Final Design Report Group 6 (Latest) PDF

CHE 4170 Design Project
Production of Ethylene glycol from various feedstocks:

DMO (dimethyl oxalate) route
G6 Engineering Sdn Bhd.

Wong Yoong Chin 26541920
Tan Hao Yang 25888463
Muhamad Dzaki Fadhlurrohman 24728497
Chew Ai Hsin 25547534
Chew Shi Phay 26351331
Chong Koon Meng 25915428
Alexander Lim Zhi Chin 24729175
G6 Engineering Sdn Bhd
Statement of Authorship
G6 Engineering Sdn Bhd declares the following:

We, the undersigned, declare the originality of all contents presented in this report with
the exception of those acknowledged and referenced to be the work of others.
Signed by the following:
__________________________ __________________________
Chong Koon Meng Wong Yoong Chin
Project Manager Senior Process Engineer
__________________________ __________________________
Muhamad Dzaki Fadhlurrohman Tan Hao Yang
Finance Director Process Engineer
__________________________ __________________________
Chew Ai Hsin Chew Shi Phay
Environmental Engineer Process Engineer
__________________________
Alexander Lim Zhi Chin
Health and Safety Engineer
Signed on: 25th October 2017
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Acknowledgement
G6 engineering SDN BHD would like to express their deepest gratitude to the unit
coordinators of CHE 4170 Design Project. Dr. Irene Chew Mei Ling and Mr. C. M.
Balaram K. P. Nair, as well as other lecturers that have kindly provide guidance to
enlighten our thoughts and leading us to the right path with their valuable knowledge,
expertise and suggestions. Intellectual exchange with students, site visits, and PASS
sessions to ensure students acquire enough help. Several interviews were conducted
which involved experienced lecturers giving feedback and review on student’s
presentation of work in order to identify any possible sources of error and
improvements of work quality. This has significantly helped us to achieve the desired
outcome and objectives of the unit. We strongly believe skills and knowledge we learnt
and achieved in this unit will eventually benefit us significantly working as a
professional engineer in the future.
Once again, for the good mentoring we received from a brain to pick, an ear to listen,
and a push in the right direction, we’d like to thank you, most sincerely, for all of the
help, knowledges, advices and the precious time from all the involved lecturers and
guest speakers. They are as follows:
 Prof. Chan Eng Seng

 Dr. Ho Yong Kuen
 Dr. Poh Phaik Eong
 Prof. Beng Ti TEY
 A/Prof Chai, Siang Piao
 A/Prof Ta Yeong WU
 A/Prof. Meng Nan Chong
 Dr. Ooi Chien Wei
 Dr. Babak Salamati
 Dr. Saman Ilankoon
 Dr. Lee Chern Leing
 Dr. Syed Tauqir
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Executive Summary
Monoethylene glycol as a major industrial chemical is expected to have an increase in
global demand to a higher level leaving a small uncertainty on the availability of MEG
for the textile industry as well as other industrial sectors even though MEG production
is estimated to have a steady growth. Sustainable processing has also become essentially
important in the industrial development here in Malaysia. G6 Engineering Inc. has thus
engaged in the glycol industry hoping to be able to supply MEG using the Dimethyl
Oxalate route that uses synthetic gas as the feedstock which could be a potential cleaner
and safer process.
The MEG production facility is located at Tanjung Langsat Industrial Area, Pasir
Gudang, Johor Bahru. Johor was chosen as the proposed location based on the
availability of the main material, syngas, as well as other raw materials and utilities
required and the ease of transportation of materials in and out of the plant.
The main objective of the plant is to produce 100,000 metric tonnes per year of MEG
over 15 years of project lifetime. The plant has 6 main sections, namely Syngas
separation, DMO synthesis, Methyl nitrite regeneration, DMO hydrogenation,
dehydration of Methanol and MEG Purification. Technology evaluation was conducted
for each major section to choose the suitable technology in terms of reliability and
economically. Process flow diagram (PFD) was developed and mass balance was
performed by manual calculations and Aspen Plus Simulations.
Design and Specification data of each and every equipment are determined and
tabulated. Detailed design of the major equipment (Reactor, Distillation Column) and
mechanical drawing of these equipment are shown. In order to ensure a safe operation
and good control of the operation, piping and instrumentation diagram was provided on
each sections.
Safety and environmental assessment on the processing plant was carried out by
performing Life Cycle Assessment (LCA) and risk assessment. Safety assessment was
conducted which includes inherent safety design (ISD), Hazard identification (HAZID)
and Standard Operating Procedure (SOP). A detail economics evaluation is performed
to determine the viability of the project.
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Table of Contents
Statement of Authorship ................................................................................................ i
Acknowledgement ........................................................................................................ ii
Executive Summary ..................................................................................................... iii
Chapter 1: Problem definition ....................................................................................... 1
1.1 Background Information ...................................................................................... 2
1.1.1 Problem Statement ........................................................................................ 2
1.1.2 Objectives of the Project ............................................................................... 3
1.2 Process Information ............................................................................................. 3
1.2.1 Processing Objectives.................................................................................... 3
1.2.2 Feedstock and product specifications ............................................................. 4
1.2.3 Feedstock Availability ................................................................................... 5
1.2.4 Plant Availability and Capacity ..................................................................... 6
1.2.5 Scope of Design ............................................................................................ 6
1.2.6 Definition of Terminal Points ........................................................................ 8
1.2.7 Site Location ................................................................................................. 9
1.2.8 Utilities and Storage .................................................................................... 10
Chapter 2: Technology Evaluation .............................................................................. 11
2.1 Market for products and by-products ................................................................. 12
2.1.1 Introduction................................................................................................. 12
2.1.2 Market demand of MEG .............................................................................. 12
2.1.3 Market price ................................................................................................ 14
2.1.4 Market of byproducts: Nitric acid and DMC ................................................ 14
2.2 Feedstocks characteristics .................................................................................. 15
2.3 Preliminary Economics ...................................................................................... 16
2.3.1 Fixed Capital Cost ....................................................................................... 16
2.3.2 Operating Costs ........................................................................................... 16
2.3.3 Working Capital .......................................................................................... 17
2.3.4 Cash Flow ................................................................................................... 17
2.3.5 Sensitivity Analysis ..................................................................................... 18
2.4 Technology evaluation ....................................................................................... 19
2.4.1 Syngas separation ........................................................................................ 19
2.4.2 DMO synthesis............................................................................................ 22
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2.4.3 MN synthesis .............................................................................................. 25

2.4.4 Dehydration of methanol ............................................................................. 27
2.4.5 DMO purification ........................................................................................ 28
2.4.6 DMO hydrogenation ................................................................................... 28
2.4.7 MEG purification ........................................................................................ 30
Chapter 3: Process synthesis & Flowsheet Development ............................................. 32
3.1 Process synthesis ............................................................................................... 33
3.1.2 DMO synthesis............................................................................................ 36
3.1.3 Methyl nitrite synthesis ............................................................................... 37
3.2 Process description ............................................................................................ 42
3.2.2 DMO synthesis............................................................................................ 44
3.2.3 MN synthesis .............................................................................................. 45
3.3 Process flow diagram (PFD) and effluent summary ........................................... 49
3.4 Process Optimization ......................................................................................... 61
3.4.1 Original Heat Exchanger Network before Heat Integration. ......................... 61
3.4.2 Pinch Analysis ............................................................................................ 61
3.4.3 Heat Exchanger Network after Heat Integration .......................................... 63
3.4.4 Network Optimization with Process Changes .............................................. 66
3.2.5 Advanced Network Optimization ................................................................ 67
Chapter 4: Mass and Energy Balance .......................................................................... 70
4.1 Mass Balance..................................................................................................... 70
4.1.1 Major Equipment in Syngas Separation ....................................................... 70
4.1.2 Major Equipment in DMO synthesis ........................................................... 74
4.1.3 Major Equipment in Methyl Nitrite Synthesis .............................................. 76
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4.1.4 Major Equipment in Hydrogenation ............................................................ 80

4.1.5 Other Major Equipment In The Plant ........................................................... 82
4.1.6 Mass balance for Minor Equipment ............................................................. 87
4.2 ENERGY BALANCE ....................................................................................... 88
4.2.1 DMO Synthesis ........................................................................................... 88
4.2.2 Methyl Nitrite Synthesis .............................................................................. 89
4.2.3 Hydrogenation............................................................................................. 91
4.2.4 Condenser ................................................................................................... 92
4.2.5 Reboiler ...................................................................................................... 93
4.2.6 Heat Exchanger ........................................................................................... 94
4.2.7 Pump ........................................................................................................... 95
4.2.8 Compressor ................................................................................................. 96
Chapter 5: Specification of equipment items ............................................................... 99
5.1 Introduction ....................................................................................................... 99
5.1 Specification sheets (by Chong Koon Meng) ................................................... 100
5.1.1 Description of equipment .......................................................................... 100
5.1.2 Specification Sheet for gas-liquid separator S-101 ..................................... 101
5.1.3 Specification Sheet for overhead condenser E-107 .................................... 102
5.1.4 Specification Sheet for kettle reboiler E-108.............................................. 103
5.2 Specification sheets (by Muhamad Dzaki Fadhlurrohman) ............................... 104
5.2.2 Specification sheet for heat exchanger E-103 ............................................ 105
5.2.3 Specification sheet for reboiler E-302 ........................................................ 106
5.2.4 Specification sheet for adsorption column V-102....................................... 107
5.3 Specification sheets (by Chew Shi Phay) ......................................................... 108
5.3.2 Specification sheet for reboiler E-501 ........................................................ 109
5.3.4 Specification sheet for distillation column D-301 ...................................... 112
5.4 Specification sheets (by Chew Ai Hsin) ........................................................... 113
5.4.3 Specification sheet for gas-liquid separator S-601 ..................................... 115
5.4.4 Specification sheet for adsorption column V-103....................................... 116
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5.5 Specification sheets (by Wong Yoong Chin) .................................................... 117

5.5.3 Specification sheet for gas-liquid separator S-201 ..................................... 119
5.5.4 Specification sheet for distillation column D-702 ...................................... 120
5.6 Specification sheets (by Alexander Lim Zhi Chin) ........................................... 121
5.6.2 Specification sheet of condenser E-706 ..................................................... 122
5.6.3 Specification sheet of overhead reboiler E-709 .......................................... 123
5.6.4 Specification of gas-liquid separator S-701................................................ 124
5.7 Specification sheets (by Tan Hao Yang) .......................................................... 125
5.7.2 Specification sheet of heat exchanger E-402 .............................................. 126
5.7.3 Specification sheet of gas-liquid separator S-401 ....................................... 127
5.7.4 Specification sheet of MEG purification column D-701 ............................. 128
Chapter 6: Detailed Design Items .............................................................................. 129
6.1 Absorber Column V-101.................................................................................. 130
6.1.1 Design Definition and Specification .......................................................... 130
6.1.2 Designing of Column Steps ....................................................................... 132
6.1.3 Mechanical Design .................................................................................... 136
6.1.4 Skirt Design .............................................................................................. 138
6.1.5 Nozzle Sizing ............................................................................................ 138
6.1.6 Specification Data Sheet and Mechanical Design ...................................... 139
6.2 Tray Distillation Column D-101 ...................................................................... 139
6.2.1 Design and Specifications ......................................................................... 139
6.2.2 Mechanical Design Calculations ................................................................ 141
6.3 Dimethyl Oxalate Reactor R-201 ..................................................................... 147
6.3.1 Definition of Design and Specification ...................................................... 147
6.3.2 Basic of Performance ................................................................................ 148
6.4 Methyl Nitrite Reactor R-402 .......................................................................... 153
6.4.1 Definition of Design and Specification ...................................................... 153
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6.4.2 Basis of Performance ................................................................................ 155

6.4.3 Reactor sizing ........................................................................................... 155
6.5 Distillation column D-501 ............................................................................... 164
6.5.1 Definition of design specification .............................................................. 164
6.5.2 Basis of performance ................................................................................. 165
6.5.3 Mechanical design ..................................................................................... 169
6.6 Hydrogenation Reactor R-601 ......................................................................... 172
6.6.1 Definition of the Design and Specifications ............................................... 172
6.6.2 Basis of Performance ................................................................................ 173
6.7 Vacuum Distillation Column (D-703) .............................................................. 177
6.7.1 Definition of the Design and Specifications ............................................... 177
6.7.2 Basis of performance ................................................................................. 177
6.7.3 Mechanical design ..................................................................................... 181
Chapter 7: Piping & Instrumentation Diagram .......................................................... 202
7.1 Pressure swing adsorption columns V-102 and V-103 to separate hydrogen from
synthetic gas .......................................................................................................... 203
7.1.1 Control philosophy .................................................................................... 203
7.1.2 Advanced control strategy ......................................................................... 203
7.1.3 Standard operating procedure (SOPs) – Maintenance for V-102 and V-103
.......................................................................................................................... 204
7.1.4 Piping and instrumentation diagram .......................................................... 204
7.2 Distillation column D-101 to separate carbon monoxide from toluene ............. 204
7.2.3 Standard operating procedure (SOPs) – Shut down and maintenance for D-
101 .................................................................................................................... 206
7.3 Syngas separation COSORB absorber and flash evaporator ............................. 206
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7.3.2 Advanced control system .......................................................................... 207
7.3.3 Standard operating procedure (SOPs) ........................................................ 208
7.4 Dimethyl oxalate synthesis .............................................................................. 208
7.4.2 Advanced Control Strategy........................................................................ 210
7.4.3 Standard operating procedure (SOPs) during maintenance ......................... 210
7.5 Methyl nitrite (MN) synthesis .......................................................................... 211
7.5.1 Control Philosophy.................................................................................... 211
7.5.3 Standard operating procedures (SOPs) during maintenance ....................... 212
7.6 Separation of required reactants (methanol and DMO) ..................................... 213
7.6.3 Standard operating procedure (SOPs) ........................................................ 214
7.7 DMO hydrogenation ........................................................................................ 215
7.7.2 Advanced control philosophy .................................................................... 215
7.7.3 Standard operating procedure for maintenance .......................................... 216
7.8 Monoethylene glycol (MEG) purification ........................................................ 216
7.8.2 Advanced control strategy for D-703 ......................................................... 217
7.8.3 Standard operating procedure (SOPs) for D-703 ........................................ 217
7.8.4 Controls for distillation column D-701 and D-702 ..................................... 218
Chapter 8: Safety and Environmental Assessment ..................................................... 244
8.1 Introduction ..................................................................................................... 245
8.2 Part A – Safety ................................................................................................ 246
8.2.1 Syngas Separation ..................................................................................... 246
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8.2.2 DMO Synthesis ......................................................................................... 257

8.2.3 MN Synthesis ............................................................................................ 266
8.2.4 DMO Purification and Dehydration ........................................................... 277
8.2.5 MEG Purification ...................................................................................... 285
8.3 Part B – Environmental.................................................................................... 293
8.3.1 Life Cycle Assessment .............................................................................. 293
8.3.2 Risk Assessment ....................................................................................... 298
Chapter 9: HAZOP Study ......................................................................................... 309
9.1 Introduction ..................................................................................................... 310
9.2 HAZOP Meeting Minutes ................................................................................ 311
9.2.1 Meeting Minutes for DMO Synthesis Process ........................................... 311
9.2.2 Meeting Minutes for Dehydration Process ................................................. 317
9.3 Piping & Instrumentation Diagram .................................................................. 321
Chapter 10: Plant Layout........................................................................................... 326
10.1 Site Selection and Location ............................................................................ 327
10.2 Plant Layout Philosophy ................................................................................ 328
10.3 Plant Layout Limitation ................................................................................. 329
10.3.1 Wind Direction ........................................................................................ 329
10.3.2 Separation Distance ................................................................................. 329
10.4 Plant Layout Justification for Process Sections .............................................. 330
10.5 Plant Layout Justification For Non Process Sections ...................................... 331
10.5.1 Security House ........................................................................................ 331
10.5.2 Loading Bay and Weighing Bridge .......................................................... 331
10.5.3 Carpark ................................................................................................... 331
10.5.4 Administration Building .......................................................................... 331
10.5.5 Control Room.......................................................................................... 332
10.5.6 Cafeteria.................................................................................................. 332
10.5.7 Medical Centre ........................................................................................ 332
10.5.8 R&D Laboratory ..................................................................................... 332
10.5.9 Warehouse and Mechanical Workshop .................................................... 332
10.5.11 Utilities Room ....................................................................................... 332
10.5.12 Cooling Tower ...................................................................................... 332
10.5.13 Boiler House ......................................................................................... 333
10.5.14 Electrical Room..................................................................................... 333
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10.5.15 Tank Farm ............................................................................................. 333

10.5.16 Fire Fighting Station .............................................................................. 333
10.5.17 Emergency Assembly Point and Emergency Exit .................................. 333
10.5.18 Flare Tower ........................................................................................... 333
10.5.19 Wastewater Storage ............................................................................... 334
10.5.20 Pipe Rack .............................................................................................. 334
10.5.21 Main Road............................................................................................. 334
10.5.22 Accommodation and Recreational Park ................................................. 334
10.6 Plant Layout Drawing .................................................................................... 335
Chapter 11: Economic Evaluation ............................................................................. 336
11.1 Revenue obtained from products .................................................................... 337
11.2 Fixed Capital Cost ......................................................................................... 337
11.2.1 Inside Battery Limits (IBL) ..................................................................... 337
11.2.2 Outside Battery Limits (OBL) ................................................................. 338
11.2.3 Engineering Cost ..................................................................................... 338
11.2.4 Contingency Cost and other costs ............................................................ 338
11.2.5 Start-Up Capital ...................................................................................... 338
11.2.6 Total Fixed Capital Cost .......................................................................... 339
11.3 Operating Cost ............................................................................................... 340
11.4 Working Capital ............................................................................................ 342
11.5 Total Capital Cost .......................................................................................... 343
11.6 Project Profitability Analysis ......................................................................... 343
11.6.1 Cash Flow Table ..................................................................................... 343
11.6.2 Payback Period........................................................................................ 347
11.6.3 Net Present Value (NPV) ........................................................................ 347
11.6.4 Internal Rate of Return (IRR) .................................................................. 347
11.7 Comparison Study ......................................................................................... 348
11.8 Sensitivity Analysis. ...................................................................................... 350
11.9 Conclusion and Profitability .......................................................................... 351
Chapter 12: Project Viability ..................................................................................... 352
12.1 Technical Viability Including Safety .............................................................. 353
12.2 Economic Viability ........................................................................................ 354
12.3 Environmental Viability ................................................................................. 355
12.4 Strategic and Technology Impacts ................................................................. 356
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12.5 Other Factors Affecting Project Viability ....................................................... 357

12.6 Recommendations ......................................................................................... 357
12.7 Conclusion..................................................................................................... 358
References ................................................................................................................ 360
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Chapter 1:
Problem
definition
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1.1 Background Information

1.1.1 Problem Statement
Ethylene Glycol (EG) is an organic compound with the formula ( CH2 OH)2 is
commonly used as a raw material in the production of polyester fibers and widely being
used as coolant and antifreeze agent in automobile industry (Industry and Engineering
Chemistry, pp624-626). EG is produced from ethylene through the intermediate
ethylene oxide (EO) and the yield of monoethylene glycol (MEG) from this reaction can
achieve up to 90% with other by-products such as diethylene and triethylene glycol.
The global MEG demand was around 21 million tonnes in 2010 and forecasts suggest
that the demand will exceed 28 million tonnes per year by 2015 and 34.1 million tonnes
by 2020 (Monoethylene Glycol, Shell, 2017). The world production of MEG has
increased by 15% and attains an amount of 26 million tonnes in the year of 2014. Saudi
Arabia is the world largest MEG producer which contributes to 25% of the global MEG
production and followed by China, India and US. Among the MEG produced, 55% of
MEG is consumed in China and Asia is the first place with 73% consumption of MEG
shown in Figure 1.1.1.1 due to the increase in population, availability of raw materials,
cheaper labour cost and strong economy development in Asia-Pacific. The average
yearly price of MEG in global market is expected to be $1,000 USD per tonnes and
$900 USD per tonnes in Asia market. It is predicted that the price of MEG will grow by
14.5% to $1,145 USD by 2020. (Monoethylene Glycol Price Trend, 2017).
Figure 1.1.1.1: World Consumption of

Monoethylene Glycol (MEG) in 2016
The industrial process of MEG

synthesis can be simplified into
two categories: EO intermediate
route and syngas processes. EO intermediate route is currently the dominant commercial
process. Ethane is extracted from natural gas and undergoes steam cracking to produce
ethylene and further oxidized into EO, subsequently water is added to form EG.
However, EO as one of the most reactive and highly toxic industrial chemicals should
2
be avoided based on Inherent Safety. On the other hand, EG synthesis from syngas
processes required synthesis gas products such as methanol, formaldehyde and synthesis
gas itself. All the process routes are being analysed and compared based on principles of
sustainability to select the best route option to synthesis MEG.
1.1.2 Objectives of the Project

G6 Engineering Sdn Bhd aims to provide professional judgement and expertise in the
specific field to produce ethylene glycols focusing on the production of mono-
derivatives (MEG).
 Selecting the best available feedstocks required for the process and meeting the
product specifications.
 Choosing the process route to synthesis EG.
 Designing major equipment and optimizing plant capacity and utilization for the
processing plant.
 Providing a construction plan by choosing a suitable location to construct the

processing plant.
The objectives stated above should be fulfilled in order to meet the rising demand of
MEG globally and achieving sustainability in environmental, economic and social
aspects. A balance of selection between the technology and the feedstock must be
optimized without compromising environmental benefits as well as the profitability of
the whole project.
1.2 Process Information

1.2.1 Processing Objectives
A manufacturing plant for production of MEG is proposed to fulfil the growing global
demand. The main objective of this project is to provide a detailed design of
manufacturing plant of MEG from the specified list of feedstocks through different
combination of process routes available. A sustainable design of the plant will be made
through the optimisation of overall process systems to maximising the process
efficiency and quality of the desired product as well as minimising the emission and
waste produced throughout the whole processes of the plant.
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1.2.2 Feedstock and product specifications

1.2.2.1 Feedstock
Table 1.2.2.1.1: Syngas specification
Components Chemical Unit Molar Composition
Formula
Hydrogen Gas H2 % 57.70
Carbon Monoxide CO % 30.90
Methane CH4 % 11.31
Water H2 O % 0.09
Table 1.2.2.1.2: Oxygen specification (VERISEQ® pharmaceutical grade gases - Oxygen, 2017)
Component Chemical Unit Linde specification
Formula
Oxygen O2 % ≥99.5
Water H2 O Ppm ≤67
Carbon Monoxide CO Ppm ≤5
Carbon Dioxide CO2 Ppm ≤300
Odour - not detected
Table 1.2.2.1.3: Methanol specification

Test Unit ASTM D-1152/97 Specification
Purity wt% ≥99.85
Apparent Specific Gravity -
20/20℃ 0.7920-0.7930
25/25℃ 0.7883-0.7893
Distillation Range, max ℃ 1.0℃ max (to include 64.6℃ ±0.1)
Non-Volatile Matter mg/100ml 5 max
Water wt% 0.10% max
Acidity (free acid as acetic acid) wt% 0.003% max
Acetone wt% 0.003% max
Hydrocarbons - To past test
Permanganate Time minute 50 minutes min
Table 1.2.2.1.4: Nitric oxide specification

Purity 99.9%-99.99%
Appearance Colourless
Dot Class 2.3
Grade Standard Industrial grade, Electron grade
Table 1.2.2.1.5: Nitrogen specification (The Linde Group, 2013)

Purity 100%
Appearance Colourless
Grade Standard Industrial grade
4
1.2.2.2 Product
EG is currently widely used in producing polyester fibres. To produce these polyester,
certain quality needs to be achieved. Table 1.2.2.2.1 below shows the quality of EG.
Table 1.2.2.2.1: Quality needed for Ethylene Glycol
Specification Quality
Minimum purity, % 99.9
Maximum Diethylene Glycol, % 0.05
Maximum acidity, ppm 20
Maximum iron, ppm 0.1
Maximum chlorides, ppm 0.2
Minimum UV Transmit @220nm, %T 70
Maximum water, % 0.05
Maximum Colour, Pt-Co Units 5
1.2.3 Feedstock Availability

At maximum rate, the reactors in the plant operate within an hour thus the target
production rate of MEG within the plant is measured in kmol/hr. The yearly target for
the rate of the production is 100000 tonnes/year which is roughly 205.33 kmol/hr. For
this goal to be achieved the quantity of feedstocks required is as follows. The amount of
syngas required is 1642.23 kmol/hr. The amount of O2 is 53.19 kmol/hr, while the
amount of both nitric oxide (NO) and methanol required is estimated to be 814.07
kmol/hr. However, these numbers and quantity are only a predicted value based on a
simple calculation and thus its accuracy is low.
Syngas can be obtained from PETRONAS Gas Berhad (Linde Engineering, 2016) and
Linde Malaysia Sdn Bhd will be the supplier of oxygen and nitrogen (Linde Industrial
Gases, 2017). Methanol and NO is only required for the start-up of the production in the
plant as it is produced within the reactors in the plant and could be use in recycle to
produce Methyl Nitrate (MN). NO is obtained from Chengu Taiyu Industrial Gases Co
Ltd in China (Chengdu-taiyu-industrial-gases-co-ltd.imexbb.com, 2017) and methanol
is supplied from PETRONAS Methanol (Labuan) Sdn Bhd (Petronas, 2017).
5
1.2.4 Plant Availability and Capacity

MEG accounts for more than 90% of the total EG production. Global demand for
glycols is increasing by significant percentages over the years, however, the industry is
facing five years of oversupply and will eventually lead to new capacities increasing
faster than the demand itself. Therefore, the plant is designed to have a capacity to
produce a moderate 100,000 tonnes of MEG per annum. (Ihs.com, 2017)
The working capacity of the plant will be at 80% for the first operation year only and
will start working at full capacity for the subsequent years. Plant availability will also be
targeted at 24 hours per day with 330 working days per year. The remaining 35 days per
year will be used to schedule for shutdown maintenances. Regular shutdowns every 6
months for a 2 weeks duration will allow ample time to inspect, repair and replace
equipment in the plant to ensure smooth operation throughout the year.
1.2.5 Scope of Design

The scope of this project is to design a plant that produces MEG which uses syngas as
the main feedstock of the process. Figure 1.2.5.1 shows the overall process flow of the
production of MEG through the DMO route. Various aspects such as the technical,
economic, social and environmental aspects while designing this plant were also
considered to ensure project feasibility.
Figure 1.2.5.1: Block flow diagram of MEG production through DMO route
1.2.5.1 Technical Aspect

For the technical aspect, the technology selection is based on its efficiency, less
hazardous conditions and cost effectiveness to install and maintain. The technologies
selected will be summarized in Process Flow Diagram (PFD) which includes the
6
equipment involved and stream conditions such as temperature and pressure. All inlet
and outlet streams conditions were also identified through Mass and Energy Balances
to determine the recycling streams to ensure the plant design is efficient and sustainable.
Appropriate assumptions and simplifications will also be made to obtain some variables
used to perform further calculations. To estimate capital and operating costs, detailed
sizing and design of equipment is performed and the detailed specifications will also
be included. Process streams properties, material selection, design, operating
temperatures and pressures will all be included in the data sheets. Detailed mechanical
design for the major equipment in the plant will be included through calculations for
stress, design loads, nozzle sizing, insulation, and vessel supports. To scale drawings of
each major equipment’s detailed design will be drawn showing the top, front and side
views with detailed cross-sections of parts included.
1.2.5.2 Social and Environmental Aspect

Piping and instrumentation diagram (P&ID) is developed for all the nodes included
within the system boundary. With the use of safety assessment techniques such as the
Bow-Tie analysis and HAZOP study, key hazards in the process were identified and
evaluated. Inherent safety design (ISD) practices will also be incorporated to eliminate,
minimise, substitute, moderate and simplify the plant design to reduce any possible
hazards and risks. The Life Cycle Assessment (LCA) will also be carried out based on a
cradle-to-gate approach to evaluate on the impact categories of the MEG production
plant such as Global Warming Potential and resource depletion to name a few to
determine the sustainability of the proposed design.
1.2.5.3 Economic Aspect

The economic viability of the project is evaluated through performing a market
evaluation on the plant. Fixed capital costs and working capital will be estimated based
on the inside battery limits (IBL) and outside battery limits (OBL) of the plant with a
reasonable allowance which includes storage of feedstocks and products for 1 week of
production and other utilities. The net present value (NPV), internal rate of return (IRR)
and payback period will also be estimated and presented in the cash flow table. The
economic analysis of the proposed plant, employment opportunities, operating stages
7
and construction stages will also be estimated to ensure full evaluation on the economic
aspect of the plant.
1.2.6 Definition of Terminal Points

Terminal points show the material and energy streams that enter and exit the defined
system boundary. In this process plant, the system boundary is defined from syngas
separation to MEG purification which involves raw materials, product, utilities and
waste. The transfer of these components across the system boundary is shown in Table
1.2.6.1.
Table 1.2.6.1: Definition of terminal points across system boundary

Inlet
Means of
Raw Material Description
Transport
Syngas Main feedstock used for MEG production Pipeline
Used for MN regeneration section to synthesize
Oxygen Pipeline
MN
Used for MN regeneration section alongside
Methanol Tank truck
with oxygen
Nitric oxide Required in small amount during plant start-ups Cylinder
Catalysts required in syngas separation
Catalyst processes, DMO synthesis as well as DMO Shipload, truck
hydrogenation in MEG production
Organic solvent Used in COSORB process to separate syngas Tank truck
Means of
Utilities Description
Transport
Electricity Energy used to power the plant Cable wire
Supplied to heat exchangers and distillation
Cooling water Pipeline
columns as well as jackets of reactors
Natural gas Used as fuel gas for process heating Tank truck
Generated through heat recovery and used in
Steam Pipeline
process heating
Nitrogen Acts as blanket for DMO synthesis Cylinder
Outlet
Means of
Product Description
Transport
Main product of the plant to be stored and Storage tank,
MEG
transported out of the plant tank truck
Means of
Waste Description
Transport
Produced in syngas separation and MEG
Wastewater purification and sent to the nearby waste Pipeline
treatment facility
By-products Sent to purge or flare Pipeline
8
1.2.7 Site Location

The site location for the proposed monoethylene glycol (MEG) plant for G6
Engineering Sdn Bhd is selected after considering the availability of a vacant land, the
availability of feedstocks, and transportation of feedstocks and products.
Figure 1.2.7.1: Map of Tanjung Langsat Industrial Estate, Johor showing the selected site
The proposed location of the MEG plant will be in Tanjung Langsat Industrial Estate,
Johor Bahru with the coordinates 1.46009 N, 103.9956 E. The uninhibited land
available is approximately 58 acres which is sufficient for potential plant expansions in
the future. This location is chosen as the syngas production facility in Johor is
approximately 22km from the proposed site and can be transported via pipelines.
Oxygen and nitrogen can be obtained from a nearby facility through pipelines. Aside
from that, methanol and NO can be imported and shipped to the nearby port.
Aside from that, the selected location also gain access to the nearest highway and
shipping port which is a few kilometres away to the respective transportation method.
Utilities such as water and electricity are also readily available nearby (Pwc.global-
arena.com, 2017). The details of the site location are shown in Figure 1.2.7.1. The
buffer zone limit set by the Department of Environment for the MEG plant is satisfied
as distance from the chosen location to the nearest residential area is 5 km and the
nearby school is also 3 km away from the site. It is also far from the Environmentally
Sensitive Areas (ESA) and other human receptors such as recreational areas.
9
1.2.8 Utilities and Storage

The utilities involved in MEG production vary from powering the plant to maximising
heat recovery. All utilities involved and their costs are summarised in the table below.
Table 1.2.8.1: Utilities costs (Production of Ethylene Glycols from Various Feedstocks, 2017)
Utilities Cost of supply/treatment
Electricity: -22KV/415V/3 Phase/50Hz RM 0.35/kWh
Natural gas: LHV 34.6MJ/m3-Mains Pressure-10 Bar(g) RM 26.33/MM Btu
Towns water RM 3.30/m3
Cooling water Towns Water + RM 0.3/m3
Saturated steam (10 Bar(g)) RM 100/Tonne
Nitrogen: Liquefied Gas (10 Bar(g)) RM 0.80/NM3
The electricity required in powering the plant is supplied by Tenaga Nasional Berhad
(TNB) Pasir Gudang whereas towns water and water is supplied by Syarikat Air Johor
(SAJ). Natural gas is supplied by Gas Malaysia Berhad, which is located nearby the
facility. Steam can be generated on-site through heat integration system.
The storage of raw materials such as syngas and oxygen is not required as these
materials are supplied through pipelines. However, methanol which is flammable is
stored in small quantities in a medium sized storage tank enclosed with bund walls to
prevent leakage. Meanwhile, NO which is nontoxic, is also stored in small quantities in
a small storage tank due to its low demand. Organic solvent and catalysts are each
stored in a storage tank. For utilities, water is stored in two large reservoirs which are
installed in the facility in case of water disruption or shortages. Cooling water is sent to
a cooling tower to be recycled. Nitrogen are supplied via compressed cylinders. Lastly,
the MEG product is first filled in a large storage tank before being transported out of the
facility.
10
Chapter 2:
Technology
Evaluation
11
2.1 Market for products and by-products

2.1.1 Introduction
Synthesis of monoethylene glycol (MEG) can be split into two categories which is the
ethylene oxide (EO) intermediate route and dimethyl oxalate (DMO) route. Under the
EO intermediate route, it is further split into peroxidation route, Dow Meteor Process
and Shell Omega Process. MEG is an organic compound and it is commonly used in the
production of polyester fibre and as antifreeze, as well as a heat transfer agent and
solvents coupler (Yu and Chien, 2017). Figure 2.1.1.1 shows the market segmentation
percentages of MEG. The main focus will be on the DMO route, where biomass-based
synthetic gas (syngas for short) along with oxygen and nitrogen is used to synthesize
MEG. Most of the MEG produced in the country are either being used locally or
exported to countries in the Asia-Pacific region, especially China, South Korea and
Taiwan.
Figure 2.1.1.1: Market segmentation of

MEG (Quasar Group Consulting, 2017)
2.1.2 Market demand of MEG
Figure 2.1.2.1: Global Consumption of MEG Figure 2.1.2.2: Local capacity and Supply
in 2016 demand for MEG in Malaysia
12
As seen from Figure 2.1.2.1, China is the world’s largest consumer of MEG in the year
2016 and is expected to be increasing steadily as MEG is an important compound in
chemical industry. In year 2015, the global demand for MEG was 28 million tonnes and
it is expected to increase to about 34 million tonnes by the year 2020 (Shell, 2017). As
observed from Figure 2.1.2.2, the demand for MEG is seen to grow steadily through the
years to come.
Figure 2.1.2.3: Biomass-based syngas Figure 2.1.2.4: Oxygen availability as

availability as feedstock (Gasification and feedstock (Grand view research, 2017)
syngas Technologies Council, 2017)
Figure 2.1.2.5: Nitrogen availability as feedstock (Jones, 2017)
As the main focus is on DMO route, the feedstock used would be syngas, oxygen and
nitrogen. From Figure 2.1.2.3, it was observed that the availability biomass-based
syngas is quite low but is expected to grow in the future (Gasification and syngas
Technologies Council, 2017). Figure 2.1.2.4 and 2.1.2.5 shows the availability of
oxygen and nitrogen as feedstock and therefore there would be enough inventories of
feedstocks for the production of MEG. Therefore, in Figure 2.1.2.6 it is understandable
that the volume of MEG produced shows a gradual increase. Based on the market
evaluation, the base capacity of the plant is set at 100,000 tonnes of MEG per annum to
fulfil the demand-supply gap.
13
Figure 2.1.2.6: Volume of production (ktonnes) and revenues (US$ mil) earnings of MEG
2.1.3 Market price

The price for MEG was determined to be roughly USD$1000 per tonnes in global
market whereas for Asia market, it is around USD$900 per tonnes (RM3800 per
tonne). Prices are expected to grow by 14.5% by the year 2020 (Monoethylene Glycol
Price Trend, 2017).
2.1.4 Market of byproducts: Nitric acid and DMC

Nitric acid is one of the by-product formed from methyl nitrite (MN) regeneration
section with dilute (≈1%) streams which can be sold with further purification. It is an
inorganic compound which can be used for applications such as fertilizers, explosives,
dyes and pharmaceuticals, which majority are used to produce ammonium nitrate for
fertilizers production (Heller, 2012). According to HIS Markit (2017), Eastern Europe is
the largest consumer for nitric acid in the year 2016. The global demand for nitric acid
was expected to grow at the Compound Annual Growth Rate (CAGR) of 10% during
2015-2022 and by 2022 it was expected to reach about USD$15 billion as the demand
for crops and vegetables are rising rapidly in recent years.
DMC on the other hand, is a versatile and eco-friendly compound. It can be used as
VOC exempt solvent, paints and in the manufacture of polycarbonate, fuel additives and
Li-ion battery (Special Materials Company, 2011). DMC is mostly used for
polycarbonate due to its transparent and strong properties. The global demand was at
USD $14 billion in the year 2015 and is expected to increase steadily to USD $22
billion by the year 2024 (Global Market Insights, 2016). Although it has a stable market,
the amount of DMC able to be separated is of small amount and thus will be treated as a
waste.
14
2.2 Feedstocks characteristics

The feedstock required for the manufacture of monoethylene glycol (MEG) from DMO
route is syngas, oxygen, nitric oxide (NO) and methanol. Syngas is the most essential
raw material in the process whereas oxygen, NO and methanol are utilized in DMO
synthesis. The economics and selection criteria of feedstock are evaluated as below
whereas the specifications of feedstock are attached in Chapter 1.
Syngas consists of mainly hydrogen, carbon monoxide and carbon dioxide as well as a
small amount of methane and gas yield such as nitrogen, argon and hydrogen sulphide.
The molar composition of syngas is attached in Chapter 1. The source of syngas is
obtained from biomass whereby it has a lower efficiency and yield compared to that
from natural gas. However, the carbon footage of syngas from biomass is reduced and
the sustainability of the environment is achieved by reducing resource depletion. The
production of syngas from biomass is also more economical compared to that from
natural gas (Fendt et al., 2015).
For oxygen, it is supplied via pipelines from Linde Malaysia. As pure oxygen is
impractical to be obtained, it is essential to ensure high purity of oxygen to improve the
efficiency of the process. The oxygen supplied from Linde Malaysia has a purity of up
to 99.5%, with the remaining of a small amount of water, carbon monoxide and carbon
dioxide. As the remaining components in supplied oxygen can be assumed to be
negligible, it does not affect the efficiency of the process. Components such as carbon
monoxide and carbon dioxide can act as inert gases as they do not react to produce by-
products. Hence, it is more economical to obtain oxygen at this purity instead of pure
oxygen.
NO is required to kick-start the process during plant start-ups which is supply through
pipelines from Chengu Taiyu Industrial Gases Co Ltd. The purity of NO supplied is
99.9% with standard industrial grade. As NO is costly, it is regenerated and recycled in
the plant, thus reducing the amount of fresh NO required in the plant which
subsequently leads to reduction of production costs.
Lastly, methanol is required in a few sections as a reactant and stabilization medium. As

methanol is a product from MEG production, it is constantly being regenerated and
reused in the process. However, a small amount of methanol is required to top up to the
15
recycling methanol stream due to insufficient amount of methanol produced. The top-up
methanol is supplied through pipelines from Petronas Methanol (Labuan) Sdn Bhd.
Hence, the purity of methanol supplied should be 99.85%, with the remaining
components of water and acetone. As methanol is volatile and highly flammable, it is
stored in a pressurized tank at low temperature to prevent flashing which leads to fire
and explosion from BLEVE.
2.3 Preliminary Economics

2.3.1 Fixed Capital Cost
The fixed capital cost is estimated for this MEG production plant in Malaysia which
produces MEG at 100,000 tonnes per annum. Detailed calculations can be found in
Appendix A2.3 of the report. Important assumptions to be made in this section are as
follow:
 Exchange rate of 1 USD to RM 4.27 as per 1 Aug 2017.
 Inflation index for chemical plants in Malaysia in year 2017 is estimated to be

596.
Purchased equipment cost for this plant is RM 87.40 million and the final estimated
fixed capital cost for this plant set up by G6 Engineering Inc. is at RM 948.10 million.
2.3.2 Operating Costs

Certain assumptions were made to determine the operating cost of the plant:
 The plant capacity is 100,000 tonnes per annum.
 The plant is operating at 100% capacity.
 15 plant operators and 1 plant supervisor are working per shift with 4 shifts per
day.
 Selling price of MEG is the global current price which is USD $ 1000/tonnes
 Maintenance labor and Maintenance materials are fixed at 2.5% of the fixed
capital.
 Insurance and Property Taxes are fixed at 1% of the fixed capital
 Book Depreciation is fixed at 7.5% of the fixed capital.
 Plant Overhead is fixed at 50% of the fixed labor.
 Operating supplies is fixed at 10% of the fixed labor.

16
 Corporate Administration cost is fixed at 3% of production cost.
 Research and Development cost is fixed at 2% of production cost.
 Selling expenses cost is fixed at 5% of production cost.

Based on all the assumptions made above, the minimum viable selling price per kg of
MEG is calculated to be MYR 1772.20 per tonnes of MEG produced.
2.3.3 Working Capital

Assumption made in working capital:
 100% capacity utilization
 Syngas is supply by pipeline; the stock of syngas is taken for period of 1.5 weeks
 Oxygen gas, methanol and nitric oxide is supplied daily; stocks for these
chemicals is taken for a period of 1.5 weeks
 Work in progress inventory is negligible
 Since the MEG produced will be exported overseas, a period of 6 weeks of

storage in plant is recommended
 The period for debtors and creditors for the plant are assumed to be 6 weeks
Based on these assumptions, the working capital of the plant is calculated to be RM
57.03 million.
2.3.4 Cash Flow

Assumptions made to generate the cash flow table are as follows:
 Economic life is assumed to be throughout 15 years of operation.
 1 year is used for detailed design and 2 years will be required for constructing and
commissioning of the plant.
 Capacity Utilization for the first year of operation only is at 80% and will increase
to 100% for the subsequent years of operation.
 Discount rate of 10% is applied.
 Tax depreciation rate is 6.7% of the fixed capital cost investment until fully
depreciated.
 Tax payment rate at 28%.
17
The complete cash flow table can be found in Appendix A2.6 of the report. After
calculations are performed, the Net Present Value (NPV) after 15 years patio is
determined to be RM 407.79 million. The payback period is 6 years with an Internal
Rate of Return (IRR) of 17.0%.
2.3.5 Sensitivity Analysis

The sensitivity analysis of the project is estimated by varying a few important criteria in
the table below.
Table 2.3.5.1: Summary of Preliminary Economics of plant
Components Value (MYR Million/year)
Capital Expenditure 948.10
Sales Revenue 450.00
Variable Costs Raw Materials 45.33
Utilities 4.29
Fixed Costs 140.66
Profit Before Tax (PBT) 247.03
Profit After Tax (PAT) 195.65
IRR % (Base Case) 17.0
NPV 305.83
Payback Period 6 years
Sensitivity 10% increase in Selling Price 20.5 %
Analysis 10% decrease in Selling Price 13.3 %
(IRR) 10% decrease in Sales Volume 13.4 %
10% increase in Capital Expenditure 15.3 %
10% increase in Raw Materials Cost 16.6 %
From the preliminary cost estimation, the IRR value obtained was roughly 17 %, which
indicates that the project is a profitable project according to the estimations. However,
based on the Sensitivity Analysis, it is important to focus on maintaining the selling
price of product as a fluctuation in selling price will have the most impact on the
Internal Rate of Return (IRR) of the project.
18
2.4 Technology evaluation

2.4.1 Syngas separation
Two of the required raw materials to produce MEG using the DMO Route are CO and H2. These raw materials are obtained by separating the syngas feedstock. Syngas is made of various gases such as CO2, CH4,
CO and H2, thus making the separation rather complex and difficult. Therefore, it is of the outmost importance to find the most efficient and productive separation technology in both economic and process aspect.
2.4.1.1 Process Options

CO is obtained to react with the MN to produce DMO inside the carbonyl reactor whereas the H2 is obtained to react with DMO to produce the MEG product. Table 2.4.1.1.1 summarizes the comparison of the
different possible technologies to separate CO and H2 from syngas.
Table 2.4.1.1.1: Comparison between Syngas Separation Technologies
Process Technology
Parameters PSA (Pressure Swing Adsorption) & COSORB
Palladium Membrane Diffusion CO Cold Box
COSORB PSA
 This process combines two
 As indicated by its name, this technology purifies
 COSORB process is first used to different technologies to
hydrogen by using pressure driven diffusion across
obtain Carbon monoxide. separate the two raw materials
the palladium membranes
 COSORB process selectively required from the rest of the  Producing CO from syngas
 At 300°C, the unique crystal lattice property in the
removes CO by complexation of CO syngas composition.  Cryogenic process
palladium allows only monatomic hydrogen to pass
in toluene solvent using CuAlCl4  PSA is used to obtain H2 by  Involves three processes: methane
Working Principle through the membrane thus allowing it to be
catalyst. adsorbing the impurities on the wash, partial condensation, CO wash
separated from the rest of the gases
 The process involves three main feedstock solution.  Components separated through
 The other impurities such as H2O, CO2, CH4 and N2
sections by order: absorption,  It involves 2 adsorption different boiling points
can penetrate and become attached to the membrane.
flash evaporation and stripping. columns where the process is
 The impurities could be purged away from the cell
(Keller and Schendel, 1988) continuous. (Tobias Keller,
through a bleed port. (Connor, 2013)
2016)
CO Lean Gas from COSORB
Raw Materials Syngas Syngas Syngas
process
 Pressure: 11 atm
 Pressure: 18 atm
 Temperature: 30 °C  Pressure: 20 atm
Feed Conditions At absorber temperature and pressure  Temperature: 350 °C
 Saturated with water  Temperature: -160 °C
(Johnson et al., 2015)
(Johnson et al., 2015)
Absorber 40 °C Wash Column -169.5 °C
Reaction Flash Evaporator 40 °C Stripping Column -171.1 °C
30 °C (Golden, 2006) 400 °C (H.H.Funke, 2002)
Temperature Stripping
111 °C COCH4 Column -170 °C
Column
Absorber 2 atm Wash Column 21.3 atm
Flash Evaporator 1 atm Stripping Column 10.8 atm
11 atm (Golden, 2006) 81 atm (H.H.Funke, 2002)
Reaction Pressure Stripping
1 atm COCH4 Column 1 atm
Column
 Alumina silica gel
 Activated Carbon
Adsorbent Material Cuprous Aluminum Chloride, CuAlCl4 N/A N/A
 Molecular sieves (FRANCO,
2014)
Membrane N/A N/A Palladium Silver Alloy (Connor, 2013) N/A
19
Material
Number of Stages 3 4 1 3
 Heavy and light hydrocarbons  CO
Byproduct  CO lean gas  H2
 CO  N2
Formation  Toluene with catalyst  CH4
 N2  CH4
Product Recovery 90 % of H2 recovered
98 % of CO recovered 99 % of Hydrogen recovered (Connor, 2013) 95% of CO recovered
Rate (Johnson et al., 2015)
Purity of product 99 % 99.5 % (Johnson et al., 2015) 99 % (Connor, 2013) 99.99 %
Electrical power: 0.49 kW/ Nm3 of CO
Energy
Reboiler heat: 1.00 MJ/ Nm3 of CO N/A N/A Specific energy: 18 – 600 kWh/t of CO
Consumption
Cooling water: 5.50 MJ/ Nm3 of CO
Level of
Industrial Large Scale Industrial Large Scale Small to Medium Scale Industrial Large Scale
Commercialization
10000 Nm3/h
Capacity 5500 Nm3/h 11 Nm3/h (Connor, 2013) 100 Nm3/h – 30,000 Nm3/h
(Mahler-ags.com, 2013)
From three of the feasible options listed above, the combined COSORB and PSA method is chosen for the syngas separation section of the plant due to its advantages. When comparing the chosen method with
the CO cold box method to separate CO from syngas, the main advantage that the COSORB process has is that it works under relatively moderate temperatures and pressures, which will lead to reduction in cost
due to cheaper material to be used for the equipment. The CO cold box method is a cryogenic process that involves the use of liquified nitrogen to maintain temperatures well below 0 °C. (Air Liquide, 2017)
Liquified nitrogen storage will pose a significant threat to the plant if it is not handled properly. The COSORB process also uses less energy to recover more of the CO from the syngas, which increases the
efficiency of the process. Although a higher purity of product can be achieved by using the CO cold box method, it is not necessary as the purity of CO obtained from the COSORB process is enough to not pose
unwanted side reactions in the following processes in the plant. On the other hand, PSA have been chosen due to the fact that it is able to produce H2 at a much higher capacity in comparison to Palladium
Membrane. PSA is able to produce 10000 Nm3/h of H2 whereas Palladium Membrane is only able to produce 11 Nm3/h of H2. The plant requires a large amount of H2 as it is one of the raw materials required to
produce Methyl Ethylene Glycol thus the selection of PSA is justified. Furthermore, PSA is extremely efficient and productive as well. It has a hydrogen recovery percentage of 98 and is able to achieve 99%
purity. In addition to that PSA is a heatless process thus minimizing the amount of energy required for the process which in the same time would be cost efficient.
Table 2.4.1.1.2: Comparison of techniques used in pressure swing adsorption (PSA)
Parameters Adsorption
Physical Chemical
Molecular Force Weak operating force required as molecule are held due to Van der Waal’s forces High operating force required as molecules are held by chemical bond
Heat Required 30 kJ/mol 300 kJ/mol
Side-product Formed Compound formation doesn’t occur Surface compound are formed
Reversibility Reversible Irreversible
Activation Energy No energy required for start up Requires activation energy for start up
Specification Not specific in nature as all gases are adsorbed to some extent Specific in nature and occurs only when there is some possibility of compound formation
Physical adsorption is chosen for the PSA as it does not require energy to start-up the process. Furthermore, the heat required for the process is much less compared to chemical adsorption with 30 kJ/mol
compared to 300 kJ/kmol. In addition to that, there are no formation of side product in the process and thus eliminating the chances of further accumulation of impurities.
The COSORB method’s main equipment is an absorber to separate the CO from the syngas feed, there are several types of absorber options that can be suitable for the process. These options are evaluated through
their advantages and disadvantages from Table 2.4.1.1.3.
20
Table 2.4.1.1.3: Comparison between different equipment for absorption (Encyclopedia.che.engin.umich.edu, 2017)
Technology Packed Bed Column Spray Column Falling Film
Advantages  Low pressure drop  Low pressure drop  Low pressure drop
 Require only small diameter  Only one stage required, lower cost  Fairly easy cleanup procedure
 Low operating and maintenance cost  Effective for solutes with high liquid solubility  Suitable for heat sensitive fluids
 Can handle corrosive materials
 Good mass transfer
Disadvantages  Not suitable for extreme flow rates (too high or too low)  Poor mass transfer  Liquid component must be uniformly supplied
 Not suitable for high viscosity fluids  Pumping cost high  Flooding may occur
 Low residence time, leading to lower purity of separation  Evaporation may deteriorate products
 Entrainment present, lower percentage recovery  Requires continuous heat removal
2.4.1.2 Inherent Safety Design for syngas separation
To separate CO from syngas, two processes were compared based on the chemicals and equipment involved through ISI evaluation.
Table 2.4.1.2.1: ISI table for process options to separate CO from syngas
Process Options COSORB Process CO Cold Box (Uigi.com, 2017)
Parameters Description Score Description Score
Chemical Inherent Safety Index
Sub-indices of Reaction Hazards
Heat of Main Reaction No reaction 0 No reaction 0
Heat of Side Reactions No reaction 0 No reaction 0
Chemical Interaction No chemical interaction 0 No chemical interaction 0
Sub-indices for Hazardous Substances
Flammability Easily flammable 3 Non-flammable 0
Explosiveness 0 - 20 1 Non-explosive 0
Toxic Exposure TLV < 1000 2 TLV < 100 3
Corrosiveness Carbon Steel 0 Stainless Steel 1
Process Inherent Safety Index
Inventory 10 – 50 t 2 10 – 50 t 2
Process Temperature 0 - 70 °C 1 < 0 °C 1
Process Pressure 0.5 – 5.0 bara 0 25 – 50 bara 2
Process Equipment Distillation Tower 1 Compressors 3
Total ISI for COSORB process 10 Total ISI for CO Cold Box process 12
Table 2.4.1.2.2: ISI for process options to separate H2 from syngas

Process Options PSA Palladium Membrane Diffusion
Flammability Non-flammable 0 Non-flammable 0
Explosiveness 0 - 20 0 Non-explosive 0
21
Toxic Exposure TLV < 1000 2 TLV < 100 3

Corrosiveness Stainless Steel 1 Carbon Steel 0
Inventory 10 – 50 t 2 10 – 50 t 2
Process Temperature 0 - 70 °C 1 300-600 °C 3
Process Pressure 5 – 25 bara 1 50 – 200 bara 3
Process Equipment Distillation Tower 1 Equipment handling non-flammable, nontoxic materials 0
Total ISI for COSORB process 8 Total ISI for CO Cold Box process 11
By choosing the COSORB process over the CO Cold Box method to separate CO from syngas, the risk of explosion due to build up in pressure in the liquid nitrogen storage tank, extremely low operating
temperatures and high pressures are eliminated. The usage of toluene in the process is also minimized as most of the toluene is recycled back to absorber to be used as a solvent for the absorbent. Toluene also
acts as a substitute for other more hazardous organic compounds to be used as the solvent for the process. By operating under moderate temperatures and pressures, the moderate aspect of the ISD is also applied
in the design. PSA and Palladium Membrane Diffusion both doesn’t require any chemical reaction however the operating temperature and pressure for Palladium Membrane Diffusion is a lot higher compared to
PSA thus the chances of rupture and excessive heat is a lot higher as well.
2.4.1.3 Justification on technology selection
Based on the comparisons from the tables above, the process option chosen for syngas separation is the COSORB combined with the PSA process as the ISI score obtained for the COSORB and PSA process is
lower. Although this process uses toluene which has a flammability higher than the liquid nitrogen used in the CO Cold Box process, it has advantages over the operating temperatures and pressure. The operating
pressure used for the COSORB process is slightly above 2 bara which is low compared to the 25 bara pressure when using the CO Cold Box method. The process equipment will also cost less as carbon steel can
be used for all the equipment due to moderate operating conditions. Lastly, potential impact of toxic component such as liquid nitrogen being exposed is relatively more harmful as inhalation may cause dizziness,
vomiting and perforations. For the COSORB process, the equipment chosen for the absorber will be the packed bed column mainly due to its low pressure drop and cheaper operating and maintaining cost. It also
provides good mass transfer to ensure that the absorption reaction proceeds with high efficiency.
When comparing PSA and Palladium Membrane Diffusion, both processes is not made of any chemical reactions thus both process does not require heat for either main reaction or side reaction. Both processes
are non-flammable thus no comparison could be made based on that parameter. However, the difference maker lies on the fact that both the operating temperature and pressure for Palladium Membrane Diffusion
is way higher compared to PSA with 400°C and 81 atm respectively whereas the temperature and pressure for PSA is 29.5°C and 18 atm respectively.
2.4.2 DMO synthesis

Synthesizing of DMO is a very crucial step in producing MEG. DMO is synthesized by oxidative coupling of CO and MN with the aid of catalyst as shown: (Yamamoto, 2010)
2𝐶𝑂 + 2𝐶𝐻3 𝑂𝑁𝑂 → (𝐶𝐻3 𝑂𝐶𝑂)2 + 2 𝑁𝑂
During the synthesizing of DMO, a by-product of Dimethyl Carbonate (DMC) is formed from the side reaction between the reactant. The formation of DMC is unfavourable hence the reaction temperature and
pressure must be controlled in order to provide a high selectivity of DMO in the reactor. The chemical equation of formation of DMC can be shown as:
𝐶𝑂 + 2C𝐻3 𝑂𝑁𝑂 → (𝐶𝐻3 𝐶𝑂)2 + 2𝑁𝑂
22

Two process options are compared in terms of safety design, reactor options of DMO synthesis, and catalytic activity. The best technology is then selected to carry on with the final design of the process. Across
the study, the DMO synthesis is found to be most effectively carried in a vapor phased reaction (Yamamoto, 2010) to ensure a high production yield of DMO in the process.
Table 2.4.2.1.1: Comparison of reactor options for DMO synthesis

Parameters Continuous Flow Integral-Type Fixed Bed Reactor Plug Flow Reactor
Cylindrical tube filled with heterogenous catalyst
pallets with MN and CO flowing through the bed and A continuous stream of MN and CO
converted into DMO. The reactions are induced as flowing into a tubular reactor. The tube
the gases contact the catalyst when passing through in the plug flow reactor is packed with
Working Principle the bed. (NETL Technology Laboratory, 2017) heterogenous (solid) catalyst to improve
the reaction. (ACS Chemistry, 1998)
Dimensions of fixed bed reactor can be scaled and calculated based on the desired
Dimensions Length: 1.5 m; inner diameter: 27 mm; outer diameter: 32 mm (according to lab scale unit)
production rate of DMO
Raw Materials MN, CO, Palladium catalyst with proper supporting chemicals MN, CO, Palladium catalyst with proper supporting chemicals
CO stream and MN stream are both fed in vapor phase. The molar ratio of the inlet CO stream and MN stream are both fed in vapor phase. The molar ratio of the inlet
reaction feed gas was: reaction feed gas was:
Feed Condition  CO: 7-30%  CO: 7-30%
 NO: 2-10%  NO: 2-10%
 MN: 10-30%  MN: 10-30%
Reaction Temperature  Temperature: 140 °C  Temperature: 110 °C
and Pressure  Pressure: 1 atm (Yamamoto, 2010)  Pressure: 1 atm (Yamamoto, 2010)
Byproduct Formation DMC, methanol and Methyl Fomrate (MF) (NianJun Luo, Yang Ji, 2012) DMC, methanol and MF. (NianJun Luo, Yang Ji, 2012)
DMO selectivity of 95% is achieved; MN conversion rate between 85% - 90%
Conversion Efficiency The one-way conversion of CO is 65% (JingGang Fang, Baowei Wang, 2003)
(NianJun Luo, Yang Ji, 2012)
Space time yield of DMO is about 706.5 kg/m3.cat.h. (JingGang Fang, Baowei Wang,
Yield Space time yield of DMO obtained is about 400 kg/m3.cat.h (Yamamoto, 2010)
2003)
Level of High, widely applied in MEG production industry to produce DMO such as Pujing
Low, only applied to the lab scale plug flow reactor.
Commercialization Chemical in China. (NianJun Luo, Yang Ji, 2012)
Operating cost of depends on the reactor temperature and pressure. Higher reaction
Low operating cost but shutdown and maintenance may be relatively expensive.
Operating Cost temperature and pressure drop will incur a higher operating cost. (Anand P, Prakash G,
(Umich.edu, 2017)
1991)
Table 2.4.2.1.2: Comparison of catalyst used

Catalyst Palladium, Pd catalyst supported by 𝜶-𝑨𝒍𝟐 𝑶𝟑 Nanofiber Supported Palladium Catalyst
Conversion of CO 25- 40 % (Shin-ichiro Uchiumi, 1998) 10 – 30 % (Tie-JunZ. DeC, 2004)
DMO selectivity 85 – 95 % 95 – 99% depending on the type of nanofiber.
Reaction Condition 14°C, 2 bara and GSHV of 2500 L/kg.h 120°C, pressure ranges between 0.1 – 0.5 MPa and 3000 L/kg.h
Catalyst Lifetime 600 hours Approximately 200 hours
Catalyst Consumption 0.004617 wt% CO in feed 0.005907 wt% CO in feed
Level of Commercialization Pd/Fe widely being used in industry and available in the market. Low level of commercialization, lab scale.
23
2.4.2.2 Inherent Safety Design for DMO synthesis
Table 2.4.2.2.1: ISI table for different reactors available for DMO synthesis
Reactor options Continuous Flow Integral-Type Fixed Bed Reactor Plug Flow Reactor
Sym. Justification Score Justification Score
Chemical inherent safety index
𝐼𝑅𝑀 Moderately Exothermic = -1033.16J/g 2 Moderately Exothermic = -1033.16J/g 2
𝐼𝑅𝑆 Mildly Exothermic = -296.57 1 Mildly Exothermic = -296.57 1
𝐼𝐼𝑁𝑇 Chemical Interaction: Heat Formation 1 Chemical Interaction: Heat Formation 1
𝐼𝐹𝐿 Combustible (Flash Point = 75°C) 1 Combustible (Flash Point = 75°C) 1
𝐼𝐸𝑋 MN Explosive Subindex: 45 - 70 3 MN Explosive Subindex: 45 – 70 3
𝐼𝑇𝑂𝑋 Toxic Exposure Subindex: CO, TLV = 25ppm 3 Toxic Exposure Subindex: CO, TLV = 25ppm 3
𝐼𝐶𝑂𝑅 Carbon Steel 0 Carbon Steel 0
Process inherent safety index
𝐼𝐼 ISBL = 97.891 tonnes 3 ISBL = > 100 tonnes 4
𝐼𝑇 Process Temperature Subindex: 70 -150°C 1 Process Temperature Subindex: 70 -150°C 1
𝐼𝑃 Process Pressure Subindex: 0.5 – 5 bara 0 Process Pressure Subindex: 0.5 – 5 bara 0
𝐼𝐸𝑄 Equipment Safety: Fixed Bed Reactor 2 Equipment Safety: Plug Flow Reactor 2
Total 17 Total 18
Table 2.4.2.2.2: Inherent Safety Design strategies

Inherently Safer Design Strategy Parameters
1. Reduce inventory
 Hazardous raw materials are stored in a minimal amount, explosive raw material such as MN is reacted once produced. Maintain only a small amount of MN
accumulated in the system. Dilute the concentration of MN with Nitrogen gas as inert.
Minimize  Hazardous products, NO is sent to the following reactor to be converted to desired product. Ensure minimal accumulation of CO in the system.
2. Reduce occurrence of runaway reaction
Fixed Bed Reactor is cooled with cooling jacket to minimize the occurrence of thermal runaway reaction and the formation of hotspots within the reactor due to the
exothermic property of the reaction.
2.4.2.3 Justification on selection of technology and catalyst
Based on the studies carried out above, the reaction will be carried out in a Fixed Bed Reactor cooled with a water jacket using Palladium with the support of 𝑨𝒍𝟐 𝑶𝟑 as catalyst.
Table 2.4.2.3.1: Selection criteria and justifications

Criteria Justification
 Fixed Bed Reactor is chosen as temperature control of the reactor is relatively easier to be manipulated by a water cooling jacket to prevent thermal runaway reaction
occurring inside the reactor.
Safety & Health Issues
 Palladium Catalyst is chosen as the required operating pressure of palladium catalyst is relatively low compared to the use of nanofiber catalyst. Hence safety issue related
to operating pressure can be minimized.
 Palladium catalyst has a longer lifetime compared to nanofiber supported catalyst. Hence less catalyst will be required in a fixed duration and lesser catalyst will be
Environmental Impacts
disposed to the environment.
 Fixed Bed Reactor is relatively easier to operate and maintain compared to Plug Flow Reactor, loading and unloading catalyst in a fixed bed reactor consumed less time
Operability Considerations and relatively easier, hence less cost is incurred during the reloading of catalyst.
 Fixed Bed Reactor is easier to be maintained compared to plug flow reactor.
24
2.4.3 MN synthesis
The synthesis of methyl nitrite (MN) is one of the main processes to produce MEG from syngas using the DMO Route. The process reaction for MN synthesis is shown below (Li et al., 2013):
2𝑁𝑂 + 𝑂2 → 2𝑁𝑂2 (1) 2𝐶𝐻3 𝑂𝐻 + 𝑁2 𝑂3 → 2𝐶𝐻3 𝑂𝑁𝑂 + 𝐻2 𝑂 (4)
𝑁𝑂 + 𝑁𝑂2 ↔ 𝑁2 𝑂3 (2) 𝐶𝐻3 𝑂𝐻 + 𝑁2 𝑂4 → 𝐶𝐻3 𝑂𝑁𝑂 + 𝐻𝑁𝑂3 (5)
2𝑁𝑂2 ↔ 𝑁2 𝑂4 (3)
Equation 1, 2 and 4 are the main reaction of the MN synthesis while equation 3 and 5 are side reaction which will reduce the yield of the final product. Since MN is one of the main reactants involved in the
formation of DMO which will then produce MEG through hydrogenation process, the efficiency of the MN synthesis process will affect the production rate of the MEG plant. Therefore, it is important to find a
suitable technology for this process to achieve higher efficiency and productivity in both economic and process aspect. The main reactants for MN synthesis are methanol, NO and O2. Since NO is one of the by-
products formed during the DMO synthesis, it can be recycled and reused in the MN synthesis process. Therefore, methanol and O2 are the only inputs that should be obtained from other sources for MN synthesis
process.

Table 2.4.3.1.1: Comparison between catalytic and non-catalytic process
Non-Catalytic Process Catalytic Process
Parameters (Union Carbide Chemicals and Plastics Company Inc., 1990; Liu, Ji and Li, (Huashuo Technology Company Limited, China 5th Ring Road Engineering Co., Ltd.,
2010; Li et al., 2013) 2014)
 The reactants enter the packing column which has larger contact surface area  A small portion of feed gas from DMO synthesis enter the lower segment of the
for reaction to produce the desired product and leave from the top stream of reactor while the rest of feed gas mix with oxygen and enter the upper segment of
the column. reactor.
Working Principle
 The product stream will enter the following column reactor to recover the  The fresh methanol injected from the top of reactor.
remaining reactants in the product streams and undergo further reaction in  The upper segment of reactor is filled with packing material or trays
order to increase the overall yield of the desired product.  The lower segment of reactor is filled with catalyst to promote the reaction efficiently
 Methanol  Methanol
Raw Material  Oxygen  Oxygen
 Nitrogen monoxide  Nitrogen monoxide
 The NO and O2 enter the reactor at temperature at 100℃ to minimise the
formation of N2O4  NO/O2 ratio of feed stream is 4:1 to 7:1
Feed condition
 The NO/O2 ratio of feed stream is 6:1  The ratio of fresh methanol to NO fed is 1.5:1 to 3:1
 The mole ratio of methanol to oxygen is 4:1 to 12:1
 Lower section: 50 - 90℃
Reaction temperature  60℃ or less
 Upper section: 20-60℃
Reaction pressure  1.36 - 4.08 atm (20 - 60 psia)  3 - 5.5 atm
 Will produce some nitric acid through side reaction:
Catalyst Used  No side reaction (convert HNO3 produced from side reaction to NO2)
𝐶𝐻3 𝑂𝐻 + 𝑁2 𝑂4 → 𝐶𝐻3 𝑂𝑁𝑂 + 𝐻𝑁𝑂3
Catalyst Consumption -  Silicoaluminophosphate molecular sieve catalyst
 1 to 1/20 liter per volume of liquid in the lower section of reactor
By-product formation -
 Lifetime of about 1200min (Sun et al., 2017)
Conversion efficiency  water  water
25
 HNO3
 99% or higher conversion of O2 by feeding excess amount of NO and
Yield methanol  100% conversion of O2 by feeding excess amount of NO and methanol
 99 % or higher nitric oxide efficiency to alkyl nitrite
High yield due to the use of catalyst and absence of side reaction which will reduce the
Operating cost High yield by using 2 reactors in series to increase the overall yield (about 86.5%)
production rate of methyl nitrite
Equipment cost Lower operating cost without the use of catalyst Higher operating cost due to regeneration and disposal of catalyst
2.4.3.2 Selection and Justification of Technology Alternatives
Based on the comparison of technologies shown in the tables above, non-catalytic process is chosen to carry out the regeneration of methyl nitrite. Since both of the processes carry out similar reaction for MN
synthesis, the raw material used and by-product formed from the reaction are similar. The overall yield and conversion efficiency of both processes are high. Thus, the main factor that affects the selection of
technology is the operating and equipment cost. For non-catalytic process for MN synthesis, it has higher equipment than catalytic process since it required additional column to recover the remaining reactants
and undergo further reaction in order to meet the desired yield. Although non-catalytic process has higher equipment cost than catalytic process, its operating cost is lower than the catalytic process. The catalytic
process requires periodic renewal and regeneration of deactivated catalyst in order to maintain the optimum performance of the process. These renewal and regeneration of catalyst are a long-term expense for the
process and thus the overall cost of catalytic process is much higher than the non-catalytic process. Besides, the operating temperature and pressure of catalytic process is higher than the non-catalytic process.
Thus, catalytic process has higher energy requirement to maintain the operating condition of the reactor.
For the selection of main equipment, tray column is chosen for this process. Since the reaction of this process is occur within liquid and gaseous reactant, a higher liquid-vapour contact efficiency is required to
meet the optimum reaction condition of the process. The liquid-vapour contact in cross flow of tray column is more effective than the counter-current flow in packing column. Besides, tray column is easier to
make inter stages cooling to remove heat produced during the reaction. Thus, it is more suitable for the exothermic reaction in this process.
2.4.3.3. Inherent safety design for MN synthesis

Table 2.4.3.3.1: ISI table for catalytic and non-catalytic process of MN synthesis
Reactor options Non-catalytic process Catalytic process
Sym. Justification Score Justification Score
IRM -121.96 kJ/mol 4 -121.96 kJ/mol 4
IRS -101.67 kJ/mol 4 -101.67 kJ/mol 4
IINT Formation of flammable gas (Methyl Nitrite) 4 Formation of flammable gas (Methyl Nitrite) 4
IFL Flash point of methanol <21°C 3 Flash point of methanol <21°C 3
IEX Methyl nitrite is explosive 3 Methyl nitrite is explosive 3
ITOX TLV of NO <100 (Osha.gov, 2017) 3 TLV of NO <100 (Osha.gov, 2017) 3
ICOR Nitric acid may be produced due to side reaction 1 Nitric acid may be produced due to side reaction 1
II Inventory: 50-200t 3 Inventory: 50-200t 3
IT 60°C 0 20 - 90°C 1
IP 1.36 – 4.08 atm 0 3 - 5.5 atm 1
IEQ Tray column 3 Tray column 3
IST Established practices 1 Established practices 1
Total ISI 29 Total ISI 31
26
Based on the comparisons obtained in the table above, the process option chosen for MN synthesis is the non-catalytic process as the ISI score obtained for the non-catalytic process is lower. Since both
processes are dealing with same chemical components, the chemical inherent safety indexes of both processes are same. The only differences between these two processes are the operating conditions. Non-
catalytic process of MN synthesis has advantages over the operating temperatures and pressure. The operating pressure and temperature of catalytic process are higher than the non-catalytic process and thus the
process pressure and temperature sub index of catalytic process are higher than non-catalytic process.
2.4.4 Dehydration of methanol

The process stream coming out from the methyl nitrate regeneration column contains water, a small percentage of nitric acid and unreacted methanol at a temperature of 60°C and 3 atm. Water and nitric acid must
be removed to ensure that the methanol is recycled back into the system with a purity of 99mol%.

Table 2.4.4.1.1: Comparison table for dehydration of methanol
Parameters Flash separation Column distillation Pervaporation
The pressurized feed stream is partially vaporized The feed stream enters the column that operates at
Separation of methanol from water through a
at a certain temperature and pressure and forms a a temperature higher than the boiling point of the
hydrophilic membrane by inducing a vacuum on
2-phase mixture in the separator with the sudden more volatile component. The distillate will
Working Principle the other side where the permeate flows. Water
pressure drop. The vapor is enriched in the more contain a higher amount of the more volatile
molecules will be passing through the membrane
volatile component whereas the liquid would component. Distillation is suitable to separate non-
and the methanol will pass by the membrane.
contain the least volatile component. azeotrope mixtures, i.e. methanol-water mixture.
Pressure: Low (< 1 atm), to vaporize more of  Temperature: 40 - 50°C
Operating Conditions Pressure: Within the range of 1 – 5 atm
methanol to be recycle back (Luyben, 2010)  Pressure: 0.2 bar (Abdallah et al., 2013)
Lower than column distillation, not able to reach High, able to reach a maximum purity higher than
Separation efficiency Low, about 45% purity at maximum
to 99% purity for methanol 99% (Kubic, 1986)
Energy consumption would be lower than column Energy consumption is high depending on the
Energy Consumption Energy consumption is low
distillation duty of condenser and reboiler
Commonly used, sometimes with a flash separator
 Scarce membrane market
Level of Commercialization Rarely utilize to obtain an almost pure methanol before the stream goes into the column (Luyben,
 Not industrial scale
2010)
 Capital costs: Relatively high
 Capital costs: Low  Capital costs: Low
Overall costs  Operating costs: High, depends on
 Operating costs: Low  Operating costs: High
frequency of membrane replacement.
From the comparison of the technologies, column distillation was chosen to carry out the dehydration of methanol. Flash separation may not be suitable for this process as the maximum purity achievable is
lower than 95% (simulated using Aspen Plus) despite having a low capital and operating costs. This is explainable since it is a single stage separator, and having to achieve a high purity of 99% more stages for
separation is required. Pervaporation is not chosen to carry out the dehydration of methanol and it is due to the low achievable purity and the low availability of the membrane required for the separation with high
capital and operating costs. It has not been scale-up for the dehydration of methanol albeit membrane separation is widely used in the separation of ethanol from water in the industry (Rhim, Kim and Lee, 1996).
As for column distillation, it is a multistage separation process, and thus with the adjustment of the necessary parameters, it is possible to achieve a high purity of more than 99% methanol to be recycled back into
the methyl nitrite regeneration column. In this case, two tray distillation columns (refer to Table 2.4.4.1.1 for selecting tray columns) will be used to achieve 99.95% purity, with the first column removing water
from the mixture and nitric acid will be removed in the second column. Heat integration can be introduced to reduce the operating cost of the column.
27
2.4.4.3 Inherent safety design for dehydration of methanol

Table 2.4.4.3.1: Inherent safety design strategies
Design strategy Parameters
Minimize  Equipment size and pipe length to feasible level
 Storage time or storage capacity of methanol product to feasible level
 Valves quantity wherever possible to prevent possible leaks into the environment
Moderate  Operating conditions of column
 Storing conditions of methanol product and industrial effluents to prevent BLEVE
Simplify  Distributed control system and switches to reduce complications for possible errors
 Fire protection systems should be kept simple
Table 2.4.4.3.2: Inherent safety index for selected technology (Rains, 2014; Terra Industries Inc, 2006; Sciencelab.com, Inc, 2013)
Process options Column distillation Flash separation
Parameters Justification Score Justification Score
Heat of main reaction No reaction 0 No reaction 0
Heat of side reaction, max No side reaction 0 No side reaction 0
Chemical interaction No chemical interaction 0 No chemical interaction 0
Flammability Methanol is easily flammable 3 Methanol is easily flammable 3
Explosiveness Explosiveness of methanol: 30.5 vol% 2 Explosiveness of methanol: 30.5 vol% 2
Toxic Exposure Nitric acid: TLV ≤ 10 4 Nitric acid: TLV ≤ 10 4
Corrosiveness Stainless steel 1 Stainless steel 1
Inventory 1-10 t 1 1-10t 1
Process temperature 70-150°C 1 70-150°C 1
Process pressure 0.5-5 bar 0 0-0.5 bar 1
Equipment safety
Isbl Distillation column 1 Separation column 1
Osbl Atmospheric storage tank 1 Atmospheric storage tanks 1
From the comparative ISI table, it was justified that column distillation is a better option to carry out dehydration of methanol although the components and the operating conditions are similar.
2.4.5 DMO purification

Column distillation is also used to carry out the purification of DMO before entering the hydrogenation reactor. The justifications of the technology selection are somewhat similar to the dehydration of methanol.
For DMO purification, the inlet stream consists of DMO, DMC and toluene. DMO is to be separated from the other 2 components with the use of one distillation column to be sent to the hydrogenation reactor.
Tray columns will be used for its ability to handle large range of flowrates (see Table 2.4.4.1.1).
2.4.6 DMO hydrogenation

The hydrogenation process of DMO involves the reaction of DMO and H2 to produce ethylene glycol (EG) and methanol. In this process, DMO reacts with H 2 to form intermediate methyl glycolate (MG), which
then further reacts with H2 to form EG and methanol. Side reaction might also take place whereby EG reacts with H 2 to form ethanol and water vapour (Zhu et al., 2016). The overall reaction to produce EG from
syngas is derived as:
28
2CO + 4H2 + 0.5O2 → EG + H2 O
The hydrogenation process occurs in a reactor with a condition of approximately 473 K and 2.5 MPa to minimise side reaction (Li et al., 2015). Catalysts are also employed in the reaction to maximise the yield.
For the past decades, DMO hydrogenation involved the use of Cu-Cr as the preferred catalyst on industrial scale whereby it has high catalytic activity. However, due to the toxicity of Cr, the catalyst is then
replaced by Cu/SiO2 with Ni support whereby the process can achieve 100% DMO conversion and 98% EG selectivity as well as having an end life of 2000 hours. Employment of this catalyst also minimises
formation of by-products such as 1, 2-BDO and 1,2-PDO (Zhu et al., 2016).
2.4.6.1 Process options

As DMO hydrogenation utilizes several types of reactors tailored to different industrial needs, it is essential to identify the appropriate reactor configurations based on reactor conditions. The table below
summarizes the difference between two technologies used for DMO hydrogenation assuming same catalyst and capacity.
Table 2.4.6.1.1: Comparison between Fixed bed and fluidized bed reactor for DMO Hydrogenation (Zhu et al., 2013)
Parameters Multi-tubular reactor Fluidized-bed reactor
Reactants enter reactor and pass through catalyst pellets packed Reactants enter reactor at high velocities to suspend catalyst powder, incurring
Working Principle
in a fixed manner fluidization behaviour of catalyst
Bed Height Ratio 7 1
Bed Diameter Ratio 10 1
Heat Transfer Efficiency High as tubular reactor has bigger heat transfer area Low as fluidized bed reactor has smaller heat transfer area
Inlet Gas Velocity Ratio 12 1
Degree of mixing Low due to lower gas velocity High due to higher gas velocity
Catalyst Consumption Low as catalyst pellets are packed and framed High due to catalysts entrained in fluid
Equipment Cost Low due to smaller height and diameter High due to higher height and diameter
Operational Cost Low due to lower inlet gas velocity High due to higher inlet gas velocity
Based on the comparison shown in the table above, it is shown that fixed bed reactor requires smaller bed height and diameter than fluidized bed reactor, thus consuming less catalysts with a higher catalyst
contact efficiency. The inlet gas velocity required for fixed bed reactor is also lower, leading to lower operating costs and pressure drop across the reactor. However, the heat transfer efficiency of fixed bed reactor
is slightly lower than that of a fluidized bed. According to the justification made, it is concluded that a fixed-bed reactor is selected for the process to reduce the costs and maximise the products. Nonetheless, as
DMO hydrogenation is an exothermic process, the temperature control of a reactor is essential to avoid runaway reaction.
2.4.6.2 Inherent safety design

As both the evaluated reactors involve similar conditions and reactants, the inherent safety index of DMO Hydrogenation for the selected reactor is evaluated and summarised as shown in Table 2.4.6.2.1.
Table 2.4.6.2.1: Inherent safety index for DMO Hydrogenation

Chemical ISI, ICI Justification Score
IRM -104.37 kJ/mol 4
IRS -34.09 kJ/mol 4
IINT H2 causes explosion, formation of flammable gas 4
IFL H2 is flammable 4
IEX 70% vol H2 4
ITOX Non-toxic reaction 0
ICOR H2 causes embrittlement, better material needed 2
Process ISI, ICI Justification Score
29
II Little storage of non-hazardous chemicals 0

IT 200 ℃ 2
IP 2.5 MPa (g) 2
IEQ Fixed-bed reactor with jacketed cooler 2
IST Established practices 1
Total ISI 29
The selection criteria for the fixed bed reactor based on inherent safer design is justified in the table below.
Table 2.4.6.3.1: Criterion for technology selection

Criteria Justification
 Eliminate latent failures that lead to major incident by designing a safe workplace.
Safety & Health Issues
 Minimize equipment size and pipe length.
 Minimize inventories and storage of chemicals to avoid leakage to environment
Environmental Impacts
 Substitute hazardous plant effluent via treatment.
 Moderate operating conditions to prevent runaway reaction.
Operability Considerations
 Simplifying complex operations such as control system layouts and equipment switches to reduce potential for error.
2.4.7 MEG purification

After hydrogenation, MEG will be produced along with methanol and some traces of impurities. The MEG purity required for industrial product is at 99.9%. Hence, purification must be done to remove almost all
the methanol and impurities that was produced in the hydrogenation part.
2.4.7.1 Process options

The purification will be carried out by using three distillation columns to achieve desired purity. The table below is a summary of possible distillation columns that can be used to purify the MEG.
Table 2.4.7.1.1: Comparison of several types of distillation column (Visual Encyclopedia of Chemical Engineering, 2017)
Parameters Multi-stage column Packed column Vacuum column
 Feed enters middle of column. Less volatile
 Pressure inside will be maintained at vacuum to
components will transfer from vapor to liquid  Feed mixture enters column, liquid will flow down the
lower the temperature required to vaporize the
stream. column whereas vapor flows up.
liquid.
Working Principle  More volatile components exit the condenser  Feed will pass through the packing which maximize
 Used for heat sensitive products, low
whereas less volatile components exit the reboiler. the vapor-liquid surface contact to ensure an efficient
viscosities liquids and liquids which tend to
 Number of trays/stages determine the purity separation.
foam or foul.
obtained and height of column.
Type of trays:
Type of packings:
 Sieve
Types  Random/Dumped N/A
 Valve
 Stacked
 Bubble cap
 Temperature, oC: 100  Temperature, oC: 100  Temperature, oC: Greater than 70
Feed Conditions
 Pressure, atm: 7  Pressure, atm: 7  Pressure, atm: less than 1
Flowrates Wide range Low Wide range
 Shell: Carbon Steel
Material Shell: Carbon Steel Shell: Carbon Steel
 Tray: Carbon Steel
30
Purity High High High

Equipment Cost High Low High
Operational Cost High Low High
2.4.7.2 Justification of technology selection
From the three types of columns listed in the table above, multistage column will be used for all 3 columns. However, the last column will be operating under vacuum condition. The multi-stage column was
chosen for all three distillation columns since multi-stage column can achieve higher purity when compared to packed column as the purity of multi-stage column can be varied by varying the number of stages in
the column. Besides, it is also easier to carry out maintenance in a multi-stage column by installing manhole to enable easy access into the column. One more advantage of selecting multi-stage column is its
ability to handle a wide range of flow rates. This is due to the plant having quite a high flowrate for this purification part. Although the equipment cost for packed column is much cheaper, multi-stage column is
still preferred to ensure that the purity of products needed can be achieved.
2.4.7.3 Inherent safety design

For purification of MEG, three different distillation columns were compared and multi-stage column was selected. The ISI will be carried out for multi-stage column and packed column.
Table 2.4.7.3.1: ISI for distillation column in MEG purification (CAMEO Chemical, 2017)
Type of Column Multi-stage column Packed column
Flammability CO, H2 are very flammable 4 CO, H2 are very flammable 4
Explosiveness CO, H2: 20 – 45 2 CO, H2: 20 – 45 2
Toxic Exposure TLV > 10000 0 TLV ≤ 1000 2
Corrosiveness Stainless Steel 1 Stainless Steel 1
Inventory 50 – 200 t 3 50 – 200 t 3
Process Temperature 150 – 300 oC 2 150 – 300 oC 2
Process Pressure 0.5 – 5.0 bara 0 0.5 – 5.0 bar 0
Process Equipment Distillation Tower 1 Distillation Tower 1
By selecting multi-stage column, 100% of the hydrogen can be completely removed in the first column. This will eliminate the chances of an explosion that could be cause by the hydrogen (due to its explosive
limits of 18% to 60% with presence of air) if hydrogen is let to cycle within the plant. Next, the number of distillation column could be minimized by using multi-stage column as this column was able to provide
the required purity by just using three columns. Besides, inventories and chemical storage are also minimized by recycling methanol within the plant. The operating conditions were then moderated to ensure that
the purification could run smoothly and the purity required could be obtained. The control system layouts and equipment switches were then simplified to reduce the errors that might occur.
31
Chapter 3:
Process synthesis
& Flowsheet
Development
32
3.1 Process synthesis

Taking a basis of 100,000 metric tonnes of monoethylene glycol (MEG) per annum, the
process synthesis and flowsheet was developed. First of all, syngas is separated into
carbon monoxide and hydrogen, followed by the synthesis of dimethyl oxalate (DMO)
and methyl nitrite (MN) synthesis, in which synthesized DMO will be further purified
before going into DMO hydrogenation. Methanol produced from the MN synthesis is to
be recovered and recycled to save on material costs. Lastly, MEG produced will go
through a purification steps to get the desirable purity for commercial purpose. More
details are further elaborate below.

The separation of syngas is the first procedure to undergo for this plant. CO and H2 are
among the main reactants needed to produce MEG through the DMO Route, and it is
required to be fed continuously into the system. The main components of the syngas
obtained from biomass are CO, H2, and CH4 gas. To separate the CO and H2 from
syngas, a combination of two types of technologies is used, where CO is first absorbed
from the syngas through the COSORB (absorption of carbon monoxide) process.
COSORB process is made of 3 steps, the first step is to absorb Carbon Monoxide from
the rest of the syngas composition using Toluene solvent dissolved in cuprous
aluminium chloride. The second step is to use flash gas-liquid separator to ensure that
the presence of undesired gas is totally removed. The Last step is to separate the Carbon
Monoxide from the Toluene Solvent using a stripper column. The second process is
done to separate H2 from the unabsorbed gases from the absorber column using the
Pressure Swing Adsorption (PSA) process. Pressure Swing adsorption is a two stage
adsorbing system which utilized the difference in the Partial Pressure of the gas
components to separate them from one another. The process is made of two columns
however only one of them would operate during the operation. This is because the
process is made of pressurization and depressurization steps. Pressurization occurs
when the adsorption process is going on and once the pressure of the column exceeded
the maximum Pressure it will be depressurized and the other column would be used for
operation purposes.
33
3.1.1.1 COSORB process

The COSORB Process uses an absorbent to selectively remove the CO from the syngas
at moderate operating conditions. This process can achieve a 98% recovery of CO with
a 99% purity (Keller and Schendel, 1988).
 The syngas will first go through a dehydration step to remove all moisture
content to prevent complications of the separation process as moisture will cause
the separation process to be less efficient.
 The syngas will then go through a heat exchanger to increase its temperature up
to 100°C and a compressor to further increase its pressure to 2 atm which is the
operating conditions of the first absorbing column.
 Toluene which acts as the solvent and Cuprous Aluminium Chloride absorbent
is first mixed with a 1:1 ratio and enters the packed bed absorbing column after
going through a heat exchanger and pump to achieve 100°C and 2 atm
(Gunardson, 1998). The amount of absorbent fed also follows a 1:4 ratio to the
CO contained in the syngas as 1 mole of absorbent will be able to absorb up to 4
moles of CO (Hogendoorn, van Swaaij and Versteeg, 1995).
 Both entering streams into the absorber are fed counter-currently to ensure
maximum efficiency. The top outlet of the absorber contains 2% of the
unseparated CO and the remaining unabsorbed H2 and CH4 gases. The bottom
outlet of the absorber contains mostly CO with trace amounts (< 1%) of H 2 and
CH4 gases.
 The CO rich stream from the absorber is fed to a gas-liquid separator which
operates at 8 atm to separate out remaining trace amounts of other gases to be
recycled back to the absorbing column. The liquid outlet stream of the separator
will be at 40°C and contains only CO, toluene, and Cuprous Aluminium
Chloride.
 The liquid outlet stream then goes through a heat exchanger to increase its
temperature up to 111°C to match the operating conditions of the distillation
column to be fed to. At 111°C and 1 atm, the toluene mixture will vaporize in
34
the distillation column and the CO gas can flow out as the top product of the
column.
 The remaining toluene will condense back into the column as the condenser will
be operating at 100°C which is lower than the boiling point of toluene. The CO
rich stream leaves the distillation column at 100°C, 1 atm, and 99% purity with
trace amounts of toluene to be fed into the DMO Synthesis process in the plant.
 The toluene and absorbent will leave the distillation column as the bottom
products and recycled back into the first absorbing column to be reused.
3.1.1.2 Pressure Swing Adsorption (PSA) process

As CO have been mostly extracted using the COSORB process, Hydrogen now need to
be extracted using PSA process. PSA technology is able recover 90% of hydrogen as
well as obtaining a 99.99% purity. The main principle theory behind the PSA
technology is to physically bind gas molecules to a solid adsorbent inside the column.
Thus, allowing separation of gas molecules from one another.
 The CO lean gas at the top of the absorber at the process is going to be the feed
for the adsorption columns.
 The CO lean gas is made of mostly H2 and CH4 and a little bit of CO leftover
which have not been separated by the COSORB process.
 The condition in which the CO lean gas leaves the absorber is at 40°C and 2
atm.
 Therefore, to meet the required operating condition of the PSA columns which
are 30°C and 11 atm the CO lean gas feed need to go through some process.
 The CO lean gas need to be first fed to a compressor to increase its pressure
from 2 atm to 11 atm.
 The compressing process however also leads to an increase in temperature by

292°C
35
 Therefore, it goes through 2 heat exchangers in which the temperature is first

reduced to 130°C in the first heat exchanger and then 30°C in the second heat
exchanger.
 The CO lean gas is then fed to the PSA technology which is made of two
Adsorption Column to separate H2 from the other gasses.
 99.99% purity of H2 product would then be able to leave the column at the top of
the column.
 The adsorbed gasses which are CH4 and CO then purged at the bottom of the
column.
3.1.2 DMO synthesis

DMO is required as a reactant for hydrogenation process to produce MEG. The
synthesis of DMO required CO and methyl nitrite (MN) as reactant, the reaction is
carried out in vapor phase reaction, hence a fixed bed reactor is chosen to be the design.
CO is being supplied from syngas separation operation which separate CO from other
gases with a purity as high as 99%. MN is being fed into the reactor from the MN
regeneration operation.
The fixed bed reactor is packed with palladium catalyst supported by Al2 O3 which is in
solid form. The lifetime of the palladium catalyst is about 600 hours and prolong
catalyst lifetime can be achieved by controlling the reaction temperature. The operating
pressure of the reactor is controlled at 3 bara and the operating temperature is 140°C.
Two chemical reactions will take place in the reactor and the chemical equations are
shown below:
2CO + 2C𝐻3 𝑂𝑁𝑂 −→ (𝐶𝐻3 𝑂𝐶𝑂)2 + 2 𝑁𝑂 ------ (Desired Product)
𝐶𝑂 + 2C𝐻3 𝑂𝑁𝑂 −→ (𝐶𝐻3 𝐶𝑂)2 + 2𝑁𝑂 ------ (Undesired By-product)
Temperature and pressure are the key parameters to control in order to achieve
selectivity of DMO as high as 95% and a conversion of MN of 90 % with a proper
control of reaction pressure. Dimethyl Carbonate (DMC) produced as by-product in the
reactor will then be removed later in DMO purification process. Due to the highly
explosive property of MN, it was recommended to add nitrogen as a diluent in the
36
reactor due to its inert property. Nitrogen is added in with a ratio of 1.5:1 with respect to
volume ratio of MN. Formation of DMO and DMC is an exothermic reaction. In order
to achieve optimum temperature and prevent runaway reaction from occurring, the
reactor is jacketed with DowTherm A as cooling medium.
3.1.3 Methyl nitrite synthesis

The design of the methyl nitrite synthesis process is done based on “Onion Diagram”
approach which starts the design from the reactor and follows by the separation system
required, heat exchanger network design of the process and utility system. The results of
the process synthesis in methyl nitrite synthesis are shown in table below.
Table 3.1.3.1: Summary of process synthesis of MN synthesis process

Process Synthesis (“Onion Diagram” approach)
Reactor (R-401, R-402 & R-403)
 The reactions involved in methyl nitrite synthesis are shown below:
1. 2𝑁𝑂 + 𝑂2 → 2𝑁𝑂2
2. 𝑁𝑂 + 𝑁𝑂2 ↔ 𝑁2 𝑂3
Main
3. 𝐶𝐻3 𝑂𝐻 + 𝑁2 𝑂3 → 𝐶𝐻3 𝑂𝑁𝑂 + 𝐻𝑂𝑁𝑂
Reactions
4. 𝐶𝐻3 𝑂𝐻 + 𝐻𝑂𝑁𝑂 → 𝐶𝐻3 𝑂𝑁𝑂 + 𝐻2 𝑂
5. 𝑁2 𝑂3 + 𝐻2 𝑂 → 2𝐻𝑂𝑁𝑂
Side 1. 2𝑁𝑂2 ↔ 𝑁2 𝑂4
Reactions 2. 𝐶𝐻3 𝑂𝐻 + 𝑁2 𝑂4 → 𝐶𝐻3 𝑂𝑁𝑂 + 𝐻𝑁𝑂3
 The side reactions due to formation of N2O4 will reduce the yield of methyl nitrite
and produce undesired nitric acid.
 In order to minimise the side reactions and maximise the overall yield of the
process, the methyl nitrite synthesis process is designed to consist of 3 reactors.
The functions and conditions of each reactor are shown below:
 R-401
 The formation of nitrogen dioxide (NO2) is occurred in R-401
 The nitrogen monoxide (NO) and oxygen (O2) are supplied in ratio of 6:1 to
ensure that the conversion of oxygen supplied into nitrogen dioxide achieved at
least 99%.
 Some of the dinitrogen trioxide (N2O3) and dinitrogen tetroxide (N2O3) will
also formed in R-401. In order to minimise the formation of N2O4, the
operating temperature of R-401 is set at 100℃ to shift the equilibrium between
NO2 and N2O4 almost all the way toward the NO2.
 R-402
 The methanol is supplied in ratio of 12 moles to 1 mole of oxygen supplied in
R-401 to ensure that all nitrous acid formed in R-402 is converted to methyl
37
nitrite and water.

 The operating temperature and pressure of R-402 are set at 60℃ and 4 atm to
improve the yield of the methyl nitrite.
 A tray column is selected due to the effective liquid-vapour contact of column.
 The methyl nitrite which is in vapour phase will leave from the top of the
column while the methanol, water and nitric acid will leave from bottom of
column.
 R-403
 A smaller reactor using same operating condition as R-402 to convert the
remaining NO leaving R-402 in order to achieve higher overall conversion of
NO.
 A packing column is selected since it is cheaper than tray column when handle
with less quantity of component and smaller tower diameter.
 Safety concern – A cooling jacket are installed since the reactions involved are
exothermic to maintain the temperature and prevent runaway reaction. Nitrogen
will also feed into reactor as diluents since methyl nitrite are explosive.
 Economic aspect – The third reactor (R-403) increase the overall conversion of
NO and thus less fresh NO is needed to supply to the system.
Separation system (S-401)
 A flashing column is used to separate most of the methyl nitrite formed in R-402
from remaining NO before entering R-403 to minimise the size required for the
reactor. It operates at temperature of -20°C and pressure of 10 atm. The vapour
stream will enter R-403 while the liquid stream will be heated to 140°C and
recycle to DMO synthesis.
Heat Exchanger Network
 Most of the stream involved in this process required to be heated or cooled to
desired temperature before entering the reactor and thus, the heat recovery of the
process is essential to achieve higher energy efficiency. A proper heat exchanger
network will be designed to achieve optimum heat recovery of the plant.
Utility system
 10 barg saturated steam is selected for heating process involved in this section.
For cooling purpose, cooling water at 29°C is commonly used for temperature less
than 100℃ while Dowtherm is selected for process stream higher than 100°C.

The initial condition of the process stream is at 20°C and 1 atm. The process stream
consists mainly dimethyl-oxalate (DMO), methanol, dimethyl carbonate (DMC),
toluene and water. The remaining components are of insignificant amount and can be
ignored. Before the process stream enters the purification column (D-301) that operates
at a temperature of 112°C, it is pumped to a pressure of 2 atm to prevent backflowing of
38
the process stream. The stream will be vaporized in the column and the volatile
impurities mainly DMC and toluene will exit from the top. The impurities will then pass
through a condenser operating at 97.5°C and 1.3 atm. DMO will be separated from the
impurities due to its higher boiling point as compared to the other components and exit
the column as a bottom product. Any DMO that exits at the top will then be condensed
back into the column. The reboiler of the column operates at 184.8°C and 1.8 atm in
which it is used to redirect the light key components back into the column to be
vaporize and exit as top product. DMO will then leave the column as a bottom product
and going into the hydrogenation process. The top product contains mostly DMC and
toluene in vapour form enters a condenser (E-303) to condense into liquid at a
temperature of 30°C.

This process involves with 2 distillation columns to achieve a methanol purity of 99%
which will be sent to a holding tank that also collects the recycled methanol recovered
from MEG purification process. The initial condition of the process stream is 17.2°C
and 3.5 atm and contains mostly methanol and other impurities such as water, nitric acid
and toluene. The stream is first heated to a temperature of 60°C and pumped it to a
pressure of 5 atm to prevent backflow of process streams as the column (D-501) will be
operating at a pressure of 4.8atm. The first distillation column (D-501) is operating at a
temperature of 1122°C. With the same concept as the previously mentioned purification
column, the process stream will vaporize in the first column and methanol with other
volatile components would exit from the top. The condenser of the first column operates
at 108.2 °C and 4.3 atm and this will condense any heavy key components that are
present at the top column. Methanol has a low boiling point compared to the condenser
operating temperature thus it leaves the first column as a vapour distillate and enters the
second distillation column. The second column operates at a temperature of 111°C and
the condenser in the second column is operating at a temperature of 101.1°C and 3.6
atm. At this pressure, nitric acid has a higher boiler point compared to methanol.
Therefore, it exits the column as the bottom products whereas methanol exits as a
vapour distillate. The bottom products from the two columns will be cooled to 30°C
before it is collected in the waste tank as the allowable storage temperature for nitric
acid is below 38°C (Poly Processing, 2017). The purified methanol at 99mol% is then
39
condensed back to liquid at 32°C and 3.5 atm to be stored in a pressurized holding tank
to prevent the methanol from vaporizing.

The reactor (R-601) for hydrogenation process takes place in a catalytic fixed-bed
reactor. The hydrogenation of DMO converts DMO to intermediate methyl glycolate
(MG) and methanol, then to MEG and methanol. During the reaction, the catalyst CuNi-
SiO3 is used in order to enhance the reaction. The optimum operating condition of the
reactor for the catalyst employed is at 200°C and 25 bara. High reaction temperature
introduces the side reaction which converts MEG to ethanol and water. The residence
time of the reactant is set to be less than 5 seconds to avoid over-hydrogenation of
DMO, which leads to production of ethanol as well. The chemical reaction taking place
in the reactor is shown as following:
𝐷𝑀𝑂 + 2𝐻2 ↔ 𝑀𝐺 + 𝑀𝑒𝑡ℎ𝑎𝑛𝑜𝑙 …Eqn (1)
𝑀𝐺 + 2𝐻2 ↔ 𝑀𝐸𝐺 + 𝑀𝑒𝑡ℎ𝑎𝑛𝑜𝑙 …Eqn (2)
𝑀𝐸𝐺 + 𝐻2 ↔ 𝐸𝑡ℎ𝑎𝑛𝑜𝑙 + 𝐻2 𝑂 …Eqn (3)
The ratio of hydrogen to DMO (HDMR) fed to the reactor is maintained at 45, which is
the optimum condition for the best selectivity and yield. Based on the result from Aspen
simulation, the selectivity and yield achieved is 99% and 97% respectively. As DMO
hydrogenation takes place at high temperature and pressure condition, safety concerns
are introduced such that to reduce the likelihood of major accidents. The safety
approach taken is introduction of jacketed cooler around the reactor as the reaction
involved is exothermic. A small amount of H2 and CO is purged to flare tower to
remove impurities in the reactor. H2 is also directly fed to the reactor to avoid mixing of
H2 and reactants at the pipeline as it is flammable and explosive. As for economic
concern, unreacted H2 is recycled back to the reactor to ensure that the HDMR remains
in the optimum range which is 40-80. From Aspen, the HDMR was obtained to be 45.
For separation system, a flash drum (S-601) is used in the system to separate product
stream from the reactor into liquid and vapor products. The flash drum operates
adiabatically in an isobaric condition at 100°C and 23.8 bara to remove most of the H2
and CO as vapor product to be purged and recycled. A flash drum is employed as its
40
costs are lower as well as high purity of the separated streams can be achieved. This
could reduce the equipment size as well as the complicity of the plant design.
Heat recovery is introduced for cooler E-602 and the jacket cooler of reactor R-601 by
using Dowtherm G. The cooling utility is first fed into E-602 at 40°C with an outlet
temperature of 170°C, then fed directly into the jacket cooler with an outlet temperature
of 172.5°C. The usage of Dowtherm G is costly, thus prompting the heat integration is
essential. Further optimization of heat recovery through integration will be done in the
later parts of the project.
Lastly, for the utilities system, hot and cold Dowtherm G ranging from 40°C to 355°C
is used in the hydrogenation process. As both equipment operates at high temperature
which requires high target temperature, the usage of cooling water and steam is not
feasible. Hence, Dowtherm G is the appropriate utility to be used in DMO
hydrogenation process.

The first column will be having an operating condition of 192 oC and 7 bara. The
condenser will be at 4 bara and reboiler at 5 bara. The flow rate entering the column is
684.785 kmol/hr containing 32.26% MEG, 66.5% methanol and other components at
very small amount. The top product will remove all the H2 and most of the methanol.
The H2 is to be removed first to ensure that no recycling of H2 within the system as it
will cause explosion (Crowl and Jo, 2007). The top product is then separated again by
using a flash separator at 30oC and 2.6 bara to separate the H2 and methanol. H2 will
then be sent to waste and the recovered methanol will mix with a fresh methanol stream
and sent to a holding tank. The bottom product of the first column is then fed into the
second column with operating condition of 211.43 oC and 7 bara. For the second
column, the condenser will be at 3.5 bara and reboiler at 4 bara. This column is to
remove all the other impurities remaining such as methanol, water, DMC, and nitric
acid. The top product will be the impurities which will be sent to a cooler to be cooled
down before going to waste tank for waste treatment. As for the third column, it will
operate at vacuum condition with 169.4oC and pressure less than 1 atm. The condenser
will have a pressure of 0.5 bara and reboiler at 0.8 bara. A steam ejector will be
included to help the distillation column to enter vacuum condition by inserting steam
41
into the column to remove low key hydrocarbon causing an empty space created in the
column which is known as vacuum (Marpudi, 2012). There will also be a vacuum
regulator installed to ensure that the distillation will always be in vacuum condition.
Vacuum condition is used to lower the boiling point of EG so that the product will come
out as liquid phase (Naik et al., 2017). At 0.8 bara, it was determined that the boiling
point is 191oC and the temperature obtained was at 189oC which means that the product
will still be in liquid phase. The third column is used to remove the remaining bits of
impurities and ensure that the MEG purity of equal or greater than 99.95% was
obtained. The MEG will exit from the bottom of the column which will then be cooled
to 30oC and pumped to 1bar into a storage tank. As for the remaining impurities such as
MG and methanol, it will exit the top of the column which will also be cooled to 30 oC
and sent to a waste treatment.
3.2 Process description

3.2.1.1 COSORB process
The use of the COSORB process is to separate CO from the other gases in the syngas.
The syngas is fed at surrounding temperature of 32°C, and 1 atm. Under this pressure
and temperature, the components in the syngas are all in vapor form. The easiest
separation method is to separate the components by their boiling points, which is -191.5
°C for CO, -252.9 °C for H2, and -161.5 °C for CH4. However, it is difficult to separate
these gases from each other as their boiling points are relatively close and at negative
temperatures, which will require the equipment to operate under very low temperatures,
therefore the COSORB process is chosen as the operating conditions are moderate. The
dehydrated syngas will first enter the compressor (C-101) which will compress the
syngas to 2atm and then enters a heat exchanger (E-102) to increase its temperature to
meet feed conditions of 100°C and 2 atm for the absorbing column (V-101). Toluene is
also mixed with the Cuprous Aluminium Chloride absorbent in a mixing tank before
going through heat exchanger E-101 and pump P-101 and eventually enters V-101 at
feed conditions. The bottoms outlet of V-101 will consist mainly of CO, toluene,
Cuprous Aluminium Chloride and a small amount of other gases that is dissolved in the
solvent. This stream is fed into a flash evaporator S-101 which operates at 1 atm to
42
separate out the unwanted other gases and recycle it back to V-101 to leave the
COSORB process. Liquid stream from S-101 flows through a valve to achieve 1 atm
and another heat exchanger E-106 to heat the stream up to 110°C. This CO-rich stream
is then fed to distillation column D-101 which will separate the CO out from the toluene
and absorbent mixture. The reboiler for this column E-108 will operate at 120°C to
vaporize the toluene stream carrying any CO and condenser E-107 condenses the top
products to 100°C which will convert the toluene back into liquid form and flow back
into the column. The bottom outlet of D-101 which consists of only toluene and
Cuprous Aluminium Chloride absorbent will be recycled back into absorber V-101 to
be reused.
3.2.1.2 PSA process

The CO lean from gas from V-101 is made of mostly H2, CH4 and a little bit of leftover
CO. The stream is at 40°C and 2 atm therefore it needs to go through a few processes
prior to entering the PSA adsorption columns. The CO lean gas is first compressed to 11
atm at the C-102 compressor. The gases also experience a temperature increase inside of
the compressor as it increases all the way to 292°C. Therefore, it need to go through
cooling process using 2 heat exchanger which are E-103 and E-104. At E-103 the
temperature decreases from 292°C to 130°C whereas the temperature decreases from
130°C to 30°C at E-104. The gas is then fed to either V-102 or V-103 which are both
adsorption column. The gas is only fed to either one of the column where the gasses are
adsorbed by solid adsorbent material. In this case the adsorbent material is activated
carbon which is able to adsorb CO whereas zeolites are used to adsorb CH4. PSA works
at constant temperature and requires no heating process as the process is based on the
pressure changes. Adsorption is based on its isotherms which give the relationship
between the partial pressure of a gas molecules with its equilibrium loading. Gases
which are highly volatile with low polarity such as H2 and helium does not have the
properties to be adsorbed within the column. This would then allow it to be separated
away from the other gases. The adsorption process takes place in a high pressure and
this process is called pressurization. The adsorption process would then stop once the
equilibrium loading is reached where the adsorbing material is loaded and the adsorbed
gas need to be purged. 90% of H2 is recovered as product and the rest would be used to
purge the adsorbed gas in the column. This is done in a low-pressure condition and is
43
hence called the depressurization. While the depressurization process is going on within
the column, the CO lean gas is fed to the other column and when this column reaches
the equilibrium loading point, the gas would then be fed to the other column. The 2-
column system allow the process to be a continuous which allow for higher percentage
of recovery and purity.
3.2.2 DMO synthesis

CO supplied from syngas separation system (stream 21) is passed through a compressor
(C-201) and to be compressed from 1 bara to 3.3 bara. Due to the isenthalpic
compression manner, the temperature in (stream 22) increased to 282.2°C, which is way
higher than the operating temperature of the reactor. Hence, CO is cooled with a heat
exchanger (E-201) to 140°C (stream 23) and 3.2 bara before feeding into the reactor.
DowTherm 4000 is chosen to be the cooling medium for E-201 heat exchanger as the
temperature of process stream is required to cool from a very high temperature (282.2°C
to 140°C)
MN is supplied from MN regeneration process (Stream 47) from a pressurized storage

vessel which is operating at 3.5 bara and it is then passed through a heat exchanger (E-
203) to be heated to 140°C before feeding into the reactor as shown in stream 48.
Saturated steam at 10 barg is used as heating medium for E-203 to 140°C.
Fixed bed reactor (R-201) is chosen to be the design for DMO synthesis process and a
pressure drop of 0.2 bara across the reactor is assumed at the current stage. Due to the
exothermic property of the reaction, the reactor is cooled with DowTherm A feeding
into the jacket at 40°C, 1.5 barg to prevent thermal runaway reaction. The reactor must
be maintained at its operating temperature which is 140°C to ensure a high selectivity of
DMO and low formation of by-product, DMC. Due to high concentration of MN exist
in the reactor as reactant and its explosive property, nitrogen at 3.2 bara and 140°C
(stream 24) is fed into the reactor as a diluent to ensure the MN is kept below the
explosivity limit.
The product exiting from the reactor (stream 25) with vapor fraction 1 is cooled with
heat exchanger (E-202) from 140°C to 20°C before entering to a gas liquid separator
(stream 26). DowTherm 4000 is chosen to be the cooling medium, entering the heat
exchanger at 10°C and 1.5 bara. The process stream is then being fed into a gas liquid
44
separator, (S-201) in order to separate the two-phase mixture. The operating

temperature of the gas liquid separator is at 20°C and 1 bara. The liquid exiting the
separator, (stream 62), is then being sent to the DMO purification unit to carry out
further purification. The vapor phase exiting the separator, (stream 27), is then being
transferred into a pressurized storage vessel which is operating at 1 bara and 20°C.
From the storage vessel, 10% of the vapor stream will be purged, (stream 104) and the
remaining 90% (stream 28) will be sent into a compressor (C-203) to be compressed
from 1 bara to 4 bara and sent to MN regeneration system.
3.2.3 MN synthesis
In this process, MN (CH3ONO) is formed through several stepwise reactions between
nitrogen monoxide (NO), O2 and methanol. The main source of the NO is supplied from
DMO synthesis process since it is one of the by-products formed during DMO synthesis
reaction. This NO-rich stream will flow through the compressor (C-202) to increase its
pressure to 4 atm before mixing with fresh O2 and NO gas streams which have
compressed to a pressure of 4 atm using compressors (C-402 and C-401) respectively.
Since the temperature of these gas streams are highly increased after compression, heat
exchanger (E-401) is used to cool down this gas stream from 204.6°C to 100°C before
entering the first reactor (R-401). The pressure drop occurring in each heat exchanger is
assumed to be 0.1 atm and thus mixed gas stream will leave E-401 at 3.9 atm and
100°C.
In the first reactor (R-401), nitrogen dioxide (NO2) is form through the reaction between
NO and O2. The total NO and O2 fed in this stage are in ratio of 6 moles of nitrogen
monoxide to 1 mole of oxygen to ensure that all oxygen supplied is reacted with NO to
produce sufficient NO2 for subsequent reaction for synthesis of MN. The reactor’s
operating temperature is maintained at 100°C to minimise the formation of dinitrogen
tetroxide (N2O4). The pressure drop occur in each reactor is assumed to be 0.4 atm and
thus the product stream will leave the reactor (R-401) at 3.5 atm and 100°C.
After all the oxygen in reactor (R-401) has reacted, the NO2 formed and remaining NO
will enter the second reactor (R-402) at temperature of 100°C. In this reactor, NO2 will
react with NO to produce dinitrogen trioxide (N2O3). The dinitrogen trioxide formed
will then react with methanol to produce MN and water. Some nitric acid (HNO3) is
45
also produced through the side reaction involved in this process. The methanol involved
in this reaction is fed into the reactor (R-402) at a ratio of 6 moles of methanol to 1
mole of nitrogen dioxide fed. The methanol used in the reactor is supplied from the
holding tank that store the methanol recycled from methanol dehydration process and
MEG purification process. Since the methanol is stored at 32°C and 2.5 atm, it will be
pumped and heated to 3.5 atm and 60°C using pump (P-401) and heat exchanger (E-
403) before entering the reactor (R-402). The operating temperature of reactor (R-402)
will maintain at 60°C. The MN formed and remaining NO will leave the reactor in
vapour phase from top of the column at 60°C and 3.1 atm while water and nitric acid
will be mixed with remaining methanol and leave the reactor in liquid phase from the
bottom of the column. The methanol rich stream will then enter the following
dehydration process to recover methanol from water and nitric acid.
The third reactor (R-403) of this process will undergo a similar reaction as second
reactor (R-402) to further react the remaining NO. Before entering the third reactor (R-
403), the stream containing NO and MN from second reactor (R-402) will pass through
condenser (E-402) and vapour-liquid separator (S-401) to condense and separate the
MN from the gas stream at -20°C and 10 atm. The condensed MN will leave from the
bottom of the vapour-liquid separator (S-401) and enter the heat exchanger (E-405) to
heat up to 100°C before mixing with top product stream of third reactor (R-403).
Meanwhile, the NO containing gas stream will leave the vapour-liquid separator (S-
401) from top and enter a heat exchanger (E-404) and a Joule-Thompson pressure
reduction valve to change the temperature and pressure of gas stream to 60°C and 3.9
atm respectively before mixing with fresh oxygen stream and enter the third reactor (R-
403).
Similar as second reactor (R-402), third reactor (R-403) operating at 60°C and the MN,
water and nitric acid are produced in the reactor. The total mole ratio of NO to O2 fed is
6:1 while the mole ratio of methanol fed to O2 fed is 12:1. The methanol used in this
reactor (R-403) is also supplied from same methanol holding and is compressed and
heated by P-402 and E-406 to 60°C and 3.9 atm before entering the reactor. The nitric
acid and water formed are leaving from the bottom of reactor (R-403) with unreacted
methanol and enter the following dehydration process. The MN formed in reactor (R-
46
403) will leave from top of column mixed with MN stream leave from vapour-liquid
separator (S-401) before it is recycled back to the DMO synthesis process. Since all
reactions involved in this process are exothermic, all three reactors will be installed a
cooling jacket which uses cooling water as the cooling medium.

Once DMO is synthesized in the reactor and separated from the other vapour
components, it should go through a purification step to achieve a high purity reactant for
the hydrogenation process to increase the final quality of the MEG product. The process
stream going into the purification column (D-301) has a mixture of DMO, methanol and
other impurities. As the flowrate of the bottom stream is quite large, the possibility of
DMO solidifying is unlikely and thus it is not necessary to add a solvent (i.e. methanol)
into the stream (Yu and Chien, 2017). The top product would enter a flash separator (S-
301) which separates the gases and are send to the flare tower. The bottom product of
the separator contains methanol and methyl nitrate would then be send out to a
wastewater treatment facility. A process flowsheet that uses Aspen software to simulate
the process is shown in the Appendix A3.1.

The goal for this process is to recover the unreacted methanol from the MN regeneration
reactor so that it can be recycled back into the system. The dehydration process involves
two distillation columns to achieve a methanol as pure as 99mol%. The process stream
coming out from reactor contains mostly methanol and other impurities such as MN and
water. This stream will be heated to a higher temperature and is pumped into the first
distillation column (D-501). Since methanol has a relatively low boiling point compared
to water, it exits the column as top product with nitric acid and enters a second
distillation column (D-502) for further purification of methanol. The second distillation
column is used to separate nitric acid from methanol, where methanol exits as a vapor
distillate and nitric acid leaves the column as a bottom product. The vapor distillates
will the go through a phase change to liquid phase before it goes into a holding tank
(TK-401). The bottom product from the first and second column will be cooled and
collected in a waste tank which will be send to a wastewater treatment facility. An
Aspen flowsheet for this process is shown in the Appendix A3.1.
47

DMO hydrogenation process converts DMO to MEG via reactions with H2. Liquid
DMO at 152°C is sent to a pump (P-601) to increase the pressure from 2.84 bara to 25
bara with a small increment on temperature. The pump duty is shown to be 0.036 MW
based on Aspen simulation. The DMO from pump outlet is then sent to a heat
exchanger (E-601) to be heated to vapour at an outlet temperature of 310°C with a
pressure drop of 0.2 bara. The heating utility used is Dowtherm G at 3 bara, which has a
temperature of 355°C. The heating duty of E-601 is found to be 4.53 MW. The vapour
DMO is then sent to a fixed-bed catalytic reactor (R-601) to undergo hydrogenation. At
the same time, H2, which is available in the holding tank T-601 at 11 bara and 30°C, is
compressed to 25 bara and 151.8°C by compressor C-601 with a duty of 0.97 MW. The
compressed H2 is then sent to R-601 for hydrogenation reaction. Inside the reactor,
DMO hydrogenation process takes place in a fixed bed reactor which operates at 200°C
and 25 bara. The duty of the reactor is -0.48 MW, showing an exothermic reaction. The
reactor is constantly being cooled using Dowtherm G available at 170°C to maintain at
operating temperature. After the reaction, the reactor outlet stream, which is at 24 bara
and 200°C is sent to a cooler (E-602) to be cooled to 100°C with a pressure drop of 0.2
bara using Dowtherm G at 40°C. The cooling duty is shown to be -18.75 MW. The
partially condensed stream is then sent to an adiabatic flash drum (S-601) to separate
liquid and vapor at isobaric condition. 1% of the vapor outlet is purged whereas the
remaining is compressed to 25 bara and recycled to the reactor. The liquid product
stream is then sent to MEG purification section to extract MEG.

In MEG purification, the feed will be coming from the hydrogenation process which
contains mainly MEG, methanol, Water, H2 and a few more compounds which are
present in very small amount. The main equipment would be three distillation columns
(D-701, D-702, D-703) where all the unwanted components are separated out to obtain
MEG with a purity of 99.9% at the end of the distillation. The first column (D-701) is
used to separate out all the H2 and most of the methanol. The top product of D-701 will
contain mainly of H2 and methanol which will then be fed into a separator (S-701) to
obtain the methanol which will be mix with a methanol top up stream and then sent to a
holding tank (TK-401) while the H2 will be sent to waste. The second column is then
48
used to separate the remaining methanol and other components. The top product will be
send to a cooler to be cooled down and finally send to waste whereas bottom product
will enter the third column to separate the remaining components to obtain the desired
purity of MEG. There is a cooler and a pump at the bottom product to cool the product
and then pump it into a storage tank. A flow sheet for this process is shown in the
Appendix A3.1.
3.3 Process flow diagram (PFD) and effluent summary

PFD for each section are shown on A3 size with mass balance and utilities table. A
master PFD for the overall process is shown after the individual sections. A summary of
the effluent streams coming out from the MEG plant is shown after the PFDs.
49
50
51
52
53
54
55
56
57
58
59
60
3.4 Process Optimization

Process optimization is required to be done by carrying out process heat integration
after developing the Process Flow Diagram. By carrying out optimization, the amount
of fresh utilities required and the energy usage within the processing plant will then be
minimized by recovering the heat energy from the process stream.
3.4.1 Original Heat Exchanger Network before Heat Integration.

Figure 3.4.1.1: Heat Exchanger Network Before Process Integration
The stream data extraction table is shown in Appendix A3.2 Table A3.2.1. The
minimum hot utility is found to be 118955.35 kW and the minimum cold utility is
found to be 95673.75 kW. A total number of 41 heat exchanger units are required.
3.4.2 Pinch Analysis

The composite curves are generated by using a ∆ Tmin of 6°C. The problem table
algorithm and cascade are attached in Appendix A3.2.2. Based on the cascade the
minimum hot utility is 37015.9kW and minimum cold utility required is 60386.6kW.
61
The pinch temperature is determined to be 120.1°C with hot pinch temperature at

123.1°C and cold pinch temperature at 117.1°C. Hot and Cold composite curves and the
grand composite curves are shown in Figure 3.4.2.1 and Figure 3.4.2.2.
Figure 3.4.2.1: Hot and Cold Commposite Curves
The utilities allocated are shown in Figure 3.4.2.2. Dowtherm G is used with specific
heat of 2.717 kJ/kg.K and entering the system at 355 °C and a duty of 13524.3 kW.
High pressure saturated steam (20barg) is required in 7773.82 kW with inlet
temperature of 214°C and saturated steam of 10bar is required with 15699 kW and inlet
temperature of 184.12°C as heating utilities.
Several cooling utilities are used in this process, Dowtherm 4000 and cooling water.
The duty required by dowtherm 4000 is 1795.21 kW and duty of cooling water is
1.238 𝑥 107 𝑘𝑊.
Figure 3.4.2.2: Grand Composite Curve
62
3.4.3 Heat Exchanger Network after Heat Integration

The thermodynamic data for individual heat exchange unit is tabulated in Appendix
A3.2.1. All the heat exchangers used are shell and tube configuration. The composition
of the stream entering the heat exchanger can be found from the Process Flow Diagram
stream table. The heat exchanger network after heat integration is shown in Figure
3.4.3.1 and Figure 3.4.3.2
Figure 3.4.3.1: Heat Exchanger Network Above Pinch
Figure 3.4.3.2: Heat Exchanger Network Below Pinch
63
Certain heat exchangers are removed in the later part. Example, heat exchange system
that includes reactors are to be removed as reactor has a very high operability risk hence
it must be cooled or heat by fresh utilities. Mixing of other process stream between the
reactor and the cooling medium can lead to catastrophic disasters.
Heat exchangers that contain hazardous components such as vapor methanol and
Methyl Nitrite, are removed from heat exchanger network optimization as leakage of
these hazardous components. Heat exchangers removed from the network are shown
below in Table 3.4.3.1
Table 3.4.3.1: Hazardous Heat Exchanger Table
Heat Exchanger Removed Justifications

E-103, E-104 High Pressure Stream (20barg)
E-203, E-401, E-402, E-404, E- Hazardous streams (Methyl Nitrite, Explosive and
405 Flammable)
E-502, E-503, E-505, E-506, E- Hazardous streams (Hydrogen and Methanol Vapor,
508, E-601, E-602, E-701, E- Flammable)
710
GCC Placement
64
Figure 3.4.3.3: Equipment placement on GCC
The figure above shows the placement of equipment such as distillation columns and
reactors on the GCC. Based on the figure, it is observed that several equipment have a
temperature range near to the pinch temperature. Hence, process changes can be made
in order to reduce the total utility needed. The process changes are discussed in the table
below.
Table 3.4.3.2: Process changes for MEG production plant
Equipment Process change
D-101 Increases pressure to increase operating
temperature to above pinch to decrease
hot and cold utility
R-201 Remains unchanged; exothermic reactor
placed above pinch to decrease hot
utility
R-401 Increases pressure; exothermic reactor
utility
R-402 Increases pressure; exothermic reactor
65

utility
R-403 Remains unchanged; operating
temperature too low to increase to above
pinch. Trade-off for operating cost too
large
R-601 Remains unchanged; exothermic reactor
utility
temperature to above pinch;
D-702 Remains unchanged; Operating
temperature too high to decrease to
below pinch. Trade-off for operating
cost too large
D-703 Decreases pressure to decrease
operating temperature to below pinch to
decrease hot and cold utility
3.4.4 Network Optimization with Process Changes

Aspen Energy Analyser is used to analyse the optimum delta T min by determining the
temperature at the lowest total cost (capital and operating costs). After energy analyser
was carried out, the ∆𝑇𝑚𝑖𝑛 is found to be 7.5°C. A new PTA and Composite Curve are
constructed with 7.5°C ∆𝑇𝑚𝑖𝑛 is shown in Appendix A3.2.3 and A3.2.5, heat exchanger
network is shown below:
Figure 3.4.4.1: Heat Exchanger Network After Heat Integration
66
Different Heat Exchanger Network, (HEN) parameters are compared and shown in
Table 3.4.4.1.
Table 3.4.4.1: Heat Exchanger Network Comparisons.
Comparison Parameters HEN 1 HEN 2 HEN 3

6 6 7.5
Pinch Temperature (oC) 120.1 120.1 183.55
Minimum Hot Duty (kW) 118955.35 37000 12978.14
Minimum Cold Duty (kW) 95673.75 60386.66 5009.08
Number of HE 41 50 26
Total Cost Index (Costs/s) - 0.182 0.06875
Capital Costs Index (Costs/s) -
Based on Table 3.4.4.1, Heat exchanger network number 3 has the most optimum
design with ∆𝑇𝑚𝑖𝑛 of 7.5oC with a pinch temperature of 183.55oC. The minimum hot
duty is 12978.14kW and cold duty is 5009.08kW.
3.2.5 Advanced Network Optimization

As the pinch temperatures of 184 °C is determined for hot pinch and 179 °C is
determined for cold pinch from the previous section, the generation of electricity is not
67
feasible in this plant. The generation of the lowest pressure steam will also require
temperatures significantly higher than 184.13 °C as LP steam has a saturation
temperature of 184.13 °C and a pressure of 10 bar. If any process steam is to be used to
generate the steam, it should be much higher than the saturation temperature of that
steam to ensure that the process is cost efficient. As electricity generation is not feasible
in this plant, the carbon footprint before and after heat integration is compared. The
assumptions made for carbon footprint estimation is explained in Appendix A3.2.
The table below shows the carbon intensity and carbon footprint before heat integration.
Table 3.2.5.1: Carbon Intensity and Footprint before heat integration

Carbon Carbon
Energy Percentag Energy Duratio Power Intensity Footprint
Source e Used (kW) n (h) (kWh) (kg CO2 (kg CO2
per year) per year)
Natural 50035828 12508957
0.5 63176.551 250179142
Gas 3.9 1
35025079 350250798. 12258777
Coal 0.35 44223.5857
8.7 7 9.6
7920
Hydropo 17689.4342 14010031 14010031.9 1961404.4
0.14
wer 8 9.5 5 73
10007165. 8005732.54 80057.325
Oil 0.01 1263.53102
68 3 43
622445705. 24971881
Total 1.0
2 2.3
The same calculations were performed for after the heat integration was performed and
the duty required for utility heating used was reduced to 12978.14 kW. The new carbon
footprint calculated was 68044907.15 kg CO2 per year. Therefore, the difference in
carbon footprint before and after heat integration is calculated below,
𝐶𝑎𝑟𝑏𝑜𝑛 𝑓𝑜𝑜𝑡𝑝𝑟𝑖𝑛𝑡 𝑟𝑒𝑑𝑢𝑐𝑒𝑑 = 622445705.2 − 68044907.15

= 554400798.1 𝑘𝑔 𝐶𝑂2 𝑝𝑒𝑟 𝑦𝑒𝑎𝑟
𝐶𝑎𝑟𝑏𝑜𝑛 𝑓𝑜𝑜𝑡𝑝𝑟𝑖𝑛𝑡 𝑟𝑒𝑑𝑢𝑐𝑒𝑑 = 5.544 × 108 𝑘𝑔 𝐶𝑂2 𝑝𝑒𝑟 𝑦𝑒𝑎𝑟
The carbon footprint after heat integration is reduced by a significant percentage of
89%
68
69
Chapter 4: Mass
and Energy
Balance
4.1 Mass Balance

4.1.1 Major Equipment in Syngas Separation
CO-Lean Gas
4.1.1.1 Absorber (V-101) Toluene Solvent

V-101
Syn-Gas Feed
CO-Rich fluid
Figure 4.1.1.1.1: Sketch of Absorber (V-101)
Basis of Calculation:
Absorber V-101 column is the first equipment within the plant. Syngas is the feed inlet
going into the column where its composition is made of Hydrogen, Carbon Monoxide
70
and Methane. The purpose of Absorber V-101 column is used to extract Carbon
Monoxide from the rest of the syngas composition. The solvent used to absorb Carbon
Monoxide from Syngas is Toluene Solvent dissolved in Cuprous Aluminium Chloride.
𝑘𝑚𝑜𝑙
The amount of Syngas Fed to the column is 2060.339 ( ). The value is obtained
ℎ𝑟
based on the required amount of Hydrogen and Carbon Monoxide for the reactors to
produce MEG (Mono Ethylene Glycol). The molar composition percentage of the
components for the Syngas feed are 57.702%, 30.98 % and 11.314% for Hydrogen,
Carbon Monoxide and Methane respectively.
Assumptions made for the Calculation:
1. 98% of Carbon Monoxide is absorbed at the bottom of the column

2. 1% of Hydrogen and Methane Gas is absorbed at the bottom of the Column
3. 100% of the Toluene Solvent goes to the liquid outlet of the column
4. Isothermal Condition
Key Calculation step
1. The amount of Toluene Solvent used in V-101 column is determined based the
literature review which stated that the ratio between the Syngas Feedstock and
Toluene Solvent used is:
4 mol Syngas/ 1 mol Toluene Solvent.
1 mol Cuprous Aluminium Chloride / 1 mol Toluene Solvent.

2. Once the molar flow rate is obtained mass flow rate of each component and the
total molar flow rate of the Syngas Feed and Toluene Solvent is obtained using the
following formula :
𝑚𝑠𝑦𝑛𝑔𝑎𝑠 = (𝑛ℎ𝑦𝑑𝑟𝑜𝑔𝑒𝑛 x 𝑀ℎ𝑦𝑑𝑟𝑜𝑔𝑒𝑛 ) + (𝑛𝐶𝑎𝑟𝑏𝑜𝑛 𝑀𝑜𝑛𝑜𝑥𝑖𝑑𝑒 x 𝑀𝐶𝑎𝑟𝑏𝑜𝑛 𝑀𝑜𝑛𝑜𝑥𝑖𝑑𝑒 ) +

(𝑛𝑚𝑒𝑡ℎ𝑎𝑛𝑒 x 𝑀𝑚𝑒𝑡ℎ𝑎𝑛𝑒 )
3. The amount of Gas component absorbed is obtained by Multiplying the Inlet Mass
Flow Rate of each respective gas component with the Absorption Percentage
4. The Total Mass Flow Rate at the bottom of the Column is obtained by summing all
the mass flow rate of the Absorbed Gas as well as the Toluene Solvent Used
71
5. The mass fraction of each component is done by dividing the Mass flow Rate of
each component with the Total Mass Flow Rate
6. The Amount of Gas unabsorbed at the Top of the column is obtained by getting
the Difference between the inlet mass flow rates of the gas with the mass flow rate
of the absorbed Gas. The Total Mass Flow rates at the top is then obtained by
summing them all up
7. The mass fraction is then obtained by dividing the Amount of Gas unabsorbed
with the total Mass flow rate at the top of the column.
Mass Balance Summary
Table 4.1.1.1.1: Mass balance summary of Absorber (V-101)

Syngas Composition Syngas Inlet Toluene Inlet Top Column Bottom
𝑘𝑔 𝑘𝑔 𝑘𝑔 Column
Stream( ℎ𝑟 ) Streamℎ𝑟 ) Outlet ℎ𝑟 )
𝑘𝑔
Outlet ℎ𝑟 )
Hydrogen 2377.8 - 2353.8 23.8
Carbon Monoxide 17875.2 - 358.4 17516.8
Methane 3729.6 - 3692.8 36.8
Toluene Solvent - 47580.6 - 47580.6
Total 23982.6 47580.6 6405 65158
Comparison with Aspen Simulation Value
Table 4.1.1.1.2 Results comparison between Aspen and Hand calculated values
Percentage
Stream Aspen Results Hand Calculated
Equipment Description Difference
No. (kmol/hr) Results (kmol/hr)
No (%)
1-07 Top 6493.5 6405 1.36
V-101
1-13 Bottoms 66916.3 65158 2.63
4.1.1.2 Adsorber Column (V-102/V-103)
Hydrogen Gas
V-102 V-103
CO Lean
GAs
Purge Stream
Figure 4.1.1.2.1: Sketch of Adsorber Column
72
V-102 and V-103 adsorber column is used to separate Hydrogen from the rest of the CO
Lean Gas coming out from the top of the V-101 absorber column. The two column
operates at the same condition and are made of the same specs which equal adsorbing
efficiency. When V-102 is on usage V-103 is not and vice versa, the detailed description
on how the process works is explained in Chapter 3. Therefore the mass balance on the
𝑘𝑚𝑜𝑙
two column is equal. The Feed Inlet Molar Flow Rate to the column is 1420.512( )
ℎ𝑟
Assumptions Made for the Calculation:
1. Assume Dynamic Steady State System

2. V-102 and V-103 are made of the same specs which equal adsorbing efficiency
3. Adsorption is based on Pressure Difference
4. 100% of Methane is adsorbed, 99% of Carbon Monoxide is Adsorbed and 10% of
Hydrogen is adsorbed.
5. Hydrogen molar composition in the Product Stream = 99%
6. Carbon Monoxide molar Composition in Product Stream = 1%
1. The molar flow rate of Hydrogen recovered in the Product Stream is obtained by
multiplying Inlet Molar Flow Rate of hydrogen with un-adsorbed Hydrogen
percentage
2. The total molar flow rate of the product steam is the obtained by dividing the
molar flow rate of Hydrogen recovered with its molar fraction in the product
stream.
3. Carbon monoxide recovered in the product stream is then calculated by getting the
difference between the total molar flow rates of the stream with the molar flow rate
of the hydrogen.
4. The amount of each respective gas component being adsorbed is calculated by
multiplying the Inlet molar flow rate of each respective gas with the adsorption
percentage
5. The mass flow rate of each gas is then obtained by multiplying each respective gas
molar flow rate with their respective molecular weight.
73
6. The total mass flow rate is then obtained by summing all the gas mass flow rate
and its mass fraction is calculated by dividing each gas component mass flow rate
with the total mass flow rate.
Table 4.1.1.2.1: Mass balance summary of Adsorber (V-102/V-103)

Stream Composition 𝑘𝑔 Top Column Outlet Bottom Column
Inlet Stream (ℎ𝑟 )
𝑘𝑔 𝑘𝑔
(ℎ𝑟 ) Outlet (ℎ𝑟 )
Hydrogen 2353.8 2118.6 235.4
Carbon Monoxide 358.4 299.6 58.8
Methane 3692.8 - 3692.8
Total 6405 2418.2 3987
Comparison with aspen simulation value
Percentage
No (%)
V-102/V- 1-12 Top Product 2169.9 2418.2 10.27
2013 1-13 Purge 4295.1 3987 7.2
4.1.2 Major Equipment in DMO synthesis

4.1.2.1 DMO Reactor (R-201)
Figure 4.1.2.1.1: Sketch of DMO reactor (R-201)
Basis of Calculation
2𝐶𝐻3 𝑂𝑁𝑂 + 2𝐶𝑂 → (𝐶𝐻3 𝑂𝐶𝑂)2 + 2𝑁𝑂 − − − − − − − − (𝑀𝑎𝑖𝑛 𝑅𝑒𝑎𝑐𝑡𝑖𝑜𝑛), 𝜖1

2𝐶𝐻3 𝑂𝑁𝑂 + 𝐶𝑂 → (𝐶𝐻3 𝑂)2 𝐶𝑂 + 2𝑁𝑂 − − − − − − − −(𝑆𝑖𝑑𝑒 𝑅𝑒𝑎𝑐𝑡𝑖𝑜𝑛), 𝜖2
74
Based on the production capacity of 128,000t/year of Monoethylene Glycol, the

dimethyl oxalate is calculated to be 220.34 kmol/hr.
Based on the literature review, the conversion of Methyl Nitrite is obtained to be 90%.
And the selectivity of Dimethyl Oxalate (DMO) is found to be 95% at 140 °C and
pressure of 1-5 barg. Further increase in pressure will cause a decrease in selectivity of
Dimethyl Oxalate as higher operating pressure will favor the undesired reaction which
will produce more dimethyl carbonate.
Assumptions for Mass Balance for R-201:
1. Mass balance is done on coupling reaction at steady state.

2. The reactor operates isothermal condition of 140°C and 3 barg.
3. Conversion of Methyl Nitrite is obtained to be 90% and Selectivity of Dimethyl
Oxalate is 90% over dimethyl carbonate.
4. The basis of calculation taken is based on the molar flowrate of product required to
produce 100,000 tonnes of MEG which is 220.34 kmol/hr of Dimethyl Oxalate.
1. Determining Extend of Reaction. The mass balance can be determined by

obtaining the extend of reaction, 𝜀1 𝑎𝑛𝑑 𝜀2 . Hence the final molar flowrate of the
reactant can then be determined. The formula for conversion and selectivity are
shown as below:
∈1 + ∈2
𝐶𝑜𝑛𝑣𝑒𝑟𝑠𝑖𝑜𝑛 𝑜𝑓 𝑀𝑒𝑡ℎ𝑦𝑙 𝑁𝑖𝑡𝑟𝑖𝑡𝑒 =
𝐼𝑛𝑙𝑒𝑡 𝑀𝑜𝑙𝑎𝑟 𝐹𝑙𝑜𝑤𝑟𝑎𝑡𝑒 𝑜𝑓 𝑀𝑒𝑡ℎ𝑦𝑙 𝑁𝑖𝑡𝑟𝑖𝑡𝑒
𝑀𝑜𝑙𝑒𝑠 𝑜𝑓 𝐷𝑒𝑠𝑖𝑟𝑒𝑑 𝑃𝑟𝑜𝑑𝑢𝑐𝑡 𝐹𝑜𝑟𝑚𝑒𝑑

𝑆𝑒𝑙𝑒𝑐𝑡𝑖𝑣𝑖𝑡𝑦 𝑜𝑓 𝐷𝑀𝑂 =
𝑀𝑜𝑙𝑒𝑠 𝑜𝑓 𝑈𝑛𝑑𝑒𝑠𝑖𝑟𝑒𝑑 𝑃𝑟𝑜𝑑𝑢𝑐𝑡 𝐹𝑜𝑟𝑚𝑒𝑑
2. Determining Molar Flowrate of Product. Molar flowrate of reactant can be

calculated by applying mass balance equation:
𝑀𝑎𝑠𝑠 𝑂𝑢𝑡 = 𝑀𝑎𝑠𝑠 𝐼𝑛 + 𝐺𝑒𝑛𝑒𝑟𝑎𝑡𝑖𝑜𝑛 − 𝐴𝑐𝑐𝑢𝑚𝑢𝑎𝑡𝑖𝑜𝑛
Mass Balance Result across Reactor R-201
75
Table 4.1.2.1.1: Mass balance summary of R-201

Inlet Outlet
Molecular
Components Mol Mass Mol Mass
Weight
(kmol/hr) (kg/hr) (kmol/hr) (kg/hr)
𝐶𝐻3 𝑂𝑁𝑂 61.04 492.77 30078.5900 46.9550 2866.13
𝐶𝑂 28.01 492.77 13802.4500 49.2770 1380.25
𝑇𝑜𝑙𝑢𝑒𝑛𝑒 92.14 2.23 205.34 2.2286 205.34
𝑁𝑂 30.01 85.39 2562.7000 531.2070 15941.53
𝑁2 28.0134 739.15 20706.180 739.1530 20706.18
(𝐶𝐻3 𝑂𝐶𝑂)2 118.09 - - 220.5850 26048.87
(𝐶𝐻3 𝑂)2 𝐶𝑂 90.08 - - 2.3220 209.16
Total 1812.31 67355.26 1591.73 67355.46
Comparison with aspen simulation value
Aspen Percentage
Stream Hand Calculated
Equipment Description Results Difference
No. Results (kmol/hr)
No (kmol/hr) (%)
Reactor
2-04 2884.4 1812.31 37.2
R-201 Inlet
Reactour
R-201 2-05 2661.4 1591.73 40.2
Outlet
4.1.3 Major Equipment in Methyl Nitrite Synthesis

4.1.3.1 Methyl Nitrite Synthesis Reactor (R-401, R-402, R-403)
In methyl nitrite (MN) synthesis process, a series of reactions are involved in the
formation of methyl nitrite which is one of the main reactants for DMO synthesis
process. These reactions were carried out in three different reactors (R-401, R-402, R-
403). The main reactants involved in this process were nitrogen monoxide (NO),
nitrogen dioxide (NO2), methanol (CH3OH) and oxygen (O2) while the by-products
formed during the reaction were water (H2O) and nitric acid (HNO3).The overall
reactions involved in each reactors in MN synthesis are shown below:
R – 401 : 2NO + O2  2NO2
R – 402, R – 403 : 2CH3OH(l) +NO(g) + NO2(g)  2CH3ONO(g) + H2O(l) (2.A)

76
CH3OH + 2NO2  CH3ONO + HNO3 (2.B)
Basis of Calculation
The mass balance of these 3 reactors were done based on the overall yield of the
reaction and feed into the reactor R-401 where the desired production rate of methyl
nitrite of 445.814kmol/hr is used as the basis. The molar flow rate of NO supplied from
DMO synthesis was found to be 531.207kmol/hr while an additional input of 23.639
kmol/hr of NO was needed to achieve the desired production rate. This additional input
of NO was found based on a series of calculations and iteration done using Microsoft
Excel spreadsheet.
The major assumptions used in calculation of mass balance across these 3 reactors
are shown below:
1. Steady state condition at constant temperature and pressure

2. The overall yield of methyl nitrite is 86.5%
3. The 100% conversion of O2 to NO2 is achieved in R-401with excess feed of NO
(NO:O2 = 6:1)
4. All the NO2 produced from reaction between O2 and NO will be consumed by
excess feed of methanol (CH3OH:O2 =12:1)
5. All the methyl nitrite, NO and CO leave from top of reactors (R-402/R-403) while
methanol, water and nitric acid leave from bottom of reactors (R-402/R-403)
R-401
1. The amount of oxygen fed into R-401 was found using following formula:
𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑂2 = 𝑓𝑒𝑒𝑑 𝑟𝑎𝑡𝑖𝑜 (𝑁𝑂: 𝑂2 ) × 𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑁𝑂 𝑓𝑒𝑑
2. The amount of NO2 produced from R-401 was found using following equation:
𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑁𝑂2 𝑓𝑜𝑟𝑚𝑒𝑑
= 𝑠𝑡𝑜𝑖𝑐ℎ𝑖𝑜𝑚𝑒𝑡𝑟𝑖𝑐 𝑟𝑎𝑡𝑖𝑜 × 𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑂2 𝑓𝑒𝑑
3. The amount of NO used in R-401 was found using following equation:
𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑁𝑂 𝑢𝑠𝑒𝑑 = 𝑠𝑡𝑜𝑖𝑐ℎ𝑖𝑜𝑚𝑒𝑡𝑟𝑖𝑐 𝑟𝑎𝑡𝑖𝑜 × 𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑂2 𝑓𝑒𝑑
4. The amount of NO left the R-401 was found using following equation:
77
𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑁𝑂 𝑙𝑒𝑓𝑡 = 𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑁𝑂 𝑓𝑒𝑑 − 𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑁𝑂 𝑢𝑠𝑒𝑑
R-402 and R-403
1. The actual number of MN produced was found using following formula:

𝑎𝑐𝑡𝑢𝑎𝑙 𝑀𝑁 𝑝𝑟𝑜𝑑𝑢𝑐𝑒𝑑
𝑂𝑣𝑟𝑎𝑙𝑙 𝑦𝑖𝑒𝑙𝑑 = 𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑀𝑁 𝑝𝑟𝑜𝑑𝑢𝑐𝑒𝑑 =
𝑎𝑐𝑡𝑢𝑎𝑙 𝑀𝑁 𝑝𝑟𝑜𝑑𝑢𝑐𝑒𝑑
𝑡𝑜𝑡𝑎𝑙 𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑁𝑂2 𝑓𝑒𝑑×𝑠𝑡𝑜𝑖𝑐ℎ𝑖𝑜𝑚𝑒𝑡𝑟𝑖𝑐 𝑟𝑎𝑡𝑖𝑜
𝐴𝑐𝑡𝑢𝑎𝑙 𝑀𝑁 𝑝𝑟𝑜𝑑𝑢𝑐𝑒 = 𝑡𝑜𝑡𝑎𝑙 𝑁𝑂2 𝑓𝑒𝑑 × 𝑠𝑡𝑜𝑖𝑐ℎ𝑖𝑜𝑚𝑒𝑡𝑟𝑖𝑐 𝑟𝑎𝑡𝑖𝑜 ×

𝑜𝑣𝑒𝑟𝑎𝑙𝑙 𝑦𝑖𝑒𝑙𝑑
2. The amount of NO2 used in main and side reactions was found using the following
step:
i. Assume the amount of NO2 used in main reaction
ii. Find the amount of MN produced in main reaction
iii. Find the amount of NO2 used and MN produced in side reaction
iv. Calculate the total mole of MN produced from both main and side reaction
v. Compared the total mole of MN produced with desired mole of MN
produced in reactor and repeat step i-vi until the desired value was achieved
3. The amount of H2O formed in main reaction was found using the following
equation:
𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝐻2 𝑂 𝑓𝑜𝑟𝑚𝑒𝑑
= 𝑠𝑡𝑜𝑖𝑐ℎ𝑖𝑜𝑚𝑒𝑡𝑟𝑖𝑐 𝑟𝑎𝑡𝑖𝑜
× 𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑀𝑁 𝑝𝑟𝑜𝑑𝑢𝑐𝑒𝑑 𝑖𝑛 𝑚𝑎𝑖𝑛 𝑟𝑒𝑎𝑐𝑡𝑖𝑜𝑛
4. The amount of HNO3 formed in side reaction was found using following equation:
𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝐻𝑁𝑂3 𝑓𝑜𝑟𝑚𝑒𝑑
= 𝑠𝑡𝑜𝑖𝑐ℎ𝑖𝑜𝑚𝑒𝑡𝑟𝑖𝑐 𝑟𝑎𝑡𝑖𝑜
× 𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑀𝑁 𝑝𝑟𝑜𝑑𝑢𝑐𝑒𝑑 𝑖𝑛 𝑠𝑖𝑑𝑒 𝑟𝑒𝑎𝑐𝑡𝑖𝑜𝑛
5. The amount of methanol fed into reactor was found using the following formula:
𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙
= 𝑓𝑒𝑒𝑑 𝑟𝑎𝑡𝑖𝑜 (𝐶𝐻3 𝑂𝐻: 𝑂2 ) × 𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑂2 𝑓𝑒𝑑
78
6. The mass flow rate of each component leaving the reactor was found using
following formula:
𝑀𝑎𝑠𝑠 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 = 𝑀𝑜𝑙𝑎𝑟 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 × 𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡
The result of mass balance of each reactor was shown below:
Table 4.1.3.1.1: Final mass balance result of R-401
Inlet (stream 4-05) Outlet (stream 4-07)
MW Molar flow Molar flow Mass flow
Component Mass flow
(kg/kmol) rate rate rate
rate (kg/hr)
(kmol/hr) (kmol/hr) (kg/hr)
NO 30 554.847 16645.41 369.898 11096.937
CO 28 49.277 1379.752 49.277 1379.752
MN 61 46.955 2864.249 46.955 2864.249
N2 28 739.153 20696.277 739.153 20696.277
O2 32 92.474 2959.183 0.000 0.000
NO2 46 0.000 0.000 184.949 8507.652
TOTAL - 1482.706 44544.87 1390.231 44544.87
Table 4.1.3.1.2: Final mass balance result of R-402 and R-403

R-402 R-403
[1] [2] [3]
Inlet Outlet Inlet Outlet[4]
Mola
Molar Mass Molar Mass Molar Mass r Mass
flow, flow, flow, flow, flow, flow, flow, flow,
kmol/h kg/h kmol/h kg/h kmol/h kg/h kmol/ kg/h
h
6547.1 2575.2
NO 369.90 11096.94 218.24 6547.19 218.24 85.84
9 4
1379.7 1379.7
CO 49.28 1379.75 49.28 1379.75 49.28 49.28
5 5
125.8 7676.9
MN 46.96 2864.25 366.92 22381.91 0.00 0.00
5 5
20696. 739.1 20696.
N2 739.15 20696.28 739.15 20696.28 739.15
28 5 28
1163.9
O2 0.00 0.00 0.00 0.00 36.37 0.00 0.00
5
NO2 184.95 8507.65 0.00 0.00 0.00 0.00 0.00 0.00
79
1109.6 13967. 310.6 9940.0

CH3OH 35510.20 789.73 25271.42 436.48
9 35 3 9
HNO3 0.00 0.00 16.65 1048.66 0.00 0.00 6.55 412.46
1073.7
H2O 0.00 0.00 151.66 2729.85 0.00 0.00 59.65
4
2499.9 1479.5 43754. 1376. 43754.
TOTAL 80055.07 2331.62 80055.07
3 2 51 95 51
Remarks:
[1] CH3OH for R-402 inlet is from stream 4-23 while others come from stream 4-07
[2] NO, CO, N2 and methyl nitrite flow through stream 4-08 while CH3OH, HNO3 and
water flow through stream 4-09
[3] CH3OH for R-403 inlet is from stream 4-26 while others come from stream 4-17
[4] NO, CO, N2 and methyl nitrite flow through stream 4-18 while CH3OH, HNO3 and
water flow through stream 4-19
Table 4.1.3.1.3 Outlet results comparison between Aspen and hand calculated values
Stream Hand Percentage
Equipment Aspen Results
No Description Calculated Difference
No. (kg/hr)
Results (kg/hr) (%)
R-401 4-07 - 68655.30 44544.87 35.12
4-08 Top 74631.40 51005.13 31.66
R-402
4-09 Bottom 33936.40 29049.93 14.40
4-18 Top 66114.50 32328.22 51.10
R-403
4-19 Bottom 13238.00 11426.29 13.69
4.1.4 Major Equipment in Hydrogenation

4.1.4.1 Hydrogenation Reactor (R-601)
Hydrogenation reactor (R-601) involves the hydrogenation of dimethyl oxalate (DMO)

to produce ethylene glycol (MEG) and Methanol as the main products. Ethanol and
Water are also formed as by-products. To achieve optimum yield and conversion, R-601
operates at a temperature and pressure of 210 oC and 25 bar(a) in order to. As
hydrogenation is a highly exothermic reaction, the type of reactor involved is a multi-
tubular reactor, where the process fluid goes through the tube side, whereas the coolant
media (Dowtherm oil) goes through the shell side of the reactor at an inlet temperature
of 40 oC and outlet temperature of 170 oC and pressure of 3 bar (a). The pressure drop
80
for each side of the reactor is calculated in Chapter 6, where the P drop for tube and shell
side is 1.97 bar (a) and 0.2 bar(a) respectively.
Basis for calculation:

The inlet of process fluid is taken as the basis of calculation and the flowrate and
composition of the stream is taken from the mixing of process stream and recycle
stream. The detailed calculation is attached in Appendix A4.1.4.
Key assumptions made for mass balance calculation:
1. Steady state process in an equilibrium reaction

2. Conversion of DMO to MG is 100%
3. Selectivity of EG is 99%
4. Unreacted hydrogen is recycled back to the reactor
5. Cu/SiO2 catalyst with Nickel support is employed
Key calculation steps:

1. Chemical reaction
𝐷𝑀𝑂 + 2𝐻2 ↔ 𝑀𝐺 + 𝑀𝑒𝑂𝐻…𝜁1
𝑀𝐺 + 2𝐻2 ↔ 𝐸𝐺 + 𝑀𝑒𝑂𝐻…𝜁2
𝐸𝐺 + 𝐻2 → 𝐸𝑡𝑂𝐻 + 𝐻2 𝑂…𝜁3
The two main reactions that take place in R-601 are 𝜁1 and 𝜁2 whereas the side reaction
that takes place is 𝜁3 .
2. Conversion of DMO to MG
Mole of MG formed
Conversion =
Mole of DMO reacted
3. Selectivity of EG
Amount of MG consumed in reaction
Selectivity =
Amount of MG fed in reaction
4. Extent of reaction and stoichiometric ratio
The extents of reaction 𝜁1 and 𝜁2 are calculated based on the aforementioned conversion
and selectivity whereas 𝜁3 is calculated based on stoichiometric ratio of the reaction.
81
5. Mass balance table for R-601

Table 4.1.4.1.1: Mass balance table for R-601
Component Inlet Mass Flow Rate (kg/hr) Outlet Mass Flow Rate
(kg/hr)
DMO 26022.82 0.00
H2 21044.24 19290.15
MG 0.00 198.50
MeOH 78068.45 92118.79
EG 0.00 13541.23
EtOH 0.00 101.52
H2O 0.00 39.69
Toluene 6.16 6.16
DMC 0.08 0.08
CO 15138.72 15138.72
Total 140280.47 140280.47
6. Comparison between Aspen and Hand Calculation Result

Table 4.1.4.1.2: Comparison between Aspen and Hand Calculation Result
Stream No. Equipment Aspen Results Calculated Results Percentage
(kmol/hr) (kmol/hr) Difference (%)
6-04 R-601 14967.1 13285.51 11.23
4.1.5 Other Major Equipment In The Plant

4.1.5.1 Gas-Liquid Separator
Recycled Gas
CO Rich Solvent S-101
CO Solvent
Figure 4.1.5.1.1: Sketch of Flash Drum (S-101)
Using S-101 as an example, it is a flash drum separator thar is used to separate the Gas
and Liquid Phase coming from V-101 column to ensure that no CO lean Gas is left
going into D-101 column. The total molar flow rate going into S-101 flash drum is
𝑘𝑚𝑜𝑙
933.19( ℎ𝑟
)
82
Assumptions made for the calculation:
1. Steady State condition during operation

2. The operating pressure of the separator operates within the P dew < Pbubble range
Key Calculation Step:
1. The first step taken in the calculation is to find the Equilibrium constant for all the
components. This is done using the Wilson’s Relation which is shown below:
𝑃𝑐𝑖 𝑇𝑐𝑖
𝐾𝑖 = X exp(5.37 x (1+ 𝑤𝑖 ) X (1- )
𝑃 𝑇
𝑉
2. Once all the Ki equilibrium constant is obtained the 𝐹 (Vapour outlet to Feed) ratio.
This is done using Rachford-Rice Flash equation which is shown below:

𝑍𝑖 𝑋(𝐾𝑖 − 1)
∑ =0
𝑉
1 + 𝐹 𝑋(𝐾𝑖 − 1)
𝑉
3. Microsoft Excel solver function is used to obtain the value.
𝐹
𝑉
4. Once the 𝐹 ratio is obtained the outlet liquid molar fraction for each component is
the obtained using the following formula:

𝑍𝑖
𝑥𝑖 =
𝑉
1 + 𝐹 𝑋 (𝐾𝑖 − 1)
5. The outlet vapour molar fraction of each component is then obtained using the K i
equilibrium constant and the xi liquid molar fraction using the following formula:
𝑦𝑖 = 𝑥𝑖 × 𝐾
𝑉
6. The total outlet Vapour flow rate is obtained multiplying the 𝐹 ratio with the total
Inlet molar flow.

7. The total outlet liquid flow rate is obtained by getting the difference between the
Inlet molar flow rate and the total outlet Vapour flow Rate
8. The molar flow of each component is then obtained by multiplying the molar
fraction with the total molar flow rate and the mass flow rate is then obtained by
multiplying it with each component Molecular weight.
Table 4.1.5.1.1: Mass balance summary of S-101
83
Stream Composition Stream Inlet Top Column 𝑘𝑔

Bottom Column Outlet(ℎ𝑟 )
𝑘𝑔 𝑘𝑔
Stream( ) Outlet ( )
ℎ𝑟 ℎ𝑟
Hydrogen 23.77 22.97 0.80
Carbon Monoxide 17517.01 860.79 16656.21
Methane 37.30 35.47 1.83
Toluene Solvent 34617 132.15 26857.64
Total 52195.42 1051.39 43516.48
9. Comparison between Aspen and Hand calculation result:

Table 4.1.5.1.2: Comparison of Result between Aspen and Hand calculation result
Aspen Result Calculated Result Percentage
Equipment No Stream No
(kmol/hr) (kmol/hr) difference (%)
1-14 14.20 45.882 69.05
S-101
1-17 919.00 887.312 3.45
2-07 2391.90 615.30 74.28
S-201
2-10 269.50 225.21 16.43
4-14 1961.40 1006.70 48.67
S-401
4-12 271.80 366.92 25.92
6-07 11510.70 10185.55 11.51
S-601
7-01 3031.89 3099.96 2.20
7-07 8.76 11.26 22.17
S-701
7-08 2804.46 2803.57 0.03
4.1.5.2 Multicomponent Distillation Columns
Figure 4.1.6.1 Multicomponent Distillation Column D-701

For the mass balance of multicomponent distillation columns, the short cut method is
used. Distillation Column D-701 will be used as the sample calculations as shown
below.
1. Determining Light Key and Heavy Key Components in stream
84
For the inlet stream going into D-701, Methanol is determined to be the Light Key
component and Ethylene Glycol is chosen as the Heavy Key component.
Table 4.1.5.2.1: Feed Stream composition of D-701
Feed stream
Mass flow rate Mass Molar flow Mole
Component
(kg/hr) fraction rate (kmol/hr) fraction
Carbon Monoxide 1.60 1.54E-05 0.06 1.88E-05
Hydrogen 16.70 1.62E-04 8.30 2.74E-03
Methyl Glycolate 3.30 3.22E-05 0.04 1.22E-05
Methanol 89873.20 0.87 2805.03 0.93
Ethylene Glycol 13554.50 0.13 218.38 0.07
Total 103449.37 1 3031.80 1
2. Key assumptions to be made for first iteration of D-701:

i. Purity of 99.5%is assumed.
ii. 100% separation of Hydrogen to the distillate.
iii. 99% separation of Methanol to the distillate.
iv. 0.5% separation of Ethylene Glycol to the distillate.
v. Steady State operation.
vi. Inlet into distillation column is saturated liquid, q=1.
3. Dew Point and Bubble Point calculation

The Antoine equation is used to help obtain the partial pressures of different
components in the distillate and bottoms streams. To obtain the Dew point temperature,
𝑦
the summation of all 𝐾𝑖 values should be equals to 1 and this temperature will be used as
𝑖
the operating temperature on the top of the distillation column. The top operating
temperature of the column D-701 is found to be 105.18 °C, which only have a 1.23%
difference from the simulation value using AspenPlus. The Bubble point temperature
will be obtained when the temperature used results in a summation of all xiKi values
equals to 1. This temperature will also be used as the bottom operating temperature of
the column and it is found to be 290.42 °C for D-701. The percentage difference of this
value from the simulated value is found to be 1.09% which shows the validity of the
assumptions and calculations.
4. Recalculate final values of remaining components in product streams

85
The minimum number of stages for the column is first calculated and used to find the
final values of components in the distillate and bottoms stream. The results obtained for
D-701 is tabulated below,
Table 4.1.5.2.2 Final calculated results of components in Distillate and Bottoms of D-701
Composition in Distillate Composition in Bottoms
Component
(kmol/hr) (kmol/hr)
Carbon Monoxide 0.06 0.0009
Hydrogen 8.30 0.0037
Methyl Glycolate 6.91E-05 0.0369
Methanol 2805.03 0.0016
Ethylene Glycol 1.45 216.9251
5. Determining the minimum reflux ratio and actual number of stages
The minimum reflux ratio is found by using the Underwood equations (Sinnott, 2014)
and the actual number of stages can be found by using the Erbar-Maddox Correlation.
The detailed steps of the calculations can be found in Appendix A4.1.6.
Comparing obtained results with simulated results from AspenPlus
Mass balance results obtained from AspenPlus were compared with the hand calculated
values and the percentage difference is found to be very small.
Percentage
No (%)
1-26 Distillate 607.00 600.56 1.06
D-101
1-23 Bottoms 280.31 286.75 2.25
3-04 Distillate 51.05 4.70 90.79
D-301
3-08 Bottoms 218.49 220.43 0.88
5-05 Distillate 1191.42 1169.70 1.82
D-501
5-16 Bottoms 337.36 165.16 51.04
5-08 Distillate 1146.82 1108.94 3.30
D-502
5-12 Bottoms 44.59 60.76 26.61
7-04 Distillate 2813.22 2814.83 0.06
D-701
7-09 Bottoms 218.66 216.97 0.77
7-15 Distillate 2.47 1.09 56.08
D-702
7-19 Bottoms 216.19 215.88 0.14
86
7-23 Distillate 2.18 1.08 50.58

D-703
7-27 Bottoms 214.01 214.80 0.37
4.1.6 Mass balance for Minor Equipment

4.1.6.1 Steam Ejector
Figure 4.1.6.1.1: System boundary for steam ejector.
To produce a vacuum condition of 0.8bar for the distillation column (D-703), a steam
ejector was used. For steam ejector, the mass flow rate of steam into the system is
usually only known by the vendors themselves. However, the amount of steam needed
for this steam ejector can be estimated and is shown in Appendix A4.1.7.The amount
needed was determined to be 340.19 kg/hr.
4.1.6.2 Pump, Compressor, Heat exchanger, Reboiler and Condenser
Basis of calculation:
Mass balance across these equipment is defined by:
Accumulation = Input + Generation – Output – Consumption
Assumptions made for mass balance:
1. Steady state (Accumulation = 0)

2. No generation or consumption of process fluid in these equipment
The mass balance is therefore reduced to:
Input of process fluid = Output of process fluid
87
4.2 ENERGY BALANCE

4.2.1 DMO Synthesis
4.2.1.1 DMO Reactor R-201
Coupling reaction to produce dimethyl oxalate is an exothermic reaction. Multi-tubular

reaction is chosen as the design for reactor for R-201, this is done to remove excess heat
generated from the reaction and to maintain the reactor at a constant temperature of
140°C in order for the conversion and selectivity of Dimethyl Oxalate to remain the
same.
The energy balance for reactor R-201 was done based on the stoichiometric ratio of
reaction and mass balance of reactors. Based on the mass balance calculations, 492.77
kmol/hr of Carbon Dioxide will react with 492.77 kmol/hr of Methyl Nitrite in order to
produce 220.585 kmol/hr of Dimethyl Oxalate, 2.322 kmol/hr of Dimethyl Carbonate
and 445.81 kmol/hr of Nitrogen Oxide.
Assumptions:
1. No heat loss to the surrounding as the reactor is insulated by mineral wools.

2. No work interaction.
Key Calculation Steps
1. The constant of heat formation of all the components are obtained from Perry’s
Handbook.
2. The heat of formation for each component is calculated using the constants
obtained at the desired temperature.
3. The net formation of heat is calculated using equation,
𝑄𝑛𝑒𝑡 = ∑ 𝑛∆𝐻𝑓,𝑝𝑟𝑜𝑑𝑢𝑐𝑡𝑠 − ∑ 𝑛∆𝐻𝑓,𝑟𝑒𝑎𝑐𝑡𝑎𝑛𝑡𝑠
4. The enthalpy change of reactants and products from 25°C to 140°C was found
using following formula:
25℃ 𝑇 25℃ 25℃
𝑛𝑖 ∫ 𝐶𝑝𝑖 𝑑𝑇 + 𝑛𝑖 ∫ 𝐶𝑝𝑖 𝑑𝑇 = 𝑛𝑖 ∫ 𝐶𝑝𝑖 𝑑𝑇 − 𝑛𝑖 ∫ 𝐶𝑝𝑖 𝑑𝑇 = 0
𝑇 25℃ 𝑇 𝑇
Detail calculation is shown in Appendix A4.2.1. Result of the energy balance

calculation is shown in table 4.2.1.1.1
88
Table 4.2.1.1.1: Energy Balance Result Table

𝑛1 ∆𝐻1 𝑘𝐽
−2.5966 × 105
ℎ𝑟
𝑛𝑖 ∆𝐻𝑟𝑥𝑛,𝑇𝑟𝑒𝑓 𝑘𝐽
−6.01 𝑥 107
ℎ𝑟
𝑛2 ∆𝐻2 𝑘𝐽
−1.538 𝑥 106
ℎ𝑟
R-201 Duty, Q -𝟏𝟕𝟏𝟗𝟑. 𝟖 𝒌𝑾
4.2.2 Methyl Nitrite Synthesis

4.2.2.1 Methyl Nitrite Synthesis Reactor (R-401, R-402, R-403)
Basis of calculation
The energy balances of reactors (R-401, R-402 and R-403) were done based on the
stoichiometric ratio of reaction and mass balance of reactors. Based on the
stoichiometric ratio, oxygen gas is the limiting reactant in R-401. 92.474kmol/hr of O2
will react with 184.949kmol/hr of NO to produce 184.949kmol/hr of NO 2. For R-402
and R-403, NO2 is the limiting reactants. In R-402, 184.949kmol/hr of NO2 will react
with 151.658kmol/hr of NO and 319.962kmol/hr of methanol to produce
319.962kmol/hr of methyl nitrite. In R-403, 72.747kmol/hr of NO2 will react with
59.653kmol/hr of NO and 125.852kmol/hr of methanol to produce 125.852kmol/hr of
methyl nitrite. T
Assumptions made in calculation are shown below:
1. No heat loss to surrounding

2. The reaction temperature of R-401 is 100℃ while reaction temperature of R-402
and R-403 are 60℃
3. The standard temperature of heat of formation is 25℃
Key calculation step
1. The heat of reaction at standard temperature was calculated from heat of

formation:
∆𝐻𝑟𝑥𝑛,25℃ = ∑ 𝑣𝑖 ∆𝐻𝑓 (𝑃𝑟𝑜𝑑𝑢𝑐𝑡) − ∑ 𝑣𝑖 ∆𝐻𝑓 (𝑅𝑒𝑎𝑐𝑡𝑎𝑛𝑡 )
89
2. The duty of the reactor at 25℃ was found using following formula:
𝐷𝑢𝑡𝑦 𝑎𝑡 25℃ = 𝑛𝑜 𝑜𝑓 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑟𝑒𝑎𝑐𝑡𝑎𝑛𝑡𝑠/𝑝𝑟𝑜𝑑𝑢𝑐𝑡𝑠 × ∆𝐻𝑟𝑥𝑛,25℃
3. The duty of the reactor at optimum temperature of reactor, T℃ was found using
following formula:
𝐷𝑢𝑡𝑦 𝑎𝑡 𝑇℃ = 𝑒𝑛𝑡ℎ𝑎𝑙𝑝𝑦 𝑐ℎ𝑎𝑛𝑔𝑒 𝑜𝑓 𝑟𝑒𝑎𝑐𝑡𝑎𝑛𝑡𝑠 𝑓𝑟𝑜𝑚 𝑇℃ 𝑡𝑜 25℃ + 𝐷𝑢𝑡𝑦 𝑎𝑡 25℃

+ 𝑒𝑛𝑡ℎ𝑎𝑙𝑝𝑦 𝑐ℎ𝑎𝑛𝑔𝑒 𝑜𝑓 𝑝𝑟𝑜𝑑𝑢𝑐𝑡𝑠 𝑓𝑟𝑜𝑚 25℃ 𝑡𝑜 𝑇℃
4. The enthalpy change of reactants from T℃ to 25℃ was found using following
formula:
25℃
𝑒𝑛𝑡ℎ𝑎𝑙𝑝𝑦 𝑐ℎ𝑎𝑛𝑔𝑒 𝑜𝑓 𝑟𝑒𝑎𝑐𝑡𝑎𝑛𝑡𝑠 𝑓𝑟𝑜𝑚 𝑇℃ 𝑡𝑜 25℃ = ∑ 𝑛𝑖 ∫ 𝐶𝑝𝑖 𝑑𝑇
𝑇
5. The enthalpy change of products from 25℃ to T℃ was found using following
formula:
𝑇
𝑒𝑛𝑡ℎ𝑎𝑙𝑝𝑦 𝑐ℎ𝑎𝑛𝑔𝑒 𝑜𝑓 𝑝𝑟𝑜𝑑𝑢𝑐𝑡𝑠 𝑓𝑟𝑜𝑚 25℃ 𝑡𝑜 𝑇℃ = ∑ 𝑛𝑖 ∫ 𝐶𝑝𝑖 𝑑𝑇
25℃
6. The enthalpy change of unreacted component can be negligible since it will be

cancelled out based on the formula of duty above.
25℃ 𝑇 25℃ 25℃
𝑛𝑖 ∫ 𝐶𝑝𝑖 𝑑𝑇 + 𝑛𝑖 ∫ 𝐶𝑝𝑖 𝑑𝑇 = 𝑛𝑖 ∫ 𝐶𝑝𝑖 𝑑𝑇 − 𝑛𝑖 ∫ 𝐶𝑝𝑖 𝑑𝑇 = 0
𝑇 25℃ 𝑇 𝑇
Based on the calculation above, the duty of the reactors is found and shown in table
below. The detailed calculation can be found in Appendix A4.2.2.
Table 4.2.2.1.1: Result for R-401, R-402 and R-403

Unit R-401 R-402 R-403
∆𝐻𝑟𝑥𝑛1 ,𝑇𝑟𝑒𝑓 : -64.879 ∆𝐻𝑟𝑥𝑛1 ,𝑇𝑟𝑒𝑓 : -64.879
∆𝐻𝑟𝑥𝑛 ,𝑇𝑟𝑒𝑓 kJ/mol -114.140
∆𝐻𝑟𝑥𝑛2 ,𝑇𝑟𝑒𝑓 : -67.298 ∆𝐻𝑟𝑥𝑛2 ,𝑇𝑟𝑒𝑓 : -67.298
Main reaction 1: Main reaction 1:
-9.839E+06 -3.870E+06
Duty at Tref kJ/hr -1.055E+07
Side reaction 2: Side reaction 2:
-1.120E+06 -4.406E+05
Duty at T kW -2966.834 -3080.393 -1205.162
Aspen
kW -10482.30 -10768.30 -1848.22
Result
Percentage % 71.70 71.39 34.79
90
difference
4.2.3 Hydrogenation
4.2.3.1 Hydrogenation Reactor (R-601)
Key assumptions made for energy balance calculation:
1. R-601 operates at isothermal condition

2. Specific heat capacity, Cp and heat of formation, Href values are taken from Perry’s
Chemical Handbook (2008)
3. Negligible potential and kinetic energy
Key Calculation steps:

1. Calculating specific heat capacity generated by the reaction
The Cp value for each component is calculated from the formula:
The values of C1, C2, C3, C4 and C5 are taken from Perry’s Chemical Handbook
(2008). The total Cp value for each reaction is calculated by the formula shown below:
2. Calculating heat of reaction at T = 25 oC

The Href value for each component is taken from Perry’s Chemical Handbook (2008).
The total Href value for each reaction is calculated by the formula shown below:
𝑎𝐴 + 𝑏𝐵 → 𝑐𝐶 + 𝑑𝐷
𝑑 𝑐 𝑏
𝐻𝑟𝑟𝑒𝑓 = 𝐶𝑝𝑑 + 𝐶𝑝𝑐 − 𝐶𝑝𝑏 − 𝐶𝑝𝑎
𝑎 𝑎 𝑎
3. Calculating energy of each component entering and leaving R-601

Energy = ṅ × Cp × T
4. Calculating duty of R-601

Q = Reactor duty,
91
Q = Energy entering system − Energy leaving system

+ Rate of heat of reaction + Rate of work done on system
5. Calculating mass flowrate of coolant (Dowtherm oil) required

Q = ṁ × CP × ∆T
6. Comparing calculated duty and duty extracted from Aspen simulation

Table 4.2.3.1.1: Comparison of duties and percentage error
Calculated duty (kW) 8626.13
Duty from Aspen simulation (kW) 7064.39
From the table above, the percentage error of calculated duty and duty from Aspen
simulation is found to be 18.10 %. As the percentage error is below 30%, therefore it is
within the acceptable range.
From the calculated duty, the mass flowrate of coolant required is calculated to be
147820.17 kg/h
4.2.4 Condenser
Figure 4.2.4.1: System boundary of condenser E-502
System boundary for condenser is shown in Figure 4.2.4.1. Few assumptions were made
to perform energy balance over a condenser.
1. Steady state
2. Negligible sensible heat in condenser
Duty of condenser is calculated based on the mass flowrates of inlet of condenser. The
key steps are shown below.
92
1. The flowrates of each component in the inlet of condenser are determined using
the formula:
𝑚̇𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡.𝑖𝑛𝑙𝑒𝑡 = 𝐷𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 (1 + 𝑅)
2. The amount of heat released during condensation for one component is
calculated using the formula:
𝑄𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 = 𝑚̇𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡.𝑖𝑛𝑙𝑒𝑡 × 𝑙𝑎𝑡𝑒𝑛𝑡 ℎ𝑒𝑎𝑡𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡
3. The duty of the condenser is then calculated by adding up the amount of heat
released by all the components in the inlet stream.
𝐷𝑢𝑡𝑦 𝑜𝑓 𝑐𝑜𝑛𝑑𝑒𝑛𝑠𝑒𝑟, 𝑄 = ∑ 𝑄𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡
4. The amount of cooling utility required is calculated using the formula:
𝑄
𝑚̇𝑐𝑜𝑜𝑙𝑖𝑛𝑔 𝑢𝑡𝑖𝑙𝑖𝑡𝑦 = 𝐶
𝑝.𝑐𝑜𝑜𝑙𝑖𝑛𝑔 𝑢𝑡𝑖𝑙𝑖𝑡𝑦 ×(𝑇𝑜𝑢𝑡𝑙𝑒𝑡 −𝑇𝑖𝑛𝑙𝑒𝑡 )
Duties of each condenser and the utilities required are summarized in Table 4.2.4.1.
Refer to Appendix A4.2.4 for detailed calculations.
Table 4.2.4.1: Energy balance of condenser
Percentage difference
Condenser Duty calculated (kW) Duty from Aspen (kW)
(%)
E-107 304.87 297.50 2.42
E-301 1025.32 144.11 85.94
E-303 54.31 601.67 90.97
E-502 14382.79 5140.01 64.26
E-505 18018.98 32865.04 45.17
E-508 14640.26 13024.75 11.03
E-701 27567.56 1086.78 96.06
E-703 401.31 494.95 18.92
E-706 1389.53 1593.84 12.82
4.2.5 Reboiler
Basis of calculation:
For reboilers, a few assumptions were made before carrying out the energy balance. The
assumptions are:
i. Steady state
ii. Sensible heat is negligible for reboilers
iii. The duty for reboiler will be determined based on the mass flow rate of boil
up stream.
93
Figure 4.2.5.1 System boundary of reboiler (E-702).

The duty for E-702 was calculated to be 22152.09 kW and the utility mass flow rate
was 153.67 kg/s. The calculations for the duty and mass flow rate will be shown in
Appendix A4.2.5
The duty and utility flow rate for each reboiler in the whole plant was calculated by
using the same steps as shown in Appendix A4.2.5 and the values were then tabulated
below.
Table 4.2.5.1: Energy balance results of Reboiler

Reboiler Duty calculated (kW) Duty from Aspen (kW) Percentage difference (%)
E-108 116.40 107.94 7.27
E-302 962.65 2968.05 67.57
E-503 20572.39 18493.69 10.10
E-506 36610.50 32311.79 11.74
E-702 22152.09 28728.60 22.89
E-705 185.93 373.18 50.18
E-709 695.39 887.73 21.67
4.2.6 Heat Exchanger

For a heat exchanger that handle fluids that does not undergo phase change in the
process, the steps below are used to calculate their respective duties.
1. Obtain Cp value for inlet mixture stream

The Cp value for each component of the inlet stream should be obtained and the average
Cp value is calculated through multiplying them by their respective molar ratios. A
sample calculation for this step can be seen in Appendix A4.2.6.
2. Calculating Duty of heat exchanger
94
The duty of the heat exchanger can be calculated by just using a simple equation as
shown below.
𝐷𝑢𝑡𝑦 𝑜𝑓 𝐻𝑒𝑎𝑡 𝐸𝑥𝑐ℎ𝑎𝑛𝑔𝑒𝑟 = 𝑚̇𝐶𝑝 ∆𝑇 = 𝑚̇𝐶𝑝 (𝑇𝑜𝑢𝑡 − 𝑇𝑖𝑛 )
Where,
𝑚̇ = Mass flow rate of inlet stream (kg/s); 𝐶𝑝 = Specific heat capacity of the mixture;
∆𝑇 = Required temperature difference of inlet and outlet stream
Table 4.2.6.1: Energy balance result of heat exchanger

Equipment No Type of Duty Duty from Percentage
Duty Calculated Aspen (kW) Difference (%)
(kW)
E-101 Heating 135.49 50.73 62.56
E-102 Cooling 1664.60 1527.50 8.24
E-103 Cooling 2422.21 2070.52 14.52
E-104 Cooling 2173.85 1222.13 43.78
E-105 Cooling 10.54 8.87 15.84
E-106 Heating 2863.42 2557.66 10.68
E-109 Cooling 459.25 202.34 55.94
E-201 Cooling 828.96 419.85 49.35
E-202 Cooling 3174.21 4588.44 44.55
E-203 Heating 2926.36 2352.26 19.62
E-401 Cooling 1642.18 2134.37 23.06
E-402 Cooling 1087.69 1795.21 39.42
E-403 Heating 874.22 918.29 4.80
E-404 Heating 617.16 1470.01 58.02
E-405 Heating 492.06 2031.91 75.78
E-406 Heating 343.86 397.03 13.39
E-501 Heating 2176.51 1717.28 21.10
E-504 Cooling 337.63 626.86 46.14
E-507 Cooling 163.87 108.73 33.65
E-601 Heating 20889.90 20118.18 3.69
E-602 Cooling 57216.25 45466.40 20.54
E-704 Cooling 6.36 16.14 60.59
E-708 Cooling 6.11 13.61 55.11
E-710 Cooling 1384.53 1544.14 10.34
4.2.7 Pump
1. Using the initial velocity, the diameter and the area of the pipe is calculated.
2. The actual velocity is then obtained
95
3. Reynolds number is then calculated and by using the moody chart the friction
factor can be tabulated.
4. Bernoulli’s equation is then used to calculate the shaft work, −𝑊𝑠 . The equation
is shown below:
−Ws ∆P ∆u2 Pf,total
= + + ∆z +
g ρg 2g ρg
5. Pump model selection is then done based on the volumetric flow rate of the
pump as well as it total head.
6. The efficiency of the pump is then tabulated based on the type of pump and the
real duty of the Pump can then be calculated.
Figure 4.2.7.1: Pump Result Table

Equipment
Duty calculated (kW) Duty from Aspen (kW) Percentage difference (%)
No
P-101 5.65 1.10 80.53
P-102 4.15 3.75 9.54
P-301 4.08 1.03 74.75
P-401 4.13 1.09 73.61
P-402 5.41 1.99 63.22
P-403 2.57 1.58 38.52
P-501 5.30 5.01 5.47
P-601 112.82 190.92 40.91
P-701 0.15 0.11 29.95
P-702 1.69 0.17 89.80
4.2.8 Compressor
Key Calculation Steps
The energy balance in the compressor is assumed to be operating at a steady state

therefore it is concluded that there are no accumulation and loss in the system.
1. Shultz method is used to obtain the work of the compressor and it is obtained using
the following formula:
𝑛−1
𝑛 𝑃
W= P1V1 (𝑛−1) [𝑃2 𝑛 − 1]
1
2. n constant is obtained using the following expression:

1
n = 1−m
3. m constant is obtained using the following expression:

96
γ−1
m= γ X 𝐸
𝑝
Where 𝐸𝑝 = Efficiency of the compressor (Sinnot figure 3.6)
4. γ constant is obtained using the following expression :

𝐶𝑝
γ= 𝐶
𝑝 −𝑅
𝑘𝑗
Where: Cp is the molar heat capacity(𝑘𝑚𝑜𝑙.𝑘 )
𝑘𝑗
R is the is the universal gas constant = 8.314 𝐾.𝑘𝑚𝑜𝑙
5. The molar heat capacity is obtained using the following formula:

𝐶𝑝ℎ𝑦𝑑𝑟𝑜𝑔𝑒𝑛
= a + bT + CT2 + DT3
𝑅
Where: a, b, c, d = gas constant

6. Using all the expressions mentioned above, all the necessary value obtained to
calculate the Work done has been obtained.
7. The duty is then calculated by multiplying the Work Done with the Mass Flow
Rate going into the compressor and dividing it with the efficiency
Table 4.2.8.1: Energy Balance Result of Compressor
Equipment
Duty calculated (kW) Duty from Aspen (kW) Percentage difference (%)
No
C-101 276.85 1662.99 83.35
C-102 3692.54 3171.46 14.11
C-103 36.39 8.87 75.63
C-201 1383.67 849.82 38.58
C-202 2176.89 3406.34 36.10
C-401 39.81 149.81 73.43
C-402 235.87 148.33 37.12
C-601 690.02 973.78 29.14
C-602 2507.94 1704.02 32.06
97
98
Chapter 5:
Specification of
equipment items
5.1 Introduction
All equipment items are required to have specification sheets as it is a very important
document to transmit the information on the detailed design for the fabrication of the
equipment. It is important to have cross-checking for every design of equipment to
ensure that the information transmitted to the fabricators are accurate and reliable. This
is also to minimize the mistakes that could be present in the design specification sheets
and reduce the confusion between fabricators and designers.
This chapter covers the specification sheets of 28 selected equipment in the

monoethylene glycol production plant. The table below shows the matrix for the
designer and their respective checkers for this Chapter of the project. It is noted that the
specification sheets for detailed design in Chapter 6 are checked by the designer
themselves.
99
Table 5.1.1: Designer and checker for all equipment selected

Checker
KM DZ SP AH YC AL HY
Designer
Koon Meng (KM) D-101 E-107 E-108 S-101
Dzaki (DZ) V-101 E-103 E-302 V-102
Shi Phay (SP) D-501 E-503 E-504 D-301
Ai Hsin (AH) R-601 E-602 S-601 V-103
Yoong Chin (YC) D-702 R-201 E-201 S-201
Alex (AL) E-709 S-701 D-703 E-706
Hao Yang (HY) E-402 S-401 D-701 R-402
Specification sheets of selected equipment are attached after a short write up on the
description of equipment. Calculations can be found in Appendix A5.
5.1 Specification sheets (by Chong Koon Meng)

5.1.1 Description of equipment
The design of the Gas-Liquid Separator S-101 is carried out by sizing the diameter of
the vessel based on the calculated vapor residence time first. The assumption made is
that the vapor residence time is equal to the actual residence time in the vessel. The
liquid holdup time is determined to be 3 minutes and the volume needed for the liquid is
calculated. The height of the vessel is also calculated based on several estimations of
column height based on its diameter (Sinnott, 2014). As for thickness of the vessel, the
calculated thickness required for the head is higher which is 7.3 mm including corrosion
allowance, and is used as the thickness of the whole vessel. Dry Pressure Drop across
the Demister Pad in the separator is calculated to be 1.49 mbar which is acceptable.
100
For overhead condenser E-107, the overall Coefficient is first estimated and has a value
of 840 W/ m2.°C. The condenser’s heat transfer area required is calculated based on the
log mean temperature difference obtained. The layout for the condenser is initially
estimated and confirmed to be viable through checking the shell side and tube side
velocity and the percentage difference between calculated and estimated Overall
Coefficient values. The percentage difference between the two values is found to be
29.6% which indicates that the initial estimates are acceptable. Lastly, the tube side and
shell side pressure drop are checked to ensure that it falls within the acceptable range.
The design of kettle reboiler E-108 starts off with estimating the Overall Coefficient, U
to calculate the heat transfer area required. The numbers of tubes required are also
calculated based on the area. The overall coefficient is then checked with the estimated
value by calculation of the heat flux and boiling coefficient and has percentage
difference of less than 30%. The maximum allowable heat flux is also much higher than
the actual heat flux calculated. Lastly, the layout of the reboiler is determined and the
vapor velocity is checked to ensure the design is viable.
5.1.2 Specification Sheet for gas-liquid separator S-101

ASME Section
Toluene 2-phase Design
Item Description Service VIII Division 1,
Separator separator Code
2010 Edition
Equipment Label S-101 Orientation Vertical
DESIGN DATA NOZZLE DATA
Operating Size
1 bar Service
Pressure ID (mm) OD (mm)
Operating
40⁰ C Inlet 80 88.9
Temperature
Design Pressure 4.5 bar Gas Outlet - -
Design
70⁰ C Liquid Outlet 80 88.9
Temperature
Hold-up Time 3 minutes Drain 80 88.9
Carbon Steel SKETCH
Material
CS-A
Max Allowable 78.57 bar
101
Stress
Density of Steel 7700 kg/m3
Inner Diameter 1.04 m
Height of Cylinder 6.46 m
Height of Heads
1.00 m
(Top & Bottom)
Total Height 7.46 m
Vessel Thickness 7.3 mm
FLUID PROPERTIES NOTES:

Liquid: 867.0 kg/m3
Density
Vapour: 0.084 kg/m3
Flow Rate 18.59 kg/s COMPANY NAME DATE
Volumetric
10.247 m3/s G6 Engineering Sdn Bhd 30 SEPTEMBER 2017
flowrate
DEMISTER PAD Drawn by: KM SHEET
Type Knitted Wire Mesh Checked by: AH
Material SS GR. 304 TITLE
Thickness 0.1 m 1 OF 1
Data Specification Sheet for MEG
Density 150 kg/m3 Separator (S-601)
5.1.3 Specification Sheet for overhead condenser E-107

Toluene Toluene
Item Description Service Design Code TEMA 1999
Condenser Condenser
Equipment Label E-602 Type Shell and Tube Orientation: Horizontal
PERFORMANCE OF ONE UNIT

Shell Side Tube Side
Fluid Allocation Carbon Monoxide, Toluene DowTherm 4000 30% Ethylene
-
Vapor Glycol
Flowrate kg/s 8.62 1.61
Fluid Properties IN OUT IN OUT
Temperature ⁰C 111 100 40 90
Density kg/m3 1.657 2.005 1044.22 1013.29
Viscosity Pa.s 0.007 0.007 1.22 × 10-5 1.22 × 10-5
Specific Heats kJ/kgK 1.448 3.831
102
Pressure bar(a) 1 1
Velocity m/s 0.257 0.438
Pressure Drop bar 0.58 0.29
Fouling Resistance m2K/W 0.0002 0.0002
Film Transfer Coefficient W/m2K 313.97 326.46
Heat Duty kW 297.50
Overall Heat Transfer
W/m2K 840
Coefficient
Required Heat Transfer Area m2 10.25
DESIGN DATA
Material for Shell and Carbon Max Allowable Pressure:
NOTES:
Tube Steel CS-A 78.57 MPa
TUBES
Design Pressure 4.5 bar Pitch Triangular
No. of Tube per Pass 2 Pitch Distance 20 mm
Length 4.88 m Bundle Diameter 177 mm
Thickness 1.2 mm Total Tubes 50
Size for Tube Pipe
16 mm
(Schedule 40)
SHELL
Design Pressure 4.5 bar Diameter 226 mm
No. of Shell per Pass 1
Baffle Spacing 1808 mm
Thickness 9 mm
Shell-bundle Clearance 49 mm Baffle Cut 25%
Size for Shell Pipe
17 mm
(Schedule 40)
SKETCH COMPANY NAME DATE: 1/10/2017
Drawn by: KM
Checked by: DZ
SHEET 1 OF 1
5.1.4 Specification Sheet for kettle reboiler E-108

Kettle
Item Description Service Toluene Reboiler Design Code TEMA 1999
Reboiler
Equipment Label E-108 Type Kettle Reboiler Orientation Horizontal
SHELL SIDE TUBE SIDE
Fluid Allocation
Toluene Liquid Saturated Steam
Temperature ⁰C 80.0 110.6 184.1 184.1
Density kg/m3 867.0 3.2 5.147 1000
Pressure bar 1 10
Mean Temperature
Difference
⁰C 73.52
2
Heat Flux kW/m 36.76
103
Heat Duty kW 107.94

W/m2K 500
Coefficient
Required Heat Transfer
m2 2.936
Area
DESIGN DATA
Carbon
Material for Shell and
Steel CS- Max Allowable Pressure 78.57 MPa
Tube A
TUBE SIDE
Design Pressure 4.5 bar
Pitch Triangular
No. of Tube per Pass 2
Length 4.88 m Bundle Diameter 92.5 mm
Thickness 1.2 mm
Size for Tube Pipe Total Tubes 12
16 mm
(Schedule 40)
SHELL SIDE
Design Pressure 4.5 bar Diameter 185 mm
No. of Shell per Pass 1 Liquid level from
140 mm
Thickness 9 mm base
Vapor Velocity 0.177 m/s
Maximum allowable vapor Surface area of liquid 0.387 m2
3.286 m/s
velocity
SKETCH OF E-108 COMPANY NAME DATE
G6 Engineering Sdn Bhd 1 October 2017
Drawn by: KM SHEET

Checked By: SP
TITLE
1 OF 1
Data Specification Sheet for Kettle Reboiler
(E-108) for Distillation Column
5.2 Specification sheets (by Muhamad Dzaki Fadhlurrohman)

E-103 is heat exchanging equipment which is used to cool down the CO Lean Gas
mixture that have been previously compressed in C-102. The Inlet temperature of the
Gas mixture is 292⁰ C and it is aimed to be cooled down to 130⁰ C. In the other hand
the cooling median used is Dowtherm G which has an inlet temperature of 40 ⁰ C and
an outlet temperature of 90⁰ C. In addition to that the operating pressure of the Gas
mixture is 11 bar whereas the operating pressure for the cooling media is 3 bar. The heat
exchanger is made of a 1one Shell and 2 passes and stainless steel is utilized as the
material for construction with the basis of ASME BPV Code 2010 as reference. The
duty of the Heat Exchanger is 2319.53 kW and its overall heat transfer coefficient was
104
𝑊
found to be 465.643 𝑚2 .𝐾. Furthermore, the length, thickness and inner diameter was
found to be 4m, 2mm and 16mm respectively. Detailed calculations can be seen in
Appendix A5.2.1 and its overall spec-sheet can be seen in section 5.2.2.
E-302 is a heating reboiler equipment which is used to heat up and maintain the outlet
temperature of the process fluid coming out of D-301 column. Saturated steam at 20
barg is used as the heating median for the process. The inlet and outlet temperature of
the process fluid is 184.8 ⁰ C, whereas there is temperature decrease from 214.987⁰ C
to 140.987⁰ C for the saturated stream. The duty of the reboiler was found to be
𝑊
2319.53 kW whereas the overall heat transfer coefficient was found to 2968.05 𝑚2.𝐾. It
also found that the tube sheet length and thickness of the tube side are 6m and 1.7mm
respectively. Detailed calculations can be seen in Sppendix A5.2.2 and its overall spec-
sheet can be seen in section 5.2.3.
V-102 is in adsorption column involve in is the PSA process. Its duty is to extract
Hydrogen from the CO Lean Gas mixture coming from V-101. Hydrogen need to be
separated from other composition of the mixtures which are CO and Methane. The
operating temperature and Pressure of the column are 30 oC and 11 bar(a) respectively.
In the other hand the construction specification of the column has been calculated and is
found to be 4.56m and 20.05 m respectively. The purity of the hydrogen at the outlet of
the column is 99% whereas its recovery is 98%. Detailed calculations can be seen in
Appendix A5.2.3 and its overall spec-sheet can be seen in section 5.2.4.
5.2.2 Specification sheet for heat exchanger E-103

Lean CO Heat
Cooler Exchanger
Type: AFT
Equipment Label E-103 Type Shell and Tube
Orientation: Horizontal
Fluid Allocation - CO lean gas Dowtherm G
Density kg/m3 2.82 2.82 1056 1056
Viscosity Pa.s 0.000147 0.000147 0.000325 0.000325
Thermal Conductivity W/m.K 0.147 0.2568
Pressure bar(a) 11 3
105

Heat Duty kW 2319.53
W/m2K 456.643
Coefficient
DESIGN DATA
Material for Shell and Stainless
Max Allowable Pressure: 10 bar NOTES:
Tube Steel
TUBES
Design Pressure 2.2 bar(a) Pitch Triangular
Pass 2 Bundle Diameter 366.4 mm
Length 4m Diameter 20 mm O/D
Thickness 2 mm Total Tubes 162
SHELL
Design Pressure 2.2 bar (a) Diameter 20 mm O/D
Baffle Spacing 91.1 mm
Thickness 2 mm

Drawn by: DZ
Checked by: SP
SHEET 1 OF 1
5.2.3 Specification sheet for reboiler E-302

Reboiler
Item Description Service Reboiler Design Code TEMA 1999
for D-301
Equipment Label E-302 Type Kettle Reboiler Orientation: Horizontal

Fluid Allocation - DMO process fluid Saturated steam
Temperature ⁰C 184.8 184.8 214.987 214.987
Density kg/m3 788.649 788.649 10.047 10.047
Viscosity Pa.s 0.00028 0.00028 0.0000317 0.0000317
Pressure bar(a) 2 20
Velocity m/s - 31.720
106

W/m2K 2968.05
Coefficient
DESIGN DATA
Stainless
Material for Shell and Tube Max Allowable Pressure: 50 bar NOTES:
Steel
TUBES
Design Pressure 20 bar(a) Pitch Triangular
Pass 2 Bundle Diameter 526.253mm
SHELL
Design Pressure 2 bar(a) Diameter 19 mm O/D
Baffle Spacing -
Thickness 1.7 mm
Shell-bundle Clearance 54 mm Baffle Cut -

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Checked by: AH
SHEET 1 OF 1
5.2.4 Specification sheet for adsorption column V-102

Location Outdoor
Item
PSA Adsorption Column
Description
Orientation Vertical
Equipment
V-102
Label
Vessel Design ASME Section VIII Division I, 2010
Type of Column Packed Column
Code Edition
As per Material
Specifications Pipe Sizing, Schedule 40
Requisition
Joint Efficiency 1.0
Size
MATERIAL SPECIFICATIONS Flange
Mark Service
Heads ASME: SA-516 GR. 70 Rating
ID (m) OD (m)
Shell ASME: SA-516 GR. 70
Skirt SA-516 GR. 70
Process
Stainless Steel 304 N1 1500 0.30 0.32
Packing Inlet
Grade A
107
Type of Packing Activated Carbon

Process
Packing Support N2 1500 0.25 0.27
Gas Injection Outlet
Type
Liquid SKETCH:
Distributor Orifice
Type
Maximum Allowable Stress
1380 bar
DESIGN DATA
Design Pressure 1210 bar(a) Operating Pressure 1100 bar(a)
Design Temperature 50⁰ C Operating Temperature 30⁰ C
DIAMETER THICKNESS TANGENT
Shell 4.56 m I/D 0.21 m - -
Heads 4.56m I/D 0.21 m Heads type Torispherical
Packing 4.56 m I/D 18.23 m (height) - -
Cylinder
20.05 m Head Height (each) 0.91 m
Height
NOTES: COMPANY NAME DATE
G6 Engineering Sdn Bhd 28 SEPTEMBER 2017
Drawn by: DZ SHEET

Checked by: YC
TITLE
1 OF 1
Data Specification Sheet for PSA
Adsorption Column (V-102)
5.3 Specification sheets (by Chew Shi Phay)

The first equipment is a kettle reboiler E-503 that controls the temperature for the
distillation column D-501 and to boil-up most of methanol back into D-501. It utilizes
10 barg saturated steam as a heating medium for the process fluid which contains
mostly water, methanol, dimethyl oxalate and nitric acid. The saturated steam has a
temperature of 184.1°C whereas the temperature of the process fluid is at 122.1°C and a
pressure of 4.8 atm(a). The duty of the reboiler was extracted from Aspen as 18493.69
kW. An initial value of overall heat transfer coefficient was used to initiate the
calculations, and after a few iterations the final coefficient is determined to be 145.8
108
W/m2K. A specification sheet on the design of the reboiler is shown in Section 5.3.2.
Detailed calculations can be found in Appendix A5.3.1.
The second equipment is a heat exchanger E-504 used to decrease the temperature of
the process fluid from 122.1°C to 50°C. In this heat exchanger, Dowtherm 4000 is used
as a coolant and it has an inlet temperature of 40°C and outlet temperature of 80°C. The
operating pressure of the process fluid at the shell side is at 4.8 atm(a) whereas the
operating pressure of the coolant at tube side is at 1.5 barg. The duty of the cooler E-504
is found to be 626.86 kW as extracted from Aspen and the overall heat transfer
coefficient is determined to be 669.35 W/m2K. A specification sheet on the design of
the heat exchanger is shown in Section 5.3.3. Detailed calculations can be found in
Appendix A5.3.2.
The third equipment is a dimethyl oxalate purification column D-301 to remove

impurities such as dimethyl carbonate and toluene present in the process stream. The
tray distillation column operates at a pressure of 1.8 atm and a temperature ranging from
97.5°C to 184.8°C. From Aspen simulation, the number of stages for the distillation is
found to be 23 stages with a reflux ratio of 0.2. A specification sheet on the design of
the heat exchanger is shown in Section 5.3.4. Detailed calculations on the column can
be found in Appendix A5.3.3.
5.3.2 Specification sheet for reboiler E-501

Reboiler
Item Description Service Reboiler Design Code TEMA 1999
for D-501
Type: AKU
Equipment Label E-503 Type Kettle Reboiler
Fluid Allocation - Methanol process fluid Saturated steam
Temperature ⁰C 122.1 122.1 184.1 184.1
Density kg/m3 8.594 8.594 5.683 5.638
Viscosity Pa.s 0.0002 0.0002 0.00015 0.00015
Pressure bar(a) 4.86 11.0
109
Latent Heat kJ/kg 1882.25 1999.28

W/m2K 145.8
Coefficient
DESIGN DATA
Stainless
Steel 304
TUBES
Design Pressure 12.1 bar(a) Pitch Square
Pass 2 Bundle Diameter 1900 mm
Length 2.44 m Diameter 40 mm O/D
Size for Tube Pipe
500 mm
(Schedule 40)
SHELL
Design Pressure 5.35 bar(a) Diameter 3800 mm O/D
Baffle Spacing -
Thickness 10 mm
Shell-bundle Clearance 20 mm Baffle Cut -
Size for Shell Pipe
600 mm
(Schedule 40)
Drawn by: SP
Checked by: AH

SHEET 1 OF 1

Item Bottom products
Service Cooler Design Code TEMA 1999
Description cooler to lower T
Equipment Shell and tube Type: AFM
E-503 Type
Label heat exchanger Orientation: Horizontal
Fluid Allocation - Bottom product from D-501 Dowtherm 4000
Temperature ⁰C 122.1 50 40 80
Density kg/m3 601.559 1056
Viscosity Pa.s 0.000541 0.000325
Pressure bar(a) 4.86 1.6
110

Heat Duty kW 626.86
W/m2K 669.35
Coefficient
DESIGN DATA
Stainless
Steel 304
TUBES
Design Pressure 2.75 bar(a) Pitch Triangle
Thickness 2 mm Total Tubes 176
Size for Tube Pipe
50 mm
(Schedule 40)
SHELL
Design Pressure 5.35 bar(a) Diameter 422.3 mm O/D
Thickness 10 mm
Shell-bundle Clearance 10.2 mm Baffle Cut 25%
Size for Shell Pipe
50 mm
(Schedule 40)
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SHEET 1 OF 1
111
5.3.4 Specification sheet for distillation column D-301
112
5.4 Specification sheets (by Chew Ai Hsin)

The item for the first specification sheet is E-602, a heat exchanger that cools the
process stream. The process consists of mainly unreacted hydrogen, methanol and
monoethylene glycol (MEG) whereas the coolant used is Dowtherm G. E-602 has an
operating temperature ranging from 110 oC to 210 oC whereas the coolant stream ranges
from 40°C to 170°C. The operating pressure of E-602 for process stream is 23 bar(a)
whereas that for coolant stream is 3 bar(a). The type of heat exchanger chosen is AFT
based on TEMA 1999, with two shells and four passes. The material used in
construction of both shell and tube is stainless steel based on ASME BPV Code 2010.
Based on the design code, the diameter and length of E-602 is calculated to be 2.593 m
and 6.83 m respectively whereas the wall thickness of the shell is 17 mm. The detailed
specification of E-602 can be found in the specification in the following pages.
The item for the second specification sheet is S-601, an adiabatic flash separator that
separates unreacted hydrogen and methanol from MEG. The cooled process from E-602
enters S-601 and is separated to vapor stream which contains mostly hydrogen and
methanol as well as liquid stream which contains mostly MEG and methanol. The
operating temperature and pressure of the flash separator is 110 oC and 23 bar(a)
respectively. The material used in construction of the wall of the vessel is stainless steel
to avoid hydrogen embrittlement. Based on ASME BPV Code 2010, the diameter and
length of S-601 is calculated to be 1.51 m and 7.57 m respectively whereas the wall
thickness of the vessel is 10 mm. The detailed specification of S-601 can be found in the
specification in the following pages.
The item for the third specification sheet is V-103, an adsorption column in PSA. The
column removes CO and methane from hydrogen, producing hydrogen with a purity of
99%. The operating temperature and pressure of the column is 30 oC and 11 bar(a)
respectively. The material used in construction of the vessel is stainless steel 304 Grade
A to avoid hydrogen embrittlement. Based on Sinnott & Towler (2009), the diameter
and length of vessel is calculated to be 4.56 m and 20.05 m respectively whereas the
wall thickness is 21 mm including corrosion allowance. The detailed specification of V-
103 can be found in the specification in the following pages.
113

MEG Heat
Cooler Exchanger
Type: AFT
Fluid Allocation - Dowtherm G Hydrogenation Process
Density kg/m3 1031.40 1031.40 0.9 0.9
-5
Viscosity Pa.s 0.007 0.007 1.22 × 10 1.22 × 10-5
Pressure bar(a) 3.0 23
Heat Duty kW 18750
W/m2K 300
Coefficient
DESIGN DATA
Tube Steel
TUBES
Size for Tube Pipe
42 in. Flange Rating 2500
(Schedule 40)
SHELL
Thickness 17 mm
Size for Shell Pipe
(Schedule 40)
Drawn by: AH
Checked by: YC
SHEET 1 OF 1
114
5.4.3 Specification sheet for gas-liquid separator S-601

ASME Section
MEG 2-phase Design
2010 Edition
Operating Size Flange
23 bar Service
Pressure ID (in.) OD (in.) Rating
Operating
110⁰ C Inlet 30.624 32 2500
Temperature
Design Pressure 25.3 bar Gas Outlet 30.624 32 2500
Design
130⁰ C Liquid Outlet 22.624 24 2500
Temperature
Hold-up Time 2 minutes Drain 2.067 2 150
Stainless SKETCH
Material
Steel
Max Allowable
2080 bar
Stress
Height of Heads
0.754 m
(Top & Bottom)
Total Height 7.573 m
Vessel Thickness 10 mm

Liquid: 1110 kg/m3
Density
Vapour: 0.9 kg/m3
H2: 0.215
Mass
MEG: 0.201 G6 Engineering Sdn Bhd 28 SEPTEMBER 2017
Fraction
Methanol: 0.584
DEMISTER PAD
Knitted Wire
Type
Mesh
Material SS GR. 304 Drawn by: AH SHEET
Thickness 0.1 m Checked by: AL
TITLE
1 OF 1
Density 150 kg/m3 Data Specification Sheet for MEG
Separator (S-601)
115
5.4.4 Specification sheet for adsorption column V-103

Location Outdoor
Item
PSA Adsorption Column
Description
Orientation Vertical
Equipment
V-103
Label
Vessel Design ASME Section VIII Division I, 2010
Type of Column Packed Column
Code Edition
As per Material
Specifications Pipe Sizing, Schedule 40
Requisition
Joint Efficiency 1.0
Size
MATERIAL SPECIFICATIONS Flange
Mark Service
Heads ASME: SA-516 GR. 70 Rating
ID (m) OD (m)
Shell ASME: SA-516 GR. 70
Skirt SA-516 GR. 70
Process
Stainless Steel 304 N1 1500 0.30 0.32
Packing Inlet
Grade A
Type of Packing Activated Carbon
Process
Packing Support N2 1500 0.25 0.27
Gas Injection Outlet
Type
Liquid SKETCH:
Distributor Orifice
Type
Maximum Allowable Stress
1380 bar
DESIGN DATA
Design Pressure 1210 bar(a) Operating Pressure 1100 bar(a)
Design Temperature 50⁰ C Operating Temperature 30⁰ C
DIAMETER THICKNESS TANGENT
Shell 4.56 m I/D 0.21 m - -
Heads 4.56m I/D 0.21 m Heads type Torispherical
Packing 4.56 m I/D 18.23 m (height) - -
Cylinder
20.05 m Head Height (each) 0.91 m
Height
NOTES: COMPANY NAME DATE
28 SEPTEMBER
2017
Drawn by: AH SHEET

Checked by: HY
TITLE
1 OF 1
Data Specification Sheet for PSA Adsorption
Column (V-103)
116
5.5 Specification sheets (by Wong Yoong Chin)

E-201 is used to cool carbon monoxide stream from 226.40°C to 140°C by using
Dowtherm 4000 as cooling medium. The heat duty acquired from Aspen Plus
simulation is 419.85kW. Dowtherm 4000 enters the shell side at 40°C and 1.5 barg and
leave at 80°C and 1.4 barg. E-201 has one shell pass and 2 tube pass configurations.
Carbon Steel A285 Grade A is chosen to be the constructing material for this
equipment as there are no corrosive components present in the stream. Outer tube
diameter of 25mm is chosen with a triangular pitch of 31.30mm pitch distance.
Separator S-201 is used to separate the vapor and liquid line of the dimethyl oxalate
products coming out from the reactor. The operating pressure of the separator is 1barg
with an operating temperature of 20°C. Design pressure is calculated to be 2.97 barg
and design temperature of 50°C. The hold-up time of liquid is set to be 10 minutes.
Carbon Steel A285 Grade A is chosen to be the constructing material for this
equipment. The gas liquid separator is installed in a vertical orientation with a height
of 7.57m with a vessel thickness of 7mm. Demister pad is required to be fitted inside
the gas liquid separator with an area of 𝟑. 𝟗𝟑𝟓𝒎𝟐 .
Distillation Column D-702 is used to purify the final product which is monoethylene
glycol from impurities such as methanol, methyl nitrite, dimethyl oxalate and etc. The
design temperature of this column is 308°C and the design pressure is 7.37barg.
Carbon Steel A285 A285 Grade A is chosen to be the material of constructing the
column. The column has 8 number of stages with a reflux ratio of 11.41.
Torispherical head is chosen to be the cover head with a thickness of 4.53mm. The
height of torispherical head has a height of 0.253m. The total height of the column is
7.3m.
117

CO Heat
Cooler Exchanger
Type: AFT
Fluid Allocation - Dowtherm 4000 Carbon monoxide
3
Volumetric flowrate m /s 0.00273 1.726
Temperature ⁰C 40 80 226.4 140
Density kg/m3 1044.20 1044.20 2.635 2.635
Viscosity Pa.s 1.34 × 10-3 1.34 × 10-3 2.45 × 10-5 2.45 × 10-5
Pressure bar(g) 1.5 3.3
Film Transfer Coefficient W/m2K 1820 116
Heat Duty kW 419.85
W/m2K 91.6
Coefficient
DESIGN DATA
Material for Shell and Carbon steel Max Allowable Pressure:
NOTES:
Tube A285 Grade A 5.5 bar(g)
TUBES
Design Pressure 3.63 bar(g) Pitch Triangular
No. of Tube per Pass 125 Pitch Distance 31.3 mm
Length 5.0 m Diameter 21.8 mm I/D
Size for Tube Pipe
25 mm Reactant flowrate 1.726 m3/s
(Schedule 40)
SHELL
Design Pressure 1.65 bar(g) Cross Flow Area 0.0157 m2
Thickness 17 mm
Shell Diameter 627 mm Baffle Cut 25%
Drawn by: YC
Checked by: AL
SHEET 1 OF 1
118
5.5.3 Specification sheet for gas-liquid separator S-201

ASME Section
DMO 2-phase Design
2010 Edition
1 barg Service
Pressure ID (mm) OD (mm) Rating
Operating
20⁰ C Inlet 600 609.6 2500
Temperature
Design Pressure 2.97 barg Gas Outlet 850 863.6 2500
Design
50⁰ C Liquid Outlet 65 73 2500
Temperature
Hold-up Time 10 minutes SKETCH
Material Carbon Steel

Height of Heads
0.754 m
(Top & Bottom)

Liquid: 906.14 kg/m3
Density
Vapour: 1.203 kg/m3
DMO: 0.269
CO: 0.362
Mass
NO: 0.1534 G6 Engineering Sdn Bhd 28 SEPTEMBER 2017
Fraction
Others (N2, DMC):
0.2156
DEMISTER PAD
Knitted Wire
Type
Mesh
Material CS A285 Drawn by: YC SHEET
Area 3.935 m2 Checked by: HY
TITLE
1 OF 1
Diameter 2.24 m Data Specification Sheet for DMO
Separator (S-201)
119
5.5.4 Specification sheet for distillation column D-702

Item Location Outdoor
MEG Purification Column
description
Equipment Orientation Vertical
D-702
label
Vessel design ASME Section VIII Division 1,
Type of Column Conventional Distillation Column
code 2010 Edition
As per material Nozzle data, Based on ASME/ANSI B16.5-1996 Pipe Flanges and
Specifications
requisition Flanged Fittings, Schedule 40
Design Data and Specification
Stream Feed Distillate Flowrate Bottom Flowrate
Mass Flow Rate(kg/hr) 13565.56 146.27 13419.28
Mol Flow Rate (kmol/hr) 218.67 2.475 216.19
Column Specification Physical Properties of Fluid
Number of Stages 8 Physical Properties Above Feed Below Feed
Reflux Ratio 11.41 Vapor Density (𝒌𝒈/𝒎𝟑) 5.58 5.92
Feed Stage 5 Liquid Density (𝒌𝒈/𝒎𝟑 ) 744.85 742.91
Cylindrical Column Section Vapor Flowrate (kg/s) 0.447 0.615
Shell Material Carbon Steel Liquid Flowrate (kg/s) 4.175 0.574
A285
Shell Diameter 1.22m Surface Tension N/m 0.0281 0.0283
Shell Thickness 7 mm Nozzle Sizing
Liquid Vapor
Design Temperature 308°C Description Inlet
Outlet outlet
Design Pressure 7.37 barg Material CS-A285 CS-A285 CS-A285
Cover Head Section Nominal Size (mm) 20 50 15
Type of Head Torispherical Schedule 40 40 40
Thickness of Cover 4.53 mm OD (mm) 26.7 60.3 21.3
Total Head Height 0.253 m Thickness (mm) 1.69 5.44 1.27
Internal Section NOTES:
Plate Thickness 5mm
Hole diameter 5mm
Weir height 60mm
Weir Length 921 mm
Downcomer Area 0.14 𝑚2
Net Area 1.029 𝑚 2
Total Pressure Drop 12.39 mm liquid
Column Height 7.3 m
SKETCH COMPANY NAME: DATE
29 SEPTEMBER
2017
Drawn by: YC SHEET
Checked by: KM
TITLE
Data Specification Sheet for 1 OF 1

MEG Purification column
(D-702)
120
5.6 Specification sheets (by Alexander Lim Zhi Chin)

The first equipment is the condenser E-706 for distillation column D-703. The purpose
of this condenser is to condense the vapor leaving the column. There are two types of
condenser, a partial condenser and a total condenser. For this condenser, a total
condenser was chosen. Hence, the distillate product will all be in liquid phase. The
operating conditions for this condenser are, 175.91oC for temperature and 0.5bar for
pressure.
The second equipment is the reboiler E-709 for distillation column D-703. The purpose
of this reboiler is to heat up the liquid leaving the bottom of the column to ensure that
some of the liquid will vaporise and be fed back into the column. This vapor will then
help with the separation process within the column. The operating conditions for this
reboiler are, 189.33oC for temperature and 0.8bar for pressure.
Separator S-701 is a two-phase separator. A horizontal separator will be chosen as the

orientation. This is because a long liquid holdup time is required for this separator. The
purpose of this separator is to separate methanol from hydrogen gas so that methanol
can be recycled back into the system. The operating conditions for this separator are,
30oC for temperature and 2.6bar for pressure.
121
5.6.2 Specification sheet of condenser E-706

Condenser Heat
for D-703 Exchanger
Equipment Type: AFT
E-706 Type Shell and Tube
Label Orientation: Horizontal
Fluid Allocation - Process stream Dowtherm G
Temperature ⁰C 175.91 170.49 40 50
Density kg/m3 0.88 813.98 1031.4 1023.6
Viscosity Pa.s 9.79 × 10-6 5.31 × 10-4 0.0061 0.0046
Specific Heats kJ/kgK 2.87 2.97 1.616 1.651
-5
Thermal Conductivity W/m.K 2.18 × 10 0.2 0.124 0.123
Velocity m/s 14.1 3.17 3.01 3.02
W/m2K 401.72
Coefficient
m2 24.87
Area
DESIGN DATA
Material for Shell and Tube Stainless Steel 304 NOTES:
TUBES
Size for Tube Pipe
250 mm
(Schedule 40)
SHELL
Design Pressure 0.55 bar (a) Diameter 488.22 mm O/D
Thickness 4 mm
Size for Shell Pipe
450 mm, in 32mm, out
(Schedule 40)
Drawn by: AL
Checked by: HY
SHEET 1 OF 1
122
5.6.3 Specification sheet of overhead reboiler E-709

Reboiler for Heat
D-703 Exchanger
Equipment
E-709 Type Kettle reboiler Orientation: Horizontal
Label
Fluid Allocation - Process stream Saturated steam @ 20 barg
Fluid Properties IN OUT OUT IN OUT
Temperature ⁰C 189.33 189.33 189.33 214 140
Density kg/m3 798.56 10.05
Viscosity Pa.s 0.00047 3.17 × 10-5
Velocity m/s 3.18 12.94 3.18 8.29 8.29
2
Fouling Resistance m K/W 0.0004 0.0002
Heat Duty kW 888.08
W/m2K 143.02
Coefficient
m2 36
Area
DESIGN DATA
Material for Shell and Tube Stainless Steel 304 NOTES:
TUBES
Size for Tube Pipe
300 mm
(Schedule 40)
SHELL
Design Pressure 0.88 bar (a) Diameter 851.20 mm O/D
Thickness 3 mm
Size for Shell Pipe
32mm, in 400mm, out 32mm, out
(Schedule 40)
Drawn by: AL
Checked by: KM
SHEET 1 OF 1
123
5.6.4 Specification of gas-liquid separator S-701

ASME Section
Methanol 2-phase Design
2010 Edition
Equipment Label S-701 Orientation Horizontal
Operating Size
2.6 bar Service
Pressure ID (mm) OD (mm)
Operating
30⁰ C Inlet 860.78 900
Temperature
Design Pressure 2.86 bar Gas Outlet 43.14 50
Design
80⁰ C Liquid Outlet 125.7 150
Temperature
Hold-up Time 10.12 minutes
Stainless
Material
Steel 304 SKETCH
Max Allowable
2080 bar
Stress
Length of
6.75 m
Cylinder
Height of Heads
0.58 m
(Top & Bottom)
Total length 7.9 m

Density
Vapour: 0.49 kg/m3
Mass H2: 0.003
G6 Engineering Sdn Bhd 30 SEPTEMBER 2017
Fraction Methanol: 0.997
Drawn by: AL SHEET

Checked by: DZ
TITLE
1 OF 1
Data Specification Sheet for
Methanol Separator (S-701)
124
5.7 Specification sheets (by Tan Hao Yang)

Heat exchanger (E-402) is used to cool the gaseous product stream from top of reactor
(R-401) from 60°C to -12°C by using Dowtherm 4000 as the cooling medium. The
Dowtherm 4000 is supplied at -30°C and will leave the heat exchanger at -20°C. Since
the gaseous product stream that leave from R-401 contain some nitric acid which is
more corrosive than Dowtherm 4000, it enters from the shell side of heat exchanger.
The total heat transfer to the Dowtherm 4000 is calculated to be 1514.39 kW and thus
the total mass flow rate of Dowtherm 4000 was found to be 49.636 kg/s.
The gas-liquid separator (S-401) is used to separate the methyl nitrite from the other gas
mixture before entering the reactor (R-403) in order to increase the rate of reaction of
methyl nitrite synthesis in R-403. The operating temperature and pressure of S-401 is
set at -12°C and 10 bar respectively. Since there have some undesired nitric acid contain
in the feed stream of S-401, stainless steel type 304 was selected as the constructing
material of this separator. The height and the diameter of S-401 is calculated to be
4.579m and 1.829 m respectively. A minimum liquid hold-up time of 10 minutes was
used to calculate the liquid hold up height required for the S-401. The wall thickness of
the separator was calculated based on ASME BPV Code and the thickness of S-401 was
found to be 9.421 mm.
Distillation column D-701 is the first column for the purification of MEG process. It
was simulated through Aspen Plus, where this column consists of 20 stages with a
reflux ratio of 0.04. In this column, hydrogen and carbon monoxide will be fully
removed. A high percentage of methanol is also removed in this first column. After this
column, the bottom product will then be passed into the following column D-702 for
further purification by removing the remaining impurities. This column is operating at
5bar and a temperature of 258.79°C.
125
5.7.2 Specification sheet of heat exchanger E-402

MN Heat
Cooler Exchanger
Type: AEM
Fluid Allocation - Dowtherm G Gas mixture from R-402
Temperature ⁰C -30 -20 60 -12
Density kg/m3 1107.91 1107.91 4.193 4.193
Viscosity Pa.s 0.033 0.033 1.22 × 10-5 1.22 × 10-5
W/m2K 101.25
Coefficient
DESIGN DATA
Tube Steel
TUBES
Size for Tube Pipe
(Schedule 40)
SHELL
Thickness 17 mm
Size for Shell Pipe
(Schedule 40)
Drawn by: HY
Checked by: KM
SHEET 1 OF 1
126
5.7.3 Specification sheet of gas-liquid separator S-401

ASME Section
2-phase Design
Item Description MN Separator Service VIII Division 1,
separator Code
2010 Edition
10.13 bar Service
Pressure ID (in.) OD (in.) Rating
Operating
-12⁰ C Inlet 30.624 32 2500
Temperature
Design Pressure 11.15 bar Gas Outlet 15 16 2500
Design
-13⁰ C Liquid Outlet 2.067 2 2500
Temperature
Hold-up Time 10 minutes Drain 2.067 2 150
Stainless SKETCH
Material
Steel
Max Allowable
1380 bar
Stress
Height of Heads
0.932 m
(Top & Bottom)
Vessel Thickness 9.421 mm

Density
Vapour: 15.12 kg/m3
CO: 0.43
N2: 0.17
Mass
Methanol: 0.04 G6 Engineering Sdn Bhd 1 OCTOBER 2017
Fraction
MN: 0.28
NO: 0.09
DEMISTER PAD
Knitted Wire
Type
Mesh
Material SS GR. 304 Drawn by: HY SHEET
Thickness 0.1 m Checked by: DZ
TITLE
1 OF 1
Density 150 kg/m3 Data Specification Sheet for MN
Separator (S-401)
127
5.7.4 Specification sheet of MEG purification column D-701
SKETCH
128
Chapter 6:
Detailed Design
Items
129
6.1 Absorber Column V-101

Syngas separation is a key section in the dimethyl oxalate (DMO) route process as it
provides the plant with the required raw materials for the production process of
monoethylene glycol (MEG) which are carbon monoxide (CO) and hydrogen (H2). V-
101 column is one of the main equipment in the absorption and purification process of
CO.
V-101 column is a counter-current absorber which functions at an elevated temperature

(40°CO) and a pressure above the atmospheric pressure (2 atm). The gas inlet to the
absorber is the Syngas feedstock which have been previously compressed and cooled to
match the operating condition of the column. The liquid solvent used for the absorption
process is toluene which also have been pumped and heated to match the operating
condition of the column. V-101 absorber is would absorb 98% of the carbon monoxide
from the rest of the Syngas composition.
The syngas feedstock would enter the V-101 column from the bottom whereas the
toluene solvent would enter from the top of the column. Furthermore, the absorption
process is further enhanced by using a catalyst of Cuprous Aluminium Chloride which
have been dissolved along with the toluene solvent. This would ensure the efficiency of
the absorption rate and achieve its aim of 98% recovery.
At the top of the column, the outlet stream is made of the CO lean gas that have been
separated from CO. Whereas downstream would be filled with the CO-rich solvent
which would then be send to a flash unit and stripper unit for further purification.
6.1.1 Design Definition and Specification

The detailed calculations for this section are found in Appendix A6.
6.1.1.1 Operating Condition
One of the reasons for choosing absorption using toluene and Cuprous Aluminium
Chloride solvent is due to the fact that its operating condition is relatively moderate
compared to other Syngas process methods such as Cryogenic Distillation. A summary
of the operating condition is shown below.
130
Table 6.1.1.1.1: Operating Condition for V-101

V-101 Column Operating Condition
Flow Type Counter-Current
Operating Temperature °C 40 °C
Operating Pressure (bar, a) 2.0265 bar (a)
CO Recovery% 98
6.1.1.2 Column Type Selection
There are two type of Absorber Column which are tray column and packed bed column.
Selection of the column type is done based on the parameters and operating condition of
the column. A summary of the column favourability is shown below:
Table 6.1.1.2.1: Condition for different type of column

Packed Column Tray Column
Able to handle different type of liquid
Small Diameter Column(<0.6m)
solvent inlet
Less agitation of liquid by vapor High Liquid residence Time
Lower Pressure Drop Dirty service (easier to clean)
More Choices in materials of
High Liquid Flow Rate
construction for packing
Exotherms requiring cooling coils inside
Less Liquid entrainment.
column
Based on the table above, it was decided that the parameters and condition favours tray
column. This is due to the fact that the Inlet Liquid Flow Rate is relatively high.
Furthermore, tray column can handle more type of liquid inlet. The liquid inlet is an
organic Toluene which have been dissolved in Cuprous Aluminium Chloride. The
solvent is extremely complex thus it will be more appropriate to use tray column.
Although the solvent is also corrosive and column packing is favoured in terms of
corrosion, the material used for the tray column would be Stainless Steel 34, and would
be able to prevent corrosion. Last but not least, the diameter of the column is relatively
larger than the preferred diameter of the packed column which is less than 0.6 m,
therefore tray column is selected.
6.1.1.3 Stream Properties and Flow Rates

A summary of the flow rates and compositions of all the streams involved in V-101
would be shown below. Its temperature and pressure would also be shown.
131
Table 6.1.1.3.1: Properties of streams

Liquid Liquid
Gas Inlet Gas Outlet
Stream Inlet Outlet
Stream Stream
Stream Stream
Temperature (°C) 40 40 40
Pressure bar 2.0265 2.0265 1.01325 1.01325
Total Mass Flow Rate (kg/hr) 23982.025 34617.34 6493.5 66916.3
Individual Component Mol Flow Rate (kg/hr)
Hydrogen 2377.7 - 2353.93 23.777
Carbon Monoxide (CO) 17874.495 - 357.49 17517.005
Methane 3739.830 3702.532 37.298
Toluene - 13494.895 - 13494.895
Copper Aluminium Chloride - 21122.444 - 21122.44
6.1.1.4 Selection of Material
Stainless Steel 304 is used as the material for both the column and the tray. Despite its
relatively more expensive price, the usage of Stainless Steel 304 is necessary as it is
able to prevent corrosion. The solvent liquid inlet is rather corrosive thus it is important
to use the right material to minimize corrosion as much as possible. To further verify
the selection of Stainless Steel, a stress analysis as well as hydrotesting has shown that
Stainless Steel is able to withstand the weight of the column and its domed head.
Furthermore, mineral wool with a thickness of 50mm has been selected as it functions
as a resistance to moisture. Insulation for heat isn’t required for V-101 as the operating
condition is relatively moderate.
6.1.1.5 Internal Of V-101

Low Pressure drop is required for the column, therefore sieve tray is selected instead of
bubble cap and valve plates. In addition to that sieve tray is relatively easier to maintain
and is cheaper compared to bubble cap and valve plates.
6.1.2 Designing of Column Steps

The detailed calculations for this section are found in Appendix A6.1.1.
6.1.2.1 Properties that have been obtained from previous work.
The density of both the inlet Gas Stream and Liquid Stream is obtained from Aspen
Simulation that was worked on prior. Furthermore, the number of trays is also estimated
using Aspen Simulation. A summary of these properties is shown below:
132
Table 6.1.2.1.1: Density of stream

𝒌𝒈 𝒌𝒈
Inlet Gas Stream Density ( ) Inlet Liquid Stream Density ( )
𝒎𝟑 𝒎𝟑
2.81 820
Number of Trays
7
6.1.2.2 Diameter of the Column

Diameter of the column is obtained by finding the Area of the Column by Dividing the
Volumetric Flow rate with the maximum Design Velocity. The first step taken was to
use the both Inlet Mass Flow Rate for the Gas and Liquid steam as well their density to
find the flow parameter. The flow parameter would then allow the K1 constant to be
obtained based on the figure 11.29 in Sinnott (2008). The K1 constant is then used to
find the maximum design flooding velocity. Once the velocity is obtained, all the
parameters required to find the area have been obtained which would then enable the
diameter to be calculated.
Table 6.1.2.2.1: Summary of obtained results

Flow Maximum Design
K1 Constant Area(m2) Diameter(m)
Parameter Flooding Velocity(m/s)
0.1484 0.106 1.361 1.524 1.485
6.1.2.3 Provisional Plate Design
The plate tray design is done by first rounding up the Diameter of the column. The
diameter of the Column is round up to 1.5 m. Using the new diameter, the Area of the
column is obtained. Using the Area of the column, the Downcomer, Net area and Hole
area is calculated and obtained. Downcomer area is assumed to be 6% of the column
area whereas the Hole area is assumed to 10% of the Active Area. The Weir length is
obtained from figure 11.33 in Sinnott (2008) whereas the Weir Height and Hole
diameter and Plate Thickness is obtained from Sinnott (2008) based on the material of
the tray which is stainless steel.
Table 6.1.2.3.1: Summary of plate design

Column Diameter m 1.5
Column Area 𝑚2 1.767
Downcomer Area 𝑚2 0.106
Net Area 𝑚2 1.66
Active Area 𝑚2 1.555
Hole Area 𝑚2 0.1555
133
Weir Length m 0.975

Weir Height mm 50
Hole Diameter mm 6
Plate thickness mm 3
6.1.2.4 Check Weeping
Check weeping is done to check whether liquid leakage through the hole will not be
excessive. This is done by calculating the weep point velocity at maximum liquid rate.
The assumptions made on the calculation are the fact that the turn down rate is 70%.
Using this assumption both the actual minimum vapor velocity and minimum design
vapor velocity is calculated. There actual minimum vapor velocity is larger than the
minimum design vapor velocity therefore leakage is controlled.
Summary of the Result is shown below:
𝑚
 Actual Minimum vapor velocity = 10.634 𝑠
𝑚
 Minimum Design vapor Velocity = 8.063 𝑠
6.1.2.5 Plate Pressure Drop

Pressure drop on the plate is due Residual Pressure drop, dry plate Pressure Drop, the
weir and static head of liquid on the plate.
Table 6.1.2.5.1: Pressure drop calculated

Drop due to Total
Drop Due to Drop due to Drop due to
head of Pressure
Residual(mm) dry plate(mm) weir(mm)
liquid(mm) Drop(mm)
15.244 75.948 50 52.495 196.858
6.1.2.6 Down-comer Liquid Back up
To make sure no flooding occurs, liquid level in the down comer need to be ensured to
be less than the total height of the top of the outlet weir on the plate. The restriction of
flow and control the liquid level is done by the down comer outlet. Therefore, its Back
1
up in the Down-comer needs to be less than × (plate spacing + Weir Height).
2
Residence time is calculation as well. Plate spacing is taken as 0.6 m.
Summary of the result is shown:
1. Back up in the Down-comer=311.189 mm

1
2. X (plate spacing + Weir Height =325mm
2
134
3. Residence time= 2.814 s
6.1.2.7 Check Entrainment

The actual percentage flooding is obtained by using the maximum vapor flow rate. This
value need to be less than the design flooding percentage. The fractional entrainment
value is obtained as well by using figure 11.31 in Sinnott (2008). Summary of the result
is shown below:
 Actual Percentage Flooding = 68.882 %, which is less than the 80% design
value
 Entrainment Value = 0.047, which is less than the allowable 0.1 value
6.1.2.8 Perforated Area.

The validation of the hole pitch is done by calculating the total area for perforation and
obtaining the Hole area and perforated area ratio using figure 11.35 in Sinnott (2008).
The range for the ratio is between 2.5 to 4.
Summary of the result is shown:

 Perforated Area = 0.5428 m2
 Hole area and perforated area ratio = 2.2 which is slightly less than 2.5 thus still
acceptable
6.1.2.9 Number of holes
Number of Holes = 5500
6.1.2.10 Height of the column
The height of the column is determined by the following factor shown in the following
table.
Table 6.1.2.10.1: Calculated values for height of column
Htray (number of tray x thickness of tray) 0.201 m

Htspacing (number of tray -1) x tray spacing 3.6 m
Height of the ellipsoidal head (0.371 X 2) m
Height for liquid holds up 1.467 m
height for Low liquid level 0.2 m
Clearance between high liquid level and inlet nozzle 0.45 m
Clearance between inlet device and top level 1.05 m
135
Diameter of Nozzle (0.59 + 0.466) M

Height of vessel 8.567 m
6.1.2.11 Wall thickness selection

The selection of wall thickness is done based on the diameter of the vessel. This is
illustrated in appendix. The thickness of the wall is found to be 7mm.
6.1.3 Mechanical Design

The detailed calculations for this section are found in Appendix A6.1.2.
6.1.3.1 Dead Weight Calculation
The total dead weight is obtained based on several sections. These sections along with
its load are shown below:
Table 6.1.3.1.1: Total dead weight calculated

Factors Load(kN)
Weight of Vessel 28.028
Weight of Internal Fitting 13.953
Weight of External Fitting 41.573
Weight of Insulation 24.373
Weight of Domed(torispherical) Head 2.058
Total Load(kN)
110.009
Several assumptions are made for the factors when calculating the Total Dead Weight
Calculation which include:
Table 6.1.3.1.2: Assumptions of certain parameter’s weight

Nozzles and Manways for Contacting plate,
Caged Ladder Steel Platform
absorption column steel
𝑁 𝑘𝑁 𝑘𝑁
360𝑚 1.7 𝑚2 1.15 1.2𝑚2
6.1.3.2 Wind Loading

The wind loading is determined based on the wind speed of the Plant Location which is
𝑚
3.618 𝑠 . The Wind loading per unit length, bending moment are then obtained. They
𝑁
are 19.368 𝑚 and 592.837 Nm respectively.
136
6.1.3.3 Stress analysis.

To ensure that the Material along with its thickness is able to absorb total load of the
vessel as well as withstand the possible wind loading exerted on the vessel, a stress
analysis is done prevent any possible buckling. The maximum compressive stress need
to be calculated and check. The maximum compressive stress need to be less than the
maximum allowable stress. Several other stresses need to be calculated for the
maximum compressive stress to be obtained and this is summarized below.
Table 6.1.3.3.1: Calculated values for each type of stress

Type of Stress Value (MPa)
Longitudinal 10.856
Hoop 21.7125
Dead Weight 3.319
Bending 0.00144
Resultant Longitudinal (Upwind) 7.538
Resultant Longitudinal (Downwind) 7.535
Greatest principle stress 14.174
difference(upwind)
Greatest principle stress(downwind) 14.177
Critical Buckling 86.741
Maximum compressive 3.321
Maximum allowable 135
As seen above the greatest principle stress (downwind) is below the maximum
allowable stress and the maximum compressive stress is below the critical buckling.
Thus, material is justified.
6.1.3.4 Hydrotesting
Stress analysis need to be done again, however this time with the assumption that the
column is filled with liquid. This is done by adding the Load of the Liquid with the
Total Dead Load.
Total load with liquid = Total Dead Load + Load of Liquid
= 113.416kN + 128.591 kN = 242.008kN
Stress analysis is then done with the new Total Load.
137
Table 6.1.3.4.1: Calculated values for stresses with new total load
Type of Stress Value (MPa)
Greatest principle stress difference(upwind) 17.832
Greatest principle stress(downwind) 17.835
Critical Buckling 86.741
Maximum compressive 6.978
Maximum allowable 135
6.1.4 Skirt Design

The skirt is used to support the vertical volume. It is important for the skirt thickness to
be strong enough to withstand both the dead weight and bending moment imposed. The
thickness of the skirt is assumed to be the same as the vessel which is 7mm. The height
of the skirt is assumed to be 1.5m. The skirt specification is shown below:
Table 6.1.4.1: Specification for skirt

Bending stress 0.0084 MPa
Dead Weight Stress (Test and Operating) 0.931 and 0.443 MPa
Resultant tensile stress 0.434 MPa
Resultant compressive stress 0.939 MPa
Maximum allowable design stress, Ss 89 MPa
Welded Joint Efficiency, E 85%
Base angle of conical skirt, 𝜽𝒔 90°
SsEsin𝛉𝐬 75.65 MPa
𝒕
0.125E.(𝑫𝒔𝒌)sin𝜽𝒔 10.843 MPa
𝒐
As seen above the Resultant tensile stress is less than SsEsin θs and the Resultant
𝑡
compressive stress is less than 0.125E( 𝐷𝑠𝑘 )sin𝜃𝑠 . This then justifies the thickness of the
𝑜
skirt.
6.1.5 Nozzle Sizing

There are 4 nozzles in V-101. They are sized based on their diameter and it is calculated
using the streams density and velocity based on Tioga Pipe Dimension and Weight.
Summary of the nozzle sizing is shown below:
Table 6.1.5.1: Calculated sizes for nozzles

Nozzle Number D0 (mm) Schedule Wall thickness (mm) Di (mm)
N-1 660 40 7.92 640.92
N-2 88.9 40 5.49 77.92
138
N-3 355.6 40 11.13 333.34

N-4 114.3 40 6.02 102.26
6.1.6 Specification Data Sheet and Mechanical Design

The specification data sheet of V-101 and the detailed mechanical drawing of the vessel
based on the side and top views will be shown at the end of this chapter.
6.2 Tray Distillation Column D-101

6.2.1 Design and Specifications
Step 1: Determining Light Key and Heavy Key Component
In this separation process, mainly Carbon Monoxide and Toluene are involved. The
density of Carbon Monoxide at the operating conditions are less than that of Toluene so
CO will be evaporated out from the top of the distillation column and toluene will be
the bottom product.
Step 2: Determining Density of Vapor and Density of Liquid in D-101
As the densities determined here will be used to design the entire column’s diameter,
the maximum flow through the column at any given time should be used.
Table 6.2.1.2: Properties of flow through D-101

For maximum flow through the column
Phase Density (kg/m3) Maximum Flow rate (kg/s)
Liquid, L 867.0 11.114
Vapor, v 1.628 8.377
Step 3: Column Diameter sizing
One of the key assumption made in this step is that the distillation column is designed at
90% flooding at its maximum flow rate. The downcomer area is also estimated to be
12% of the cross-sectional area of the column. The diameter of the column is calculated
through the Souders and Brown equation which relates to the maximum allowable
superficial vapor velocity in the column. The diameter obtained for Distillation Column
D-101 is 2.40 m.
139
Step 4: Plate Design
The hole active area is estimated to be 10% of the active area calculated. The liquid
flow arrangement was also determined to be a Cross flow (single pass) type after
calculations were made. The design suitable for the trays are tabulated as follow,
Table 6.2.1.3: Design Parameters calculated for Plate Design

Design Parameters Value/Selection Units
Cross Section Area of Column, 𝐴𝑐 4.291 m2
Downcomer Area, 𝐴𝑑 0.515 m2
Active Area, 𝐴𝑎 3.261 m2
Hole Active Area, 𝐴ℎ 0.326 m2
Plate Thickness 5 mm
Weir Length, 𝑙𝑤 1.753 m
Weir Height 40 mm
Weir thickness 5 mm
Weir Crest, ℎ𝑜𝑤 28.256 mm liquid
Step 5: Hole Design
The width of calming zone is chosen to be 100 mm and support ring is chosen to be 75
mm as the diameter of the column is above 1.5 m (Sinnott, 2014). By calculating the
unperforated area using the geometry of the plate, the perforated area, Ap can then be
found to be 2.201 m2.
With a recommended hole diameter of 5 mm as the chosen hole diameter, the hole pitch
could be calculated by using the equation,
2
𝐴ℎ ℎ𝑜𝑙𝑒 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟,𝑑ℎ
= 0.9 [ ]
𝐴𝑝 ℎ𝑜𝑙𝑒 𝑝𝑖𝑡𝑐ℎ,𝑙𝑝
This equation relates hole area and perforated area calculated to the hole arrangements.
The hole pitch is determined to be 12.32 mm. The arrangements of holes are also
chosen to be triangular pitch to ensure a more compact arrangement to account for the
large amount of holes needed per plate. The total number of holes is then determined
through dividing the hole active area with the area of a single hole. Lastly, the number
of holes per plate can be found as the optimal number of plates is known through using
the Aspen Plus simulation.
140
Figure 6.2.1.3: Number of holes calculated

Total number of holes required 16608 holes
Number of holes per plate 1845 holes per plate
Step 6: Entrainment and Weeping Checking
The percentage flooding was also calculated by using the actual velocity divided by the
90% of the flooding velocity for safety measures and is found to be 0.009 %, which
indicates that flooding is very unlikely to happen in the operation of this column.
The weeping velocity is calculated through the use of the Weep-point correlation graph
found on Figure 11.32 (Sinnott, 2014) and is found to be 9.356 m/s. To check for
weeping, the actual minimum vapor velocity is calculated by assuming a 70% turn-
down and is 11.041 m/s. This value is significantly larger than the weeping velocity and
the calculation ensures that weeping is also unlikely to happen during operation. Hence,
the design of the Distillation Column is free from flooding and weeping.
6.2.2 Mechanical Design Calculations

Step 1: Design temperature and pressure
The highest operating temperature of the distillation column is 111 °C. 30 °C will be
added to the operating temperature as the Design temperature of the column for safety
measurements. (Sinnott, 2014) The column operates under 1 atm which is 0 barg. For
vessel that operates between 0 – 35 barg, the design pressure would be the maximum
operating pressure plus 3.5 barg. (NORSOK STANDARD - PROCESS DESIGN, 1997)
Therefore, the Design pressure is set to be 3.5 barg.
Step 2: Material Selection for Vessel
As the vessel is operating under moderate conditions of 111 °C, 1 atm and handles non-
corrosive fluids, Carbon Steel is initially selected to go through stress analysis and try to
minimize the cost for the equipment. The material properties are tabulated below.
Table 6.2.2.1: Selected Material properties

Material Carbon Steel
Grade CS-A
Product Form Sheet
Minimum Tensile Strength (MPa) 275
Minimum Yield Strength (MPa) 140
141
Tensile Strength at 141 °C (MPa) 276

Yield Strength at 141 °C (MPa) 122
Maximum Allowable Stress at 141 °C (MPa) 78.6
To calculate the maximum allowable stress, four different conditions were also used
(Sinnott, 2014) and the smallest value that is obtained among the four conditions is
chosen as the maximum allowable stress.
Table 6.2.2.2: Selection of Maximum Allowable Stress
Specified minimum tensile strength at room temperature divided by
78.571 MPa
3.5
Tensile Strength at temperature (141 °C) divided by 3.5 78.857 MPa
Minimum yield strength at room temperature divided by 1.5 93.333 MPa
Yield Strength at temperature (141 °C) divided by 1.5 81.333 MPa
The smallest value obtained from the table above is 78.571 MPa and is used as the
maximum allowable stress for material to be used for D-101.
Step 3: Vessel Head Selection
For low pressure applications, torispherical heads are normally used due to the fact that
their cost of fabrication is lower. As for this Distillation Column, the operating pressure
is at 0 barg which classifies under low pressure application, therefore the torispherical
head is chosen.
Step 4: Vessel Wall Thickness
For calculation of vessel wall thickness, the equations below are used for either vessel
body or vessel head. (Sinnott, 2014)
Table 6.2.2.3: Equations used to calculate thickness of wall

Equation used for Vessel Body Equation used for Vessel Head
Pi Di 0.885Pi Rc
𝑡 = 2SE−1.2P t = SE−0.1P
i i
Where,
Pi = Internal Design Pressure, MPa;
Di = Internal Diameter, mm;
S = Maximum allowable stress, MPa;
E = Welded-joint efficiency (Taken as 1)
Rc = crown radius, mm
142
The calculated wall thickness for the body of the vessel is to be 6.7 mm and 13 mm for
the vessel head. The minimum requirement for a vessel which falls under 2 to 2.5m in
diameter is to have a wall of 9 mm thickness. Therefore, the thickness of the whole
vessel is chosen to be 13 mm as it is the larger value and fits the requirement for the
minimum thickness of wall required. 2 mm corrosion thickness allowance was also
included in the determination of vessel wall thickness.
Step 5: Nozzle Sizing
The nozzle is sized based on the volumetric flow rate of fluid through a pipeline, the
relationship between fluid density and optimal velocity of flow through the pipeline is
used to first determine the velocity required for each and every stream. (Sinnott, 2014)
The pipe area required is then calculated by,
𝑉𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝐹𝑙𝑜𝑤
𝑃𝑖𝑝𝑒 𝐴𝑟𝑒𝑎 𝑟𝑒𝑞𝑢𝑖𝑟𝑒𝑑 = 𝑂𝑝𝑡𝑖𝑚𝑎𝑙 𝑉𝑒𝑙𝑜𝑐𝑖𝑡𝑦
After the diameter of pipe is determined through acquiring the pipe area, a DN of pipe is
chosen to be used for the nozzle. The initial pipe chosen will go through thickness
calculations to find the actual diameter of the pipe and is checked to see if the initial
chosen DN of pipe fits the required conditions. The actual pipe diameter is calculated
by,
𝐴𝑐𝑡𝑢𝑎𝑙 𝑃𝑖𝑝𝑒 𝐷𝑖𝑎𝑚𝑒𝑡𝑒𝑟 = 𝑂𝑢𝑡𝑒𝑟 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟 − (2 × 𝑡ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠 𝑜𝑓 𝑝𝑖𝑝𝑒)

The calculation steps above are repeated for all streams entering and exiting the
Distillation Column D-101 for the nozzle sizing. The naming in the table below
corresponds to the Detailed Drawing for Tray Distillation Column D-101.
Table 6.2.2.4: Nozzle Sizing for Distillation Column

Nozzle Specifications
Nozzle Label Nozzle Description Nominal Size
N1 Vent Gas Outlet 125 mm
N2 Top Product Gas Outlet 660 mm
N3 Pressure Relief Valve 125 mm
N4 Inlet Stream 711 mm
N5 Top Reflux Inlet 73 mm
N6 Bottom Reboiler Inlet 559 mm
N7 Level Indicator Sensor 30 mm
N8 Bottom Product Liquid Outlet 73 mm
143
N9 Drain Nozzle 60 mm
N10 Nitrogen Purge Inlet 125 mm
N11 Manway 1 600 mm
N12 Manway 2 600 mm
N13 Manway 3 600 mm
Step 6: Height of Vessel
The straight height of the vessel is calculated through the sum of different heights in the
column such as tray heights, overhead height and sump volume height. The time
accounted for the sump volume is a 3 mins liquid hold up time. The detailed
calculations to obtain the straight height of the vessel can be found in Appendix A6.2.6.
Table 6.2.2.5: Calculated values for Height of Vessel
Vessel Straight Height (m) 14
Torispherical Head Height (m) 0.22
Height of Vessel 14.44
The equation used to find the Height of the vessel (excluding skirt height) is as follow,
𝐻𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑉𝑒𝑠𝑠𝑒𝑙 = 𝑆𝑡𝑟𝑎𝑖𝑔ℎ𝑡 ℎ𝑒𝑖𝑔ℎ𝑡 + (2 × 𝐻𝑒𝑎𝑑 ℎ𝑒𝑖𝑔ℎ𝑡)
Step 7: Total Weight of Vessel
The total weight of the vessel is made up of various weights in and out of the column.
Before performing weight calculations, the insulation thickness should first be found.
The assumption made is that the all the conductive heat transfer from the different
layers of walls is fully transferred to the convective heat transfer from the outermost
wall to the surrounding air. (Cheresources.com Community, 2017) The insulation
material is chosen to be Mineral Wool and with the use of Aluminium Cladding.
The data used to obtain the insulation thickness is tabulated below.
Table 6.2.2.6: Values for insulation thickness calculation

Radius of Vessel Wall (m) 1.2
Thickness of Vessel Wall (m) 0.013
Thickness of Cladding (m) 0.002
Vessel Temperature (°C) 111
Desired Temperature of Wall (°C) 48
Temperature of Surrounding Air (°C) 30
Thermal Mineral Wool 0.05
Conductivity Carbon Steel 35.351
144
(W/m.K)
Insulation thickness required (mm) 12
After obtaining the thickness of insulation, the total weight of the vessel can be
determined. The dead weight of the vessel is calculated through the use of Equation
13.73 (Sinnott, 2014).
𝑊𝑣 = 𝐶𝑤 𝜋𝜌𝑚 𝐷𝑚 𝑔(𝐻𝑣 + 0.8𝐷𝑚 )𝑡 × 10−3

Where,
𝑊𝑣 = Total weight of the shell, excluding internal fittings, such as plates, N;
𝐶𝑤 = Factor to account for weight of nozzles, manways, internal supports (1.15 for
distillation columns);
𝐻𝑣 = height, or length, between tangent lines, m;
g = gravitational acceleration, 9.81 m/s2 ;
t = wall thickness, mm;
𝜌𝑚 = density of vessel material, kg/m3 ;
𝐷𝑚 = Mean diameter of vessel = (𝐷𝑖 + 𝑡 × 10−3 ), m
Table 6.2.2.7: Various weights to make up weight of column
Parameters Value Units
Dead Weight of Vessel 139.05 kN
Weight of Chosen Heads (2 heads) 9.354 kN
Weight of Insulation 1.864 kN
Weight of Internals (9 Trays) 22.87 kN
Weight of Ladder 2.358 kN
Weight of Liquid Holdup (3 mins) 19.622 kN
Total Weight of Vessel 195.118 kN
Step 8: Stress Analysis
As the height of the vessel is less than 20m, the bending moment of the vessel due to
wind loading need not to be considered. The longitudinal stress and hoop stress due to
the internal pressure of the vessel are calculated using the equations below,
Pi Di
𝐻𝑜𝑜𝑝 𝑆𝑡𝑟𝑒𝑠𝑠, 𝜎ℎ = = 60.13 𝑀𝑃𝑎
2t
Pi Di
𝐿𝑜𝑛𝑔𝑖𝑡𝑢𝑑𝑖𝑛𝑎𝑙 𝑆𝑡𝑟𝑒𝑠𝑠, 𝜎𝐿 = = 30.07 𝑀𝑃𝑎
4t
145
Wz
𝐷𝑒𝑎𝑑 𝑤𝑒𝑖𝑔ℎ𝑡 𝑠𝑡𝑟𝑒𝑠𝑠, 𝜎𝑤 = = 2.865 𝑀𝑃𝑎
π(Di +t)t
For stress checking, the resultant longitudinal stress is calculated to be 32.935 MPa. The
hoop stress is also calculated to be 60.13 MPa. The maximum allowable stress of the
material is determined to be 78.571 MPa. Therefore, the principal stresses are lower
than the maximum allowable stress.
Step 9: Support Calculation
The support chosen here is the skirt support as the Distillation Column stands about 15
m. The maximum wind speed in Malaysia is also used as 20 km/h in the support
calculations. An initial guess was used as the skirt support thickness and is used to
check if the calculated values meets the criteria for design.
Criteria for Design:

𝜎𝑠 (𝑇𝑒𝑛𝑠𝑖𝑙𝑒) < 𝑆𝑠 𝐸𝑠𝑖𝑛𝜃
𝑡
𝜎𝑠 (𝐶𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒 ) < 0.125𝐸𝑦 ( 𝐷𝑠𝑘 ) 𝑠𝑖𝑛𝜃
𝑠
The values used for calculations are tabulated below.

Table 6.2.2.8: Support Calculation
Wind Speed, Uw (km/h) 20
Dynamic Wind Pressure, 𝑃𝑤 (N/m2) 28
Maximum Bending Moment, M (Nm) 8233.85
Bending Stress of Skirt, 𝜎𝑏𝑠 (MPa) 0.124
Water Load for vessel, 𝑊𝑣 (kN) 63.33
Dead weight stress of skirt, 𝜎𝑤𝑠 (MPa) 0.585
𝜎𝑠 (𝑇𝑒𝑛𝑠𝑖𝑙𝑒) (MPa) -0.461
𝜎𝑠 (𝐶𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒 ) (MPa) 0.709
Skirt thickness chosen (mm) 14
The calculated value is the most optimum when the skirt thickness chosen was 14 mm,
therefore, the determined thickness for skirt support is 14 mm.

The specification data sheet of D-101 and the detailed mechanical drawing of the vessel
146
6.3 Dimethyl Oxalate Reactor R-201

6.3.1 Definition of Design and Specification
Dimethyl oxalate, (DMO) is required further in the process of producing monoethylene
glycol. DMO can be synthesis in the presence of Palladium catalyst with the support of
aluminium oxide. The reaction is carried out in a reaction temperature of 140°C and
operating pressure of 3barg. The reactant for the synthesizing of DMO is CO, and
Methyl Nitrate (MN). Due to the explosive property of MN when presence in high
concentration, nitrogen gas is being fed into the reactor as inert as well as to act as a
diluent for the high concentration of MN. Synthesizing DMO is a vapor phase reaction
whereby the reactant enters the reactor in vapor phase and exits the reactor as vapor
phase as well. No phase change occurs in the reactor hence a multi-tubular fixed bed
reactor is being designed in order to carry out the reaction. Both reactants enter the
reactor at the bottom and leave together as products and unreacted reactant at the top of
the reactor.
The chemical equations of the process are shown below:
2CO + 2C𝐻3 𝑂𝑁𝑂 −→ (𝐶𝐻3 𝑂𝐶𝑂)2 + 2 𝑁𝑂 ------ (Desired Product)
𝐶𝑂 + 2C𝐻3 𝑂𝑁𝑂 −→ (𝐶𝐻3 𝐶𝑂)2 + 2𝑁𝑂 ------ (Undesired By-product)
Table 6.3.1.4: Reactor Stream Table

Description Reactant Inlet Product Outlet
Vapor Fraction 1.0 1.0
Temperature (°C) 140 130
Pressure (barg) 3.2 2.9
Volumetric Flowrate 29198.65 30450
Density (𝑘𝑔/𝑚3 ) 8.9 3.2161
Total Mass Flowrate (kg/hr) 97930.9 97930.9
Individual Component Flowrate (kg/hr)
Dimethyl Oxalate 0.5 26329.7
Carbon Monoxide 48003 35447.8
Nitrogen Oxide 1502.9 15024.3
Methyl Nitrate 30243.1 2740.9
Toluene 292.2 292
Dimethyl Carbonate 4.0 213.1
Nitrogen 13984.4 13984.4
147
Water 95.6 95.6

Methanol 3713.4 3713.4
Nitric Acid 89.6 89.6
Under the reaction temperature and pressure, the conversion of MN to DMO (Desired
Product) is around 90%. The high conversion can be achieved ONLY with the proper
control of reaction pressure and temperature since higher reaction pressure will
contribute to lower selectivity of DMO and forming more Dimethyl Carbonate (by-
product). Hence the monitoring of pressure and temperature of the reactor is crucial in
order to produce high purity of DMO.
6.3.2 Basic of Performance

6.3.2.1 Reactor Sizing
Step 1: Reactor Type
As determined in Chapter 2: Technology Evaluation, multi-tubular fixed bed reactor is

chosen to be the design of this process as high heat transfer area is achievable compared
to jacketed fixed bed reactor. The reactant enters the reactor at the bottom and flows
upward whilst the product will leave at the top of the column.
Step 2: Catalyst Properties
Table 6.3.2.1.1: Catalyst Properties (Nian Jun L, 2012)

Properties Selection Justification/ Source
Type Palladium Higher selectivity on DMO and
supported on higher conversion of MN
Aluminium Oxide
Particle Diameter (mm) 60 -
Shape Solid Cylinder -
Catalyst Consumption 0.004617 wt% of
CO
Step 3: Catalyst Bed Mass Volume
Based on the volume of the bed calculated, the mass of catalyst can be determined by
obtaining the porosity of the catalyst inside the tube of the reactor. The formula to
calculate the weight of and volume of the catalyst is shown in Table 6.3.2.1.1.
148
Step 4: Sizing the Reactor
The sizing of reactor was carried out based on the gas hour space velocity (GHSV)
of 3000 ℎ−1 . The height and the diameter of the reactor was sized based on the tube
length and the tube flow area. Minimum heat transfer area required to achieve the duty
of the reactor is determined. Number of tubes required to achieve an optimum velocity
of the process stream as well as meeting the heat transfer area required is being iterated
and determined.
Table 6.3.2.1.2: Calculation Summary on Reactor Sizing

Parameter Method and Equation Value
k = 2.49 x 10-5
𝑏𝑢𝑙𝑘 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 mol/h.gcat.Pa0.5
Mass of Catalyst, W𝑐 (kg) 1− ∈ = 𝑎𝑐𝑡𝑢𝑎𝑙 𝑑𝑒𝑛𝑠𝑖𝑡𝑦
W𝑐 = 853 kg
Total W𝑐 = 2560 kg
𝑇𝑜𝑡𝑎𝑙 W𝑐
Volume of Catalyst Bed (m3) 𝑉𝐶 = 2.56
𝐵𝑢𝑙𝑘 𝐷𝑒𝑛𝑠𝑖𝑡𝑦
𝑉̇
Volume of Reactor (m3) 𝐺𝐻𝑆𝑉 = 𝑉 10.15
Diameter of Reactor (m) Shell side Diameter 2.157
ℎ𝑒𝑖𝑔ℎ𝑡
7.9
Height of Reactor (m) = 𝑡𝑢𝑏𝑒 ℎ𝑒𝑖𝑔ℎ𝑡
+ ℎ𝑒𝑎𝑑 ℎ𝑒𝑖𝑔ℎ𝑡
𝑉
Residence Time in Reactor (s) 𝑅𝑒𝑠𝑖𝑑𝑒𝑛𝑐𝑒 𝑡𝑖𝑚𝑒 = 𝑉̇ 1.2
6.3.2.2 Heat Exchange System

Due to the exothermic property of the reaction, cooling of reactor is required and crucial
to prevent thermal runaway reaction. The operating temperature of the reaction is
140°C. Based on Aspen plus simulation, the duty of the reactor is found to be 9400 kW.
Dowtherm 4000 is used as cooling medium to provide cooling effect to the reactor
constantly. Dowtherm 4000 is chosen in this case is being used instead of cooling water
due to the ability of Dowtherm in cooling process stream that has a higher temperature.
Details of heat transfer system and configuration is shown below:
Table 6.3.2.2.1: Heat Exchange System Data

Tube Side Shell Side
Number of Tubes 948 Bundle diameter 2.091
Number of tube pass 1 Shell Diameter 2.157
External diameter of Tubes 50 mm Number of Pass 1
149
Internal diameter of tubes 45.80mm Baffle Cut 25%

Tube Pitch 62.50mm Inlet Temperature 40°C
Wall Thickness 2.10mm Outlet Temperature 80°C
Tube Side Velocity 5.416 m/s Shell Side Velocity 0.328m/s
Length of Tube 7m
Inlet Pressure 3bar
6.3.2.3 Reactor Internal Fittings and Sizing

Sieve Mash
Sieve mash is placed at the top as well as at the bottom of the tube sheet in order to
prevent the catalyst from spilling out of the tube as the velocity inside the tube side is
very high. Without the sieve mash the catalyst might be constantly lost and leave the
tube side along with the product formed. Sieve mash is responsible to trap the catalyst
as well as the inert material in the tube side and only be removed during unloading and
replacement of catalyst. The thickness of the sieve mash is 0.1m and has a sieve size of
1mm.
Vapor Distributor
Vapor distributor is required to form trickles of vapor flow to ensure high surface area
of contact of reactant with the catalyst packed inside the tube. Vapor distributor is also
responsible to distribute the reactant flow uniformly into the all the tubes present in the
reactor. (Intra-Process, 2017)
Gasket
Gaskets are used to ensure a leak-tight joint between the tube sheet and torispherical
cover head. Selection on gaskets is done by following ASME BPV Code Sec VIIID.1.
Several factors must be considered when selecting a gasket material such as reactor
temperature and pressure as well as the assembly and disassembly of the joint. Rubber
gasket is used as the operating temperature of the reactor is only 140°C. (Ram Gasket
Solutions, 2017)
6.3.2.4 Reactor Structure and Support

Torispherical head is used as cover head of the reactor as the operating pressure of the
reactor is only 3barg, which is way below 15 barg. (Sinnott, Trowler, 2015) The
150
torispherical head is connected with the tube sheet along with the reactor with bolts.
Number of bolting required is found to be 59 bolts.
Double gusset plate lug support with 4 legs is chosen as the desired support system of
the reactor. Skirt support is not recommended as the torispherical head is required to be
removed during maintenance purposes. The reactor is fitted inside the platform in which
platform support in the interval of 3m is required to support the reactor.

6.3.3.1 Material Selection and Justification
Table 6.3.3.1.1: Equipment Material Selection
Parameters Material Justification/ Source
Reactor Carbon Steel Carbon steel is suitable for equipment which corrosion
Construction A285 Grade factor is negligible. Stainless steel is not required as there
A is little or none corrosive components present in the
equipment. Carbon steel is relatively cheaper compared to
other construction material. (Meps, 2017)
Insulation Mineral Used to maintain temperature of reactor and also as
Wool personnel protection. Mineral wool is chosen as it is an
excellent heat insulator. Besides, density of mineral wool
is low making it light, cheap and easy to apply. (Sinnot &
Towler, 2009)
Cladding Aluminium To protect and cover insulation. Aluminium is chosen for
it being light and fire resistant
6.3.3.2 Vessel Wall Thickness

The wall thickness of the vessel is calculated based on ASME Section VIII Thin Walled
Pressure Vessel Standard. The design pressure is calculated by assuming a 10% higher
than maximum allowable working pressure. The constructing material of the vessel is
chosen to be carbon steel which has a S value of 88.94MPa. Welded joint efficiency is
assumed to be 1.0 to allow for full radiography examination. Corrosion allowance is set
to be 2mm which is the minimum as stated in ASME code. Method of calculating
different thickness of the vessel is shown in Table 6.3.3.2.1.
Table 6.3.3.2.1: Calculations of Wall Thickness

Parameter Method and Equation Value (Including
Corrosion allowance
of 2mm)
151
Vessel Shell Thickness 𝑐𝑖𝑟𝑐𝑢𝑚𝑓𝑒𝑟𝑒𝑛𝑡𝑖𝑎𝑙 𝑡 11

(mm) 𝑃𝑖 𝐷𝑖
=
2𝑆𝐸 − 1.2𝑃𝑖
Torispherical Closure 0.885𝑃𝑖 𝑅𝑐 9.57

𝑡=
Thickness (mm) 𝑆𝐸 − 0.1𝑃𝑖
Insulation Thickness (mm)Typical thickness for a vessel 50
operating with a temperature
of 130oC is 50mm
Tubesheet Thickness (mm) Comparing Shear thickness 51
and Bending Thickness,
whichever is greater.
6.3.3.3 Lifting Lug

Lifting lug is required to be welded on torispherical head in order to lift the cover head
during maintenance purposes. The design and calculation of lifting lug will be carried
out following the Pressure Vessel Handbook, 12th Edition. Details of the dimensions
are shown in Table 6.2.3.3.1.
Table 6.3.3.3.1: Lifting Lug Detail

Description Values
Diameter (mm) 38.10
Thickness (mm) 19.05
Height (mm) 152.40
Length (mm) 254.00
6.3.3.4 Inspection Hole

Manhole is not required however an inspection hole is required to check on the tube
status in order to spot any rusting or leakage of tubes. The inspection hole is sized based
on ASME BPV Code Section VIII, Div 1, UG-46, The dimension of inspection hole
has an internal diameter of 300mm.
6.3.3.5 Pressure Relief Valve (PRV)

According to Asme BPV code Section VII, pressure relief valve must be fitted on all
type of pressureized vessel. Pressure relief valve prevents catastrophic failure of vessel
152
by releasing the vapor content in the vessel to relief the pressure. The set point of
pressure relief valve is 90% below the design pressure. Which is 4.65 barg. The nozzle
size of the PRV was chosen to have a nominal diameter of 125mm.
6.3.3.6 Nozzle Sizing

Nozzle size can be calculated by ensuirng the velocity of liquid streams is within 1-3m/s
and velocity of vapor stream is within 15-30 m/s (Sinnot & Towler, 2015). All the
nozzles selected follow the pipe size at Schedule 40. The detail nozzle sizes are shown
in Table:
Table 6.3.3.6.1: Nozzle Detail

Tube side Shell side
Schedule 40 Schedule 40
Outer Diameter 812.8 mm Outer Diameter 273.1mm
Thickness 17.48mm Thickness 9.3 mm
Process Stream 17.85 m/s Process Stream 1.2m/s
Velocity velocity

The specification data sheet of R-201 and the detailed mechanical drawing of the vessel
6.4 Methyl Nitrite Reactor R-402

6.4.1 Definition of Design and Specification
The synthesis of the methyl nitrite will be occurred through a series of reaction using
methanol, nitrogen monoxide and oxygen. Since methyl nitrite synthesis is a gas-liquid
reaction, the packing column is selected for this process due to its high interfacial
contact area for liquid and gas during the operation. In this process, the operating
condition for the packing column reactor is set at 60℃ and 7atm to maintain the overall
yield of the product. During the synthesizing process, the gas feed stream will enter
from the side of packing column, flow up and passing through the bottom of packing
section of column. The reaction will take place on the surface of the packing material
when the gas is in contact with methanol which flow down from the top of the packing
153
section. The gaseous product (methyl nitrite) will then flow out from top of the column,
while the liquid by-product (H2O and HNO3) will flow out from the bottom of the
column. The stream composition processed by the packing column is tabulated in Table
6.4.1.1 below. The main limitation during the design of the reactor is the rate of reaction
which affected by the partial pressure of NO in the reactor. Based on Table 6.4.1.1,
there have large amount of unreacted CO from previous process remain in the gas
stream which reduce the partial pressure of main reactant and thus reduce the reaction
rate.
Table 6.4.1.1: information of stream in and out of reactor

Gas Inlet Liquid Inlet Gas Outlet Liquid Outlet
Temperature, ℃ 100 60 60 60
Pressure, atm 7 7 6.5 6.5
Density, kg/m3 3.50 569.82 4.19 620.07
Volume
19628.72 70.14 17809.3 54.80
Flow,m3/h
Total Mass
68680.78 39965.22 74668.27 33978.06
Flow, kg/h
Component Mole Flow, kmol/h
DMO 1.81 - - 1.80
CO 1138.87 - 1138.83 0.11
NO 361.60 - 213.88 0.06
Methyl nitrite 39.80 - 343.23 7.97
Toluene 1.17 - 0.28 0.88
DMC 0.65 - 0.04 0.60
N2 449.26 - 449.22 0.04
Water 1.43 - 3.69 145.34
Methanol 68.61 1247.27 83.08 921.38
HNO3 0.52 - 0.91
NO2 180.00 - - -
Total 2243.71 1247.27 2233.17 1093.99
154
6.4.2 Basis of Performance

The main reaction of methyl nitrite synthesis is shown below:
2𝐶𝐻3 𝑂𝐻 (𝑙 ) + 𝑁𝑂(𝑔) + 𝑁𝑂2 (𝑔) → 2𝐶𝐻3 𝑂𝑁𝑂(𝑔) + 𝐻2 𝑂(𝑙 )
The nitrogen dioxide is firstly synthesized in R-401 by reacting nitrogen monoxide and
oxygen before entering packing column reactor (R-402). The nitrogen monoxide and
nitrogen dioxide will then react to form dinitrogen trioxide (N 2O3) before they start to
react with methanol. Since the formation of dinitrogen trioxide is an equilibrium
reaction, nitrogen monoxide will be supplied in excess in order to swift the reaction to
the side of formation of N2O3. Therefore, the overall conversion of NO2 in this reaction
can reach approximately 100%. Besides, since this reaction is a heterogeneous reaction
of gaseous and liquid, the reaction will greatly affect by the interfacial contact surface
area of the reaction. Thus, a packed column with higher interfacial contact area due to
its packing material is selected for this process. The sizing of the reactor will also based
on the contact surface area required of the reaction. The chemical and physical
properties of component needed in calculation are mostly extracted from Aspen Plus or
relevant content from website.
6.4.3 Reactor sizing

Based on the literature ( Liu, Ji and Li, 2009), the reaction kinetic on methyl nitrite
synthesis from methanol and dinitrogen trioxide is shown below:
kmol 𝑃𝑁𝑂 0 57.416

𝑅𝑀𝑁 ( ) = 2 𝐶 √𝐷𝑁𝑂 × 6.546 × 10 9 exp (− ) × 𝐶0
m2 s 𝐻𝑁𝑂 𝑅𝑇
The surface area required for reaction was then calculated using this rate of reaction by
the following equation.
1 𝑑𝑁𝐴 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝐴 𝑓𝑜𝑟𝑚𝑒𝑑 𝑚𝑜𝑙𝑒𝑠 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 𝑜𝑓 𝐴 𝑓𝑜𝑟𝑚𝑒𝑑

𝑟"𝐴 = ( )= =
𝑆 𝑑𝑡 (𝑠𝑢𝑟𝑓𝑎𝑐𝑒)(𝑡𝑖𝑚𝑒) (𝑠𝑢𝑟𝑓𝑎𝑐𝑒)
Based on the calculation performed, the rate of reaction of this process is 8.3 x 10 -7
kmol/(m2.s) and the surface area needed is 104211.86 m2. Since this process required a
large contact surface area, a structural packing column was used. A structured packing
material with higher interfacial contact area per unit volume of packing material was
155
selected to provide higher surface area with smaller column volume. In this case, the
Gempak 4A structured packing with 452 m2/m3 surface area is chosen as packing
material. The volume of packing section is calculated using this surface area per unit
volume and a volume of 230.56 m3 of packing section is required achieve desired
production rate of methyl nitrite. The detail calculation is shown in Appendix A6.4. The
properties of the structured packing chosen are shown in following table:
Table 6.4.3.1: Properties of packing material used

Type Material Void fraction, Surface area, Packing factor, m-
Ɛ m2/m3 1
Gempak 4A Ceramic 0.91 452 105

The packing material made of ceramic is selected due to its corrosion resistance. Since
some of nitric acid will be synthesized in the reactor due to side reaction, a packing
material with good acidic corrosion resistance is necessary.
6.4.3.1 Column diameter and pressure drop

The column diameter and pressure drop of a packing column can be determined by the
following design procedure:
Step 1: Select a suitable packing
From previous section, a Gempak 4A structured packing with higher surface area per
unit volume of packing was selected. The packing factor, Fp of this type of packing is
105 m-1 and will be use in the following calculation.
Step 2 Select a suitable liquid to gas ratio, G L/GG

𝑚𝑎𝑠𝑠 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒
Since gas and liquid mass velocity = 𝑐𝑟𝑜𝑠𝑠 𝑠𝑒𝑐𝑡𝑖𝑜𝑛𝑎𝑙 𝑎𝑟𝑒𝑎 , and the cross-sectional area of
𝐿
GL 𝐴𝑐 𝐿
column is constant. The liquid-to-gas ratio, G = 𝑉 = 𝑉 , where L and V are the liquid
G
𝐴𝐶
and gas mass flow rate respectively. Based on the calculation, the liquid-to-gas ratio of
0.58 was calculated.
Step3. Calculate the flooding pressure drop

The pressure drop at flooding can be calculated by following equation:
∆𝑃𝑓𝑙𝑜𝑜𝑑 = 0.115𝐹𝑝0.7
156
This equation was developed by Kister and Gill and can used to predict the flooding
pressure drop from 9 to 60 ft -1. The Gempak 4A ‘s packing factor still fall within the
range and the flooding pressure drop calculated was 1.301 in.H 2O/ft packing height.
Step4.Calculate the flow parameter

The equation to calculate the flow parameter is shown below:
𝐺 𝜌 0.5
Flow parameter = (𝐺𝐿 ) ( 𝜌𝐺)
𝐺 𝐿
By substituting all value, the flow parameter was calculated to be 0.046. This value will
then used to found capacity parameter of 1.58 from following graph with flooding
pressure drop.
Figure 6.4.3.1.1: Relation between capacity parameter, pressure drop and flow parameter
Step5. Calculate gas velocity, vG and gas mass velocity, GG

𝜌𝐺 0.5
Since capacity parameter =𝑣𝐺 (𝜌 ) 𝐹𝑝0.5 𝑣 0.05 , gas velocity of 3.64 ft/s was found
𝐿 −𝜌𝐺
from equation. The gas mass velocity can be found by multiplying gas density and gas
velocity. The gas mass velocity at flooding was found to be 0.795 lb m/s.ft2.
Step6. Select a suitable percentage of flooding velocity for design and find a new
value of GG
50% of the flooding velocity rule was used in this case. the new gas mass velocity was
found to be 0.398 lbm/s.ft2 and the new capacity parameter was found to be 0.79. By
using 0.79 of capacity parameter and same flow parameter of 0.046, the pressure drop
of 0.15 in.H2O/ft of packing height was found.
157
Step7.The column cross-sectional area and internal diameter

The column cross-sectional area, Ac can be found by dividing gas mass flow rate, V by
the gas mass velocity. The cross-sectional area of column of 105.757 ft 2 (9.825 m2) was
found.
The inner diameter of column was then calculated using following equation:
4𝐴𝑐
𝐷𝑖 = √
𝜋
Therefore, the diameter of the column was 11.604 ft (3.537 m)
6.4.3.2 Height of Packing section

Since the column cross-sectional area of 9.825 m2 was found and the volume of packed
column is known, the height of the packing section needed can now be calculated
through the following equation:
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑝𝑎𝑐𝑘𝑖𝑛𝑔
𝐻𝑝 = = 23.466 𝑚
𝑐𝑟𝑜𝑠𝑠 𝑠𝑒𝑐𝑡𝑖𝑜𝑛𝑎𝑙 𝑎𝑟𝑒𝑎
Since the height of every packed section is recommended not to be more than 8m to
prevent uneven distribution of down coming liquid flow. Thus, the packed bed will need
to split into 3 sections with same height. Thus, the height of each packed section is
7.822 m.
6.4.3.3 Column Internals

Liquid distributer and Redistributors
Liquid distributors are usually use in a packing column above each packing section to
provide a uniform liquid distribution with low gas pressure drop. It typically located
200mm above the packing in order to provide enough space for gas to leaving the
packing. Based on the literature review (Packed columns: Design and Performance), the
diameter of orifice was recommended to be 0.375 inch for carbon steel and the
minimum liquid level of 2 inches. The number of hole is then be calculated to be 389. A
Model 1016/1017 Trough Distributor/Redistributor is selected as liquid rate fall within
158
the operating range of this type of distributor and it is suitable for larger diameter
column
Bed limiters
Bed limiter is typically used in metal and plastic random packing column to prevent the
fluidization of the top of the bed. Most of the structured packing column do not need the
bed limiter and thus the R-402 do not need a bed limiter due to low potential of packing
displacement during upset condition.
Support plate
Every packing column need to have a support plate to carry the weight of the packing
and have high percentage of free passage for process stream in the reactor to allow
unrestricted flow of both liquid and gas stream through the support plate. The support
plate selected for this column is Model 134 support grid (Packed Tower Internals
Guide, 2001). This type of support grip is normally used for structured packing and
allows free and uniform passage for gas and liquid to flow. This ensures that the
packing capacity is not limited by the support plate.
Height of column
The height of each section of column was shown in following table, the height between
each column internal are taken from literature (Packed Tower Internals Guide, 2001)
Table 6.4.3.3.1: Height of each section of the column

Component Value, m
Inner diameter 3.537
thickness of insulation 0.050
Liquid hold up 0.595
Total height of bed 23.466
Height of each head without insulation 0.897
Height of each bed 7.822
Height of each support plate 0.150
Height between Liquid level and gas feed nozzle 0.5 00
Height between support plate and gas feed nozzle 0.897
Height of manway 0.600
159
Height between top of bed and bottom of distributor 0.200

height of distributor/distributor 0.300
Height between top of redistributor and next support plate 0.750
Height of distributor bottom to liquid feed 0.450
Height of distributor bottom to bottom of head 0.801
Height of cylindrical shell 29.409
Total height with head 31.303

The operating pressure and temperature of R-402 are 7 atm and 60℃ respectively and
the design pressure and temperature are set at 7.7 atm and 85 ℃ respectively. The
mechanical design of R-402 will be done based on this design condition.
6.4.4.1 Column shell thickness

Based on ASME BPV Code (Sec.VIII D.1 Part UG-27), the wall thickness of the
cylindrical shell can be calculated using following equation:
𝑃𝑖 𝐷𝑖
𝑡=
2𝑆𝐸 − 1.2𝑃𝑖
where the maximum allowable stress, S which will be used for carbon steel (SA-516)
shell is 118 N/mm2 at temperature range from -30 ℃ to 250℃. Thus, the shell thickness
of column is determined to be 13.586 mm with 2mm of corrosion allowance. The detail
calculations are shown in Appendix A6.4.5.
6.4.4.2 Selection of column head and thickness

Based on Towler and Sinnott (2009), torispherical head is more economical for column
up to pressure of 15bar. However, besed on the equation from ASME BPV Code, the
head thickness calculated for torispherical head is much thicker than ellipsoidal head.
Thus, a ellipsoidal head will probably be the more economical column head for this
condition. The equation and calculation result of these 2 type of head are shown below:
0.885𝑃𝑖 𝑅𝑐
Torispherical head: 𝑡= = 20.440𝑚𝑚
𝑆𝐸−0.1𝑃𝑖
𝑃𝐷
𝑖 𝑖
Ellipsoidal head: 𝑡 = 2𝑆𝐸−0.2𝑃 = 11.548 𝑚𝑚
𝑖
160
Since the wall thickness for whole column should be constant, the larger thickness from
cylindrical shell of 13.586 mm is chosen for the thickness of whole column. The detail
calculations are shown in Appendix A6.4.6.
6.4.4.3 Nozzle sizing

The sizes of the nozzles on the column are determined based on the pipe size of the
process stream involved in this column. The pipe size of the process stream can be
determined by using volumetric flow rate and fluid velocity. Based on Towler and
Sinnott textbook, maximum gas and liquid velocity are 30m/s and 3 m/s respectively.
The optimum velocity of fluid can be found by fluid density based on the table
developed by Simpson (1968). The equations of each steps of pipe sizing are shown
below:
𝑣𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒

𝑐𝑟𝑜𝑠𝑠 𝑠𝑒𝑐𝑡𝑖𝑜𝑛𝑎𝑙 𝑎𝑟𝑒𝑎 𝑜𝑓 𝑝𝑖𝑝𝑒 =
𝑓𝑙𝑢𝑖𝑑 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦
4×𝑐𝑟𝑜𝑠𝑠 𝑠𝑒𝑐𝑡𝑖𝑜𝑛𝑎𝑙 𝑎𝑟𝑒𝑎 0.5

𝐼𝑛𝑛𝑒𝑟 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟 𝑜𝑓 𝑝𝑖𝑝𝑒 𝑎𝑡 𝑎 𝑔𝑖𝑣𝑒𝑛 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦 = ( )
𝜋
The inner diameter calculated for a given velocity will then scale up to the nearest
standard nominal pipe size (Pipe Dimensions and Weights, 2013). The results of the
calculation are shown below and the detail calculations are shown in Appendix 6.4.10.
Table 6.4.4.3.1: Result of nozzle sizing

Parameter Gas Inlet Gas Outlet Liquid Inlet Liquid Outlet
Schedule 40 40 40 40
Nominal pipe size, in 24 24 3.5 3.5
Outer pipe diameter,
609.6 609.6 101.6 88.9
mm
Thickness, mm 17.4 17.4 5.7 5.5
Inner pipe diameter, mm 592.2 592.2 95.9 83.4
Actual velocity, m/s 19.795 17.960 2.697 2.786
6.4.4.4 Weight Load

The table below has shown the summary of weight loading of the packing column
reactor. The detailed calculations are shown in Appendix A6.4.7.
161
Table 6.4.4.4.1: Result of Weight load

Component Weight, kN
Shell of Column 429.345
Insulation 41.675
Packed bed 193.882
Caged ladder 10.587
Platform 124.695
Total Weight without liquid 800.184
6.4.4.5 Stress Analysis

The results and equation of the stress analysis are shown in following table. The
detailed calculation of stress analysis is shown in Appendix A6.4..7.
Table 6.4.4.5.1 Result of stress analysis

Stress Formula Result , N/mm2
𝑃 𝐷𝑖
Longitudinal stress 𝝈𝑳 = 50.117
4𝑡
𝑃 𝐷𝑖
Hoop stress 𝝈𝒉 = 100.234
2𝑡
𝑊
Dead weight stress 𝜎𝑤 = 𝜋×(𝐷 +𝑡)×𝑡 5.280
𝑖
Bending stress 𝜎𝑏 = ±
𝑀𝑥 𝐷𝑖
( 2 + 𝑡) ±16.788
𝐼𝑣
Resultant longitudinal 𝜎𝑧,𝑢 = 𝜎𝐿 − 𝜎𝑤 + 𝜎𝑏 61.625

stress (upwind)
Resultant longitudinal 𝜎𝑧,𝑑 = 𝜎𝐿 − 𝜎𝑤 − 𝜎𝑏 28.049
stress (downwind)
Greatest difference between σh − 𝜎𝑧,𝑑 72.185
principle stresses
𝑡
Critical buckling stress 𝜎𝑐 = 2 × 104 (𝐷 ) 76.234
𝑜
Maximum compressive σ𝑚𝑎𝑥 = 𝜎𝑤 + 𝜎𝑏 22.068

stress
The calculation of stress analysis is justified when:
162
1. The greatest difference between principle stresses < maximum allowable stress
of a material (118.N/mm2)
2. The maximum compressive stress on the vessel < critical buckling stress
6.4.4.6 Hydrostatic testing

A similar calculation method as stress analysis will be used in hydrostatic testing of
packing column reactor (R-402). During the hydrostatic testing, the packed column will
be filled with liquid and thus the total weight of the column has changed.
The result of the hydrostatic testing is shown in following table and detailed calculation
is shown in Appendix A6.4.8.
Table 6.4.4.6.1: Result of Hydrostatic testing

Stress Formula Result , N/mm2
𝑃 𝐷𝑖
Longitudinal stress 𝝈𝑳 = 50.117
4𝑡
𝑃 𝐷𝑖
Hoop stress 𝝈𝒉 = 100.234
2𝑡
𝑊
Dead weight stress 𝜎𝑤 = 𝜋×(𝐷 +𝑡)×𝑡 18.397
𝑖
Bending stress 𝜎𝑏 = ±
𝑀𝑥 𝐷𝑖
( 2 + 𝑡) ±16.788
𝐼𝑣
Resultant longitudinal 𝜎𝑧,𝑢 = 𝜎𝐿 − 𝜎𝑤 + 𝜎𝑏 48.508

stress (upwind)
Resultant longitudinal 𝜎𝑧,𝑑 = 𝜎𝐿 − 𝜎𝑤 − 𝜎𝑏 14.932
stress (downwind)
Greatest difference between σh − 𝜎𝑧,𝑑 85.302
principle stresses
𝑡
Critical buckling stress 𝜎𝑐 = 2 × 104 (𝐷 ) 76.234
𝑜
Maximum compressive σ𝑚𝑎𝑥 = 𝜎𝑤 + 𝜎𝑏 35.185

stress
The calculation of stress analysis is justified when:
163
1. The greatest difference between principle stresses < maximum allowable stress
of a material (118.N/mm2)
2. The maximum compressive stress on the vessel < critical buckling stress
6.4.4.7 Skirt Support

A straight cylindrical skirt is selected as the vessel support of packing column reactor.
Skirt support is recommended to use for tall vertical column. A 2m height of skirt
support with 10 mm of thickness was used to do the initial calculation of skirt design.
The result of the calculation is shown in following table and the detailed calculation is
shown in Appendix A6.4.11.
Table 6.4.4.7.1: Properties of Skirt support.

Parameter Result
Height of support, m 2
Thickness, mm 12 ( with 2mm corrosion allowance)
Maximum compressive stress, N/mm2 50.476
Maximum tensile stress, N/mm2 18.521
Maximum Design Compressive Stress, N/mm2 70.143
Maximum Design Tensile Stress. N/mm2 75.65

6.5 Distillation column D-501

6.5.1 Definition of design specification
The distillation column D-501 is one of the columns designed to separate methanol
from water and other impurities so that it is recycled back as a reactant for the
regeneration of methyl nitrite and help reduces the cost of feedstocks. The methanol
leaves the column as a distillate product and enters a second distillation column for
further purification to ensure high quality of reactant and to prevent the build-up of
164
impurities in the regeneration process. Water and other remaining impurities will be
removed as bottom products and is collected in the waste tank for wastewater treatment.
D-501 is a tray distillation column, and the design of equipment will focus on the
conceptual and mechanical design of column and the column internals. D-501 operates
at a pressure of 4.8 atm and temperature ranging from 108.2°C to 122.1°C. Higher
pressure is required for this process due to a small difference in the boiling points of
methanol and water. Properties of process streams across D-501 are shown in Table
6.5.1.1 below.
Table 6.5.1.1: Properties of process stream across D-501

Stream Feed (stream 55) Distillate (stream 58) Bottoms (stream 56)
Temperature (°C) 60.1 108.2 122.1
Pressure (atm) 5.0 4.8 4.3
Component mass flowrate (kg/hr)
Dimethyl oxalate 212.8 0.0 212.8
Carbon monoxide 4.2 4.2 0.0
Nitric oxide 1.9 1.9 0.0
Methyl nitrite 698.2 698.2 0.0
Toluene 81.5 81.5 0.0
Dimethyl carbonate 54.2 19.0 35.2
Nitrogen 1.7 1.7 0.0
Water 3919.8 887.3 3032.5
Methanol 40782.2 35845.8 4936.4
Nitric acid 1474.0 667.0 807.0
Total 47230.6 38206.6 9024.0
The individual component balances for each component are taken from Aspen
simulation. Reflux ratio of 0.45 and boil-up ratio of 5.6 is determined. Methanol leaves
the column at a purity of 93.8wt% which will be further increase once it leaves the
second distillation column. D-501 is also equipped with a partial condenser (E-502) and
a kettle reboiler (E-503) with Dowtherm 4000 30% ethylene glycol and saturated steam
at 10 barg as the heat transfer utilities. The kettle reboiler (E-503) will be included as a
minor equipment.
6.5.2 Basis of performance

6.5.2.1 Approach of designing distillation column
Conventional distillation process is chosen since it mainly involves the separation of
methanol from water. Tray column is chosen due to its ability to handle a broad range of
165
flowrates and its ease of maintenance. There are traces of DMO and DMC that comes
from the DMO synthesis process which enters the MN regeneration process as well as
MN and nitric acid produced in the MN regeneration process. The feed stream contains
the liquid product mixture from 2 reactors and it has a temperature of 17.2°C and
pressure of 3.45 atm after mixing the 2 streams. Detailed calculations will be shown in
Appendix A6.5.
6.5.2.2 Selection of material

Stainless steel 304 is chosen as the material for the distillation column and the internal
trays. This is due to the presence of nitric acid in the process stream which is corrosive
in carbon steels. Using stainless steel 304 in the presence of nitric acid is also better
choice as nitric acid helps to increase the corrosion resistance of stainless steel with its
powerful oxidising nature (British Stainless Steel Association, 2017). Stress analysis
were conducted on stainless steel 304 and it can be concluded that it is able to support
the dead weight of loading including the liquid hold up.
Insulation layer for distillation column is selected to be mineral wool with aluminium
cladding. Mineral wool is widely used in the industrial application (Thermal Insulation
Association of Southern Africa, 2001) with its resistance to moisture. Aluminium is
chosen for its high corrosion resistance and the ease of welding and forming wherever
needed.
6.5.2.3 Internals
Among the 3 available types of plates, sieve tray is used for D-501 due to large flowrate
of 47230.6 kg/hr fed into the column. Aside from that, it is the cheapest option that
gives the lowest pressure drop and it is comparatively easy to maintain.
6.5.2.4 Design calculations (key equations and assumptions)

Step 1: Determination of light key and heavy key component
In the process where water and methanol are the main components, methanol will be the
light key component as it has a lower density compared to water. This property allows
methanol to evaporate and water to be collected at the bottom of the distillation column
and send out for treatment.
Step 2: Determining density at top and bottom column

166
Table 6.5.2.4.1: Density of streams across D-501extracted from simulation

Temperature (°C) Density (kg/m3)
Feed 111.6 592.768
Distillate 108.2 4.697
Bottoms 122.1 421.064
The distillate density in Table 6.5.2.4.1 does not take account for the density of liquid
present in the vapour flowrate leaving the rectifying section since the distillate is in
vapour state. The liquid density can then be calculated by extracting data of the mass
fraction for each component multiply with their respective density (refer to A6.5).
Likewise, the bottoms density does not include density of vapour present in the liquid
flowrate leaving the stripping section as the bottoms is in liquid state. Hence, density of
vapour can be calculated using the same method as mentioned earlier (refer to A6.5).
Table 6.5.2.4.2: Density at rectifying and stripping section

Liquid density (kg/m3) Vapour density (kg/m3)
Rectifying (top) section 742.304 4.658
Stripping (bottom) section 419.802 5.930
Step 3: Determine column diameter
Few assumptions were made to determine the column diameter. After a few iterations,
the distillation column is designed at 75% flooding at the maximum flowrate with a
downcomer area at 13% of total area. The maximum vapour flowrate is the main factor
that determines the size of the column which is calculated based on the cross sectional
area of column. From the calculations, the top column requires a larger diameter of 2.03
m whereas the bottom column only requires a diameter of 0.28 m (due to a smaller
vapour flowrate). Thus, the final diameter for the column is set to be 2.1 m.
Step 4: Provisional plate design (trial plate layout)
Once a column diameter is set, the downcomer area and the net area can be calculated.
Downcomer area = 0.13 × column area
Net area = column area − downcomer area
Active area is calculated to determine the hole area which is assumed to be 13% of the
active area after iterations. Assumptions on weir length and height, hole diameter and
plate thickness are carried out for testing.
167
Table 6.5.2.4.3: Properties of trial plate

Weir length 1.63 m
Weir height 50 mm
Hole diameter 6 mm
Plate thickness 3 mm
Step 5: Check for weeping
The minimum design velocity (weeping velocity) is calculated based on the maximum
liquid flowrate. The goal is to ensure that the operating minimum vapour velocity
exceeds weeping velocity. Initially set to 10%, the hole area is increased to 13% of the
active area to satisfy the requirement.
Step 6: Check for plate pressure drop
Pressure drop for each plate is calculated to be 263.4 mm liquid, and total pressure drop
of the column is calculated to be about 4741 mm liquid (0.46 atm).
Step 7: Checking for downcomer backup
Downcomer area and plate spacing should be designed to prevent the liquid level from
exceeding the top of outlet weir as this would cause the column to flood. In addition to
that, the downcomer backup should be smaller than the limit (half of the plate spacing
and weir height). After a few iterations, using a plate spacing of 0.9 m and weir height
of 50 mm will gives a backup value of 0.437 m which is smaller than the limit of 0.475
m to prevent flooding. Downcomer residence time is calculated to be 5.0 s.
Step 8: Checking for entrainment
Velocity of maximum vapour flowrate and percentage flooding is calculated. Ideally the
max percentage flooding should be lower than the design percentage flooding, which
was set to 75%. Fractional entrainment smaller than 0.1 is preferred.
Table 6.5.2.4.4: Entrainment result

Max vapour velocity 1.09 m/s
Percent flooding 70%
Fractional entrainment 0.061 < 0.1
Step 9: Perforated area
168
Plate layout including perforated area and calming zone is designed. Hole pitch is
calculated and checked. Based on the calculation, lp/dh is found to be 2.51 which is in
the range of 2.5 to 4.
Step 10: Determining number of holes
The area for one hole is calculated which is used to calculated the number of active
holes in a plate. The number of holes is calculated to be 11785 holes on the sieve plate.
6.5.3 Mechanical design

6.5.3.1 Stress calculation
Step 1: Define design pressure and temperature
Operating pressure of the column is 4.8 atm whereas operating temperature is within the
range of 108.2°C to 122.1°C. Design pressure is set to 10% higher of operating
pressure, which is 5.28 atm. The design temperature is set to 125°C.
Step 2: Selection of material
Stainless steel 304 is chosen. Table 6.5.3.1.1 shows a summary of SS304 properties
based on ASME 2010 code.
Table 6.5.3.1.1: Summary of SS304 properties

Max tensile Min yield Max Max allowable
Material Grade
strength strength Temperature stress (at 125°C)
Stainless 304 515 MPa 205 MPa 816°C 107 MPa
steel
Step 3: Selection of head
Torispherical head is chosen for D-501 as the operating pressure is below 15 bar.
Step 4: Thickness of wall
Since the wall thickness of torispherical head is calculated to be larger than the
cylindrical wall thickness, the column wall thickness is chosen to be 9 mm.
Step 5: Height of column
Table 6.5.3.1.2: Height of column

Height of total trays (no. of trays × plate thickness) 0.06 m
Height of total plate spacing (plate spacing × (no. of trays + 1)) 17.40 m
169
Height of torispherical head 0.68 m

Height of vessel at tangent line 17.46 m
Height of vessel 18.14 m
Height of vessel (including skirt support of 2 m) 20.14 m
An allowance of an extra plate spacing of 0.9 m is provided to account for liquid hold
up and other fittings such as nozzles.
Step 6: Determine dead weight load
Mineral wool and aluminium cladding are used for insulation purpose therefore the
weight of material used is considered in the dead weight of vessel. Caged ladder is also
used to access the platforms that have an additional diameter of 0.7 m.
Table 6.5.3.1.3: Dead weight of vessel

Weight of shell + fittings 100.28 kN
Weight of plates 74.81 kN
Weight of insulation layer 20.98 kN
Weight of torispherical heads 6.04 kN
Total dead weight of vessel 202.1 kN
Step 7: Determine the wind load
The wind speed in Johor is approximately 24.1 km/h. A factor of 3 is considered to

account for sudden wind gust. Wind loading per length is calculated to be 976.25 N/m
and bending moment of distillation column is calculated to be 148720.27 Nm.
Step 8: Stress analysis
Stress analysis is required to check if the material and wall thickness can withstand the
weight load and the wind load. Calculated stresses are tabulated in Table 6.5.3.1.4.
Table 6.5.3.1.4: Calculated stresses

Stresses (N/mm2)
Hoop stress 62.42
Longitudinal stress 31.21
Dead weight stress 3.39
Bending stress 4.75
Resultant upwind stress 32.57
Resultant downwind stress 23.07
Max difference of stresses (downwind) 39.35
Critical buckling stress 85.0
Maximum compressive stress 8.1
170
Maximum allowable design stress 107.0
The maximum difference in stresses occurs at the downwind side and this value is
smaller than the maximum allowable design stress. Aside from that, the maximum
compressive stress is also calculated to be lesser than the critical buckling stress.
Therefore, design is satisfactory.
6.5.3.2 Hydrotesting calculation

Hydrotesting is required to check if the design of distillation column can withstand the
maximum force exerted when the column is fully filled with water. Stress analysis is
carried out again in this condition.
Table 6.5.3.2.1: New dead weight of column for hydrotesting

Weight load without water 202.1 kN
Weight load in fully filled condition 611.2 kN
New weight load 813.3 kN
Table 6.5.3.2.2: Stress analysis for hydrotesting

Stresses (N/mm2)
Hoop stress 62.42
Longitudinal stress 31.21
Dead weight stress 13.64
Bending stress 4.75
Resultant upwind stress 22.34
Resultant downwind stress 12.82
Max difference of stresses (downwind) 49.6
Critical buckling stress 85.0
Maximum compressive stress 18.39
Maximum allowable design stress 107.0
Both criteria are met, thus design is satisfactory.
6.5.3.3 Design for support

Skirt supports are chosen to be used for distillation column since it is one of the
commonly used supports for tall towers, aside from bracket supports. This is due to its
suitability for supporting tall towers that is likely to experience wind loading. Aside
from that, skirt support does not impose any additional loads acting on the vessel shell.
An initial skirt thickness of 9 mm is used to check if the design is satisfactory.
Table 6.5.3.3.1: Skirt design calculation

Bending stress 5.9 N/mm2
171
Dead weight stress (hydraulic test) 10.2 N/mm2

Dead weight stress (operating) 3.4 N/mm2
Maximum tensile stress 2.5 N/mm2
Maximum compressive stress 16.2 N/mm2
Maximum allowable design stress 138 N/mm2
Joint factor 0.85
Base angle of skirt 90°
Limit for tensile stress 104.9 N/mm2
Limit for compressive stress 96.7 N/mm2
The maximum tensile and compressive stresses are lower than their respective limit
values. Thus, the design is satisfactory.
6.5.3.4 Nozzle sizing

The inner diameter of each nozzle is calculated based on the volumetric flowrate of the
streams. The respective fluid velocity is found based on the respective density of each
stream.
Table 6.5.3.4.1: Nozzle sizing for each stream

Nominal pipe size Thickness
Nozzle Schedule ID (mm) OD (mm)
(mm) (mm)
N1 100 40 102.26 114.3 6.02
N2 750 40 742.94 762.0 9.53
N3 150 40 154.08 168.28 7.11
N4 400 40 381 406.4 12.7
N5 125 40 129.9 143.00 6.55

6.6 Hydrogenation Reactor R-601

6.6.1 Definition of the Design and Specifications
The detailed design equipment involved in DMO hydrogenation process is the
hydrogenation reactor (R-601). Hydrogenation reaction occurs in the reactor whereby
DMO dissolved in methanol reacts with hydrogen to produce monoethylene glycol
(MEG) and methanol. By-products such as ethanol and water are also produced in a
small amount. Catalysts are also used in the reaction to enhance the selectivity of the
products.
172
The reactor R-601 operates at a temperature and pressure of 210oC and 25 bar(a). The
mass flowrate of the process, which consists of mainly DMO, methanol and hydrogen is
55.67 kg/s. The outlet of the process consists of mainly MEG, unreacted hydrogen,
methanol and a small amount of by-products. As the reaction is a highly exothermic
reaction which has a heat duty of 9.02 MW, multi-tubular reactor is employed as R-601.
The process is allocated to the tube side whereas the coolant is allocated to the shell side
of the reactor. The coolant used is Dowtherm G, which has a temperature of 40 oC and 3
bar(a). The mass flowrate of the coolant is 93.05 kg/s to maintain the reactor at the
temperature of 210oC. The temperature of the outlet of the coolant is 170oC. Dowtherm
G is used as it does not vaporize at high temperature and does not cause fouling of the
heat exchanger.
The type of catalyst employed in the reaction is CuNi/Si-O2, which has a lifetime of 6
months. The catalyst is chosen as it gives a selectivity of 99% and deters formation of
poisonous by-products such as 1, 4-Butanediol. The weight hourly space velocity
(WHSV) of the catalyst is assumed to be 4 h-1, which gives the mass of catalyst required
as 50.1 tonne. Based on the mass of catalyst required, the number of tubes required is
calculated to be 1892. The specification of the tube will be discussed in the following
section.
6.6.2 Basis of Performance

The type of reactor involved is a 1 shell 1 pass reactor, which is of type AFT based on
TEMA (1999). Triangular pitch of tube pitch 0.063 m is chosen as the fluid in shell side
is relatively clean. The sizing of the shell side of the equipment is performed based on
Kern’s method. The vessel has a shell diameter of 3 m, with a 25% baffle cut and
spacing of 0.9 m. The baffle thickness is assumed to be 15 mm. The number and
diameter of tie rod is also assumed to be 10 and 0.016 based on the optimum condition
as stated in Sinnott & Towler (2009). From the specification, the velocity of Dowtherm
G at the shell side is 0.17 m/s. Based on Kern’s method, the pressure drop across the
shell side of the reactor is 0.12 bar(a).
For tube side, the specification of the tube chosen for the reactor has an outer diameter
of 50 mm and a wall thickness of 2.1 mm based on Sinnott & Towler (2009). The tube
of OD 50 mm is chosen to minimize pressure drop across the tube. As the residence
173
time required for the process is 1.5 s and the velocity of the process is assumed to be 10
m/s at the inlet, hence a reactor with a length of 15 m is required. According to Ergun
equation, the velocity of process across each tube is 1.63 m/s, which gives a pressure
drop of 1.97 bar(a) across the tube.
The specification of tubesheet is discussed in the following section. A sieving mesh is

attached to the tubesheet to hold the catalyst in place.

6.6.3.1 Material of Construction
As R-601 is considered a pressurized vessel, the detailed design of the reactor is
performed according to ASME BPV Code Section II Part D (2010). The material
chosen for the construction of both the shell and tube of the reactor is stainless steel 304
Grade A. The maximum allowable stress of the material is 2080 bar at 210 oC.
6.6.3.2 Stress Analysis

The stress analysis of R-601 is performed and attached in Appendix A6.6.2. Based on
ASME BPV Code (2010), the minimum thickness of the shell is calculated to be 21
mm. Mechanical design and stress analysis of the vessel is then and it is found that the
maximum stresses on the vessel exceed the maximum allowable stress of the vessel.
The shell thickness is then gradually increased and the stress calculation is iterated until
a shell thickness of 25 mm. The loadings and stresses analysis of R-601 are tabulated as
shown below.
Table 6.6.3.2.1: Loads and stresses of R-601

Dead weight of vessel (kN) 4724.67
Bending moment (Nm) 553519.94
Hoop stress (MPa) 149.36
Resultant upwind stress (MPa) 57.84
Resultant downwind stress (MPa) 51.58
Greatest stress difference (MPa) 200.93
Critical buckling stress (MPa) 164.63
Maximum compressive stress (MPa) 23.104
174
6.6.3.3 Internals
In R-601, a tubesheet is bolted to both ends of the shell to hold the tubes in place. A
sieving mesh of thickness 2 mm is also attached to the tubesheet to support the packed
catalyst. The sieve diameter, xsv is 250 𝜇m, slightly smaller than the size of catalyst,
which is 300 𝜇m.
The type of tubesheet used in the shell is floating head, constructed with stainless steel
304 Grade A which has a maximum allowable stress of 208 MPa (ASME, 2010). The
tubesheet, which has a diameter of 2.99 m, has a thickness of 150 mm. The tubesheet is
attached to 10 tie rods of diameter 16 mm.
The tubesheet is bolted to the closure of the shell with nuts. Bolt diameter of 100 mm is
chosen. As a result, 28 bolts are required with a bolt spacing of 326 mm.
6.6.3.4 Pipe Sizing

The pipe sizing calculation is performed and attached in the appendix. The pipe and
nozzle sizing for all inlets and outlets are tabulated below. The material used in
construction of pipe and nozzle is chosen to be stainless steel 304 Grade A according to
ASME (2010), to avoid hydrogen embrittlement. The flange rating and pipe schedule is
also taken into consideration in pipe sizing (Sinnott & Towler, 2009).
Table 6.6.3.4.1: Pipe sizing of R-601
Nominal Pipe Size Pipe ID Pipe OD

Nozzle Schedule
(mm) (mm) (mm)
PRV (N1) 20 40 21 27
Process outlet (N2) 1050 40 1048 1067
Atmosphere (N3) 20 40 21 27
Coolant inlet (N4) 850 40 848 864
Coolant outlet (N5) 850 40 848 864
Process inlet (N6) 850 40 848 864
Drain valve (N7) 20 40 21 27
Steam purging (N8) 20 40 21 27
Nitrogen purging (N9) 20 40 21 27
175
Table 6.6.3.5.2: Flange details of R-601 (ASME BPV Code, 2010)

Flange Diameter
Flange Flange OD Number
Nozzle thickness of bolts
Rating (mm) of bolts
(mm) (mm)
PRV (N1) 150 229 22 6 25
Process outlet (N2) 2500 1219 68 10 100
Atmosphere (N3) 150 229 22 6 25
Coolant inlet (N4) 300 1016 68 8 100
Coolant outlet (N5) 300 1016 68 8 100
Process inlet (N6) 2500 1016 68 8 100
Drain valve (N7) 150 229 22 6 25
Steam purging (N8) 150 229 22 6 25
Nitrogen purging
150 229 22 6 25
(N9)
6.6.3.5 Heads and Support

The type of closure the vessel endorses is 2:1 ellipsoidal head as for pressurized vessel,
it is more economical to use an ellipsoidal head (Sinnott & Towler, 2009). The closure
has a height of 0.75 m and a thickness of 20 mm including corrosion allowance. The
diameter of the closure is same as the vessel, which is 2.99 m.
Brackets are chosen as the support of the vessel as the vessel is in vertical orientation
and the brackets are able to withstand the loadings and stresses of the vessel. The
material chosen for the construction of the brackets is stainless steel 304 Grade A
(ASME, 2010). The number of brackets required is 6, which the detailed drawing is
attached in the appendix. The length of the plate and the bracket is assumed to be 200
mm. Based on Sinnott & Towler (2009), the plate thickness is calculated to be 65 mm.
6.6.3.6 Insulation
As R-601 involves a highly exothermic reaction, insulation is required to ensure the
safety of the surrounding and the plant. For R-601, mineral wool of 50 mm thick is
chosen as the layer of insulation as it has a low density, which minimizes the mass load
on the vessel. Based on the stress analysis, the weight of insulation is calculated to be
176
9.1 kN. Besides, the thermal conductivity of mineral wool is 0.035 W/m.K, which is
relatively low.

6.7 Vacuum Distillation Column (D-703)

6.7.1 Definition of the Design and Specifications
For this section, a detailed description of the design of a tray vacuum distillation column
(D-703) will be explained. The main purpose for this column is to separate the product,
Ethylene Glycol (EG), from Methyl Glycolate (MG) and other impurities. A good
design is required to ensure that the product obtained is at a high purity. The purity
required for the EG is to be 99.9% and above. Hence, this column will be design in such
a way that the purity required can be achieved.
This column is set to vacuum condition due to EG having a high boiling point. Hence,
the vacuum condition will reduce the boiling point of EG and ensure that the product
leaving the column is in liquid phase instead of vapor phase. At a vacuum condition of
0.8bar, the boiling point of EG is at 191oC (trimen.pl, 2017) and the temperature of the
column outlet was obtained to be 189oC which is lower than the boiling point. By using
Aspen Plus, a purity of 99.99% was achieved.
Now, the column is to be designed under the same conditions and to ensure that the
purity of the column can be achieved. The detailed design will be mainly according to
the steps stated in the Chemical Engineering Design book (Sinnott & Towler, 2009).
The details for all the stream entering and exiting the column will be shown in A6.1.
6.7.2 Basis of performance

6.7.2.1 Number of stages and reflux ratio
Firstly, the number of stages for this column was obtained from Aspen Plus by using the
RadFrac column. The number of stages obtained was 13 stages and it was also
determined that the feed stage would be at the 9th stage. Next, the reflux ratio was also
obtained from Aspen Plus which is 45.70.
177
6.7.2.2 Design procedure

All detailed calculations are done in A6.1.
Step 1: Selection of plates
There are several different types of plates that can be selected from such as sieve plate,
bubble-cap plates, and valve plates. When selecting plates, a few criteria must be
considered to ensure that the plate chosen is the most suitable for the column. The
criteria for selecting plates are the cost, the pressure drop, the capacity, etc. For this
column, sieve plate was chosen. This is because sieve is considered to be the cheapest
and also sieve plates has the lowest pressure drop among the other plates (Sinnott &
Towler, 2009).
Step 2: Determine the diameter of column
After selecting the type of plates, the first thing to determine is the diameter of the
column. The main assumption for this step is that the design was assumed for 85%
flooding at maximum flowrate and that the downcomer area was to be 12% of the net
area. Then, the diameter was obtained by first determining the superficial vapor velocity
then followed by the cross-sectional area. After obtaining the cross-sectional area, the
column diameter can then be obtained. The column diameter was calculated to be 2.6m.
Step 3: Designing the plate
With the diameter known, the plate is then to be designed. The hole area was first
assumed to be 10% of the active area. After doing the calculations, it was also
determined that the liquid flow is a cross flow. The calculated design parameters are
tabulated in the table below:
Table 6.7.2.2.1: Summarised design parameters for plate design.

Parameters Values
Column Area, Ac 5.31 m2
Downcomer Area, Ad 0.64 m2
Net Area, An 4.67 m2
Active Area, Aa 4.04 m2
178
Hole Area, Ah 0.404 m2

Weir length 1.98 m
Since this is a vacuum distillation column, a few more assumptions were made for the
weir height, hole diameter, and plate thickness.
Weir height, hw = 9mm

Hole diameter, dh = 8mm
Plate thickness = 5mm
Step 4: Hole design
Firstly, the width for calming zone was chosen to be 100mm and support ring to be
75mm. According to Sinnott, these dimensions are suitable for column with diameter
larger than 1.5m. By using the geometry of the plate to calculate the unperforated area,
the perforated area, Ap, was also then obtained to be 3.27m2. After obtaining the
perforated area, the hole pitch can then be determined with the following equation,
𝐴ℎ ℎ𝑜𝑙𝑒 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟 2
= 0.9 ( )
𝐴𝑝 ℎ𝑜𝑙𝑒 𝑝𝑖𝑡𝑐ℎ
The hole pitch was then determined to be 21.59mm. The hole arrangement was chosen
to be triangular pitch. This is because a triangular pitch can provide a more compact
arrangement which is suitable for large number of holes. The number of holes per plate
for this column was determined to be 8028 holes.
Step 5: Head selection
The most common type of head selected is usually the torispherical head as it is the
cheapest for column operating under 10bar. Since the highest pressure for this
distillation column is 0.8 bar, hence torispherical head was chosen.
Step 6: Determine thickness of vessel

179
For the thickness calculation, two different equations will be used. One equation for the
wall thickness of vessel and the other equation for the thickness of the head. The
equations are as follow,
𝑃𝑖 𝐷𝑖
𝑡= = 𝑤𝑎𝑙𝑙 𝑡ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠
2𝑆𝐸 − 1.2𝑃𝑖
0.885𝑃𝑖 𝑅𝑐
𝑡= = ℎ𝑒𝑎𝑑 𝑡ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠
𝑆𝐸 − 0.1𝑃𝑖
With the two equations above, the wall thickness was calculated to be 12.94mm
whereas the head thickness was 22.79mm. Since the head thickness is larger, hence the
whole column will follow the thickness of the head. A 2mm corrosion allowance is then
added to the thickness. Hence, the final thickness is set to be 25mm.
Step 7: Determine the height
The height of the distillation column is the sum of the two heads and the cylindrical
height of the column. The cylindrical height will consist of the tray heights, overhead
height, and sump volume height. The total height was then determined to be 14.27m.
The height for the heads was calculated to be 0.6m per head.
Step 8: Check weeping and entrainment
The weeping velocity was first calculated using the following formula and also Figure
11.32 from Sinnott (pg 724)
[𝐾2 − 0.9(25.4 − 𝑑ℎ )
𝑢ℎ =
(𝜌𝑣 )2
The weeping velocity was calculated to be 16.22m/s. Then, the actual minimum vapor
velocity was calculated by assuming 80% turn-down which was obtained to be
32.21m/s. With the actual minimum vapor velocity being significantly higher than the
weeping velocity calculated, it indicates that weeping will be very unlikely to occur for
this column.
For entrainment, the percent flooding was calculated to be 76.3. The value calculated
was well below the early assumed 85%. This indicates that flooding is also highly
unlikely to occur in this column.
180
6.7.3 Mechanical design

Step 1: Design temperature and pressure
The highest temperature and pressure for this distillation column is 189.33 oC and
0.8bar. To obtain the design temperature, 50oC will be added to the operating
temperature whereas for design pressure, it will be 10% higher than the operating
pressure (Sinnott, 2009). Hence, the design pressure was determined to be 239.33oC
whereas design pressure was 0.88bar.
Step 2: Material selection
For this distillation column, it operates at 189.33oC and 0.8bar. For such moderate
conditions, carbon steel is usually chosen as the material. However, for this column,
corrosive material is present. Hence, carbon steel will not be chosen whereas stainless
steel 304 would be used instead. The properties of the materials which will be used for
calculations are tabulated below,
Table 6.7.3.1: Summarized properties of stainless steel 304.

Material Stainless Steel 304
Minimum Tensile Strength, MPa 517.11
Minimum Yield Strength, MPa 206.84
Maximum Temperature, oC 815.56
Maximum Allowable Stress, MPa 88.94
Step 3: Determine the total weight of vessel
The weight of a column can be made up of many different components. However,

before getting to the total weight, the thickness for insulation was first determined.
Mineral wool was chosen as the insulation material and a thickness of 50mm was
assumed to be the thickness with a 1mm aluminium cladding.
With the thickness of insulation known, the total weight can then be obtained. The first
weight would be the dead weight which is calculated based on the following equation,
𝑊𝑣 = 𝐶𝑤 𝜋𝜌𝑚 𝐷𝑚 𝑔(𝐻𝑣 + 0.8𝐷𝑚 )𝑡
181
Then, the weight of plates and contents was calculated followed by the weight of heads
and lastly the weight of insulation. The weights calculated are tabulated in the table
below,
Table 6.7.3.2: Summarised table of total weight.

Dead weight, kN 282.17
Weight of plates and contents, kN 82.82
Weight of heads, kN 59.06
Weight of insulations, kN 13.61
Total, kN 437.67
Step 4: Stress Analysis
The bending moment due to wind load is not that important as the column’s height is
less than 20m. The maximum wind speed in Malaysia was determined to be 25.2km/h
and the value obtained for wind load was 11.87kN/m which can be considered to be
very small. Next, the stress due to internal pressure is then calculated. The values
obtained are all tabulated in the table below,
Table 6.7.3.3: Values obtained for stresses due to internal pressure.

Hoop Stress, σh 45.76 MPa
Longitudinal Stress, σL 22.88 MPa
Dead Weight Stress, σw 2.12 MPa
The resultant longitudinal stress, σz, was then determined for both upwind and
downwind. The values obtained was 20.79MPa for upwind and 20.73MPa for
downwind. The greatest difference between the hoop stress and resultant longitudinal
was determined to ensure that it is lesser than the maximum allowable stress. The
greatest difference was determined to be in the downwind side with a value of
25.03MPa which is well below the maximum allowable stress of 88.9MPa.
Lastly, the elastic stability was checked. This is done by first determining the critical
buckling stress and compare it to the max compressive stress of the column. The critical
buckling stress was determined to be 183.02MPa whereas the maximum compressive
182
stress was only 2.15MPa. Since the maximum compressive stress is well below the
critical buckling stress, hence the design for this distillation column was considered to
be satisfactory.
Step 5: Support calculations
For the supports, a straight skirt design was selected for the column. By using the wind
load determined earlier, the bending moment at the base of the skirt is then determined
to be 18.42kNm with a column height of 16.27m including the height of the skirt. The
skirt thickness was first assumed to determine whether the criteria for the skirt design
can be satisfied.
Criteria for skirt design,
𝑡𝑠𝑘
𝜎̂𝑠 (𝑡𝑒𝑛𝑠𝑖𝑙𝑒) ≤ 𝑆𝑠 𝐸𝑠𝑖𝑛𝜃 𝑎𝑛𝑑 𝜎̂𝑠 (𝑐𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒) < 0.125𝐸𝑌 ( ) 𝑠𝑖𝑛𝜃
𝐷𝑠
The σs(tensile) and σs(compressive) was determined to be 0.15MPa and 0.16MPa

respectively. Then, it was determined that the criteria were satisfied with a skirt
thickness of 23mm. Hence, a 2mm corrosion allowance was added to the thickness
which then gives a skirt thickness of 25mm.
Step 6: Nozzle sizing
The nozzle was sized based on the velocity of fluid through the pipeline. The velocity
was determined by relating density to velocity (Sinnott, 2009). The pipe area was
determined first to obtain the diameter of the nozzle.
𝑚𝑎𝑠𝑠 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒

𝑎𝑟𝑒𝑎 𝑟𝑒𝑞𝑢𝑖𝑟𝑒𝑑 =
𝑑𝑒𝑛𝑠𝑖𝑡𝑦 × 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦
The DN of the pipe is then determined after obtaining the diameter of the pipe. After
getting the DN, the actual diameter of the pipe is then calculated to check whether it is
suitable to be used.
𝑎𝑐𝑡𝑢𝑎𝑙 𝑑𝑖𝑎𝑚𝑒𝑡𝑒 = 𝑜𝑢𝑡𝑒𝑟 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟 − (2 × 𝑡ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠)
The above steps were the same for all nozzles exiting and entering the column. The
nozzle sizing for this distillation column is then tabulated in the table below.
183
Table 6.7.3.4: Nozzle sizes for distillation column.

Nozzle Label Nozzle Description Nominal Size, mm
N1 Feed Inlet 50
N2 Pressure Relief Valve 15
N3 Top Gas Product 450
N4 Level Indicator Sensor 32
N5 Bottom Liquid Product 50
N6 Drain Nozzle 65
N7 Top Reflux Inlet 32
N8 Bottom Reboiler Inlet 300
N9 Manhole 700
N10 Manhole 700
N11 Manhole 700

184
185
186
186
187
188
ITEM Hydrogenation
SERVICE REACTOR DESIGN CODE TEMA 1999
DESCRIPTION reactor
EQUIPMENT MULTITUBULAR TYPE: AFT
R-601 TYPE
LABEL REACTOR ORIENTATION: VERTICAL
SHELL SIDE TUBE SIDE
FLUID ALLOCATION DOWTHERM G Hydrogenation Process
FLOW RATE 93.05 kg/s 55.67 kg/s
FLUID PROPERTIES IN OUT IN OUT
TEMPERATURE 40⁰ C 170⁰ C 210⁰ C 110⁰ C
DENSITY 1031.40 kg/m3 1031.40 kg/m3 0.9 kg/m3 0.9 kg/m3
1.22 x 10-5
VISCOSITY 0.007 Pa.s 0.007 Pa.s 1.22 x 10-5 Pa.s
Pa.s
SPECIFIC HEAT 1.616 kJ/kgK 14.510 kJ/kgK
THERMAL CONDUCTIVITY 0.124 W/mK 0.272 W/mK
PRESSURE 3 bar(a) 25 bar(a)
VELOCITY 0.17 m/s 1.63 m/s
PRESSURE DROP 0.12 bar 1.97 bar
FOULING RESISTANCE 0.0002 m2K/W 0.0002 m2K/W
FILM TRANSFER COEFFICIENT 257.08 W/m2K 107.60 W/m2K
HEAT DUTY 9022.43 kW
OVERALL HEAT TRANSFER
70 W/m2K
COEFFICIENT
REQUIRED HEAT TRANSFER AREA 955.46 m2
DESIGN DATA
STAINLESS NOTES:
MATERIAL FOR TUBE AND MAX ALLOWABLE
STEEL 304 N1: Nozzle for pressure
SHELL PRESSURE: 2080 bar
GRADE A relief valve
TUBES
N2: Nozzle for process
DESIGN PRESSURE 27.5 bar(a) PITCH TRIANGULAR
NO. OF TUBE/PASS 1892 PITCH DISTANCE 63 mm outlet
BUNDLE N3: Nozzle to
PASS 1 2887 mm atmosphere
DIAMETER
LENGTH 15 m DIAMETER 50 mm O/D N4: Nozzle for coolant
THICKNESS 2.1 mm TOTAL TUBES 1892 inlet
SIZE FOR TUBE PIPE N5: Nozzle for coolant
34 in. FLANGE RATING 2500
(SCHEDULE 40) outlet
SHELL
DESIGN PRESSURE 3.3 bar (a) DIAMETER 2987 mm O/D
N6: Nozzle for process
NO. OF SHELL/PASS 1 inlet
BAFFLE SPACING 896 mm N7: Nozzle for drain
THICKNESS 25 mm
SHELL-BUNDLE valve
100 mm BAFFLE CUT 25%
CLEARANCE N8: Nozzle for steam
purging
SIZE FOR SHELL PIPE
34 in. FLANGE RATING 300 N9: Nozzle for nitrogen
(SCHEDULE 40)
purging
COMPANY NAME DATE
G6 ENGINEERING 27 SEPTEMBER 2017
DRAWN BY: AI HSIN CHEW CHECKED BY: ALEXANDER LIM
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Chapter 7:
Piping &
Instrumentation
Diagram
202
7.1 Pressure swing adsorption columns V-102 and V-103 to separate

hydrogen from synthetic gas
7.1.1 Control philosophy
Operating pressure of both adsorption columns are at 1.14 MPa while the operating
temperature is 30 °C. Flow transmitters FT-101 and FT-102 are connected to the inlet
and outlet stream going into the columns respectively. The transmitters transmit the
signal to flow indicators FI-101 and FI-102 which sends the data to a Flow Ratio
Controller FFC-101. The flow ratio controller will analyse the information obtained and
compare the value to the set point given. If the set point if not achieved, it means that
the column being pressurised is slowly to lose its efficiency due to the adsorbent
material being occupied. FFC-101 will control sets of three-way valves to open and
close in order to direct the gas flow into another column. The aforementioned
pressurised column will now go through depressurisation to release the gas adsorbed to
the materials and to be used again for later process. This process is repeated to generate
a steady amount of product gases.
7.1.2 Advanced control strategy

A Safety Instrumentation System (SIS) is implemented in the two columns as the
operating pressures are high. Pressure transmitters PT-101 and PT-102 transmits data of
pressure in each column to a pressure indicator PI-101. If the pressure of any column is
getting higher than the set point, the PAH-101 alarm will first go off and operator
intervention will be needed to find the cause of the increase in pressure. If the problem
is not solved in time and the pressure increases again, the PAHH-101 alarm will go off
and the SIS-101 system will be activated. SIS-101 controls SV-101 to close and SV-102
to open which directs all of the gas flow into a flare system to ensure no inlet gas flow
to the columns. The pressure safety valves on each column is also designed to burst at
an operating pressure 5% above the set point value and is directed to a flare system. The
operation will require a shut down and the pressure safety valves will need to be
replaced.
203
7.1.3 Standard operating procedure (SOPs) – Maintenance for V-102 and

V-103
When the columns undergo maintenance procedures, the inlet gas flows into the
columns are stopped. The nozzle located on every part of the column will be blocked by
blinds to ensure no leakage into the adsorption columns. The nitrogen gas inlet nozzle is
opened, and nitrogen purge stream enters the columns and leaves through another flare
outlet nozzle. The harmful gases are required to be purged out completely before any
maintenance can be done for both columns and any human intervention inside of the
columns.
7.1.4 Piping and instrumentation diagram

The piping and instrumentation diagram (P&ID) for this section is attached at the end of
the chapter.
7.2 Distillation column D-101 to separate carbon monoxide from

toluene
The operating pressure of distillation column D-101 is at 101.3 kPa and the operating
temperature of the column is at 111 °C which is above the boiling point of toluene. The
flow of Carbon Monoxide (CO) and Toluene from S-101 is in liquid form and flows to
heat exchanger E-106 to be heated up to the operating temperature of D-101 prior to
entering it. Saturated steam at 10 barg enters the tube side of E-106 and heats the
process fluid going through the shell side of the heat exchanger. The shell side outlet of
E-106 is connected to a temperature control loop which consists of TW-101, TT-101
and TIC-101. When the temperature of the outlet stream does not meet the required set
point, it is first detected by the thermowell which transmit a signal through the TT-101
to the TIC-101 which is connected to the Control Valve, TCV-101. A pneumatic signal
is sent from the controller to the valve to adjust the opening of the valve, in turn
adjusting the flow rate of steam flowing into E-106 to either increase or decrease the
temperature of the process stream coming out. The temperature outlet of E-106 is
crucial in aiding the separation of components in the following distillation process.
As for D-101, the first control is a level indicator controller LIC-101 connected to the
column through a level transmitter LT-101. This level controller helps ensure that the
204
liquid level in the distillation column does not build up to a certain level that can cause
backflow into the nozzle of the reboiler inlet into the column by adjusting the flowrate
of the bottoms into the reboiler E-108. A temperature control loop which consists of
TW-102, TT-102 and TIC-102 will also be connected to the reboiler inlet stream into
the distillation column. When the temperature of the vapor stream coming out of the
reboiler deviates from the set point, TIC-102 will control the flowrate of the saturated
steam going into the reboiler E-108 by adjusting the opening of TCV-102. A Flow Ratio
Controller FFC-101, is also connected to the vapor outlet stream of reflux drum T-101
through a flow transmitter FT-101, and the liquid outlet stream of the reflux drum
through FT-102. This flow ratio control helps ensure that the reflux ratio of the
distillation column is at a constant value. If the ratio does not meet the set point, FFC-
101 will send a pneumatic signal to the flow control valve, FCV-101 to adjust the
flowrate of the condensate reflux going back into the distillation column to change the
reflux ratio. For the kettle reboiler E-108, an alarm system is also implemented. The
alarm system consists of LT-102, LI-101, LAL-101 and LAH-102. When the liquid
level in the reboiler gets too high or too low, the alarm will sound, and the level of the
liquid will be indicated to the operator. A LAH-101 alarm is also connected to CO
Storage Tank TK-101 to indicate when the liquid level gets too high in the storage tank.

The alarms implemented in this P&ID will all require operator intervention when it is
sounded. When the LAH-101 alarm connected to the TK-101 sounds, the operator
needs to drain the liquid through the drain valve at the bottom of the tank. There is also
a level indicator to determine when the draining procedure needs to be stopped. TK-101
stores mainly CO gas and sounding of the alarm is not likely to happen under normal
operating conditions as there is only little liquid build-up. As for the alarm system
connected to reboiler E-108, when the liquid level high alarm sounds, the operator
needs to drain the liquid level through the drain valve on the shell side of the reboiler.
This is to ensure that the liquid level in the reboiler stays roughly constant and will not
affect the efficiency of the boil up. There will also be bypasses for all streams
containing any control valves to account for maintenance on the control valves. The
control systems will adjust to any change in set point value of more than 10% for good
205
separation between components. The control valves are also designed to be either fail
close or fail open in the case of an emergency.
7.2.3 Standard operating procedure (SOPs) – Shut down and maintenance

for D-101
During shut down or maintenance of distillation column D-101, all pumps will be
closed as the operation is seized. For any maintenance procedure that requires operators
to enter the distillation column, the column would first undergo some operating
procedures. The control valves and isolation valves connected to the column will first
be closed to stop any flow of streams entering the column. Ring spacers will also be
switched to block off all of the nozzles on the distillation column to ensure no fluids are
entering the column in the case of leakage. The drain valve is first opened up to drain all
the liquid contained in the sump volume part of the column. Next, the nozzles for
nitrogen purge and to flare system will be opened open to allow the column to undergo
nitrogen purging to remove all the harmful CO gas in the column. After the column is
free of CO gas, the column is then safe to be manually cleaned from the inside to
remove any clogging or blockage that might lead to the shut-down of the process.

the chapter.
7.3 Syngas separation COSORB absorber and flash evaporator

To ensure a maximum efficiency in the Plant operation, a sufficient and effective
control philosophy is required. Operating conditions such as temperature and pressure
need to be maintained at optimum condition not only to maximize the operation but also
to prevent any possible leakage, flooding, or any rupture within the plant which can lead
to accidents which could resulted in disasters.
The level of the liquid inside column V-101 is controlled by connecting a Pneumatic
Control valve to a Liquid Indicator Controller in the operating room which have
transmitted the data from the transmitter. The Pneumatic valve controls the output flow
of the column. When the Liquid Level within the column reaches a level beyond the
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normal operating condition, the Pneumatic Control Valve would command the liquid
output of the column to flow in a higher rate thus reducing the liquid level within the
column.
In a heat exchanging equipment it is extremely crucial to monitor the operating

temperature of the equipment. To control the temperature from being either too high or
too low, a Pneumatic Control Valve attached to the either the heating or cooling media
is connected to a Temperature Indicator Controller. In E-101, a Temperature
Transmitter (TT-101) which reads the temperature of the heat exchanger would transmit
the data the to the control room which would then control the inlet flow rate heating
media of saturated steam. The inlet flow rate of the heating media can be adjusted
accordingly to ensure that the temperature is within the operating range.
C-101 is used to increase the pressure of the process fluid. In a case in which the wanted
pressure change is not achieved the Pressure Transmitter, PT-101 would send the data
to the control room which would then command the Process Fluid to be recycled and
eventually be recompressed in order for the process fluid achieve the wanted pressure
change.
7.3.2 Advanced control system

A Ratio Control (RC-101) is implemented prior to the V-101 column. In order for
optimum operating condition, the ratio of the two-inlet stream going into the column
need to be maintained within 1:4 ratio for the syngas stream going into the column. A
flow transmitter is connected to both of the inlet streams. Syngas stream is defined as
the “wild” stream between the two-inlet stream as it is the main feedstock to the column
whereas toluene solvent stream is the controlled stream. A Ratio Controller signal is
connected to both of the transmitter which would then allow the reading of the flow
ratio between the two streams. In a case where the wanted ratio is not achieved, it is the
Toluene Solvent steam that is being controlled and adjusted, this is to ensure that the
amount of feedstock syngas is not disturbed.
207
7.3.3 Standard operating procedure (SOPs)

7.3.3.1 Start-up procedure
A common start up-procedure for an absorber column is to go through the pressuring up
process prior to liquid introduction into the column. This is due to the fact that a
pressurized liquid will have a higher boiling point at higher temperature, this would
eliminate the potential of large thermal stressed due to liquid flashing occurring at
relatively low temperature. These thermal stresses can lead to brittle failure and
unnecessary joint or flange leaks.
Another common start up procedure is the process of cleaning the column from any
undesirable material which can potentially affect operation. This is done by purging
cleaning by wither steam or nitrogen stream which would is able to purge these
impurities.
7.3.3.2 Shut down procedure

The first step is shut down procedure of an operating column such as V-101 is to close
all potential heating or cooling sources into the column. Draining all the liquid within
the column using a drain valve such as DV-117 to remove any liquid within the column.
It is also important to ensure all the control valve as well as the drainage and control
valves are all closed once the draining process have completed.

the chapter.
7.4 Dimethyl oxalate synthesis

CO streams, nitrogen and methyl nitrite (MN) streams are fed into the reactor R-201 at
a temperature of 140°C and pressure of 3.2 barg. CO and MN are both reactants whilst
nitrogen is acting as diluent since high concentration of MN will lead to explosion. The
reaction is moderately exothermic hence constant cooling of the reactor is required in
order to prevent run-away reaction from occurring which leads to catastrophic events or
explosion due to explosive properties of MN in the reactor.
208

The temperature of the reactor is maintained at 140°C by manipulating the flowrate of
Dowtherm 4000 entering the multi-tubular reactor R-201. The temperature of the
reactor is controlled by a feedback control system labelled as TT-202 and TIC-202,
which will send a continuous pneumatic signal to FCV-201 to adjust the flowrate of
DowTherm 4000. The flowrate of CO and MN entering the reactor is measured and
controlled by a flow transmitter FT-209, FT-206, FIC-206 and FIC-208 which will send
a continuous pneumatic signal to FCV-208 and FCV-206 to control the flowrate
entering the reactor. The reactor R-201 has two special hose to allow for maintenance
purposes to clean the tube side of the reactor. Another set of temperature control system
is placed at the direct outlet of the reactor, TI-211, TALL-206 and TAHH-207 to
monitor the outlet temperature, this will be further explained in section 7.3.2. Since the
reaction is very much dependent on the reaction pressure which is 3 barg, a pressure
control system is installed on the reactor to control the pressure from building up.
All the inlet and outlet streams of the reactor R-201 is being isolated by an isolation
valve during maintenance. Drain valve DV-219 is placed at the bottom of the reactor to
drain any Dowtherm 4000 that is still accumulated inside the reactor during
maintenance. Vent valve IV-244 is placed directly at the top of the reactor and is
normally in closed position since vent valve is only required to be in open position
during maintenance purposes. Special hoses that are connected to the reactor consist of
steam and nitrogen whereas steam is used to clean the tube side of the reactor and
nitrogen is to depressurize the system. 2 sets of pressure safety valve (PSV-203 and
PSV-204) is being installed at the top of the reactor to overpressure of the reactor by
relieving the process streams to the flare system. 2 sets of pressure relief valve is used to
ensure that the reactor is always protected by one pressure relief valve even when the
other is undergoing maintenance due to malfunctioning.
Both the compressor, C-201 and C-202 is protected by an anti-surge control and an anti-
choke control. The pressure difference between inlet and outlet of the compressor
measured by (PT-205, PT-206 and PT-217, PT-218) is being sent to a pressure
differential indicator control (PDIC-205 and PDIC-213) whereby the flowrate of the
recycle line can be controlled by (PFC-205 and PFC-213) to prevent surging occurring.
209
To prevent choking from occurring, the flowrate entering the compressor is being
measured by a flow transmitter and an indication controller will send a continuous
pneumatic signal to pneumatic valve to control the flowrate. Since compressor is
relatively expensive compared to other equipment, hence the control system of the
compressor is relatively complex to prevent failure of compressors.
7.4.2 Advanced Control Strategy

The normal operating temperature of the reactor is 140°C, which will be measured by
TT-202 and controlled by TIC-202. During an event where the temperature inside the
reactor becoming higher than the operating temperature, the flowrate of Dowtherm 4000
will be controlled by (FCV-201) to allow for higher flowrate of Dowtherm into the
reactor to decrease the pressure. The pneumatic control valve (FCV-201) is controlled
by the continuous pneumatic signal sent by TIC-202. Since the operating pressure of the
reactor is not categorized as relatively high pressure so the pressure control of the
reactor is relatively simpler. The pressure of the reactor will be measured by PT-210
which will send the electrical signal to PI-201. During an event where the pressure of
the reactor reaches a pressure higher than the expected pressure, PAHH-204 will sound.
The operator can then manipulate the flowrate of reactant flowing into the reactor.
However, if at the same time the temperature of the product leaving the reactor reaches
a temperature higher than the expected, TAHH-207 will be sound. Combination of these
2 alarms will then be controlled by safety instrumental system which will then send a
pneumatic signal to emergency shutdown valve (ESV-201 and ESV-202) to prevent
ANY flow of reactant entering the reactor. Furthermore, the pressure safety valve will
have a setpoint of 4.653 barg which is 10% below the design pressure, if the pressure of
the reactor exceeds the setpoint of the pressure safety valve the process stream inside
the reactor will be automatically released to the flare tower in order to depressurize the
reactor.
7.4.3 Standard operating procedure (SOPs) during maintenance

During maintenance of equipment, all the process stream lines are being isolate with an
insolation valve to prevent any flow going into the equipment. Drain valve and vent
valve attached on the equipment will then be manually turn on to vent or drain any
process liquid into a temporary storage tank or to vent system. A special hose will then
210
be connected to the equipment to supply steam to wash and nitrogen to depressurize the
system. All the pneumatic control valves are protected by a bypass line and isolation
valves to ensure the flow of process stream is continuous even the pneumatic valve is
undergoing some maintenance.

The piping and instrumentation diagram (P&ID) for DMO synthesis is attached at the
end of the chapter.
7.5 Methyl nitrite (MN) synthesis

The MN synthesis process involved a series of reaction that using nitric oxide (NO),
oxygen and methanol as reactant. A total of three reactors are involved in the MN
synthesis process to increase overall yield of the product. The first reactor (R-401) will
undergo the NO oxidation reaction to produce a certain amount of nitrogen dioxide
(NO2). The main reactants for first reactor are oxygen and NO. The product synthesized
in R-401 is one of the main reactant for subsequent reaction in R-402 and R-403. Both
R-402 and R-403 undergo same reaction for MN synthesis using NO2, NO and
methanol as reactant. The R-403 is operating in series with R-402 to further convert the
unreacted component into desired product. The desired product and unreacted gaseous
by-product from R-403 will pass to subsequent DMO synthesis process as one of the
main reactant. The liquid by-product and unreacted methanol will send to subsequent
dehydration process to recover the unreacted methanol in the process stream.
7.5.1 Control Philosophy

The oxygen and nitrogen gas are compressed to 7 bar by entering compressor C-402
and C-401 before entering the reactor (R-401). These compressors are protected from
surge by using a pressure differential controlling devices (PDIC-401 and PDIC-402) to
measure and control the pressure difference across the pump. If a low differential
pressure is detected by pressure transmitters (PT-401 and PT-402), The pressure
controller (PV-401 and PV-402) will open to allow the process fluid to recycle back to
the inlet of compressor. Since the temperature of gases increase sharply after
compression, these 2 reactants will then mix with the nitrogen monoxide rich stream
from C-202 of previous section and enter a heat exchanger (E-401) to cooled down to
100℃ before entering the R-401. The cooling medium involved in this cooling process
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is Dowtherm 4000. The desired temperature of the process stream is achieving by

controlling the flow rate of the Dowtherm entering E-401 from tube sides.
The flow rate of the reactants that fed into R-401 is controlled by a flow controller
(FIC-401) to maintain the production rate of NO2. If the flow transmitter (FT-401)
detects a high variation of flow rate of reactant, the controller valve (PV-405) will
adjust the opening of valve to maintain a desired flow rate. The NO 2 from R-401 will
mixed with other unreacted gas and enter the R-402. The methanol which is one of the
main reactant for R-402 is send from a holding tank (TK-401). A level control device is
implemented in TK-401 control the liquid level in the tank. When the level sensor (LE-
401) detect a large liquid level drop or rise, the level transmitter (LT-401) will send
signal to the level indicator controller (LIC-401) to adjust the flow rate of the outlet
stream by the level control valve (PV-406). The alarm system integrated with level
indicator controller (LIC-401) will activate when the liquid level exceeds the designed
liquid level of the tank. This liquid level control system is also installed in reactors, R-
402 and R-403 to control the liquid hold up level.

Since the reaction involved in MN is exothermic, a cooling jacket will be installed to
each reactor to maintain the operating temperature of the reactor. The temperature of the
reactor will be controlled by adjusting the cooling water flow rate into the reactor. Since
most of the reaction in this process involved large amount of gaseous reactant,
especially for R-401, a pressure indicator controller (PIC-405) will be used instead of
temperature controller as the pressure of gases in the reactor will highly increase with
high temperature. The pressure controller will adjust the flow rate of cooling water in
cooling jacket through control valve (PV-404). If the pressure in the reactor exceeds the
upper limit of operating pressure, pressure alarm system will activate so that the
operator on duty can take immediate action to overcome this condition.
7.5.3 Standard operating procedures (SOPs) during maintenance

During the maintenance of equipment, the isolation valve installed at inlet and outlet
pipeline will be closed while the drain valve will be opened. For example, the isolation
valve (IV-405 and IV-421) will close to prevent any further transfer of process stream
into heat exchanger E-401. The drain valve (DV-407) and isolation valve (IV-420) will
212
open to allow the process stream leaving the equipment. Since the gases involved in E-
401 is toxic and flammable, it cannot directly vent to atmosphere. A flare system will be
used to treat these hazardous process gases. When the IV-412 opened, nitrogen gas that
used for maintenance will enter E-401 to purge out excess process gases through the IV-
410 to flare system. A similar procedure of purging with nitrogen will be done during
start up process of the equipment to remove other gases in E-401.

The P&ID of methyl nitrite synthesis is attached at the end of the chapter. The detailed
calculation of pipe sizing is shown in Appendix A7.
7.6 Separation of required reactants (methanol and DMO)

Two sections from the process flow diagram will be discussed in this section which is
the dehydration of methanol and the DMO purification. Dehydration of methanol
consists of two distillation columns D-501 and D-502 and distillation column D-301 is
used for purification of DMO. All three columns are having similar controls which are
discussed in the next few sections.

The feed that goes into D-501 is a mixture of liquid that is separated from 2 MN
reactors (R-401 and R-402) with a temperature of 17.5°C. The feed stream is sent to a
heat exchanger (E-501) to heat up the process fluid to 60°C to maintain at saturation
temperature. The temperature of the outlet is controlled by the saturated steam rate. If
outlet temperature is lower than the set point, a signal will be sent to the temperature
control valve (PV-501) to increase the flowrate of the saturated steam into the heat
exchanger. The heated feed stream will enter a pump to increase the pressure to 5 atm.
Temperature of the distillation column is an important parameter for better separation.
Therefore, the temperature at the bottom column needs to be regulated by controlling
the reboiler temperature, which is controlled by the flowrate of saturated steam. The top
product will flow to a condenser where the outlet temperature is controlled by the
flowrate of Dowtherm 4000. Level control is implemented at the bottom part of column
to prevent flow of liquid back to reboiler. Flow control is added to maintain the reflux
rate back into the column. Similar controls were used for D-502, where methanol is
further dehydrated.
213
Purification of DMO is carried out after synthesis before entering the hydrogenation
reactor (R-601). This is to ensure better quality MEG is produced. The feed coming
from gas liquid separator has a temperature of 20°C and a pressure of 1 atm. The feed is
pump to a pressure of 2 atm and this is so to get a better separation of DMO from other
components. Controls of distillation column D-301 is similar to the other 2 columns.

Feedback control is commonly used for control loops. Indicators are all located in the
main control room to alert the operators in case of any accident. Pressure relief valves
are mounted on distillation columns to prevent pressure build-up which has a set point
of 5.28 atm. A level high alarm is placed at the bottom of the distillation column to
prevent the back flow of liquid back into the reboiler. Spare pumps are placed to
maintain normal operations during maintenance.
7.6.3 Standard operating procedure (SOPs)

7.6.3.1 Start-up and shut down
During start-up, valves that are controlling the coolant streams with be opened for 10
minutes. This is done to prevent overpressure and avoid potential damage to the heat
exchangers. At the same time, open the valves to allow the cold process fluid to flow
into the reboiler. Once the procedure is complete, saturated steam will then be allowed
to flow in due to its high pressure and temperature.
For shutdown process, valves for controlling saturated steam flow should be close first
to prevent any further increase in temperature of process fluid. After that the process
fluid valves are closed and the coolant is allowed to flow for a longer time period to
decrease the temperature of the equipment.
7.6.3.2 Maintenance
Steam and nitrogen will be supplied for maintenance purpose. Nitrogen is first supplied
through pipeline and unit operations to purge out all process fluid. Drain valve will then
be open to drain all liquids. Steam is used in cleaning and sterilization of the unit
operations.
214

The P&ID for the DMO purification and dehydration of methanol is attached at the end
of the chapter.
7.7 DMO hydrogenation

Piping and instrumentation diagram (P&ID) on DMO Hydrogenation section is drawn
based on the process flow diagram (PFD) with details of pipe sizing as well as the
control system and valves used in the process to ensure smooth operation. The P&ID of
this section starts from the inlet of DMO and methanol mixing tank (MX-601) to the
outlet of MEG gas-liquid separator (S-601). The main equipment involved in the P&ID
include MX-601, E-601, R-601, E-602, S-601 as well as pumps and compressors.

During normal operation, a highly exothermic reaction takes place in R-601. As R-601
needs to maintain at the operating temperature of 210 oC, Dowtherm G is constantly
being fed to the reactor to efficiently remove heat and maintain the desired temperature.
Hence, the flowrate of Dowtherm G is controlled by PV-606, TT-610 and TIC-610. TIC
is controlled by TAH and TAL, where PV-606 will open and close based on the
respective control system.
Pressure is also another factor to be taken into consideration when designing R-601. As
R-601 is a pressurized vessel at 25 bar(a), the operating condition is monitored by a
safety instrumented system. As PT-609 detects and transmits signals to SIS-609, it
analyses the signal and closes an emergency shut down valve (SD-602) when PAHH is
hit. This will stop the process from going into R-601, then relief valve (RV-603) will
come into play whereby it opens to release the pressure in the vessel.
7.7.2 Advanced control philosophy

As compressors require a minimum flowrate going in to prevent surge, hence an anti-
surge line is added to the control system for all the compressors. For C-601, a flow
transmitter (FT-607) transmits signals to anti surge controller (ASC-607). When a
minimum flowrate is detected, FALL is triggered and ASC-607 will open anti surge
valve (ASV-601) in order to allow a small amount of the process to be recycled to the
inlet of the compressor.
215
7.7.3 Standard operating procedure for maintenance

During the maintenance of the hydrogenation reactor R-601, all the process is shut
down and purged using nitrogen. MV-607 is opened manually to allow nitrogen to be
sent to R-601. When all the process fluid is purged, the remaining liquid in the vessel is
vented through drain system (DV-620). For steam cleaning, MV-608 will be opened
manually to allow steam to enter. After the maintenance, a manual valve (MV-609) is
opened to allow air to enter the vessel before starting the process.
As for equipment which requires replacement such as pump (P-601), the pump motor is
first shut off. The remaining liquid in the pump is then vented through a drain system
(DV-605). A spectacle blind is then inserted into the isolation valve (IV-605 and IV-
607) and the valves are then closed. The pump can then be safely removed. Meanwhile,
IV-608 and IV-610 is opened and the spectacle blind in the valve is then removed. The
motor of the spare pump (P-602) is then switched on to allow the process to continue.
However, it is important that IV-609 is opened during the start-up of the pump in order
to remove air present in the pump through the pump casing.

The P&ID drawings for the entire section of DMO hydrogenation are attached at the
end of the chapter.
7.8 Monoethylene glycol (MEG) purification

Three distillation columns are required to obtain high purity of MEG product. The last
column used for the purification process will be a vacuum distillation column. The
control philosophy explained will be for the last column as the control philosophy for
all three columns are quite similar except for the vacuum condition.

The operating pressure for the third distillation column, D-703, is 0.8bar which
indicates that it is in vacuum condition. This vacuum condition is obtained with the help
of a steam ejector, SE-701. There will be a pressure indicator (PI-718) before the steam
ejector which indicates the pressure inside the column. The steam ejector is then
controlled from MV-701 to ensure that the pressure within the column is 0.8bar. This is
important as pressure plays a vital role in determining the purity of the product. Due to
216
the importance of pressure, a high or low alarm was also installed at PI-718. The
temperature of the column is also another important parameter to control. The
temperature at the bottom of the column will be controlled using the flowrate of the
saturated steam entering the reboiler (E-709). After the reboiler, there will be a cooler
(E-710) to cool the product for storage. A temperature controlled (TIC-726) was
installed to control the temperature of product by controlling the flowrate of Dowtherm
G Cold. Next, a level control with high or low alarm was also installed at the bottom
liquid outlet. This is to ensure that overflow does not occur at the bottom of the column
and also to ensure that there is no sudden decrease in the liquid level.
The top condensed product (Methyl Glycolate, MG) will first be stored in a reflux drum
(RD-703) where a level control with high or low alarm (LIC-721) will be available to
prevent the drum from overflow or being empty. Next, a flow control with high or low
alarm (FIC-717) is also installed to control the flow rate of the reflux stream. This is to
ensure that the reflux ratio will remain constant and not fluctuate. After the distillate,
there will be a cooler (E-708) to cool the waste before discharging it to waste. A flow
indicator (FI-722) was placed before the cooler to ensure that the flow into the cooler is
steady. A temperature controlled (TIC-723) was also installed to control the temperature
of waste by controlling the flowrate of Dowtherm G Cold.
7.8.2 Advanced control strategy for D-703

For each controller, there will be individual high low alarm except for the temperature
control after the coolers (E-708 and E-710). The high low alarm is set to go off if the
required condition is off by ±10%. All the control valves are design to Fail Open (FO)
during an emergency except for the control valve (CV-715) for the flow rate of
saturated steam which will be Fail Closed (FC). During an emergency, the liquid within
the column will all be drained out through DV-744. Then, the flowrate of Dowtherm G
Cold into E-710 would be increase to further cool down the product to be stored. During
emergency, products obtained will be considered as off-specs product.
7.8.3 Standard operating procedure (SOPs) for D-703

7.8.3.1 Start-up procedure
Before start-up of plant, all control valves will be changed to manual mode until a
steady state inside the column is achieved. First, the column will be purged with
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nitrogen via MV-707. This is to remove oxygen gas from the column. After purging,
steam will be introduced via MV-706 to remove the nitrogen gas. The vacuum
condition is then created by adjusting the steam ejector until a pressure of 0.8bar is
achieved. The off-specs product is used as the feed into the column first until all
conditions are in steady state. After achieving steady state, the off-specs product will be
drained out through DV-744 and a new fresh feed will be supplied into the column.
7.8.3.2 Shutdown procedure

When shutting down, the spectacle blind for feed stream will be closed followed by the
shutdown of all the pumps. The flow of saturated steam into the reboiler will also be cut
off. All the control valves will then be closed except for CV-713. CV-713 is left open to
ensure that all liquid within the column has been drained out through DV-744. The
steam ejector is then shut down by closing MV-705. Finally, all remaining drain and
isolation valves will be closed.
7.8.4 Controls for distillation column D-701 and D-702

The controls for D-701 and D-702 are quite similar to D-703 except for the absence of
steam ejector as D-701 and D-702 is not operating under vacuum. There will be a
temperature differential indicator for both columns as the temperature difference within
the column is quite high from 103.89oC – 258.79oC for D-701 and 181.54oC –
249.73oC for D-702. The rest of the controls and SOPs for D-701 and D-702 are
considered similar to D-703. As for S-701, there will only be a level control with high
or low alarm (LIC-705) as the level within the separator must be controlled to prevent
overflow or a sudden decrease in level is detected which indicates that there are
problems occurring.

The piping and instrumentation diagram for all three columns will be attached at the end
of this chapter along with the pipe list data.
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231
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241
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Chapter 8: Safety
and
Environmental
Assessment
244
8.1 Introduction
This chapter focuses on the safety and environmental assessment of each section of the
plant by evaluating the safety assessment as well as the life cycle assessment (LCA) and
risk assessment. The safety assessment of each section includes inherent safety design
(ISD), hazard identification (HAZID), standard operating procedure (SOP) and the bow-
tie diagrams summarising intrinsic and extrinsic safety. The LCA investigates the
environmental impacts of monoethylene glycol (MEG) production via dimethyl oxalate
(DMO) route whereas the risk assessment summarises the key environmental emissions
as well as their respective risk ranking based on impact register.
The author of each nominated section in safety assessment, LCA and risk assessment is
tabulated below.
Table 8.1.1: Nominated section of each member for safety assessment

Major Minor Hazardous
Section Author
Equipment Equipment Scenario
Syngas Column Heat Compressor
Dzaki
Separation – PSA (V-101) Exchangers (C-101)
Yoong Reactor Heat Compressor
DMO Synthesis
Chin (R-201) Exchangers (C-201, C-202)
Methyl nitrite Reactor Reactor (R-402 Separator
Hao Yang
(MN) Synthesis (R-401) & R-403) (S-401)
DMO
Distillation Reboiler
Purification & Penny Pumps
Column (D-501) (E-503)
Dehydration
Distillation Reboiler Separator
MEG Purification Alexander
Column (D-703) (E-709) (S-701)
Table 8.1.2: Nominated section for LCA and risk assessment

Section Author
LCA Ai Hsin
Risk Assessment Koon Meng
245
8.2 Part A – Safety

8.2.1 Syngas Separation
8.2.1.1 Safety Assessment
Syngas separation is the first procedure to undergo within the plant. Carbon monoxide (CO) and hydrogen (H2) are the two raw materials
required from syngas for the production of MEG through the DMO route. The separation process to extract the two required raw materials
is relatively complex as the boiling point of the gas components within the syngas composition is similar. Therefore, the separation process
is going to go through steps which could result to potential safety being jeopardized such as, extreme temperature increase and leakage of
harmful solvents. In this section, the steps taken to reduce and limit the potential hazardous disaster as well as, enhancing safety for both
the environment and the personals surrounding the plant are summarized and discussed. operating parameters such as pressure, temperature
and flow level are continuously monitored and controlled with the appropriate control equipment, however in a case in which these
parameters deviate away from its normal condition it is important to imply an alarm system which would warn the operators of such events.
Another step which could be done to limit potential disaster is to regularly conduct maintenance on all equipment, valve, flange and
pipeline. Lastly and perhaps most importantly, the operators in charge of the plant need to well informed and educated on the Standard
Operating Procedure (SOP) of the start-up, normal operation as well as the shutdown process of the plant.
8.2.1.2 Inherent Safety Design

Table 8.2.1.2.1: Inherent Safety Design Summary
ISD
ISD Parameter Justification
Principles
The syngas feedstock to V-101 absorption column is reduced as recycled gas from the
Minimise Feedstock
vapour product from S-101 is used as feedstock
246
Cuprous Aluminium Chloride is used as the solvent used for V-101 absorption
instead of Aluminium Chloride. Cuprous Aluminium Chloride is a more efficient than
Solvent
Aluminium Chloride therefore the quantity require for an optimum absorption process
is relatively less.
Dowtherm 4000 is used as the cooling media in E-102, E-103, and E-104. Dowtherm
Substitute Cooling Media is less corrosive than Cooling Water thus it is more appropriate for the cooling
process.
COSORB (Absorption by Cuprous Aluminium Chloride) process is used for the
separation process instead of Methane Washing. The operating condition is relatively
Moderate Operating Condition moderate for COSORB as its operating temperature and pressure are 40°C and 2 atm
respectively whereas the operating and temperature and pressure for methane washing
is -169.5 °C and 21.3 atm respectively.
All the equipment, valve and flanges in the plant is labelled accordingly to limit
Equipment/Valve/Flange/Labelling
errors.
Simplify
The operators in charge must work within an appropriate duration to prevent fatigue
Appropriate working shift
and limit potential error
8.2.1.3 Hazard Identification as well as its Causes, Outcome and Mitigation

Table 8.2.1.3.1: Hazard Table for Column V-101
Type of Possible Causes Possible Outcomes Mitigation Process
Hazard
Thermal The temperature of the inlet syngas feed Skin burn could occur upon 1. Cover the column and pipeline in
Hazard and toluene solvent is excessively higher direct contact with either the which the hot process fluid is
than the design temperature of the column column or pipeline in which the present with the appropriate
due to upstream heat exchanger (E-102) hot fluid is present insulation material
malfunction. 2. Monitor the outlet temperature of
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Fire Hazard 1. Loose fittings in either pipeline or 1. Highly flammable gas such as E-101 and E-102 and maintain
valves leading to leakage of flammable H2 and Methane exposed to its temperature by controlling the
gas: the atmosphere could ignites inlet utility stream of U-101 and
 H2 (LEL-4%, UEL-75%) and starts fire. U-103 using Temperature
 Methane (LEL-5%, UEL-15%) 2. The well-being of personals Controller Indicator TIC-101 and
2. Presence of ignition sources nearby the surrounding is in danger. TIC-102
column V-101 3. Regular maintenance for the
Mechanical 1. Excessive flow of syngas feed going 1. Overpressure in column V-101 Control Valves involved, PV-
Failure/Rupture into column V-101 due to malfunction could lead to rupture 101 and PV-102
leading To of Flow Control, FCI-101 causing the 2. Major and minor pipeline 4. Regular Check-up and
Explosion pressure of the column to exceed the could undergoes potential maintenance on the Pipeline and
design pressure which could lead to rupture Valve around the Column
rupture 3. Rupture within either column 5. Ensure that the operator in
2. Faulty operation on the Pressure Relief or pipeline could lead to gases charge of operation is well
Valve. such as H2 and Methane being informed and educated on the
exposed to the atmosphere SOP of the operation thus
resulting in explosion allowing them to know then
4. Rupture and explosion can operation parameters deviates
potentially harm the well- from the normal parameters.
being of the personnel and 6. Imply an appropriate immediate
other surrounding equipment. procedure to deal with skin burns
as well as treating it.
7. Usage of Personnel Protective
Equipment (PPE) need to be
applied at all times within the
plant site.
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8. Install an appropriate first aid

and fire response procedure in a
case of emergency.
9. Immediate contact with the
nearest Fire Fighter Station and
Hospital.
10. Set-up a proper Start-up,
Maintenance and Shut-Down
Procedure.
Toxic Hazard 1. Toxic toluene solvent leakage in the 1. Toxic and poisonous 1. Ensure that the operator in
inlet of V-101 column due to loose chemicals such as Toluene charge of operation is well
fittings in either Pipeline or Valve could be exposed to the informed and educated on the
2. Faulty operation on the Pressure Relief surrounding which could SOP of the operation thus
Valve potentially harm the health of allowing them to know then
personals and operators operation parameters deviates
2. Malfunction in the Pressure from the normal parameters
Relief Valve leads to toxic 2. Usage of PPE need to be applied
gases such as CO and Methane at all times within the plant site.
being exposed to the 3. Regular Check-up and
environment. maintenance on the Pipeline and
Chemical 1. CO Rich Solvent leakage at the bottom 1. Both air and ground water Valve around the Column
Exposure outlet of the column due to Loose pollution could be resulted due 4. Monitor the Level of the Flow
Hazard Fittings in either Pipeline or Valve to either leakage of CO and within the column V-101 using
2. Drained Valves, DV-117 and DV-118 CO Rich Solvent. LIC-101 to ensure no leakage
went through malfunction have occurred.
5. Ensure Draining of fluids is done
249
in an appropriate manner without

leakage.
6. Set-up a proper Start-up,
Maintenance and Shut-Down
Procedure.
Table 8.2.1.3.2: Hazard Table for Heat Exchangers, E-101, E-102 and E-103
Type of
Possible Causes Possible Outcomes Mitigation Process
Hazard
Thermal 1. Saturated Steam at 10 Bar(g) and 1. Skin burn could occur upon direct 1. Cover the Pipeline in which the Hot
Hazard 184.123°C was fed at an excessive contact with pipeline in which the Steam is present with the appropriate
Leading to quantity to E-101 due to hot fluid is present as well as Insulation Material
Mechanical malfunction in pneumatic through leakage. 2. Imply an appropriate immediate
Failure valve(PV-101) 2. Excessive feed of Hot Saturated procedure to deal with skin burns as
2. Loose fittings in either pipe or Steam could result in the operation well as treating it.
valve leading to Leakage of Hot Temperature to exceed the Design 3. Usage of PPE need to be applied at all
Saturated Steam in U-101 the Temperature of E-101 leading times within the plant site.
pipeline. to mechanical failure.
Fire Hazard 1. Presence of Ignition sources 1. 1. The Syngas feed is made of 1. Regular maintenance for the Control
nearby Heat Exchangers such as Flammable gas such as Hydrogen Valve (PV-101)
E-101, E-103 and E-104. and Methane which could result in 2. Ensure that the operator has the
2. Loose fittings in either pipe or fire when exposed to atmosphere. necessary knowledge and skill on the
valve leading to Leakage of 2. Fire could damage both the well- SOP thus recognizing when the
Flammable Gas: being of Personals and Operators in operating parameters deviate from the
 H2 (LEL-4%, UEL-75%) charge as well as other equipment. normal condition
 Methane (LEL-5%, UEL-15%) 3. Imply an appropriate immediate
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Explosion 1. Excessive flow of Utility Stream 1. High Pressure in the Heat procedure to deal with skin burns as
Hazard into the tube side leading to high exchanger E-101 could lead to well as treating it.
pressure due to failure in control rupture and explosion. 4. Usage of PPE need to be applied at all
Valve (PV-101) 2. Pressure build up could be times within the plant site.
2. Pressure Relief Valve in the Heat excessive within the Heat 5. Install and apply the most appropriate
exchangers such as PRV-101 and Exchanger as Pressure Relief Valve Start-up, maintenance and shutdown
PRV-102 are malfunction are not able to reduce the pressure Procedure
3. Draining valves malfunction within the equipment which could 6. Regular Check-up and maintenance
4. Faulty and Inappropriate eventually result in rupture and on the Pipeline and Valve around
shutdown and maintenance explosion Heat Exchangers
Procedure 3. H2 gas exposed to the atmosphere 7. Install an appropriate first aid and fire
5. Operators mistake as SOP is not could react and forms an explosion. response procedure in a case of
followed. 4. Rupture and explosion could emergency.
damage both the well-being of 8. Immediate contact with the nearest
Personals and Operators in charge Fire Fighter Station and Hospital.
as well as other equipment.
Chemical Leakage of Process Fluid such as The Toluene Solvent is corrosive
Exposure Toluene Solvent and Syngas feed in which could damage the health of
Hazard the Shell Side of Heat Exchangers personal within the plant.
(E-101, E-102 and E-103) due to
either, Pipeline or Valve Malfunction
Table 8.2.1.3.3: Hazard Table for Compressors C-101

Type of Hazard Possible Causes Possible Outcomes Mitigation Process
Fire Hazard 1. Ignition sources located 1. Highly Flammable gas such 1. Ensure that the operator has the
nearby the Compressors as H2 and Methane exposed necessary knowledge and skill on the
251
2. Leakage of Flammable Gas to the atmosphere could SOP thus recognizing when the
such as H2 and Methane due ignites and starts fire. operating parameters deviate from the
to Loose Fittings in Pipeline/ 2. The well-being of personals normal condition
Flanges/Valves surrounding is in danger. 2. Usage of PPE need to be applied at all
3. High outlet Temperature as times within the plant site.
well as velocity due to failure 3. Regular Check-up and maintenance on
in the intercooler system the Pipeline and Valve around the
Mechanical 1. Excessive incoming flow into 1. Overpressure could lead to compressor
Failure/Explosion the Compressor leading into the compressors being 4. Install an appropriate first aid and fire
excessive pressure within the ruptured response procedure in a case of
compressor 2. Explosion of compressors due emergency.
2. Excessive internal pressure to Flammable Gas such as 5. Immediate contact with the nearest
build-up due to malfunction Hydrogen and Methane being Fire Fighter Station and Hospital.
in the drainage valve such as exposed to the atmosphere 6. Monitor the outlet Pressure of the
DV-107 and DV-108. 3. Rupture and explosion can compressors using the Pressure
3. Overpressure within the potentially harm the well- Transmitters such as PT-106.
compressor due to surge being of the personals and 7. Install a Pressure Relief Valve to
other equipment surrounding. prevent excessive pressure build up.
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8.2.1.4 Standard Operating Procedure

Start-Up Procedure
1. The first step taken before the start up procedure was to ensure that that there are no
leakage within the column by going through steam cleaning process. This is done by
closing all the valves (Isolation Valve, Bypass and Control Valve) except for IV-131
as it is fully open to allow Steam to flow into the column V-101 as well as E-101
and E-102.
2. Close IV-131 to stop steam flow and now open IV-132 to allow nitrogen flow to V-
101 as well as E-101 and E-102. At this point it is ensured that all the Vent Valves
such as DV-117 in V-101, DV-111 in E-101 and DV-114 in E-102 are open to allow
nitrogen purging. Nitrogen is used to clean and purify all the equipment from
undesired impurities and contaminants.
3. Once nitrogen cleaning and purging is finished, IV-132 is closed to stop nitrogen
Flow.
4. All control valves and alarms such as (PV-103/PV-105) and (TIC-101/LIC-101)
needs to be check, tested to ensure that they are all calibrated and installed properly.
5. During the checking and testing process all the control valves and alarms are
overridden as they need be set to manual mode.
6. Working personnel need to be placed on active stand-by mode in case of an
unexpected accident and emergency occurred during this process.
7. The availability of utility stream for E-101 and E-102 are checked to ensure
optimized cooling and heating process for Inlet Streams going into V-101.
8. Once the cleaning and checking process are completed, process fluid as well as the
utility stream flowing into E-101 and E-102 is introduced by opening IV-102, IV-
106, IV-110 and IV-112.
9. The heated toluene solvent and cooled syngas feedstock is then slowly introduced
by partially opening IV-115 and IV-116. FCI -101 and RC-101 are activated and
PV-104 is open to control the flowrate of the two streams going into the column.
10. Once the column V-101 reaches steady state obtains its operational condition which
is 2.2 bar absolute and 40°C, the column is ready for operation.
11. All isolation valves prior to column are now fully open to allow steady flow of
toluene solvent and syngas feed into the column.
253
12. All drain valves are ensured to be closed to prevent any leakages.
13. Control valves and alarms such as PV-105 and LIC-102 are now open and activated
in automatic mode for the operation procedure.
Normal Operation Procedure

1. The position of all the valves is as shown in P&ID-1-3. All control valves and
alarms are now set to automatic mode.
2. The Inlet temperature of Toluene Solvent and Syngas feed is controlled using PV-
101 and PV-102 which controls the Inlet flow of the utility stream going into E-101
and E-102 respectively.
3. The amount of Syngas and Toluene Solvent entering the column is controlled by
PV-104 control valve which also linked to Ratio Controller, RC-101 to ensure that
the ratio in which the two-inlet stream entering the column is maintained for optimal
operation.
4. To prevent flooding and control the level in which liquid is present in the column,
LIC-101 Alarms is used to indicate an event in which the level within the column
exceeds the normal parameter. PV-105 is then used to control the outlet stream of
the column allowing the liquid stream to discharge at a higher level in order for the
level to within the column to decrease and return to normal parameter.
5. Pressure Relief Valve, PRV-101 PRV-102 and PRV-103 are installed in E-101, E-
102 and V-101 respectively to relief vapour to vent in a case in which the pressure
of the equipment exceeds the design pressure.
6. Operators on site as well as the control room are given an appropriate shift duration
in to ensure optimum working condition and prevent any human error.
Shutdown procedure
1. The first step taken in Shutdown procedure is to slowly decrease the amount of
Toluene Solvent and Syngas feedstock to V-101 by partially closing IV-115 and
IV-116 using PV-104 control valve.
2. This is done to slowly decrease the pressure of the column to atmospheric pressure
and enhance safety.
3. Once this is reached, IV-115 and IV-116 are closed to ensure that there are no more
flow going in.
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4. IV-101, IV-102, IV-107 and IV-111 are also closed to ensure no inlet flow going
into E-101 and E-102.
5. E-101 and E-102 Heat Exchangers are shut down.
6. Drain valves such as DV-117 and DV-118 are then opened to remove all the liquid
content.
7. Vent valve such DV-116 is then opened to remove vapour content in the column.
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8.2.1.5 Bow Tie Diagram
Figure 8.2.1.5.1: Bow Tie Diagram for Highly Flammable Hydrogen Gas Releases
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8.2.2 DMO Synthesis

DMO production involves several processing of hazardous chemicals. CO is reacted with MN in order to produce DMO. The reaction
involved is an exothermic reaction whereby multi-tubular fixed bed reactor is used with the supply of Dowtherm 4000 to maintain the
reaction temperature at 140°C. The scope and the boundary of the safety control measure evaluation is on the Decoupling React ion to
produce DMO. The reactor, R-201 will be insulated by mineral wools to protect personnel from injuries. Several extrinsic safety measures
are detailed in this section in order to reduce the risk to an acceptable and safe operational level. Several safety control measures in this
section SOP and incorporation of process control systems, emergency processing plan, and alarm systems. Besides, all the plant operators
are required to attend the training programmes to familiarise the start-up, normal operation and shutdown procedure of the plant. A constant
maintenance across all the equipment to ensure safe operation and ensure a leakage free operation across pipelines, valves and flanges. The
inherent safety design for the production of DMO is shown below on Section 8.2.2.2. Specific hazards and mitigation measures for all the
equipment are assessed and tabulated in the section below.

Table 8.2.2.2.1: Inherent Safety Design Summary
ISD ISD
Justification
Principles Parameters
By-product Hazardous components such as methanol is eliminated and separated from the inlet stream before entering
Eliminate
reactor R-201.
Feedstock Concentration of MN is diluted with the addition of nitrogen as diluent.
Minimise Inventory The product is delivered directly via pipeline from the reactor. Hence no storage is required.
By-product The parameters of the reaction are controlled at an optimum condition to maximise the formation of DMO
257
Formation and reduce the formation of by-product.

Cooling Dowtherm 4000 is used as cooling medium in the shell side of the reactor to substitute cooling water as
Substitute
Medium Dowtherm 4000 has a higher operating temperature than water to prevent flashing of utilities.
Catalysts Catalysts required is calculated and packed in in the tube side of the reactor in a just sufficient amount.
Moderate Operating Reactor temperature is operated at a moderate reaction condition whereby temperature and pressure is
Condition maintained at 140°C and 3.5 barg.
8.2.2.3 Hazard Identification as well as its Causes, Outcome and Mitigation

Table 8.2.2.3.1: Hazard Table for Reactor R-201
Dimethyl Oxalate Synthesis, Multi-tubular Fixed Bed Reactor, R-201
Hazard Causes Potential Outcomes Mitigation Measures
Fire  Temperature control loop failures  Reactor catches fire.  Reactor is installed in between
Hazards (causes runaway reaction)  Causes thermal explosion due platform to prevent direct exposure
 Presence of ignition sources nearby. to uncontrol exothermic from sunlight.
 Leakage of process vapor from valves reaction.  Multi-tubular Reactor is used to
or flanges due to the extremely  Vessel rupture due to provide enough cooling duty.
flammable property of MN. overpressure by thermal gas  Two pressure relief valves are
expansion. installed to prevent vessel rupture.
 Injuries and fatalities (PSV-203 and PSV-204).
Explosion  Similar causes as fire hazards  Similar outcomes as above.  Temperature control loop 201 to
Hazards mentioned above.  Release of process vapor control the flowrate of Dowtherm into
 Failure of pressure relief valve causes (DMO, Nitrogen Oxide, MN the reactor.
overpressure in reactor. etc.)  Safety Instrumentation System (SIS)
 Blockage in the tube side of the reactor  Explosion injuries and is implemented (SIS-201) to shut
by catalyst. fatalities down the operation by cutting off the
 Leakage of MN reactant reactants flowing into R-201. (ESV-
258
 Uncontrolled temperature increase in 201, and ESV-202)

reactor R-201.  Regular inspection on the equipment
 MN control loop failure causes to identify leakage.
uncontrolled amount of MN entering  SOP for start-up, normal operation
reactor. and shut down is established and
Runaway  Dowtherm control loop failure leading  Causes thermal explosion or required to be followed by trained
Reactions to insufficient cooling medium feeding rupture of reactor within the operators.
into the reactor. plant.  Well established emergency plan.
 Failure in E-201 and E-203 causes of  Release of explosive reactants  Temperature control loop (TIC-201,
reactant entering R-201 at temperature causes explosion if couple TT-211) with HH/LL alarm to control
higher than normal operation. with ignition source. reactor temperature.
 Uncontrolled exothermic reaction that  Explosion injuries and
produce large amount of heat. fatalities
 Malfunction of temperature transmitter  Reactor catches fire.
causes increase temperature in reactor
and promote rate of reaction.
Thermal  Reactor operating temperature of 140°C  Direct contact with hot vessel  Vessel and pipelines are fully covered
Exposure could cause severe burn. by hot insulation with mineral wools.
Table 8.2.2.3.2: Hazard Table for HEX E-201, E-202, E-203

Heat Exchanger (HEX), E-201, E-202 and E-203
 Temperature control loop  HEX catches fire.  HEX is installed in between platform to
Fire failures (causes runaway  HEX melts down. prevent direct exposure from sunlight.
Hazards reaction)  Cause increased temperature in  Sufficient spacing between HEX and other
 Presence of ignition sources downstream. processing equipment.
259
nearby.  HEX rupture due to  Pressure relief valves are installed to prevent
 Leakage of process vapor from overpressure by thermal gas HEX rupture.
valves or flanges due to the expansion. (PSV-201, PSV-202 and PSV-205).
extremely flammable property  Injuries and fatalities  Temperature control loop to control the
of MN. flowrate of Dowtherm into the HEX.
 Similar causes as fire hazards  Similar outcomes as above.  Regular inspection on the equipment to
mentioned above.  Release of process vapor identify leakage.
 Failure of pressure relief valve (DMO, Nitrogen Oxide, MN,  SOP for start-up, normal operation and shut
Explosion causes HEX overpressure. etc.) into atmosphere. down is established and required to be
Hazards  Leakage of MN reactant  Explosion injuries and fatalities followed by trained operators.
 Blockage in tube side of HEX.  Well established emergency plan.
 Temperature control loop (TIC-203, TIC-207
and TIC-209) to control HEX temperature.
Thermal  E-201 and E-203 outlet  Direct contact with hot vessel  Vessel and pipelines are fully covered by hot
Exposure temperature at 140°C could cause severe burn. insulation with mineral wools.
Table 8.2.2.3.3: Hazard Table for Compressor C-201, C-202

Compressor C-201 and C-202
Fire  Presence of ignition sources nearby.  Compressor catches fire.  Compressor is installed in well
Hazards  Leakage of process vapor from valves  Compressor rupture due to ventilated area and have sufficient
or flanges due to the extremely overpressure by thermal gas spacing with other processing
flammable property of MN. expansion. equipment.
 Compressor overheating due to  Fire injuries and fatalities  Regular inspection and maintenance
surging leading high discharge on the equipment to identify leakage.
temperature.  Compressor is protected by anti-surge
260
Explosion  Similar causes as fire hazards  Similar outcomes as above. control (PFCV-205 and PFCV-203)
Hazards mentioned above.  Release of process vapor  SOP for start-up, normal operation
 High incoming pressure at suction side (DMO, Nitrogen Oxide, MN, and shut down is established and
causing surging of compressor. etc.) into atmosphere. required to be followed by trained
 Overpressure due to surging.  Compressor rupture due to operators.
overpressure.  Well established emergency plan.
 Explosion injuries and fatalities
Electrical  Exposed wire connection to the  Short circuit in the plant.  Establish a regular inspection and
Hazards compressor or damaged wire.  Injuries and fatalities due to maintenance to ensure good
 Presence of water around wiring. electric shock. conditions of electrical cords.

Start-Up Procedure
Start-up for CO and MN:
1. Ensure all drain valves and vent valves are in fully closed position.
2. Ensure all control valves are set into manual setting.
3. Open all isolation valves for the process stream and bypass valves (BV-204, BV-205, BV-206, BV-207, BV-209, and BV-210), to
allow for nitrogen purging from the upstream.
4. Ensure there is no “hiss” sound along the pipeline in between the purging process indicating a leak-free process.
5. DV-207, DV-208, DV-209, DV-210, DV-211, 216, DV-216, IV-215, IV-231 are closed after completion of nitrogen purging.
261
Start-up for Reactor R-201:
1. Close all drain valves, isolation valves and vent valves.

2. Open DV-219, IV-244 for nitrogen purging in order to remove air and any
impurities inside the reactor.
3. Close DV-219, IV-244 after nitrogen purging is completed.
4. Proof testing of alarm systems to ensure all the alarms are in good operating
condition.
5. Open IV-208 to allow nitrogen as diluent to enter the reactor.
6. Open IV-207 to allow coolant (Dowtherm 4000) to enter the reactor and to fill up
the reactor and IV-239 is opened when the reactor is fully filled by coolant.
7. Open IV-235, IV-222 to allow reactants to enter R-201.
8. Open IV-238 to allow product (Dimethyl Oxalate) to leave the reactor.
9. IV-242 is opened to allow operation of PSV-203.
10. Automate control valves FC-201, TCV-202, TCV-203, TCV- 204, TCV-205, FCV-
206, TCV-207, FCV-208 once the system achieve steady state operation.
Normal Operation Procedure

1. Ensure all the control valves are in automatic configuration.
2. Monitor the normal operating parameters of each equipment to ensure all the
parameters fall within the range as shown in the table below.
Equipment Control Loop Normal Operation Parameters
TIC-202 140°C
FIC-206 Approximate 6500 𝑚3 /ℎ𝑟
R-201
FIC-208 Approximate 23000 𝑚3 /ℎ𝑟
PT-210 3.0 barg
E-201 TIC-203 140°C
E-202 TIC-209 20°C
E-203 TIC-207 140°C
C-201 PDIC-205 2.2 barg
C-202 PDIC-213 3 barg
3. Daily routine inspection on pipelines, valves and instrumentations to ensure safe

operation of the process and prevent leakage from happening.
4. Maintenance planning system (MPS) is followed below in the table based on
equipment type.
262
Maintenance
Equipment Justifications
Type
Reactor  Preventive  R-201 maintenance every 2 months for
Heat Maintenance catalyst replacement.
Exchanger  Predictive  Heat exchanger and compressor
Compressor Maintenance maintenance scheduled at every 6 months.
Gas-Liquid  Equipment is too costly for having a back-
Separator up.
 Failure in equipment will directly stop the
production.
Valves and Planned  Maintenance carried out once a month.
Instrumentation Maintenance  Back-up is affordable.
 Have no severe impact on production.
5. ESV-201 and ESV-202 close to cut off reactants entering R-201, IV-234 is opened
to allow nitrogen purging when R-201 lost control.
6. Valve exercise programme is scheduled weekly.
Shutdown Procedure
Shut down for CO and MN heat exchanger and compressor:
1. Ensure all control valve is in manual setting.

2. Close IV-206 and IV-225 to cut off heat transfer fluid and steam flowing into heat
exchanger E-201 and E-203.
3. Shut down C-201.
4. Close IV-209 and IV-226 to stop carbon monoxide and methyl nitrite from
upstream entering DMO synthesis section.
5. Close IV-213, IV-219, IV-226 and IV-232 to isolate E-201 and E-203.
6. Open DV-211, DV-212, DV-213, DV-216, DV-217, DV-218, BV-206, BV-209 to
drain out all the process fluid inside heat exchanger.
7. Open IV-216, IV-217, IV-227, and IV-228 to allow nitrogen purging to carry out to
remove all the components in the process stream into a temporary storage tank.
8. Close DV-211, DV-212, DV-213, DV-216, DV-217, DV-218, BV-206, BV-209,
IV-215 and IV-231 after nitrogen purging is done.
Shut down for R-201:
1. Ensure that no reactant is flowing into R-201 by closing IV-222 and IV-235.
263
2. IV-238 is closed to isolate R-201 in order to ensure no backflow of product into R-

201
3. Shut down C-201, E-201 and E-203 to stop carbon monoxide and methyl nitrite
entering DMO reactor.
4. Allow Dowtherm 4000 to cool the reactor to achieve 50°C.
5. Open IV-244 to vent out process gases inside the reactor into a temporary venting
storage tank.
6. IV-240 is opened to ensure all the process stream in the Pressure relief valve line is
sent into flare system.
7. DV-219 is opened to drain out Dowtherm 4000 in the shell side of the reactor.
8. Open IV-236 and IV-237 for nitrogen purging to remove all the process gases in the
tube side of the reactor.
9. Close IV-244, DV-219, IV-236 and IV-237 after nitrogen purging process is
completed.
10. Perform pipeline Nitrogen purging on process streams.
264
Figure 8.2.2.5.1: Bow Tie Diagram for Direct Release of Large Scale Process Gases
265
8.2.3 MN Synthesis
MN which is one of the main reactants of DMO synthesis is produced from a series of reaction in this section. Methanol, nitric oxide (NO)
and oxygen are the main raw material required in MN synthesis. The NO which is one of the by-products of DMO synthesis is recycled and
mixed with fresh NO before entering the first reactor (R-401). The first reactor (R-401) involved formation of nitrogen dioxide while
second and third reactor (R-402 and R-403) is two similar reactors involved same reaction to produce MN. Since MN synthesis process
involved several hazardous material and exothermic reactions which could lead to some potential hazard, several safety measures are taken
this section to reduce possibility of these potential hazardous events to an acceptable level. The operating parameters such as temperature,
pressure and level of the process equipment and pipeline are monitored and controlled by proper instrumentation and alarm system. The
operators in charge of the plant will be trained and educated on the SOP of start-up, shutdown and normal operation of the process. A
regular maintenance on equipment, valves and pipeline of plant will also be conducted to ensure that all of them can be operated safely and
efficiently.

Table 8.2.3.2.1: Inherent Safety Design of MN Synthesis
 The NO feedstock to R-401 is reduced by using 2 similar reactors (R-402 and R-403) operate in series
to increase the overall conversion of the reactant.
 The NO which is the by-product of DMO synthesis is recycled as main feedstock of MN synthesis to
Feedstock
Minimise reduce the amount of fresh NO feedstock required.
 The unreacted MN from DMO synthesis is recycled. Thus, the amount of MN required to synthesis in
R-402 and R-403 is reduced and the feedstocks required can be minimised.
Flammability Stainless steel 304 is chosen as pipeline material for process stream which contain high concentration of
266
MN since MN is an oxidizing agent and a heat-sensitive explosive in the presence of metal oxides (NOAA
Office of Response and Restoration, 2017). Besides, these materials can also minimise the possibility of
leakage of MN which will form explosive mixtures with air.
Dowtherm 4000 is chosen as cooling media of E-401 and E-402 since it is cleaner and less corrosive than
Substitute Cooling media
cooling water.
The operating condition of R-401, R-402 and R-403 are controlled by the PV-404, PV-410 and PV-415
Operating
Moderate respectively. These control valves control the cooling water flow rate into the cooling jacket of each
condition
reactors.
Since MN is highly flammable and explosive, the nitrogen gas will be fed into process stream to reduce the
Flammability
concentration of MN in process stream
Equipment and All the equipment and valves involved in MN synthesis are labelled accordingly to prevent operating error.
Simplify
Valve labelling
8.2.3.3 Hazard Identification as well as its Causes, Outcomes and Mitigation

Table 8.2.3.3.1: Hazard Identification and mitigation measure for reactor R-401
Type of
Possible Causes Possible Outcome Mitigation Process
Hazard
Thermal 1. Insufficient cooling water supply to the 1. Skin burn upon direct contact with 1. Proper insulation of pipeline
Hazard cooling jacket of R-401 due to reactor or pipeline. and reactor with appropriate
malfunction in control valve (PV-404) or 2. Pressure build up in the reactor material
transmitter (PT-405) which may cause vessel rupture 2. Personnel protective equipment
2. Insufficient cooling water supply to the 3. Excessive temperature in reactor need to be worn at all time
cooling jacket of R-401 due to loose may affect the product quality and within the plant site
fitting in either pipeline or valve which production rate 3. Regular check-up and
will lead to leakage. 4. Runaway reaction maintenance on the
3. Malfunction of heat exchanger (E-401) valve/transmitter/flanges
267
which will cause a higher feed 4. Ensure all the process fluid is
temperature. fully vented to flare system
before maintenance to prevent
skin burn
5. Ensure the operators are
properly trained and has
sufficient knowledge on SOP.
Chemical 1. Leakage of process fluid due to 1. MN and CO which is toxic will 1. Regular maintenance on the
Exposure pipeline/valve/flange malfunction release to environment and threaten valve (IV-427 and PRV-402),
Hazard 2. Vent valve (IV-427) or pressure relief the human health. pipeline and flanges in plant is
valve (PRV-402) failure 2. The flammable chemicals in conducted
3. Improper shutdown or maintenance process stream such as MN and CO 2. Ensure the operators are
procedure which lead to release of reactor may cause fire hazard after contact properly trained and has
content with ignition source. sufficient knowledge on SOP
3. Skin burn upon direct contact with 3. PPE need to be worn at all time
process fluid due to high operating within the plant site
temperature 4. Install a fire sprinkler system to
Fire and 1. Excessive pressure build-up in reactor 1. Reactor rupture due to overpressure control spread of fire
Explosion due to: and explosion 5. Dilute the process stream with
Hazard a. Pressure relief valve (PRV-402) failure 2. Flammable gas such as CO will nitrogen to reduce the
b. Runaway reaction release to atmosphere and cause concentration of flammable and
c. Insufficient cooling of reactor due to flash fire or explosion if in contact toxic gas such as CO
leakage or valve (PV-404) failure. with ignition source 6. Install an appropriate and
d. Control valve (PV-405) failure lead to 3. Fire/Explosion injuries or fatalities immediate first aid and fire
excessive flow level of reactant into response procedure in a case of
reactor emergency.
268
2. Leakage of reactor content due to 7. A safety instrumented system

pipeline/valve/flange failure (SIS-405) with PAHH alarm
3. Improper shutdown or maintenance system is installed to control
procedure which lead to release of reactor solenoid valve (SV-402) so that
content the pressure of the reactor will
4. Reactor is placed near the ignition source not exceed its maximum design
Runaway 1. Pressure and temperature increase due to 1. Reactor rupture due to overpressure pressure
Reaction transmitter (PT-405) and control valve of reactor
(PV-404) failure 2. Release toxic gas such as CO
2. Insufficient cooling water supply to the which may cause difficulty
cooling jacket due to leakage from breathing and blood
pipe/valve/flange damage (MATERIAL SAFETY
3. High reactor temperature and pressure DATA SHEET: Carbon Monoxide,
will increase rate of reaction which will 2010) to atmosphere. exposure
then generate large amount of heat due to 3. Fire/Explosion injuries or fatalities
uncontrolled exothermic reaction.
Table 8.2.3.3.2: Hazard Identification and mitigation measure for reactor R-402 and R-403
Type of
Hazard
Fire and 1. Presence of air inside the reactor 1. MN and CO which is highly 1. Regular maintenance on the valve,
Explosion and pipeline flammable will be ignited by any pipeline and flanges in plant is conducted
Hazard 2. Presence of metal oxides in ignition source nearby 2. Ensure the operators are properly trained
reactor or pipeline due to 2. MN will form explosive mixture and has sufficient knowledge on SOP
corrosion with air and is heat-sensitive 3. PPE need to be worn at all time within
3. Reactor is placed near the explosive in the presence of metal the plant site
269
ignition source oxides (NOAA Office of Response 4. Install a fire sprinkler system to control
4. Leakage of reactor content due and Restoration, 2017). spread of fire
to pipeline/valve/flange failure 3. Vessel rupture due to overpressure 5. Dilute the process stream with nitrogen
5. Excessive pressure build-up in 4. Fire/Explosion injuries or fatalities to reduce the concentration of flammable
reactor due to: 5. Release of toxic gas (such as CO and toxic gas such as carbon monoxide
a. Pressure relief valve (PRV- and MN) which will affect human and methyl nitrite
406/PRV-409) failure health to the atmosphere 6. Install an appropriate and immediate first
b. Runaway reaction aid and fire response procedure in a case
c. Insufficient cooling of reactor of emergency.
due to leakage or valve (PV- 7. A safety instrumented system (SIS-
410/PV-415) failure. 412/SIS-416) with PAHH alarm system
6. Improper shutdown or is installed to control solenoid valve (SV-
maintenance procedure which 405/SV-406) so that the pressure of the
lead to release of reactor content. reactor will not exceed its maximum
Runaway 1. Transmitter (PT-412/PT-416) 1. Reactor rupture due to design pressure
reaction and control valve (PV-410/PV- overpressure of reactor 8. Install a pressure relief valve (PRV-
415) failure leading to reactor 2. Release toxic gas such as CO and 406/PRV-409) to protect reactor from
pressure and temperature MN to atmosphere overpressure
increase. 3. Cause fire and explosion of reactor 9. Using nitrogen to purge reactor content
2. Insufficient cooling water supply 4. Fire/Explosion injuries or fatalities before start-up and maintenance to avoid
to the cooling jacket of R-402/R- presence of air inside the reactor
403 due to leakage from 10. Set-up a proper Start-up, Maintenance
pipe/valve/flange and Shut-Down Procedure.
3. High reactor temperature and
pressure will increase rate of
reaction which will then
270
generate large amount of heat

due to uncontrolled exothermic
reaction.
Toxic 1. Leakage of process fluid due to 1. CO in process fluid may cause 1. Regular inspection and maintenance on
Hazard lose fitting/failure of difficulty breathing and blood the valve, pipeline and flanges of
valve/flange/pipeline damage if inhaled reactors.
2. Vessel rupture due to 2. MN in process fluid may cause 2. Ensure the operators are properly trained
overpressure or explosion dizziness or asphyxiation and has sufficient knowledge on SOP
3. Improper shutdown or 3. PPE is available on site
maintenance procedure which 4. Install an appropriate and immediate first
lead to release of process fluid aid response procedure in a case of
emergency
Corrosion 1. Presence of moisture and nitric 1. Vessel rupture or other mechanical 1. Using appropriate material such as
acid in the process stream failure may occur due to decrease stainless steel 304 as construction
in strength of material of vessel. material of pipeline involved corrosive
2. Reduce the lifetime of reactors and fluid.
its fitting
Table 8.2.3.3.3: Hazard Identification and mitigation measure for separator S-401
Type of
Hazard
Mechanic 1. Pressure relief valve (PRV-408) 1. Vessel rupture results in release of 1. Regular inspection and maintenance on
al failure separator content which contains PRV-408
Failure/R 2. Pressure transmitter (PT-415) or MN and CO 2. Install appropriate pressure and level
upture control valve (PV-413) failure 2. Fire/Explosion due to release of controller (PIC-415 and LIC-403) with
3. Corrosion due to presence of highly flammable gas (MN and alarm system to control pressure and
271
moisture or nitric acid CO) level of separator

3. Fire/Explosion injuries or fatalities 3. Install an appropriate and immediate first
4. Release of toxic gas (MN and CO) aid and fire response procedure in a case
to the atmosphere of emergency.
Chemical 1. Mechanical failure/rupture 1. MN and CO which is highly 1. Regular maintenance on the valve,
Exposure 2. Leakage of process fluid due to flammable will be ignited by any pipeline and flanges in plant is conducted
Hazard failure/loose fitting of ignition source nearby 2. Ensure the operators are properly trained
lead to valve/pipeline/flange 2. MN will form explosive mixture and has sufficient knowledge on SOP.
Fire, 3. Excessive pressure build-up with air and is heat-sensitive 3. PPE is available on site
Explosion lead to vessel rupture explosive in the presence of metal 4. Install an appropriate and immediate first
and Toxic 4. Improper start-up, shutdown or oxides aid and fire response procedure in a case
Emission maintenance procedure which 3. Release toxic gas such as CO and of emergency.
lead to release of reactor content MN to atmosphere 5. Install a pressure relief valve (PRV-408)
4. Fire/Explosion injuries or fatalities to avoid overpressure
5. Severe injury/frostbite if came into 6. Using nitrogen to purge reactor content
direct contact with process fluid before start-up and maintenance to avoid
with low operating temperature presence of air inside the S-401
7. Set-up a proper Start-up, Maintenance
and Shut-Down Procedure.
8.2.3.4 Standard Operating Procedure (SOP)

In this section, the SOP of reactors (R-401, R-402) where MN is synthesized will be summarised and shown below. Since R-402 and R-403
are similar reactors, the SOP of R-403 is similar to R-402.
272
Start-Up Procedure
Checking and Purging Process
1. Before the start-up procedure, all the equipment in this section will be check to
ensure no leakage will occur during operation by carrying out steam cleaning. All
isolation valve, drain valve, bypass valve and control valve are closed except IV-
413, IV-415, IV-439, IV-456 and IV-459 to allow steam to enter R-401 and R-402
as well as E-401, E-403 and E-406.
2. After using steam cleaning, IV-413, IV-415, IV-439, IV-456 and IV-459 will be
closed while all the vent valve (IV-420, IV-427, IV-454, IV-463, IV-469) of these
equipment (E-401, R-401, E-403, E-406, R-402) will be opened and using nitrogen
gas to purge all the fluid inside equipment to remove all the air and steam inside
this equipment. This is done by opening the isolation valve (IV-412, IV-414, IV-
438, IV-441, IV-460) to allow nitrogen gas to enter this equipment. These isolation
valves as well as vent valves are closed after finish nitrogen purging.
3. During the start-up process, all the alarm are overridden and set to manual mode by
the operators.
4. The availability of C-401, C-402, and P-402 as well as utility stream for E-401, E-
403 and cooling jackets of reactors will be checked and tested to ensure operating
temperature and pressure of inlet stream of R-401 and R-402 can be achieved.
Start-up for R-401 and R-402
1. All the drain valves and vent valve on E-401, R-401 and pipeline are close.
2. All the isolation valve for control valves are opened.
3. Fresh NO and oxygen will enter compressors (C-401 and C-402) respectively by
opening isolation valves (IV-401, IV-402, IV-406, IV-407) to achieve desired
pressure. These compressed gasses will then enter E-401 by opening IV-405 before
entering R-401.
4. IV-410, IV-411 and IV-421 of Dowtherm 4000 will be opened to allow it to enter
E-401. The flow rate of utility will be control by PV-403 until the outlet stream of
E-401 reached the desired temperature. Similar procedure will be done for cooling
water of cooling jacket of R-401.
273
5. IV-422 and IV-430 will be opened to allow inlet and outlet flow to R-402. The inlet
flow of R-401 will be controlled manually by PV-405.
6. Similar to fresh feedstocks of R-401, fresh methanol will enter a pump (P-402) and
a heater (E-403) to achieved desired temperature and pressure before entering R-
402.
7. Once the system reached steady state, control valve and alarm will be run under
automated control mode for normal operation procedure.
Normal Operating Procedure

1. All the control valve and alarm will all be set to automated control mode during
normal operation.
2. The inlet temperature of R-401 is controlled using PV-402 which controls the flow
rate of Dowtherm 4000 into E-401. Meanwhile, the operating temperature and
pressure of R-401 is controlled using PV-404 which control the flow rate of cooling
water into cooling jacket of R-401. Since pressure of gas is directly proportional to
temperature, the operating pressure of R-401 can also be controlled by same control
loop.
3. Similar to R-401, the operating temperature and pressure of R-402 is controlled
using PV-410 which control the cooling water flow rate. The inlet temperature of
methanol is controlled using PV-407 which control the flow rate of steam into E-
403. Since another inlet stream of R-401 is the outlet stream of R-401, its
temperature is depending on the operating temperature of R-401 which is controlled
using PV-404.
4. In order to prevent flooding in R-402, the liquid level in R-402 is controlled by
using LIC-402 which can control the flow rate of bottom outlet stream by adjusting
the opening of PV- 412. Level alarm (LAHH, LALL, LAH and LAL) will be
triggered when the level of liquid in R-402 is exceed or lower than normal
operating range.
5. The pressure relief valves, PRV-402 and PRV-406 of reactors R-401 and R-402
respectively will be opened to release vapour to flare system to reduce pressure of
reactor when the pressure in reactor (R-401/R-402) exceed the maximum design
pressure.
274
Shutdown Procedure
1. The compressors (C-401 and C-402) and pump (P-402) are turned off to remove the
driving force of process fluid.
2. IV-405, IV-422 and IV-455 are closed to ensure no feeds enter R-401 and R-402.
3. PV-403 and PV-407 are closed to stop supplying utility stream into E-401 and E-
403 respectively. The cooling water supplied to cooling jacket of R-401 and R-402
is stopped by closing PV-404 and PV-410.
4. All the isolation valves on upstream and downstream of reactors are closed to
ensure no process fluid will enter the reactors during maintenance process.
5. All the drain valves (such as DV-410 and DV-426 of R-401 and R-402
respectively) are opened to remove all the liquid in reactor.
6. The vent valves (such as IV-427 and IV-469 of R-401 and R-402 respectively) are
opened to remove the vapour content in reactors.
7. IV-414 and IV-460 are opened to allow nitrogen gas to flow into R-401 and R-402
respectively. The nitrogen gas will act as cooling medium to cool the reactor (R-
401/R-402) and purge the remaining process fluid in reactors to flare system via
vent valve (IV-427/IV-469).
275
Figure 8.2.3.5.1: Bow Tie Diagram for Large Release of Process Fluid.
276
8.2.4 DMO Purification and Dehydration

This section summarizes the safety aspects of dehydration process that utilizes two distillation columns, as well as DMO purification
process which utilises one distillation column. The focus will be on the dehydration tray column D-501 drawn in P&ID-5-1 as the three
columns share similar safety aspects.

Two inherent safety principles are followed for the distillation columns, which is minimize and moderate. Operating pressure of D-501 is
moderated at pressure 4.8 atm which is not consider as high pressure. The column temperature is controlled by the flowrate of saturated
steam flowrate into the reboiler E-503 through control valve PV-505. This is to prevent potential risk of fire hazard and explosion,
especially with the presence of methanol. The control valve is at a fail-closed position to prevent over-heating of column. Control valves
PV-502 and PV-506 controls the flowrate of coolant and these are set to be at fail-opened position for the purpose of decreasing
temperature of the pipelines and unit operations to prevent mechanical failure. Flammability of methanol is minimized by purging
nitrogen gas throughout the section during start-up of plant to remove air in the pipelines and equipment. This is to prevent the formation of
explosive mixture of methanol vapour and air due to its low flash point.

Table 8.2.4.3.1: Hazards, causes, potential outcomes and mitigation measures for D-501
Hazards Causes Potential outcomes Mitigation measures
 Leakages of process vapour with the  Column rupture due to  Column are placed in areas with good
Fire hazard presence of an ignition source. thermal expansion of process ventilation away from potential ignition
 Failure of control loop TIC-504 vapour, overpressure occurs sources.
277
which controls the column to vessel.  Weekly maintenance of control loop

temperature.  Column catches fire, may TIC-504. High temperature alarms
 (Highly unlikely) Leakage of air into cause fire injuries and (TAH-504) have been installed to alert
column through loose flanges or fatalities. operators in case of column
fittings. Auto ignition temperature of  Leaked methanol will burn temperature exceeding the limit.
methanol is 464°C. (Sciencelab.com, in the presence of ignition  Nitrogen purging to be carried out
Inc, 2013) source, which forms thoroughly to remove air from column
 Operator’s mistake for not following methanol vapour. and to detect any leaks from the
SOP. column.
 Build-up of pressure in column due  Column rupture due to  SOPs established for start-up, normal
to blockages of valves or equipment thermal expansion of process operation, shut down and abnormal
during normal operation. vapour, overpressure occurs events.
 Valve IV-508 not opened during to vessel.  Emergency plan is elaborated.
maintenance for steam cleaning or  Explosion due to pressurized  Routine inspection and maintenance.
Explosion nitrogen purging. leaked methanol vapour and  Training courses for operators to fully
 Air leaked into column, LEL of air mixture with the presence understand SOPs and able to handle
methanol: 6%; HEL of methanol: of ignition source. abnormal conditions.
36.5%. (Sciencelab.com, Inc, 2013)  Explosion injuries and
 Operator’s mistake for not following fatalities.
SOP.
 Leakage of process vapour or fluid  Over-inhalation of process  Proper training of handling accidental
to surrounding through loose vapour or direct contact with emissions should be provided to all
Toxic
fittings. LD50 of methanol is 5628 skin with process fluid will operators.
emission
mg/kg. (Sciencelab.com, Inc, 2013) cause irritation.  Proper PPE on site.
 Proper reporting procedures.
Thermal  High operating temperature: 101°C  Skin injuries or burns.  Proper PPE on site.
278
exposure to 122°C. (D-502 and D-301  Hot insulation of column for personnel
operates at a much higher protection.
temperature.)  Warning labels placed at obvious
location.
 Falling objects.  Injuries or fatalities.  Proper training and PPE provided.
Height-
 Accidents while climbing up the  Railings are installed on platforms.
associated
ladders during maintenance or  Caged ladders are used for safety
hazards
inspections. purpose.
 External environmental conditions,  Potential column damages.  Stainless steel cladding is installed at
Corrosion e.g. acid rain.  Leakage of process fluid. outer walls of column.
 Corrosion allowance.
Table 8.2.4.3.2: Hazards, causes, potential outcomes and mitigation measures for E-503 reboiler for D-501
 Leakages of process vapour with the  Reboiler rupture due to  Reboiler are placed in areas with good
presence of an ignition source. thermal expansion of process ventilation away from potential ignition
 (Highly unlikely) Leakage of air vapour, overpressure occurs sources.
into shell side of reboiler through to vessel.  Weekly maintenance of control loop
loose fittings and TIC-504  Reboiler catches fire, may TIC-504. High temperature alarms
Fire hazard malfunction at the same time. Auto cause fire injuries and (TAH-504) have been installed to alert
ignition temperature of methanol is fatalities. operators in case of column
464°C. (Sciencelab.com, Inc, 2013)  Leaked methanol will burn temperature exceeding the limit.
 Operator’s mistake for not following in the presence of ignition  Nitrogen purging to be carried out
SOP. source, which forms thoroughly to remove air from reboiler
methanol vapour. and to detect any leaks from the
Explosion  Build-up of pressure in tube side of  Explosion due to pressurized reboiler.
279
reboiler due to blockages of valves leaked methanol vapour with  SOPs established for start-up, normal
or equipment. This leads to tube the presence of ignition operation, shut down and abnormal
rupture and then the rupture of shell source. events.
from overpressure.  Explosion injuries and  Emergency plan is elaborated.
 Air leaked into shell side of reboiler, fatalities.  Routine inspection and maintenance.
LEL of methanol: 6%; HEL of  Training courses for operators to fully
methanol: 36.5%. (Sciencelab.com, understand SOPs and able to handle
Inc, 2013) abnormal conditions.
 Operator’s mistake for not following
SOPs.
 Leakage of process vapour or fluid  Over-inhalation of process  Proper training of handling accidental
to surrounding through loose vapour or direct contact with emissions should be provided to all
Toxic
fittings. LD50 of methanol is 5628 skin with process fluid will operators.
emission
mg/kg. (Sciencelab.com, Inc, 2013) cause irritation.  Proper PPE on site.
 Proper reporting procedures.
 High operating temperature: 122°C.  Skin injuries or burns.  Proper PPE on site.
(E-302 and E-506 operates at a much  Hot insulation of column for personnel
Thermal
higher temperature.) protection.
exposure
 Warning labels placed at obvious
location.
The following table summarizes the mechanical hazards associated with pump, albeit not a major source of hazard. It is still essential to list
out the potential outcomes and mitigation measures for the potential hazards.
280
Table 8.2.4.3.3: Hazards, causes, potential outcomes and mitigation measures for pumps
 Improper placement of pump i.e. pumps  Injuries associated  Pump covers should be installed.
placed at area that is frequently accessed with mechanical  Proper training for personnel involve in
Mechanical
by personnel. hazards. pump handling.
hazard
 Mistakes during maintenance.  Warning labels placed at obvious
 Operator’s mistake for not following SOPs location.

This section covers the SOP for distillation column, D-501 as drawn in P&ID-5-1. The system boundary includes the preheater (E-501),
pump (P-501), condenser (E-502), reboiler (E-503), reflux drum (T-501) and cooler (E-504). It is noted that the SOPs for two other
distillation columns (D-502 and D-301) are similar to D-501.
Start-Up Procedure
1. All control valves are set to manual mode and all alarms and controls are calibrated and checked for functionality respectively.
2. Nitrogen purging will be carried out to check for any leakage prior to start-up. Any form of leakages has to be addressed before
commencing plant start-up.
3. Thorough purging of nitrogen will be conducted to remove air in the column and the rest of system. All the drain valves are closed and
all the isolation valves, check valves and bypass valves are fully open to ensure complete purging throughout the distillation system.
Valve MV-501 will then be open to let nitrogen flow into the system.
4. Once the purging is complete, MV-501 and all by-pass valves will be shut closed. The process fluid will then be introduced into the
preheater E-501. IV-501 and IV-502 are opened to allow the saturated steam to heat up the process fluid to the desired feed
temperature.
281
5. Ensure pump P-501 is fully filled with fluid before start-up. IV-511 and IV-512 will
be open to allow the coolant to flow into the condenser for ten minutes before
allowing the process vapour from D-501 to enter the condenser.
6. Once the level of process fluid in the column reaches the upper limit, P-501 is
switched off. At initial stage, the column is operating under total reflux condition
and column has to be isolated. Spectacle blinds at the feed line will be closed and
control valves PV-504 and PV505 are in manual operation. Saturated steam is then
introduced into the reboiler E-503 by manipulating PV-505. Total reflux operation
will continue until steady state is achieved.
7. Once steady state is achieved, P-501 is switched on and all the valves are back to
normal operating conditions as shown in P&ID-5-1. All the control valves and
alarms in the section are then switched to automatic control.
Normal operating procedure

1. The state of valves position at normal operation is as shown in P&ID-5-1, whereby
all control loops as well as high/low alarms in the system are automated.
2. Temperature is the crucial parameters that requires control. Control schemes are
shown below.
3. Control loop FIC-501 controls the reflux flowrate into D-501. Detection of any
deviations in flowrate in pipeline 510 and 512 will cause PV-503 to take necessary
actions.
4. Control loop TIC-504 controls the temperature of D-501 to 122.1°C. Detection of
change in column temperature will cause PV-505 to manipulate the flowrate of the
saturated steam.
5. Control loop LIC-501 controls the process fluid level in D-501. Detection of any
deviations in fluid level in D-501 will activate PV-504 to take necessary actions.
6. Control loop PDI-501 shows the pressure drop in the distillation column. No
automated control scheme is set up.
7. As the high/low alarms are automated, any deviation that goes beyond the set upper
and lower limits will trigger the alarm. Operators will need to override the alarm,
switch the control valves into manual mode and take the necessary corrective
actions.
282
8. Spare pumps are assigned to P-501 (or P-501A) and P-502 (or P-502A) as they are
crucial to the process. In case of P-501 failure IV-506 and IV-507 will be open and
spare pump P-501B will be switched on. IV-504 and IV-505 will then be closed
and P-501 is drained and removed for maintenance. Similar procedures are carried
out for P-502. Alternating of pumps should be done once a week.
Shutdown procedure
1. IV-502 is shut closed in order to stop the flow of saturated steam flowing into the
preheater E-501. Allow the process stream flow for a few minutes and IV-504 is
shut close to prevent process fluid to enter the preheater. DV-503 is open to drain
out the preheater.
2. Pump P-501 is shut down followed by the closing of IV-505 to stop the flow
entering D-501. The spectacle blind at the feed inlet is then closed.
3. Pumps P-501 and P-502 are shut down and drained by opening DV-504 and DV-
511. D-501 is further isolated by closing IV-509 and IV-520. Control loops TIC-
501 and TIC-505 are set to manual control.
4. Control loops TIC-504 and FIC-501 are set to manual control; saturated steam
flowrate into D-501 is stopped by closing PV-505.
5. Once process vapour is fully condensed, coolant flowrate is shut off by closing IV-
512. Condensed process fluid is returned to D-501 by opening PV-503.
6. MV-501 is opened to allow nitrogen to flow into D-501. Nitrogen acts as a cooling
stream to decrease the temperature of the process fluid in D-501 for safety purpose
as the column temperature is higher than the flash point of the process fluid.
7. Once the process fluid reaches a temperature lower than 60°C which is shown in
the temperature indicator TI-502, all the drain valves will be opened to drain the
process fluid from the equipment and pipelines. Equipment and pipes should be
ready for maintenance.
283
Figure 8.2.4.5.1: Bow tie diagram for large scale release of fluid
284
8.2.5 MEG Purification

In this section, the safety aspects for MEG Purification will be summarised. For MEG Purification, this process will consist of three
distillation columns (D-701, D-702, D-703), a few heat exchangers (E-704, E-708, E-710), a pump (P-704) and a gas-liquid separator (S-
701). The safety aspects for all three columns are almost similar except for the last column (D-703) as it is operating in vacuum condition.
Hence, the focus will be on the system boundary of D-703, E-704, P-704 and S-701.

There will be three inherent safety design parameters which will be considered in this MEG Purification process which are eliminate,
minimize and moderate. Firstly, the presence of hydrogen within the system was eliminated from the first column (D-701) as hydrogen can
pose hazard within the plant due to its explosive property. Next, the operating pressure for D-703 was moderated to 0.8bar to ensure that
the operating temperature could be reduced and hence minimizing the chances for fire and thermal associated risks to occur.

Table 8.2.5.3.1: Hazards, causes, potential outcomes and mitigation methods of D-703.
Hazards Causes Potential Outcomes Mitigation Methods
 Ignition source nearby and leakages  Column catches fire.  Ensure columns are in well ventilated areas.
to the environment.  Rupture due to thermal  Ensure no potential ignition source near the
 Malfunction of temperature control expansion. column.
Fire
loop (TIC-724) in controlling  Fire injuries or  Regular maintenance and check-up on
Hazard
column’s temperature. fatalities. temperature control loop (TIC-724).
 SOP were not followed by operators.  Nitrogen purging is carried out at start-up and
shut-down of column to remove air in the
285
column and to check for possible leakages.

 Install fire sprinkler system.
 Train personnel to fully understand SOPs and
able to handle emergency situations.
 Leakage due to rupture.  Causes ingestion if  Proper training is provided to operator to
 Leakage due to PRV-703 not close inhaled/consumed handle accidental emissions.
Toxic
properly.  Causes irritation if  Have proper reporting procedures in case of
Emission
come into contact with emissions.
skin.  Ensure proper PPE available on site.
 High operating temperature of  Causes burn/skin  Have proper and visible warning labels/signs
Thermal column. (D-703 temperature = injuries on the column.
Exposure 189.33oC)  Ensure hot insulation for personnel
protection.
Hazards  Objects falling from above.  Serious  Properly train personnel and ensure that PPE
Related  Accidents/injuries might occur when injuries/fatalities is provided.
with climbing ladders during inspection or  Caged ladder installed for extra safety.
Height maintenance.  Railings also installed on platforms for safety.
 Steam ejector malfunction.  Buckling will occur.  Obtain approval from an experience engineer
 Wrong material selected when  Process fluid will leak. regarding design of column.
Implosion
designing.  Injuries and fatalities  Install pressure control PIC-718 and P-719 at
might occur. steam ejector.
 Due to external effects. (e.g.: acid  Column will rupture.  Install stainless steel cladding at the outer
rain)  Process fluid will leak. wall of column.
Corrosion
 A corrosion allowance thickness is applied on
the wall thickness.
286
Table 8.2.5.3.2: Hazards, causes, potential outcomes and mitigation methods of E-709.
 Ignition source nearby and leakages  Reboiler catches fire.  Ensure reboilers are in well ventilated
to the environment.  Thermal expansion of areas.
 Malfunction of temperature control vapor causes rupture and  Ensure no potential ignition source near the
loop (TIC-724) to control flow of overpressure. reboiler.
utilities into reboiler.  Fire injuries or fatalities.  Regular maintenance and check-up on
 SOPs were not followed by temperature control loop (TIC-724).
Fire
Hazard operators.  Nitrogen purging is carried out at start-up
and shut-down of column to remove air in
the column and to check for possible
leakages.
 Train personnel to fully understand SOPs
and able to handle emergency situations.
 Leakage due to rupture/lose fittings.  Causes ingestion if  Proper training is provided to operator to
inhaled/consumed handle accidental emissions.
Toxic
 Causes irritation if come  Have proper reporting procedures in case
Emission
into contact with skin. of emissions.
 Ensure proper PPE available on site.
 High operating temperature of  Causes burn/skin  Have proper and visible warning
Thermal reboiler. (E-709 temperature = injuries labels/signs on the column.
Exposure 189.33oC)  Ensure hot insulation for personnel
protection.
287
Table 8.2.5.3.3: Hazards, causes, potential outcomes and mitigation methods of S-701
 Ignition source nearby and leakages to  Pressure build up causing  Ensure separator is in well ventilated
the environment. rupture and overpressure. areas.
 Leakage of process fluid.  Fire injuries or fatalities.  Ensure no potential ignition source near
Fire &  Pressure build up due to process fluid.  Explosion injuries or the separator.
Explosion  SOPs were not followed by operators. fatalities  Regular maintenance and check-up on
Hazard separator.
 Train personnel to fully understand SOPs
and able to handle emergency situations.
 Leakage due to rupture/lose fittings.  Causes ingestion if  Proper training is provided to operator to
inhaled/consumed handle accidental emissions.
 Causes irritation if come  Have proper reporting procedures in case
Toxic
into contact with skin. of emissions.
Emission
 Ensure proper PPE available on site.
 Regular inspection and maintenance on
heat exchanger.
 Wrong material selected during  Buckling will occur.  Obtain approval from an experience
design.  Process fluid will leak. engineer regarding design of separator.
Implosion
 Injuries and fatalities
might occur.
288

This section will summarise the SOP for the distillation column, D-703, which is in
vacuum condition. The system boundary will include the condenser (E-706), reboiler
(E-709), reflux drum (RD-703), and the steam ejector system (SE-701). As for the other
two columns (D-701 and D-702), the SOPs are similar to D-703 without the steam
ejector system.
Start-Up Procedure
i. Before start-up, the column will be checked to ensure that there is no leakage.
This is done by carrying out steam cleaning.
ii. Nitrogen purging is then carried out to remove any possible air within the
column before introducing the process fluid into the column. This is done by
opening valve MV-707 to allow nitrogen to enter the column. All the isolation
and bypass valves will be opened whereas the drain valves will be closed.
iii. During start-up, all the alarms will be override. Hence, operators are required to
be present on site.
iv. After nitrogen purging, the steam ejector system will be started in order to obtain
the required vacuum condition in the column. Firstly, IV-764 will be opened to
allow Dowtherm G Cold to enter the condenser (E-706). The steam ejector is
then start-up accordingly. For the steam ejector, IV-761 and MV-705 are first
opened to all high pressure steam to enter the ejector. MV-705 was then
manipulated until the desired pressure inside the column is achieved. After
obtaining the required pressure, all the valves should be back to normal
operating conditions.
v. Off-specs process fluid will first be let into the first column (D-701) which will
then flow to D-703. Make sure that all the pumps (P-703, P-704) are filled
before start-up. IV-762 is then opened to ensure Dowtherm G Cold flows into
the condenser (E-706).
vi. As the level within the column reaches its upper limit, IV-739 is then closed.
The column is then isolated to obtain total reflux conditions. IV-758 and IV-765
are also closed. Then, FIC-717, TIC-724 and LIC-725 will be controlled
manually and saturated steam will be let into E-709 by manipulating TIC-724.
The total reflux operations will not stop until steady state is achieved.
289
vii. After achieving steady state, IV-747 is then opened and all the other valves will
then be back to normal operating conditions as shown in P&ID 7-03 All the
control valves and alarms will then be running under automated control.
Normal Operating Procedures

i. All the valves will be positioned as shown in P&ID 7-03 As for control loops
and high/low alarms, it will all be under automated system.
ii. As pressures and temperatures are important parameters which have to be
controlled to obtain the purity desired, hence, the control systems will be
explained in detail below.
iii. To control the temperature of D-703, control loop 724 is used. When there is a
change in temperature within the column, control loop 724 will then manipulate
the flowrate of saturated steam into the column to ensure that the desired
temperature is obtained. The flowrate will be controlled by PV-715.
iv. As for pressure, it is indicated by using control loop 718. There will be no
control systems for control loop 718 as the pressure is controlled by
manipulating MV-705.
v. For reflux rate, it is controlled using control loop 717. If there is any abnormal
flowrates within pipeline 730, PV-711 will then take necessary actions to obtain
the desired flowrate.
vi. The fluid level in the reflux drum (RD-703) is then controlled by the control
loop 721. If an undesirable fluid level is detected, PV-712 will then control the
flowrate in pipeline 731 to achieve the desired level within RD-703.
vii. All the alarm systems are automated. However, if any alarm is triggered, the
operators will then override the alarm, switch the control valves to manual mode
and then fix the problem.
viii. The pumps (P-703 and P-704) are crucial. Therefore, spare pumps are placed in
case of any failure in the pump. If any maintenance is required, IV-755 and IV-
756 will be closed and P-703a will be switched off and removed for maintenance
whereas IV-757 and IV-758 will be opened and P-703b will be switched on. The
same procedure will be carried out for P-704 when needed.
ix. Valve exercising should be practiced at least once every week to ensure that
there are no problems with the valves.
290
Shutdown Procedure
i. IV-747 will be closed to stop the inlet into the column. Then, the spectacle blind
on pipeline 728 will be closed.
ii. Pumps P-703a and P-704a is then switched off and DV-738 and DV-749 is
opened. The column is then isolated by closing IV-760 and IV-76. The control
loops 721, 723 and 726 are then switched to manual mode.
iii. Control loops 717 and 724 are also switched to manual mode. PV-715 is then
closed to stop the flow of saturated steam.
iv. When process vapor is fully condensed, IV-775 is then closed to stop the flow of
Dowtherm G Cold into E-706. The condensed process fluid is then sent back
into the column by fully opening PV-711.
v. MV-707 is then opened to allow nitrogen to flow into the column. The nitrogen
will act as a cooling medium to cool the contained process fluid inside the
column and also to ensure that no air enters the column when the vent is open.
vi. Then, the process fluid is let to cool down to a temperature less than 100 oC
which will be shown in the control room from control loop 716.
vii. Finally, the process fluid inside all pipelines and equipment are drained by
opening all drain valves. The drained fluid will then be stored and used as off-
spec products for start-up purposes. All equipment should be ready for
maintenance after draining.
291
Figure 8.2.5.5.1: Bow tie diagram for large scale release of fluid
292
8.3 Part B – Environmental

8.3.1 Life Cycle Assessment
8.3.1.1 Goal and Scope
The goal of this life cycle assessment (LCA) is to investigate the environmental
impacts, namely global warming potential (GWP) and resource depletion (RD) of all
sections of the MEG production plant as well as compare the sustainability of each
section through its entire life cycle. In this report, syngas is used as the main raw
material whereas the finished product is ethylene glycol (EG).
In this LCA, the approach adopted is “Gate to Gate” approach, whereby it focuses
mainly on all stages of EG production. As this LCA adopts a ‘gate to gate’ approach,
transport, use and disposal of EG is not included in this report. The processing stages of
MEG production include syngas separation, DMO synthesis, DMO purification, MN
synthesis, dehydration, hydrogenation and EG purification. In order to evaluate the
impacts, all inputs such as raw materials, water, electricity and energy as well as outputs
such as emissions and waste for all the processes involved are taken into consideration
for this LCA.
8.3.1.2 Methodology
The methodology taken in this LCA includes defining the goal and scope of the LCA,
conducting inventory analysis of raw material usage and emissions, investigating impact
assessment, evaluating results of assessment as well as concluding the LCA by
providing improvement decisions. The definition of goal and scope is the first step of
LCA and to ensure consistent performance of LCA. The goal and scope include
defining functional unit, system boundary and assumptions. Inventory analysis of raw
material usage and emissions is conducted by extracting data of raw material usage and
emissions for each of the process involved. The raw material usage includes syngas,
electricity and water whereas the emissions are gases contributing to GWP such as CO 2
and methane. The next step is evaluation of impact assessment which includes GWP
and RD. Comparison between sustainability of each process is also conducted. Lastly,
this LCA is concluded by introducing improvement decisions to reduce environmental
impacts caused by the emissions.
293
8.3.1.3 Functional Unit

In this LCA, the functional unit chosen as basis for comparison of the sustainability of
each section is 1 tonne of EG produced. The functional unit is chosen to allow
consistent comparison and investigate and evaluate impact assessment based on
environmental impacts.
8.3.1.4 Assumptions and Limitations

1. The impact categories in this LCA are restricted to GWP and RD.
2. The inputs and outputs of transportation of raw material is neglected due to
insufficient data.
3. Fugitive emissions from process equipment are not accounted for this LCA due to
insufficient data.
4. Water treatment system is not considered in this LCA due to insufficient data.
8.3.1.5 System Boundary

The system boundary, including inputs and emissions of every process for the
production of EG is shown in the figure below.
Figure 8.3.1.5.1: System boundary showing all stages of EG production

The figure above shows the system boundary for this LCA report. The stages involved
include syngas separation, DMO synthesis, MN synthesis, dehydration, DMO
purification, hydrogenation as well as EG purification. For EG production, syngas is fed
to syngas separation, namely COSORB and PSA to separate syngas into CO and H 2.
CO is fed to DMO synthesis, whereby CO reacts with MN (from MN synthesis section)
to form DMO and NO. Unreacted CO and NO is recycled back to MN synthesis for MN
regeneration, meanwhile producing water, which is sent to dehydration columns. DMO
294
product is sent to DMO purification, then hydrogenation. In hydrogenation section,

DMO reacts with H2 (from PSA) to produce EG, which is then sent to EG purification
to obtain the finished product. All the processes require electricity and water while
emitting gaseous emissions, which are summarized in the figure above.
8.3.1.6 Inventory Analysis

Table 8.3.1.6.1: Inventory Data for Input
Syngas DMO DMO MN EG
Input Dehydration Hydrogenation
Separation Synthesis Purification Synthesis Purification
Petroleum
7.48E-01 6.57E-01 1.59E-04 4.67E-02 7.73E-04 4.43E-01 2.36E-04
(kg)
Natural
5.24E+02 4.60E+02 1.11E-01 3.27E+01 5.42E-01 3.10E+02 1.65E-01
Gas (kg)
Coal (kg)
9.76E+00 8.57E+00 2.07E-03 6.10E-01 1.01E-02 5.78E+00 3.08E-03
Electricity
3.00E+02 2.63E+02 6.37E-02 1.87E+01 3.10E-01 1.78E+02 9.47E-02
(kWh)
Water (L)
6.71E+03 0.00E+00 8.29E+01 5.85E+04 0.00E+00 0.00E+00 0.00E+00
Table 8.3.1.6.2: Inventory Data for Output

Syngas DMO DMO MN EG
Input Dehydration Hydrogenation
Separation Synthesis Purification Synthesis Purification
CO (g)
2.03E+04 2.19E+05 1.05E+02 0.00E+00 0.00E+00 1.84E+03 1.24E+01
CH4 (g)
2.31E+05 0.00E+00 0.00E+00 0.00E+00 0.00E+00 0.00E+00 0.00E+00
VOCs (g)
0.00E+00 1.67E+04 2.56E+03 0.00E+00 0.00E+00 3.03E+02 1.30E+05
NO (g)
0.00E+00 9.43E+04 1.36E+02 0.00E+00 9.11E+04 8.66E+01 1.29E+03
H2 (g)
1.47E+04 0.00E+00 0.00E+00 0.00E+00 0.00E+00 2.29E+04 0.00E+00
8.3.1.7 Impact Assessment

The graphs showing comparison of the impact categories of each section are shown
below. The detailed calculations and summarized tables for each section are attached in
the Appendix A8.1.
295
Figure 8.3.1.7.1: Comparison of GWP for each section of the process
Figure 8.3.1.7.2: RD comparison for each section of the process
The impact categories that are assessed in this LCA for all the processes are
summarized in the table.
Table 8.3.1.7.1: Impact assessment for the entire process
Impact Category Impact Score
Global Warming Potential (kg CO2-eq) 14670.97
Resource Depletion (kg) 8.25 × 10−12
Based on Figures 8.3.1.7.1 and 8.3.1.7.2, it is observed that the comparison of impact
categories for each section of the process is conducted. From Figure 8.3.1.7.1, syngas
separation contributes to the highest GWP due to a large amount of CO, methane and H 2
296
emission from the separation processes. The largest contributor of GWP is followed by
DMO synthesis and dehydration whereas DMO purification and hydrogenation
contributes to little GWP. MN synthesis contributes no GWP as no waste is emitted in
this section.
From Figure 8.3.1.7.2, it is seen that syngas separation has the highest RD. The
electricity required by the process is the highest whereas the water intake is the second
highest after MN synthesis. However, as MN synthesis requires little electricity, the
impact score of RD is also less as compared to syngas separation. DMO synthesis and
hydrogenation comes after syngas separation. The graph in figure 8.3.1.7.2 shows that
the difference of RD impact score for DMO purification, dehydration and EG
purification is unnoticeable. However, based on calculations in the appendix, the section
that contributes to the least RD is DMO purification, which is6.92 × 10−16 kg.
Table 8.3.1.7.1 shows the impact score for each assessed category for the entire process.
The GWP for all the process is 14670.94 kg CO2-eq whereas that of RD is 8.25 ×
10−12 kg. This impact score is calculated based on the aforementioned functional unit,
which is 1 tonne of EG produced.
In conclusion, syngas separation contributes to the highest of both GWP and RD,
followed by DMO synthesis. DMO purification contributes the least to the total of GWP
and RD. Some improvements can be done in order to minimize the impact and increase
the environmental sustainability of the plant. As syngas separation is the main
contributor of GWP, the composition of syngas can be improved in such a way that it
emits less CO, methane and H2. The electricity and water usage of syngas separation
can also be reduced by using high efficient absorption columns. The total water usage of
the plant can also be reduced by performing water integration and water reuse. On the
other hand, the environment impact can be reduced by treating the gas before releasing
it.
297
8.3.2 Risk Assessment

8.3.2.1 Environmental Aspect and Impact Register
Goal, Objectives and Specific Targets
An Environmental Aspect and Impact Register will be carried out in this section of the
report to assess the environmental impacts of the production of MEG of this plant. The
Impact Register covers the activities in the plant during normal operation which
includes operation during cleaning and maintenance. Different criteria are taken into
consideration throughout this study. The table below shows the different criteria and
their definition to have a clearer understanding of how these criteria are assessed.
Table 8.3.2.1.1: Criteria assessed and their definitions

Criteria Assessed Definition of criteria
Defined by the any actions carried out by the organization
Activity
during normal operation.
All kinds of organization activity, services or products
Environmental Aspect
that involves interacting with the environment.
Changes to the environment made through that
environmental aspect regardless of it being beneficial or
Environmental Impact
harmful. Includes changes to the environment made
through partial involvement of organization activities.
The likelihood that a harmful
consequence might result when
Unmitigated Risk
exposed to the hazard without
(Pre-control risk)
implementation of the proposed
mitigation measures.
Risk (R)
The likelihood that a harmful
consequence might result when
Residual Risk
exposed to the hazard with the
(Post-control risk)
effective implementation of the
proposed mitigation measures.
The chance or probability of an event resulting in an
Likelihood (L)
impact occurring.
Defined by how much harm the impact could have, how
Consequence (C) many people it could affect and the duration of harmful
state.
The magnitude of the damage or harm that can be caused
Significance (S)
by the respective impacts.
Actions to be taken to help minimize potential impacts to
Mitigation Measures
the environment and reduce the likelihood of the
298
associated risks.
The procedure for the development of Environmental Aspects and Impact Register can
be seen from the table below.
Table 8.3.2.1.2: Steps for development of Environmental Aspects and Impacts Register
Identify, decide and list out the activities in the plant that are major enough
Step 1
to contribute to the environmental aspects during all operations.
Step 2 Identify the environmental aspects that are related to the activities listed out.
Step 3 Identify the environmental impacts with respective environmental aspects.
Step 4 Identify related guidelines and legislation involved.
Rank and determine the likelihood and consequence of the event and then
Step 5 evaluate the significance of identified impacts before the implementation of
mitigating measures. (Unmitigated Risk)
Propose and implement control or mitigating measures to the event
Step 6
happening.
Rank and determine the likelihood and consequence of the event and then
Step 7 evaluate the significance of identified impacts after the implementation of
mitigating measures. (Residual Risk)
8.3.2.3 Risk Assessment Methodology and Matrix

In this study, the risk assessment matrix system is adopted to help assess the risks
involved. By using this matrix as shown below, the likelihood and consequence of an
occurring event during plant operations can be quantified.
Figure 8.3.2.3.1: Risk Assessment Matrix
The quantification of both factors would be required before the significance can be
determined through the equation below.
299
𝑆𝑖𝑔𝑛𝑖𝑓𝑖𝑐𝑎𝑛𝑐𝑒 = 𝐶𝑜𝑛𝑠𝑒𝑞𝑢𝑒𝑛𝑐𝑒 𝑆𝑐𝑜𝑟𝑒 × 𝑃𝑟𝑜𝑏𝑎𝑏𝑙𝑖𝑡𝑦 𝑆𝑐𝑜𝑟𝑒
The magnitude of significance score has respective definitions and is further explained
in the table below. The detailed scores given to different activities of the plant can also
be seen in the later part of the report in form of tables.
Table 8.3.2.3.1: Significant Level and its description

Significant Level Score Description
Acceptable risk of low magnitude in which the
Low 1 to 5 impacted individuals are ready to accept, therefore
no control or mitigation is required.
Tolerable risk of moderate magnitude that is within
range where impacted individuals can still live with
Medium 6 to 10 to secure certain benefits. Risk is classified under
non-negligible and needs to be reduced further if
possible.
Tolerable risk of high magnitude that is within
range where impacted individuals can still live with
High 11 to 15 to secure benefits. Risk needs to be reduced further
as soon as possible with necessary mitigation
measure being introduced and implemented.
Intolerable risk of extreme magnitude that is
unacceptable for impacted individuals and society.
Extreme 16 to 25 When risk is still present, the plant operation should
not be continued unless risks are controlled with
appropriate mitigation measures.
8.3.2.4 Risk ranking definitions and Score justifications

To provide a score for the likelihood and consequence of an occurring event, definitions
and justifications has been developed and is to be followed to ensure a uniform scoring
throughout the assessment. The table below shows the scoring descriptions for
probability (likelihood) of an occurring event.
Table 8.3.2.4.1: Rating of Likelihood of an occurring event

Probability Rank Description Definition/Justification
Almost Will almost certainly occur. Has a 95% or greater
5
certain chance of occurring within a 12-month period.
Probably will occur. Has a 70% to 95% chance of
4 Likely
occurring within a 12-month period
3 Possible May possibly occur. Has a 30% to 70% chance of
300
occurring within a 12-month period.

Could possibly occur. Has a 5% to 30% chance of
2 Unlikely
occurring within a 12-month period.
Only likely to occur in exceptional circumstances.
1 Rare Has a 5% or less chance of occurring within a 12-
month period.
The consequence ranking will also be strictly following the rating matrix below.
Table 8.3.2.4.2: Rating of Consequence of an occurring event

Consequence
Description Definition/Justification
Rank
Non-reversible long-term impacts in less than 10
years. Significant degradation towards environment
5 Catastrophic
and has significant impact on human health and
safety.
Reversible long-term impacts in 2-10 years. Major
4 Major degradation to the environment and impact on
human health.
Moderate environmental harm that is contained on-
site or only have minor widespread harm that is
3 Moderate reversible in a span of less than 2 years. Moderate
degradation to the environment and impact on
human health.
Unplanned on-site environmental harm that does not
2 Minor spread off-site. Has insignificant impacts on the
environment and human health and safety.
Insignificant impacts that are contained strictly on-
1 Insignificant site. No environmental disturbances and impacts on
human health.
301
8.3.2.5 Environmental Aspects and Impacts Register Matrix

The Environmental Aspects and Impacts Register is done for the normal phase of operation.
Phase of Operation: Normal

Unmitigated Residual
Environmental Environmental Legislation
No. Activity Risk Mitigation Measures Risk
Aspect Impact Involved
L C S L C S
 Degradation in  Efforts to switch to  Environmental
air quality due a cleaner fuel for Quality
Emissions from
to air vehicles used for (Control of
exhaust gases
emissions transportation Emission from
coming from
 Contribute to  Perform regular Diesel Engines)
transport such as
increase in servicing on Regulations
CO, NOx, SOx
Global 5 3 15 vehicles used for 2000 3 3 9
and particulate
Warming transportation  Environmental
matters coming
Raw Materials Potential Quality (Clean
from heavy
and Products (GWP), Air)
vehicle’s brakes
1. transportation in Human Regulations
and tyres.
and out of the toxicity and 2014
plant acidification
 Noise pollution  Switch to different  Environmental
to nearby route that avoids Quality (Motor
victims and residential areas to Vehicle Noise)
Noise generated
residents the plant
from engines of 4 1 4 2 1 2
vehicles.  Perform regular
servicing on
vehicles used for
transportation
2. Pump operation Electricity  Contributes to 4 3 12  Supply pump and  National 2 3 6
302
in plant and Consumption resource compressors with Conservation

Compressor to depletion due just enough amount Strategy 1993
compress gases to usage of fuel of power to keep  Environmental
to generate operation Quality (Clean
electricity unhindered Air)
required  Invest in pump and Regulations
compressors 2014
designs that are
more energy saving
 Minimize number
of pumps required
through utilizing
gravity flow as
much as possible
 Noise pollution  Implement noise  Factories and
to nearby absorbing material Machinery
workers and to walls (Noise
Noise generated residents surrounding the Exposure)
from pump and pump and Regulations
4 1 4 2 1 2
compressor compressors 1989
operation  Earplugs to be
provided to
operators and
workers
 Water pollution  Control amount of  Environmental
Use of cooling
Wastewater if discharge blowdown water to Quality
water as cooling
generation from untreated discharge to (Industrial
3. utility in 3 4 12 1 3 3
cooling water wastewater to environment Effluents)
processes in the
blowdown environment  Treat wastewater Regulations
plant
which leads to before discharging 2009
303
aquatic and it to the

human toxicity environment
 Contributes to  Implement ways to  National
resource minimize cooling Conservation
Water consumption as water blowdown Strategy 1993
4 1 4 3 1 3
Consumption clean water is a and improve
limited recycled water
resource usage
 Contributes to  Use only thermal  National
resource fluids with just the Conservation
depletion right amount of Strategy 1993
Use of heating
through usage heating duty
utilities in Fuel
4.
processes in the Consumption
of fuel to heat 4 2 8  Performing heat 2 2 4
up utilities integration within
plant
such as thermal process streams to
fluids minimize utility
required
 Potential  Ensure that there  Environmental
pollution to are proper operating Quality
water sources procedures for (Control of
and land which operations which Pollution from
Accidental can lead to includes the Solid Waste
Catalyst handing spillage of human and handling of catalyst Transfer Station
5. of all reactors in catalyst during aquatic toxicity 3 3 9  Supervising major and Landfill) 2 2 4
the plant maintenance or maintenance Regulations
checking procedures to 2009
ensure workers
strictly follows
operating
procedures
304
 Contamination Provide proper  Environmental

of land and storage for spend Quality
Solid Waste water sources catalyst (Scheduled
Generation from if wastes not 3 3 9  Sending spent Wastes) 2 1 2
spent catalyst handled catalyst to Schedule Regulations
properly Waste Facility 2005
before disposing
 Harm land and  Regular inspection  Environmental
water source on Quality
contamination valves/flanges/pipel (Industrial
Wastewater
if leakage ines Effluents)
Syngas generation from
12  Ensure proper
occurs and is Regulations
6. Separation leakages and 3 4 2 2 4
discharged to operating 2009
process maintenance
the procedures are
procedures
environment available for
maintenance
operators to follow
 Contributes to  Implement more  National
resource effective ways to Conservation
depletion as clean equipment to Strategy 1993
Water
clean water is 4 1 4 reduce water usage 2 1 2
Consumption
Maintenance not an infinite  Only use water for
and cleaning resource cleaning when it is
7. operations on necessary
equipment in the  Contributes to  Avoid performing  National
plant resource unnecessary Conservation
Electricity depletion due maintenance and Strategy 1993
4 1 4 2 1 2
Consumption to fuel cleaning operations
consumption to to reduce frequency
generate of maintenance
305
electricity
 Potential land  Perform checking  Environmental
and water of the quality of Quality
source wastewater and (Industrial
Wastewater
contamination ensure it meets the Effluents)
generation from
if wastewater is standard before Regulations
cleaning and 3 4 12 2 2 4
discharged discharging to the 2009
washing of
directly to the environment
equipment
environment  Treat wastewater
before discharging
to the environment
 Land and water  Sludge produced to  Environmental
source be filtered and Quality
contamination stored in proper (Scheduled
if sludge enters storage and sent to Wastes)
Sludge
the soil or 3 4 12 Schedule Waste Regulations 2 2 4
Generation
water flow Facility 2005
which can lead
Wastewater to aquatic and
treatment of human toxicity
8. wastewater  Degradation in  Implement ways to  Environmental
generated in air quality due reduce the amount Quality (Clean
plant to air of wastewater Air)
emissions produced from Regulations
Air emissions
 Contribute to processes in the 2014
from aeration 4 3 12 3 2 6
increase in plant
process
Global  Situate aeration
Warming tanks away from
Potential residential areas
(GWP), nearby and consider
306
Human downwind direction

toxicity and
acidification
 Foul smell
causing
discomfort to
nearby victims
and residents
 Land and water  Ensure storage for  Environmental
source wastes are checked Quality
contamination regularly for (Scheduled
if wastes enter leakages and that it Wastes)
the soil or is sealed tightly Regulations
Temporary Leakage of water flow  Ensure that standard 2005
9. storage of wastes to the which can lead 3 4 12 operating 2 2 4
Schedule Waste environment to aquatic and procedures are
human toxicity available to
operators to handle
spillage and tools to
handle spillage are
available nearby
 Land and water  Wastewater from  Environmental
source steam ejector Quality
Wastewater
contamination system should be (Industrial
Vacuum generation from
if wastes enter treated before Effluents)
Distillation steam ejector
10. the soil or 4 3 12 discharging to the Regulations 2 1 2
Column usage which
water flow environment 2009
Operation contains
which can lead  Checking the
hydrocarbons
to aquatic and quality of
human toxicity wastewater to
307
ensure the standards

are met before
discharging to
environment
 Land and water  Ensure storage for  Environmental
source chemicals are Quality Act
contamination checked regularly 1974
if wastes enter for leakages and
the soil or that it is sealed
water flow tightly
which can lead  Provide training on
to aquatic and proper handling of
Storage of raw human toxicity chemicals to
Leakage of
materials and workers to
11. chemicals to the 3 4 12 1 4 4
chemicals to be minimize incident
environment
used in the plant occurrence
 Ensure that standard
operating
procedures are
available to
operators to handle
spillage and tools to
handle spillage are
available nearby
308
Chapter 9: HAZOP
Study
309
9.1 Introduction
A hazard and operability study (HAZOP) was carried on two different nodes which are
distillation column (D-501) and reactor (R-201). HAZOP is a study where the process or
node is carefully reviewed in a systematic manner to determine whether the deviations from
the design or operating conditions will lead to consequences which are undesirable. The
HAZOP study are usually carried out when the final design of the plant has been completed.
This study aims to identify and evaluate any malfunction and mal-operation that could cause
potential hazards which would cause serious effects on the plant. The HAZOP study will be
carried out on equipment which are involved in the nodes. After determining the potential
hazards, the following is then be determined, the causes, consequences and safeguards.
Lastly, a recommended action will be given to mitigate the situation.
The node to be examined will be from the DMO synthesis process and the dehydration
process of the plant. When carrying out the HAZOP study, each group member was given a
task which will be shown in the table below.
Table 9.1.1 HAZOP team for DMO Synthesis and Dehydration process of the plant.
HAZOP Study
Process Involved i. DMO Synthesis
ii. Dehydration
Equipment Involved R-201, E-501, P-501 and D-501
Ref. Drawing No. P&ID201 & P&ID 5-1
Group Members Role Responsibilities
Wong Yoong Chin Designer/Facilitator Designer of the studied nodes. Conduct
andalso ensuring that minutes are
recorded correctly
Chew Ai Hsin Operations Engineer Accept the completed facility and
ensuring the performance target is met.
Tan Hao Yang Maintenance Engineer Ensure all equipment undergoes
maintenance.
Chew Shi Phay Designer Designer of the studied nodes.
Chong Koon Meng Control and Responsible for the instrumentation and
Instrumentation control system of the plant.
Engineer
Muhamad Dzaki Design Team Project Making sure that the project is completed
Fadhlurrohman Engineer on time and does not exceed the budget
for the required target of product.
Alexander Lim Zhi Scribe Record meeting minutes from HAZOP
Chin review.
310
9.2 HAZOP Meeting Minutes

9.2.1 Meeting Minutes for DMO Synthesis Process
Project: Production of Methyl Ethylene Glycol (MEG) from Node Reference: P-204-300-40-CS-H consisting of IV-219 to IV-222, FCV-206, BV-207,
Table 1
Syngas Feedstock using DMO process ESV-201, and DV-212 and DV-213
Date: 7/10/2017
Node Description: Process stream containing CO into DMO synthesis reactor R-201
Group: 6
Item Guide
Parameter Possible Causes Consequences Safeguards Other Recommended Actions
No. Word
 Blocked pipe.  Pressure build up in  FIC-206 to ensure constant  Regular inspection and maintenance to ensure no
 FCV-206 malfunction pipeline causing pipe flowrate pipe/flange/valve leakage
 Pipe/flange/valve leakage rupture.  Operators should quickly response to related control valves
 IV-219, IV-220, IV-221, IV-  Leakage of CO to when alarm sounds
1 No/Low Flow 222, ESV-201 jam shut surrounding causing  Operators should ensure all isolation valves fully open and
 DV-212 and DV-213 jam toxic environment drain valves fully close during start-ups
open  No reaction in R-201
 FIC-206 signal failure  Increased flow in  Incorporated FAL/H in  Operators should be alert when FAH rings and check on
 FCV-206 malfunction downstream. pipeline valves and controllers as well as contact upstream operators to
 R-201 overpressure decrease flow in stream
2 High Flow  Possible explosion of  Regular inspection and maintenance on valves/controllers to
vessel. prevent malfunction
 Pipeline rupture
 High pressure in R-201  No reaction in R-201  ESV-201 to shut down the  Introduction of check valve
3 Reverse Flow process and prevent
backflow
 Thermal overpressure from  Pressure build up in  Control loop 203 to  Ensure proper selection of pipe material, thickness and
upstream pipeline causing pipe monitor and regulate the schedule to avoid pipe rupture
 Increased flow from rupture stream temperature  Regular inspection and maintenance on valves/controllers to
upstream  Overpressure in R-201 prevent malfunction
4 High Pressure
 Blocked pipe  Operators should quickly response when TIC-203 alarm
 FCV-206 malfunction sounds and contact upstream and downstream operators to
 IV-219, IV-220, IV-221, IV- carry out respective measures
222, ESV-201 jam shut
 Low temperature from  Underpressure in R-201  Control loop 203 to  All actions to be the similar to the actions taken when high
upstream  Backflow of stream due monitor and regulate the pressure
 Decreased flow from to high pressure in Node stream temperature  Regular inspection and maintenance on valves/controllers to
upstream 2 prevent malfunction.
5 Low Pressure
 Pipe/flange/valve leakage
 FCV-206 malfunction.
 DV-212, DV-213 jam open
311
 TT-203 signal failure  Corrosion in pipeline  TT-203 and TIC-203 to  Regular inspection and maintenance on valves/controllers to
 TIC-203 malfunction  High temperature in monitor and regulate the prevent malfunction
downstream affecting R- stream temperature  All actions to be the similar to the actions taken when high
6 High Temperature
201  Hot insulation in pipeline pressure
 Operators should be fully equipped with safety gear to avoid
direct contact of heat to skin
Project: Production of Methyl Ethylene Glycol (MEG) from Node Reference: P-206-600-40-CS-H consisting of IV-232 to IV-235, FCV-208, BV-210, ESV-
Table 2
Syngas Feedstock using DMO process 202, and DV-217 and DV-218
Date:7/10/2017
Node Description: Process stream containing MN into DMO synthesis reactor R-201
Group: 6
Item Guide
No. Word
 Blocked pipe.  Pressure build up in  FIC-208 to ensure constant  Regular inspection and maintenance to ensure no
 FCV-208 malfunction. pipeline causing pipe flowrate pipe/flange/valve leakage
 Pipe/flange/valve leakage rupture  Operators should quickly response to related control valves
 IV-232, IV-233, IV-234, IV-  Leakage of MN to when alarm sounds
235, ESV202 jam shut surrounding leading to
explosion.
1 No/Low Flow  No reaction in R-201.
 FIC-208 signal failure  Increased flow in  Incorporated FAL/H in  Operators should be alert when FAH rings and check on
 FCV-208 malfunction downstream. pipeline valves and controllers as well as contact upstream operators
 R-201 overpressure. to decrease flow in stream
2 High Flow  Possible explosion of  Regular inspection and maintenance on valves/controllers
vessel to prevent malfunction
 Pipeline rupture.
 High pressure in R-201  No reaction in R-201  ESV-202 to shut down the  Introduction of check valve.
process to prevent backflow
3 Reverse Flow
312
 Thermal overpressure from  Pressure build up in  Control loop 208 to prevent  Ensure proper selection of pipe material, thickness and
upstream. pipeline causing pipe thermal overpressure schedule to avoid pipe rupture.
 Increased flow from upstream rupture  Operators should quickly response when TIC-208 alarm
 Blocked pipe  Overpressure in R-201. sounds and contact upstream and downstream operators to
 FCV-208 malfunction. carry out respective measure
 IV-232, IV-233, IV-234, IV-  Regular inspection and maintenance on valves/controllers
4 High Pressure 235, ESV202 jam shut to prevent malfunction
 Low temperature from  Underpressure in R-201  Control loop 208 to monitor  All actions to be the similar to the actions taken when high
upstream  Backflow of stream due and regulate the stream pressure
 Decreased flow from upstream to high pressure in Node temperature  Regular inspection and maintenance on valves/controllers
 Pipe/flanges/valves leakage 1 to prevent malfunction
 FCV-208 malfunction.
 DV-218, DV-218 jam open
5 Low Pressure
 TT-208 signal failure  Corrosion in pipeline  Control loop 208 to monitor  All actions to be the similar to the actions taken when high
 TIC-208 malfunction  High temperature in and regulate the stream pressure
downstream affecting R- temperature  Operators should be fully equipped with safety gear to
201  Hot insulation in pipeline avoid direct contact of heat to skin
6 High Temperature  Regular inspection and maintenance on valves/controllers
to prevent malfunction
Project: Production of Methyl Ethylene Glycol (MEG) from

Node Reference: Reactor R-201 Table 3
Syngas Feedstock using DMO process
Date: 8/10/2017
Node Description: DMO Synthesis Reactor
Group: 6
Item Guide
No. Word
313
 Tube blockage.  Reduced rate of reaction  No safeguard  Set up of a regular inspection and maintenance schedule to
 Decreased flow in Node 1 and  Downstream process ensure no blockage of tube/valves
Node 2. affected  Set up of a scheduled maintenance as part of MPS to ensure
 Blockage and leakage in smooth operation in tube side
1 Low/No Flow
upstream and vessel  Introduction of ratio controllers (RC) in upstream to ensure
 IV-244 jam open. proportionate feed
 FCV-206 and FCV-208
malfunction
 Increased flow in Node 1 and  Downstream process  No safeguard  Operators should check on to FCV-206 and FCV-208 when
Node 2 affected high flow occurs to ensure the control valves function
 FCV-206 and FCV-208  R-201 subject to high properly
2 High Flow malfunction pressure  Regular inspection and maintenance on valve/controllers to
prevent malfunction
 Introduction of ratio controllers (RC) in upstream to ensure
proportionate feed.
 Thermal overpressure from  Pressure build up in  Control loop 202 to  Operators should response quickly when TIC-202 sounds by
upstream. vessel causing vessel prevent thermal ensuring pressure of vessel within control. Shall pressure go
 Increased flow from upstream rupture. overpressure beyond control, operators to contact other operators to
 Tube blockage  Downstream product is  PSV-203 and PSV-204 to prepare for emergency shut down procedures
3 High Pressure  PT-210 signal failure. affected, higher rate of relief pressure build up  Regular inspection and maintenance on valves/controllers to
 IV-238, IV-242, IV-245 jam formation of undesired  SIS-201 to shut down prevent malfunction
shut product over desired process in critical  Ensure proper mechanical design and selection of vessel
product conditions material and thickness to prevent vessel rupture
 Low temperature from  Underpressure in R-201  Control loop 202 to  Operators to check for open valves and leakages when TIC-
upstream  Backflow of stream due monitor and regulate the 202 alarm sounds
 Decreased flow from to high pressure in P- stream temperature  Regular inspection and maintenance on valves/controllers to
4 Low Pressure upstream 204. prevent malfunction
 Pipe/flanges/valves leakage.  Rate of reaction affected  Ensure proper mechanical design and selection of vessel
 DV-219, IV-240, IV-244 jam material and thickness
open
314
 TT-202 signal failure.  Thermal runaway  Control loop 202 to  All actions to be the similar to the actions taken when high
 TIC-202, TCV-202 reaction monitor and regulate the pressure
malfunction  Downstream product is stream temperature through  Regular inspection and maintenance on transmitter and
 Increased temperature from affected, higher rate of coolant flowrate. controller to prevent malfunction
Node 1 and Node 2 formation of undesired  Feedback controlTT-211  Operators should be fully equipped with safety gear to avoid
product over desired and TAHH-207 direct contact of heat to skin
product incorporated with PAHH-
 Possible thermal 204 to trigger the SIS to
5 High Temperature expansion in tube side shut down the operation
 Hot insulation in vessel
 Coolant used in shell-side
of R-201 to remove heat
generated by reaction
 TT-202 signal failure  Low rate of reaction in  Control loop 202 to  Operators should quickly response when TIC-202 alarm
 TIC-202 malfunction R-201 monitor and regulate the sounds and contact upstream and downstream operators to
6 Low Temperature  TCV-202 jam open stream temperature through carry out respective measures
 Decreased temperature from coolant flowrate
Node 1 and Node 2

Node Reference: P-207-700-STN-CS-P consists of IV-238. Table 4
Date: 8/10/2017
Node Description: Process stream flowing out of DMO synthesis reactor R-201
Group: 6
Item Guide
No. Word
 Pipe/flanges/valves leakage  Leakage of DMO to  Nitrogen is fed into R-201  Regular inspection and maintenance to ensure no
 IV-238 jam shut and IV-244 surrounding leading to to dilute the concentration pipe/flanges/valves leakage
jam open. flammable surrounding of flammable and  Operators should quickly response to related control valves
 PSV-203 failure  Downstream process is explosive gas when alarm sounds
1 Low/No Flow affected  Operators should ensure all isolation valves fully close
during start-ups
315
 Increased flow from Node 1  Increased flow in  Not critical as the  Ensure proper selection of pipe material, thickness and
and Node 2 into R-201 downstream occurrence is very unlikely schedule to avoid pipe rupture
 Runaway reaction occurred in  Pressure build up in
2 High Flow
R-201 pipeline causing pipeline
rupture
 Thermal overpressure from  Pressure build up in  Safeguard is being  Ensure proper selection of pipe material, thickness and
3 High Pressure upstream pipeline causing pipe considered in R-201 schedule to avoid pipe rupture.
 Increased flow from upstream rupture
 Insufficient flow from  Downstream affected  No safeguard  Regular inspection and maintenance on valves to prevent
upstream  No severe consequences malfunction
 Pipe/flanges/valves leakage
4 Low Pressure  IV-244 jam open and PSV-203
failure
 Thermal runaway reaction in  Corrosion in pipeline  TT-211 to monitor pipeline  Operators should response quickly to TAHH-207 by
R-201  High temperature in temperature and TAHH- contacting upstream and downstream operators for
 Increased temperature in Node downstream require 207 to trigger SIS to shut emergency shut down procedures
1 and Node 2. higher cooling duty in E- down the operation.  Regular inspection and maintenance on transmitter to
 TT-202 and TCV-202 failure 202  Hot insulation is installed prevent malfunction
5 High Temperature on pipeline.  Ensure proper selection of pipe material, thickness and
schedule to avoid pipe rupture
 Operators should be fully equipped with safety gear to avoid
direct contact of heat to skin
 Low reaction temperature in  No significant  No safeguard  Not recommended for over control
R-201 consequences
6 Low Temperature  Low temperature in Node 1
and Node 2
316
9.2.2 Meeting Minutes for Dehydration Process
Project: Production of Methyl Ethylene Glycol (MEG) from Node Reference: S1-501-150-40-CS-H consisting of IV-501, IV-502, PV-501, BPV-501, DV-
Table 5
Syngas Feedstock using DMO process 501 and DV-502
Date: 7/10/2017
Node Description: Saturated Steam supply to tube side of heat exchanger E-501
Group: 6
Item Guide
No. Word
 IV-501 or IV-502  Undesired flow  Install PIA 503  Weekly inspection routines to ensure all valves are functioning and leakages does not occur
jam shut of utility stream (H/L) before IV-  Operators should contact upstream operators to ensure that steam supply is normal when alarm
 BPV-501 jam shut into E-501 501 rings
 Lack of saturated leading to  Install PIA 504  Operators to be fully equipped with PPE and perform inspection on valves when alarm rings
steam going into the insufficient (H/L) after IV-502
E-501 from supply heating for the  Incorporation of
1 No/Low Flow  PV-501 malfunction. process fluid surrounding
 Pipeline/flange/valve  Leakage of high temperature
leakages temperature sensors
steam leading to
potential injury
to operators in
charge
 PV-501 jam open.  Undesired flow  Install PIA 503  All actions to be the similar to the actions taken when No/Low Flow occurs
 Over supply for of utility stream (H/L) before IV-  Materials selected for construction is suitable for the operating conditions
saturated steam going into E-501 501
into E-501 leading to  Install PIA 504
2 High Flow  BPV-501 Jam Open overheating of (H/L) after IV-502
process fluid  Incorporation of
 Pipe Rupture surrounding
leading to temperature
leakage sensors
 Lower temperature of  Insufficient  Install TIA-511  Operators should contact upstream operators to ensure that steam supply is at desired
3 Low Temperature saturated steam heating for the (H/L) before IV- temperature range when alarm rings
supply required process fluid 501
 Higher temperature  Overheating of  Install TIA-511  Actions taken to be similar to recommended actions when Low Temperature occurs
4 High Temperature of saturated steam process fluid (H/L) before IV-
supply required 501
 Lower pressure of  Lower  Install PIA 503  Operators should contact upstream operators to ensure that steam supply is at desired pressure
saturated steam temperature of (H/L) before IV- range when alarm rings
supply required saturated steam 501
5 Low Pressure
going into E-501  Install PIA 504
(H/L) after IV-
502
317
 Higher pressure of  Higher  Install PIA 503  Actions taken to be similar to recommended actions when Low Pressure occurs
saturated steam temperature of (H/L) before IV-  Materials selected for construction is suitable for more extreme operating conditions
supply required saturated steam 501  Weekly inspection routines to ensure all valves are functioning
 IV-501, IV-502 or going into E-501  Install PIA 504
6 High Pressure IV-503 not fully open  Rupture of (H/L) after IV-502
pipeline leading  Incorporation of
to leakage surrounding
temperature
sensors

Node Reference: Heat Exchanger E-501 Table 6
Date:7/10/2017
Node Description: Process stream flowing through shell side of Heat Exchanger E-501
Group: 6
Item Guide
No. Word
 Leakage of contents  Inefficient heat  No safeguard  Weekly inspection routines to ensure no leakage or blockage of streams going into E-501
from shell side or transfer between needed
1 Low Pressure tube side of E-501 two streams
 Blockage of nozzle  Low outlet flow
in shell side inlet of process stream
 Blockage of nozzle  Rupture of shell  PIA-505 (H) for  Operators should stop upstream flow in to E-501 and perform inspection on nozzles of heat
2 High Pressure in shell side outlet side of E-501 shell side of heat exchanger with fully equipped PPE
exchanger
 Low incoming  Higher duty is  Temperature  Operators to coordinate communication with operators of upstream process when low
stream temperature required for more control system 501 temperature detected in the control room
Temperatur from MN synthesis heating has been
3 Low
e reactors  Separation accounted to
 Low incoming flow efficiency affected increase flowrate
of saturated steam of saturated steam
 High incoming  Phase change  Temperature  Operators to coordinate communication with operators of upstream process when high
stream temperature might occur and control system 501 temperature alarm rings to ensure condition of stream coming in
from MN synthesis pump P-501 has been  Monthly inspection for probes and transmitter to ensure functionality of sensors
reactors might be damaged accounted to
Temperatur  High incoming flow decrease flowrate
4 High of saturated steam of saturated steam.
e
 TE-501 or TT-501  Incorporate a TIA-
malfunction 512(H) to alert
operators when
phase change
occurs
318

Node Reference: Pumps P-501A and P-501B including IV-504 and IV-506 Table 7
Date: 8/10/2017
Node Description: Process stream flowing into pump P-501
Group: 6
Item Guide
No. Word
 IV-504 jam shut  Pump cavitation  PIA-506 (L) is to  Weekly inspection routines for leakages in pipelines and nozzle blockage
 Leakage of contents  Downstream be install before P-  Operators should stop the flow of stream going into P-501A
from valves or pressure will not 501  Operators should perform inspection to identify the source of error (leakage/blockage) along
flanges be sufficient the pipeline before the pump
 Blockage at E-501
1 Low/No Flow shell side nozzle
outlet
 Low flow in  Higher pump  PIA-506 (L) is to  All actions to be similar to recommend actions taken when Low/No Flow occurs
pipeline before duty required be install before P-  Operators to coordinate communication with upstream operators to adjust pressure of stream
pump P-501 501
2 Low Pressure  Pressure of stream
coming from the
shell side of E-501
is lower
 High incoming  Thermal  Temperature  Operators to coordinate communication with operators of upstream process when high
temperature from E- expansion might control system 501 temperature occurs
501 occur has been accounted
to decrease
flowrate of
3 High Temperature saturated steam.
 TIA-512(H) is
incorporated
319

Node Reference: Pumps P-501A and P-501B including IV-505, IV-507, DV-504 and DV-505 Table 8
Date: 8/10/2017
Node Description: Process stream flowing out of pump P-501
Group: 6
Item Guide
No. Word
 Blockage at the  Downstream  PIA-507 (L) is to  Weekly inspection routines for nozzle and valve blockage
outlet of pump P- process affected be install after P-  Operators to perform inspection on outlet valve of the pump to ensure no blockage when low
501 501 pressure alarm rings
1 Low/No Flow  IV-505 jam shut  Operators to stop flow into P-501A by closing IV-504 and opening IV-506 to bypass process
stream through P-501B
 Low flow in pipeline  Downstream  Check valve CV-  Actions to be taken similar to recommended actions for when Low/No Flow occurs
after pump P-501 process affected. 501 installed after  Pump maintenance procedures should be well-informed to operators
 Pump cavitation or  Backflow to the pump P-501
2 Low Pressure
malfunction pump might  PIA-507 (L) is to
occur be install after P-
501

Node Reference: Distillation column D-501 Table 9
Date: 8/10/2017
Node Description: Process flow entering distillation column D-501
Group: 6
Item Guide
No. Word
 Low inlet flow into  Quantity of  Level control  Weekly inspection routines for inlet nozzles of D-501
column D-501 desired product system 501 has  Cleaning routines for D-501 twice per year
 Blockage at inlet is lower been implemented
nozzles of D-501  Vapor products
1 Low/No Level  Low reflux flow may flow into
back into columns reboiler, thus
decrease the
reboiler
efficiency
 Blockage at bottom  Backflow into  Check CV-503 has  Cleaning routines for D-501 twice per year.
outlet nozzle of D- reboiler E-503 been implemented  Operators to drain liquid through DV-114 when high level alarm rings
501 may occur to prevent  Monthly inspection for probes and transmitter to ensure functionality of sensors
 LE-501 or LT-501  Operating backflow into
2 High Level
malfunction temperature of reboiler E-503
D-501 not at  Level control
optimum level. system 501 has
been implemented
320
 Low outlet flow  Separation  Temperature  Monthly inspection for probes and transmitter to ensure functionality of sensors
from reboiler E-503 efficiency control system 504  Operators to check with upstream operators to ensure temperature going in to column falls
 Low temperature of affected has been within range when low temperature alarm rings.
inlet flow into D-  Quantity of implemented.  Weekly inspection for reboiler to ensure functionality
3 Low Temperature
501. distillate  Insulation of D-
 TE-504 and TT-504 decreased 501 has been
malfunction implemented to
reduce heat loss
 Low outlet flow  Leak of vapor  PAL-501 should  Weekly inspection for reboiler and valves to ensure functionality
from reboiler E-503 product poses be installed at the  Operators to inspect on leakages on nozzles with full PPE while low pressure alarm rings
 Leakage occurring potential hazard PDI-501  Operators to perform inspection on IV-508 condition
4 Low Pressure at nozzles or to surrounding
flanges in D-501 operators
 IV-508 not fully  Less distillate
closed product obtained
 High outlet flow  Column might  PRV-501 designed  Operators to inspect on working conditions of reboiler E-503 when high pressure alarm rings
from reboiler E-503 rupture and at 10% higher of  Check valves CV-501 should be installed and CV-502 has been implemented.
cause leakage operating pressure
 Less distillate is installed
5 High Pressure
product obtained  PAH-501 should
 Backflow of be installed at the
inlet streams of PDI-501
D-501
9.3 Piping & Instrumentation Diagram

The original P&ID and the modified P&ID for both processes will be shown in the following page.
321
322
323
324
325
Chapter 10:
Plant Layout
326
10.1 Site Selection and Location

The site for this Mono Ethylene Glycol (MEG) production plant was proposed to be at
Jalan Persiaran Tanjung Langsat in Tanjung Langsat Industrial Estate with coordinates
1o27’39.7”N, 103o59’47.1”E. The selected site is as shown in Figure 10.1 below where
it indicates that the vacant site covers an area of 609000m2 (60.9 hectares) which is
more than sufficient for this proposed plant.
Figure 10.1.1: Proposed site for MEG production plant.
In the process of selecting the site, a few factors were also taken into consideration. The
factors considered were mentioned in Chapter 1 of this report and is summarize below:
i. Easy to transport raw material. Raw material can be transport through

pipelines and also can be imported and shipped as it located to a nearby port.
ii. Availability of utilities such as electricity and water (Pwc.global-arena.com,
2017).
iii. Ensure that it satisfies the limits set by Department of Environment where
the plant is 5km away from the nearest residential area and 3km away from
the nearest school.
iv. Availability of land and flexibility for future expansion.
327
10.2 Plant Layout Philosophy

A number of approaches were considered in determining the layout philosophy of this
plant. Two types of layout were used for this plant which is the product layout and
process layout. Product layout is when each equipment are grouped according to its own
respective section based on the product that will be produced by each section. As for
process layout, it is when similar equipment are placed together regardless of the
product that will be produced by each section (Ingram, 2017). As mentioned, both
combinations were used where equipment will be grouped according to sections but
similar equipment in each section will be placed together. The product layout will
ensure that the production jobs can be specifically contained (Ingram, 2017) whereas
process layout will ensure that supervision can be done effectively (YourArticleLibrary,
2014). Apart from the mentioned advantages, other factors were also taken into
consideration:
 Safety
- Ensure that there is a safe distance between processing sites and other
buildings (e.g: office, facilities) to limit the probability of hazards such as
explosion from occuring.
 Plant Operation Convenience
- Equipment which needs regular maintenance and accessed regularly by
operator are to be placed near to the control room. The equipment will also
be spaced appropriately to ensure operator can access the equipment easily
for check-up and maintenance.
 Economic Consideration
- The area for equipment and piping systems should occupy as small space as
possible but not to the point where it compromise the safety of the plant.
This will help in reducing the cost as the length of pipeline needed can be
reduced.
 Future Expansion
- Ensure that there are spaces for expansion when there is a rise in product
demand.
328
10.3 Plant Layout Limitation

After designing the plant layout, there will be certain limitations which should be taken
into consideration.
10.3.1 Wind Direction

As the site was chosen at Tanjung Langsat Industrial Estate, Johor, there will be
limitation due to wind direction as this area will be affected by the monsoonal seasons,
Southern Monsoon from May to September and Northern Monsoon from November to
March. During the monsoonal season, the area will be very humid and there will also be
heavy rainfall which might cause flood within the plant. To avoid flood from occurring
within the plant, flood barriers will be constructed. Besides, the wind direction will also
affect the flare stack location. This is because at upwind location, ignition sources will
be brought closer to flare due to the wind and in downwind location, the whole plant
might be blanketed by flare (Suhaila et al.,2010).
10.3.2 Separation Distance

Equipment should be separated accordingly as there are rules which govern the distance
for certain equipment and also depending on the content of the equipment. Table 10.3.1
and Table 10.3.2 will show the recommended distance between equipment (GAPS
Guideline, 2015).
Table 10.3.2.1: Inter-unit Spacing

All dimensions are in meter
Services Process Utilities Cooling Control Pressure Flare Fire
Units Area Tower Room Storage Station
Tanks
Process 15.24
Units
Utilities Area 30.48
Cooling 30.48 30.48 15.24
Tower
Control 30.48 30.48 30.48
Room
Pressure 106.68 106.68 106.68 106.68
Storage
Tanks
Flare 60.96 91.44 91.44 91.44 91.44
Fire Station 60.96 15.24 15.24 15.24 106.68 91.44
329
Table 10.3.2.2: Intra-unit Spacing

All dimensions are in meter
Equipment Pumps Reactors Columns Compressors Heat
Exchangers
Pumps 1.52
Reactors 3.05 7.62
Columns 7.62 3.05 4.57
Compressors 15.24 9.14 15.24 9.14
Heat 3.05 3.05 3.05 9.14 1.52
Exchangers
10.4 Plant Layout Justification for Process Sections

For the equipment that are not sized, the sizing is assumed based on the standard size of
each particular equipment. The standard size of a centrifugal pump is assumed to be
0.2m in length and 0.6m in width whereas all holding tanks are assumed to have a
diameter of 3 m and a length of 10 m (Shell Global Solutions, 2009). The standard size
of a heat exchanger is assumed to be 4.88 m in length and 0.25 m in diameter, as
suggested in Sinnott (2009). For a single stage compressor, it is assumed to be 1.5 m in
length and 1.5 m in width (Grainger, 2017). The area required for each section of the
process plant is calculated based on the sizing of equipment on ground and the
minimum distance required between each equipment. The area required for each section
is shown in the table below whereas the detailed calculations of the area required are
attached in Appendix A10.1.
Table 10.4.1: Summarized area required for process sections
Section Length (m) x Width (m) Area Required (m2)
Syngas Separation 50.0 x 18.2 910.0
DMO Synthesis 39.7 x 26.2 1040.1
DMO Purification 22.9 x 8.0 183.2
MN Synthesis 52.0 x 42.0 2184.0
Dehydration 16.2 x 9.2 149.0
DMO Hydrogenation 30.0 x 37.5 1125.0
MEG Purification 20.0 x 10.5 210.0
Total Area Required (m2) 5801.4
330
10.5 Plant Layout Justification For Non Process Sections

10.5.1 Security House
There are 2 main entrances to the plant, where one is mainly for light vehicles whereas
the other one is only for heavy vehicles. Each entrance has a security house and
registration room where it houses the displays connected to all closed-circuit televisions
(CCTVs) in every corner of the plant for security purposes. The guard house operates
24 hours and only authorized personnel is granted access. Each security house has an
area of 72 m2 (12 m x 6 m).
10.5.2 Loading Bay and Weighing Bridge

The loading bay is constructed next to the heavy vehicle entrance and it allows raw
materials and finished products to be loaded and unloaded. The location of loading bay
is near to the storage tank, to ease loading and avoid spillage. A weighing bridge and 6
parking spots for trucks are also provided. The loading bay has a length and width of 36
m and 30m respectively, leading to an area of 1080 m2 whereas that of the weighing
bridge is 25 m and 3 m respectively, leading to an area of 75 m2.
10.5.3 Carpark
The carpark is located next to the main entrance and administration building. A
standardized parking space of 2.5 m in width and 5.5 m in length is provided, and a total
of 40 parking slots are allocated, with 10 slots at every row. Additional slots at the
corner, making up to 10 m long and wide, are allocated for motorcycles and bicycles,
and the width of one-way driveway is 4 m. Hence, the total area for parking lot is 1260
m2 (30 m x 42 m).
10.5.4 Administration Building

The administration building is located next to the carpark, away from main processing
sections of the plant. The building has 2 stories, where it houses reception, offices,
working area, rest area, washroom and pantries for the employees. Thus, the area of the
building is 1134 m2 (54 m x 21 m).
331
10.5.5 Control Room

The control room is located at a safe distance away from the main processing sections
of the plant. It houses all control and alarm systems for the plant, where the material of
construction is explosion-proof. The area of control room is 216 m2 (18 m x 12 m).
10.5.6 Cafeteria
The cafeteria is located near the administration building, away from the main sections of
the plant to enhance the hygiene of food and prevent food contamination. The cafeteria,
which can accommodate 100 people, has an area of 100 m2 (10 m x 10 m).
10.5.7 Medical Centre

The medical centre provides treatment and medical check-ups for the employees. It also
houses sick bays, wheelchairs, stretchers and ambulance trolleys. It is located nearby the
emergency exit of the plant to ease transportation in the event of any emergency cases.
The area of the medical centre is 200 m2 (10 m x 20 m).
10.5.8 R&D Laboratory

The lab serves as the quality control as well as product sampling lab. All research
related works are also conducted in the lab. Taking into account of major lab equipment,
hence it has an area of 200 m2 (10 m x 20 m).
10.5.9 Warehouse and Mechanical Workshop

The warehouse stores spare equipment whereas the mechanical workshop provides on-
site services such as equipment inspection, maintenance, repair, cleaning and
fabrication. The total area of this section is 72 m2 (12 m x 6 m).
10.5.11 Utilities Room

The utilities room houses the condensers for thermal oil cycle. As there are 4 types of
thermal oils used in the plant, 4 main condensers are required. Hence, the total area
required is 200 m2 (20 m x 10 m).
10.5.12 Cooling Tower

A cooling tower functions to cool and recirculate cooling water to the heat exchangers
in the main processing sections. For the plant, 2 cooling towers with the base diameter
of 4 m each are required. Hence, the area of cooling tower section is 26 m2.
332
10.5.13 Boiler House

As steam is generated on-site, a boiler house is required. The boiler house is located
near to utilities room and cooling tower. As the steam is generated at 185 oC and 10 bar,
the boiler house is constructed using insulated material to ensure safety of the operators.
As the boiler consists of equipment such as holding tank, boiler feedwater pump,
deaerator and boiler, the total area required by the boiler house is 400 m2 (20 m x 20 m).
10.5.14 Electrical Room

The electrical room is situated in the utilities section of the plant, near the utilities room.
Electrical room acts as the core of the plant as it distributes electricity throughout the
entire plant to provide power to the plant. The area of the electrical room is 35 m2 (5 m
x 7 m).
10.5.15 Tank Farm

Tank farm houses all of the raw materials and products storage tanks and water
reservoirs. The tank farm is located beside the loading bay and heavy vehicles entrance
to ease transportation. The tank farm has an area of 2880 m2 (96 m x 30 m).
10.5.16 Fire Fighting Station

The fire-fighting station is located between the control room, administration building
and main processing sections of the plant to create easy access to the cores of the plant.
The fire-fighting station houses all fire-fighting equipment such as water supply, water
pump, fire extinguishers and fire trucks. The area of fire-fighting station is 120 m2 (12
m x 10 m). In addition to that, water sprinklers are installed in every part of the plant as
a mitigation measure in the case of fire.
10.5.17 Emergency Assembly Point and Emergency Exit

The emergency assembly point is located next to the carpark, where an emergency exit
is also located nearby to the assembly point. The emergency plan for evacuation is
posted at every part of the plant to ensure the safety of all employees. The area of the
assembly point is 315 m2 (21 m x 15 m).
10.5.18 Flare Tower

Flare towers are located at the corner of the plant and away from the administration
building. To ensure health and safety, the flare towers are erected by taking the wind
333
speed and direction into consideration. Assuming each flare tower has a diameter of 2 m
and that there are three flare towers, therefore the total area allocated to the flare towers
is 10 m2.
10.5.19 Wastewater Storage

The wastewater storage is located next to the flare stack and away from administration
building for hygiene and safety purposes. All wastewater from the plant is stored in the
storage before being channelled to the nearby wastewater treatment plant. The area of
wastewater storage is 2500 m2 (50 m x 50 m).
10.5.20 Pipe Rack

Main pipe racks are installed circulating the main processing sections of the plants,
connected to utilities section as well as waste disposal section, i.e. flare stack and
wastewater storage. The pipe racks are designed at elevated height such that fire trucks
and tankers could access the areas. The height of the pipe racks is 4.5 m.
10.5.21 Main Road

Main roads are constructed to ease transportation of vehicles such as fire trucks, tankers
and ambulance. The main roads contain the entire processing sections of the plant, with
a width of 4 m.
10.5.22 Accommodation and Recreational Park

As the plant operates 24 hours, rest areas such as accommodation and recreational park
are provided to the employees. The rest areas are located away from the main
processing sections and the administration building. The total area of accommodation
and the park is 2000 m2 (80 m x 25 m).
334
10.6 Plant Layout Drawing
Figure 10.6.1 Plant Layout Drawing
335
Chapter 11:
Economic
Evaluation
336
11.1 Revenue obtained from products

The product produced in this plant is Mono Ethylene Glycol (MEG) and its sales volume and
determined selling price is tabulated below.
Table 11.1.1 Estimated revenue per year using selling price and sales volume
Estimated Annual
Sales Volume Selling price
Product Revenue (MYR
(tonnes/year) (MYR/tonne)
millions/Year)
MEG 128000 4500 576
11.2 Fixed Capital Cost

The project life of the proposed MEG plant is determined to be 15 years starting from the
year of operation. The total fixed capital cost will be inclusive of both cost for Inside Battery
Limits (IBL) and cost for Outside Battery Limits (OBL). Under the IBL costs, the direct costs
consist of items such as the purchased equipment and their installation, piping, electrical
systems and building facilities whereas the other costs such as engineering services,
construction expenses and legal expenses will be classified under indirect costs. During
calculation for these costs, the location factor and currency exchange factor will also be
considered.
11.2.1 Inside Battery Limits (IBL)

Inside Battery Limits (IBL) refers to everything inside the boundary of detailed cost
estimation for the plant such as purchased equipment costs and their installation, piping and
control instruments. The purchased equipment cost is estimated in US dollars (USD) and will
be further converted to Malaysian Ringgit (MYR) later on. The year of estimation will be
within years 1990, 1994, 2002 and 2004. The year factors will also be considered through the
use of Chemical Engineering Plant Cost Index (CEPCI) to obtain a more accurate estimation
of cost for year 2017. Key assumptions were also made to proceed with calculations are and
shown below (Chemical Engineering Plant Cost Index (averaged over year), 2017):
1. Exchange rate: 1 USD is equivalent to 4.23 MYR.

2. CEPCI values: 357.6 (Year 1990), 368.1 (year 1994), 395.6 (Year 2002), 444.2 (Year
204), 562.1 (Year 2017)
337
The total purchased equipment cost was found to be RM 79.784 million after calculation.
The direct costs and indirect costs are then estimated based on engineering plant factors to
obtain a total IBL cost of RM 370.2 million. The breakdown of values obtained will be
shown in Appendix A11.1.1.
11.2.2 Outside Battery Limits (OBL)

The Outside Battery Limits (OBL) costs are referring to the cost of facilities outside the plant
boundary such as administrative offices, cafeteria, wastewater treatment plant etc. The OBL
cost estimation of the plant is taken from a range of values between 10-40% of the plant’s
IBL cost (Sinnott, 2014). A value of 10% is taken for this MEG plant as there are fewer
facilities outside the boundary of the plant. The OBL cost is calculated to be RM 37.02
million.
11.2.3 Engineering Cost

The engineering cost comes under the IBL cost of the plant and is classified under indirect
costs. The plant produces 128,000 tonnes of MEG per year and is considered to be a
moderate scale plant, therefore is taken as 33% of the purchased equipment cost of the plant.
The engineering cost for the plant is estimated to be RM 26.329 million.
11.2.4 Contingency Cost and other costs

The contingency cost is the extra costs estimated to account for any variation in the project
during the cost estimation phase. A contingency charge of 44% of purchased equipment cost
is used and is found to cost RM 35.102 million. Other indirect costs such as Construction
expenses (RM 32.712 million), Legal expenses (RM 3.191 million) and Contractor’s fee
(RM 17.553 million) were also included by multiplying with their respective factors and is
tabulated in the Appendix A11.2. (Peters, Timmerhaus and West, 2003)
11.2.5 Start-Up Capital

Start-up capital refers to the amount of money that is required to start the operation of a plant.
In this MEG plant, the start-up capital includes the cost of raw materials (NO, O 2, methanol,
syngas), solvents (toluene, copper aluminium chloride), utilities (dowtherm 4000, dowtherm
G, steam, and cooling water), catalyst (Palladium, Cu, SiO2) and process labour wages to
start-up the plant. The assumptions made during the calculation of start-up capital are shown
below:
338
1. The amount of raw materials and utilities for plant start-up are taken as the amount of
raw materials needed during normal operation in 2 hours.
2. The amount of catalysts required for start-up capital of plant is found based on the
volume and weight of catalysts used in reactor (R-201/R-601)
3. The process labour wages for start-up capital is assumed to be 1 month
The detailed calculation of start-up capital is shown in Appendix A11.1.3.6. The summary of
the results is shown in table below:
Table 11.2.5.1: The Summary of start-up capital

Unit Price Quantity Price Price
Component
(RM/kg) (kg) (RM) (RM million)
Raw Material
Syngas 0.70 47965.20 33575.64 0.03
NO(Nitrogen Monoxide) 3.40 131550.60 447832.45 0.45
Oxygen 0.55 8640.00 4714.12 0.00
Methanol 1.61 114385.20 184617.71 0.18
Solvent
CuAlCl4(Cuprous
5.30 135965.00 721158.36 0.72
Aluminium Cholride)
Toluene Solvent 2.70 50707.00 136716.21 0.14
Catalyst
Palladum 8.64 2560.00 22118.40 0.02
Copper 50.00 10020.00 501000.00 0.50
Silicon Dioxide 21.60 40080.00 865728.00 0.87
Utilities
Dowtherm 4000 8.65 3745844.94 32410058.07 32.41
Dowtherm G 23.43 2369405.92 55513068.85 55.51
Cooling water 0.00 1926161.30 6356.33 0.01
Steam 0.10 632200.55 63220.05 0.06
Labour - -- 135500.00 0.14
Total 91.05
11.2.6 Total Fixed Capital Cost

The total capital cost of the plant can be obtained by summing up the IBL cost, OBL cost,
and the start-up capital. The final cost estimated for total fixed capital cost is RM 498.265
million.
339
11.3 Operating Cost
Operating cost is made of manufacturing and non-manufacturing cost. Manufacturing cost is
obtained by adding the Total Fix Cost and Total Variable Cost which is made of several
costing parameters such as Total Raw Material Cost, Total Utility Cost and Total Process
Labor Cost. In the other hand the non-manufacturing cost is made of variables such as
Research & Development, Selling expenses and Corporate administration. The raw materials
and utilities required have previously been tabulated in chapter 3.3.
Assumptions required for the calculation:
24ℎ𝑟 330𝑑𝑎𝑦𝑠
 The Plant is running and operates continuously for and
𝐷𝑎𝑦 𝑌𝑒𝑎𝑟
 The operating cost for the plant is assumed to be at 100% capacity utilization
 The unit prices required to calculate the operating cost such as Raw Material Price
and Electricity Price is obtained based on literature review and is tabulated in the
following Table 11.3.3.
𝑅𝑚
 The selling price of the MEG (Mono Ethylene Glycol) is taken as 4500 𝑇𝑜𝑛𝑛𝑒𝑠
 To calculate the Total Fixed cost, the several factors % need to be assumed and they
are summarized in the table below:
Table 11.3.1: Factor used in fixed cost calculation

Fixed Operating Cost Factor % Cost to be Factored
(Wages for labor with shift)
Payroll overheads 10
+ (Wage for labor without shift)
Maintenance materials and labor 8 Fix Capital Investment
Plant Overheads 50 Process Labor Cost
Insurance 2 Fix Capital Investment
Book Depreciation 5 Fix Capital Investment
Property Taxes 3 Fix Capital Investment
 The Non-Manufacturing cost also required several factors % to be taken into

consideration and they are summarized in the table below:
Table 11.3.2: Factor used in non-manufacturing cost calculation

Non-Manufacturing Cost Factor % Cost to be Factored
Research & Development 10 Total Production Cost
Selling Expenses 8 Total Production Cost
340
Corporate Administration 50 Total Production Cost
 The Process Labour Wages is din Appendix A.11.2.
Summary of Result:
Table 11.3.3: Summary of operating cost
Annual cost Cost per tonne
Production Cost (MYR of product
million/year) (MYR/tonne)
Usage rate Unit Cost
Raw Materials
(Tonnes/Year) (MYR/Tonnes)
Syngas 189942.19 700.00 132.96 1038.75
Nitrogen Monoxide 21621.60 1702.13 36.80 287.52
Oxygen 34214.40 545.62 18.67 145.84
Methanol 9214.13 1614.00 14.87 116.18
Cuprous Aluminium
1472.33 5304.00 7.81 61.01
Chloride
Palladium 33.79 8640.00 0.29 2.28
Copper 39.68 50000.00 1.98 15.50
Silicon Dioxide 158.72 2330.00 0.37 2.89
Toluene Solvent 12983.26 2696.20 35.01 273.48
Total Raw Material Cost 248.76 1943.46
Usage rate Unit Cost
Utilities
(Unit/year) (MYR/Unit)
Steam 381379937.40 0.10 38.14 297.95
Cooling Water 125175708.11 0.00 0.41 3.23
Electricity 87373836.00 0.35 30.58 238.91
Total Utility Cost 69.13 540.09
Total Variable Cost 317.89 2483.55
Salary
Process Labour Factors
(MYR/year)
Wages for labour
- 612000.00 0.61 4.78
with shift
Wages for labour
- 1014000.00 1.01 7.92
without shift
Payroll Overheads 0.10 162600.00 0.16 1.27
Total Process Labour Cost 1.79 13.97
Factor
Maintenance
8% fixed capital cost 39.86 311.42
materials and labour
Plant overheads 50% process labour cost 0.89 6.99
Insurance 2% fixed capital cost 9.97 77.85
Book Depreciation 5% fixed capital cost 24.91 194.64
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Property Taxes 3% fixed capital cost 14.95 116.78
Total Fixed Cost 92.37 721.65
Total Production Cost 410.26 3205.19
Non-manufacturing
Factors
Cost
Research and
3% production cost 12.31 96.16
development
Selling expenses 2% production cost 8.21 64.10
Corporate
3% production cost 12.31 96.16
Administration
Total Non-manufacturing cost 32.82 256.42
Total Operating Cost 443.09 3461.61
11.4 Working Capital

For the calculation for working capital, the capacity is assumed to be at 100% utilization
which amounts to 128,000 tonnes of MEG produced per year. Several key assumptions were
made to proceed with the calculations:
1. The raw materials are delivered intermittently and therefore a period of 3 weeks is
accounted for them.
2. Syngas delivery is through pipeline and is also estimated to have a period of 3 weeks.
3. Period for debtors and creditors are assumed to be 6 weeks for both.
4. Creditors include purchasing of Raw Materials, Utilities and Process Labour.
5. MEG products stock of 6 weeks is accounted.
6. Calculated operating cost of RM 3461.60 per tonne of MEG product is used.
7. Selling price of MEG at RM 4500 per tonne.
8. 52 weeks in a year.
9. There is negligible stock for the work in progress.
Table 11.4.1: Working Capital Breakdown

Working Capital
Cost of Annual Cost
Period
Component Component Demand (MYR
(Weeks)
(MYR/tonne) (Tonne/year) millions/year)
Raw Materials
Syngas 3 700.000 189942.192 7.671
Toluene 3 2696.200 12983.256 2.020
Oxygen 3 545.616 34214.400 1.077
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Nitrogen Oxide (NO) 3 3404.255 21621.600 4.246
CuAlCl4 3 5304.000 1472.328 0.451
Cu 3 432000.000 39.679 0.989
SIO2 3 21600.000 158.717 0.198
Methanol 3 1614.000 9214.128 0.858
Palladium 3 8640.000 33.792 0.017
Products
Mono Ethylene Glycol
6 399.410 128000.000 51.125
(MEG)
Debtors
Mono Ethylene Glycol
6 4500.000 128000.000 66.461
(MEG)
Creditors
Syngas 6 700.000 189942.192 -15.341
Toluene 6 2696.200 12983.256 -4.039
Oxygen 6 545.616 34214.400 -2.154
Nitrogen 3404.255 21621.600 -8.493
6
Raw Oxide (NO)
Material CuAlCl4 6 5304.000 1472.328 -0.901
Cu 6 432000.000 39.679 -1.978
SIO2 6 21600.000 158.717 -0.396
Methanol 6 1614.000 9214.128 -1.716
Palladium 6 8640.000 33.792 -0.034
Utilities 6 540.093 128000.000 -69.132
Process Labour 6 1626000 MYR per year -0.188
Total Working Capital 30.741
The total working capital is found to be RM 30.741 million per year.
11.5 Total Capital Cost

The total capital investment will just be the summation of total fixed capital and total
working capital and is found to be RM 529.006 million.
11.6 Project Profitability Analysis

11.6.1 Cash Flow Table
The cash flow analysis tabulates the net flow of money earned and spent by the project over a
certain amount of years. The project lifetime used for estimation here is of a period of 15
years starting from the first year of operation. Key assumptions were made to proceed with
the cash flow table:
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1. 2 years is accounted for construction and detailed design of the plant. (2017-2018)
2. The first operating year of the plant will be in Year 2019 and will be at 80% capacity
utilization.
3. The subsequent years will work at 100% capacity utilization.
4. Working capital to be fully recoverable at the end of the project life.
5. Tax depreciation is 6.7% until fully depreciated.
6. The corporate tax rate used in the calculations is 28%.
7. Real discount rate is used as 10%.
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The cash flow table for the MEG plant over 17 years is shown as below.
Table 11.6.1.1: Cash Flow Table (Year 1-9)
Cash Flow Table

1 2 3 4 5 6 7 8 9
Item Value Units 2017 2018 2019 2020 2021 2022 2023 2024 2025
Fixed Capital MYR Million -249.13 -249.13
Working Capital MYR Million -24.59 -6.15
Sales volume Tonne/Year 102400.00 128000.00 128000.00 128000.00 128000.00 128000.00 128000.00
Selling price MYR/Tonne 4500.00 4500.00 4500.00 4500.00 4500.00 4500.00 4500.00
Sales revenue MYR Million/Year 460.80 576.00 576.00 576.00 576.00 576.00 576.00
Variable Cost MYR Million/Year -254.31 -317.89 -317.89 -317.89 -317.89 -317.89 -317.89
Fixed Cost MYR Million/Year -92.37 -92.37 -92.37 -92.37 -92.37 -92.37 -92.37
Non Manufacturing Cost MYR Million/Year -26.26 -32.82 -32.82 -32.82 -32.82 -32.82 -32.82
Cash Flow Before Tax MYR Million/Year 87.86 132.91 132.91 132.91 132.91 132.91 132.91
Tax Depreciation 6.7 %
Tax Depreciation allowance MYR Million/Year 33.38 33.38 33.38 33.38 33.38 33.38 33.38
Taxable Income MYR Million/Year 54.47 99.53 99.53 99.53 99.53 99.53 99.53
Tax Rate 28 %
Tax Payment MYR Million/Year -15.25 -27.87 -27.87 -27.87 -27.87 -27.87 -27.87
Cash Flow After Tax MYR Million/Year -249.13 -249.13 48.01 98.90 105.05 105.05 105.05 105.05 105.05
Cumulative Cash Flow after Tax MYR Million -249.13 -498.27 -450.25 -351.36 -246.31 -141.26 -36.22 68.83 173.88
Discount Rate 0.1
Discounted Factor 0.91 0.83 0.75 0.68 0.62 0.56 0.51 0.47 0.42
Discounted Cash Flow after Tax MYR Million -226.48 -205.89 36.07 67.55 65.23 59.30 53.91 49.00 44.55
Cumulative Discounted Cash Flow After Tax MYR Million -226.48 -432.38 -396.31 -328.76 -263.53 -204.24 -150.33 -101.33 -56.78
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Table 11.6.1.2: Cash Flow Table (Year 10-17)
Cash Flow Table

10 11 12 13 14 15 16 17
Item Value Units 2026 2027 2028 2029 2030 2031 2032 2033
Fixed Capital MYR Million
Working Capital MYR Million 30.74
Sales volume Tonne/Year 128000.00 128000.00 128000.00 128000.00 128000.00 128000.00 128000.00 128000.00
Selling price MYR/Tonne 4500.00 4500.00 4500.00 4500.00 4500.00 4500.00 4500.00 4500.00
Sales revenue MYR Million/Year 576.00 576.00 576.00 576.00 576.00 576.00 576.00 576.00
Variable Cost MYR Million/Year -317.89 -317.89 -317.89 -317.89 -317.89 -317.89 -317.89 -317.89
Fixed Cost MYR Million/Year -92.37 -92.37 -92.37 -92.37 -92.37 -92.37 -92.37 -92.37
Non Manufacturing Cost MYR Million/Year -32.82 -32.82 -32.82 -32.82 -32.82 -32.82 -32.82 -32.82
Cash Flow Before Tax MYR Million/Year 132.91 132.91 132.91 132.91 132.91 132.91 132.91 132.91
Tax Depreciation 6.7 %
Tax Depreciation allowance MYR Million/Year 33.38 33.38 33.38 33.38 33.38 33.38 33.38 33.38
Taxable Income MYR Million/Year 99.53 99.53 99.53 99.53 99.53 99.53 99.53 99.53
Tax Rate 28 %
Tax Payment MYR Million/Year -27.87 -27.87 -27.87 -27.87 -27.87 -27.87 -27.87 -27.87
Cash Flow After Tax MYR Million/Year 105.05 105.05 105.05 105.05 105.05 105.05 105.05 135.79
Cumulative Cash Flow after Tax MYR Million 278.92 383.97 489.01 594.06 699.11 804.15 909.20 1044.99
Discount Rate 0.1
Discounted Factor 0.39 0.35 0.32 0.29 0.26 0.24 0.22 0.20
Discounted Cash Flow after Tax MYR Million 40.50 36.82 33.47 30.43 27.66 25.15 22.86 26.86
Cumulative Discounted Cash Flow After Tax MYR Million -16.28 20.54 54.01 84.44 112.10 137.25 160.11 186.98
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11.6.2 Payback Period
The payback period is the estimated period of time elapsed before the capital investments of
the project are recovered which also indicates the profitability of the project as a short
payback period generally indicates a more profitable project. The cumulative cash flow after
tax obtained from the cash flow table is used to plot the graph against the project lifetime in
years. The payback period graph is plotted below with the help of Microsoft Excel.
Payback Period =
7.4 years
Figure 11.6.2.1: Payback period graph (Cumulative Cash Flow Plot)

The payback period of the MEG plant project is estimated to be around 7.4 years.
11.6.3 Net Present Value (NPV)

The Net Present Value is a value used to compare the total of money invested in the present
to the value of money in the future. As a real discount rate of 10% is assumed for the Cash
flow table, it will also be used for the NPV calculations. Detailed calculation of the NPV is
shown in Appendix A11.3.1. The calculated NPV of the project after 15 years of operation is
RM 186.98 million.
11.6.4 Internal Rate of Return (IRR)

The Internal Rate of Return (IRR) sometimes called as the Discounted Cash Flow Return
(DCFR) is the discount rate which will result in the Net Present Value (NPV) of the project to
be zero. The rule of thumb is that the project is only profitable if the IRR estimated of the
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project exceeds the real discount rate imposed on the project. In this case the real discount
rate is used as 10%. The graph below shows the IRR estimated using a graph.
IRR = 16%
Figure 11.6.4.1: Graph to obtain IRR value

As shown in the graph above, the estimated IRR for the project is at 16.0%, which indicates
that the project is profitable and is able to proceed.
11.7 Comparison Study

Comparison Study is done to observe the productivity and cash flow outcome of the plant
when its capacity is changed into either larger-scale production or smaller-scale production.
𝑇𝑜𝑛𝑛𝑒𝑠 𝑇𝑜𝑛𝑛𝑒𝑠
The larger-scale capacity and smaller-scale capacity are 103500( ) and 500000( )
𝑌𝑒𝑎𝑟 𝑌𝑒𝑎𝑟
respectively. Assumptions made for the calculation are shown below:
1. The amount of Raw Materials, Catalyst, Solvent and Utilities remain the same
despite the capacity of the plant being changed
2. The labour cost remains the same as well
3. With the new Capacity, the calculation steps and assumptions made to calculate the
Operating Cost and Working Capital remains the same
4. The Cash flow calculation is also repeated using the same steps and assumptions to
obtain the new NPV, IRR% and Payback year.
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When the capacity of the plant changes the Fixed Capital, cost would change as well. The
new Capital Cost is obtained using the following formula:
𝐼𝑝 𝑄 𝐹
= (𝑄𝑝 )𝐵 ( 𝐹𝑝 )(L)
𝐼𝑟 𝑟 𝑟
Where:
𝐹𝑝
 = Inflation Index
𝐹𝑟
 Qp = Capacity of Proposed Plant

 Qr = Capacity of comparison
 Ip = Capital Investment of Proposed Plant
 Ir = Capital Investment of comparison
 L = Location Factor
 B= Exponent factor =0.6
A summary showing the changes in the outcome of key economic parameters as the Capacity
of the plant as well as its Fixed Capital varies is shown in the table below:
Table 11.7.1: Result of comparison study
𝑻𝒐𝒏𝒏𝒆𝒔 103500 128000 500000
Plant Production Capacity, ( )
𝒀𝒆𝒂𝒓
Fix Capital Cost, MYR Million 438.631 498.266 1128.540
Annual Operating Cost, MYR Million 431.493 443.086 565.611
Payback Period, Years 16.700 7.400 3.300
IRR, Internal Rate of Return, % 0.020 15.800 73.00
NPV at 10% discount rate, MYR Million -207.398 180.888 6432.93
An analysis is done based on the values tabulated in the table above. It can be concluded that
a reduction in the Plant Production Capacity would result in a negative manner economically
and need to be avoided at all cost. This could be observed from the Payback Period and
𝑻𝒐𝒏𝒏𝒆𝒔
IRR% calculated when the Plant production capacity is 103500( ), as they are 16.7
𝒀𝒆𝒂𝒓
years and 0.02 % respectively. The IRR% is much lower than the minimum profitable IRR%
which is 12%. Furthermore, it would take 16.7 years to achieve payback and start making
profit which is certainly undesirable.
In the other hand, when the plant capacity increases so would the profitability rate as the
𝑇𝑜𝑛𝑛𝑒𝑠
Payback Period and the IRR% when the capacity is 500000( ) are 3.3 years and 73%
𝑌𝑒𝑎𝑟
respectively. The values obtained indicates an extremely positive and desirable outcome as
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the duration required to recover the initial capital investment is relatively brief. Furthermore,
the IRR% is much higher than the minimum profitable IRR%. Therefore. it can be concluded
that in an economic manner, the plant is fully capable to benefit from an increase in the Plant
Production Capacity.
11.8 Sensitivity Analysis.

The purpose of conducting a sensitivity analysis is to evaluate the potential outcome of the
proposed plant Capability, when the assumed input economical parameters changes in a way
in which it could affect its capability in a negative manner. The percentage of variation is
taken as 10% and the input parameters that would be varied are: - Decrease in Sales Volume,
- Decrease in Selling Price, - Increase in capital expenditure and -Increase in Raw Material
cost. The outcome parameters that would be obtained and analyzed are NPV (Net Present
Value) and IRR (Internal Rate of Return). The following table would summarize the changes
in the outcome parameters for all the four scenarios mentioned above as well as proposed
plant assumption
Table 11.8.1: Result of sensitivity analysis
Variation Description NPV (Million MYR) IRR (%)
Base Case 180.89 15.8
Sales volume, - 10% 123.17 14
Selling Price, -10% -68.67 7.8
Capital Expenditure, +10% 98.94 13
Raw Material Cost, +10% 60.73 12.1
Based on the table above, analysis on the outcome of NPV (Net Present Value) and IRR
(Internal Rate of Return) due to the variation in the input Parameter is done. When sales
volume decreases by 10 % the IRR obtained is 14%. This indicates that the proposed Plant
would still be profitable as it is higher than the minimum profitable IRR % which is 12 %.
The drop in IRR % is also relatively small as it only decreases by 1.8%. When Capital
Expenditure increases by 10% the plant is still profitable as its IRR is 13% which is still
higher than the minimum profitable IRR %. Furthermore, the IRR% value when the raw
material cost increases by 10% is still above the minimum profitable IRR as its value of 12.1
% is right on the border of profitability. However, when the Selling Price decreases by 10%
the IRR value would be 7.8% which is less than the minimum profitable IRR %. Based on the
analysis above only, out of 4 potential variations only one would not resulted in profitability
for the plant. Furthermore, the one case in which profit might not be obtained is very unlikely
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as the selling price of the MEG (Mono Ethylene Glycol) would probably not drop anytime in
the near future as the Market Demand for MEG (Mono Ethylene Glycol) is still continuously
increasing. Therefore, it can be concluded that the capability of the proposed plant would be
able to withstand the potential variation and still made profit out of the production.
11.9 Conclusion and Profitability

Based on the profitability analysis, the project is estimated to be economically feasible to be
carried out while having a production capacity of 128000 tonnes of MEG products per year.
By using a 10% real discount rate, a Net Present Value (NPV) of RM 186.98 million is
obtained after 15 years of operation. The payback period of the project is also estimated to be
at 7.4 years including the commissioning and construction years. Internal Rate of Return
(IRR) value estimated is also quite attractive at 15.8% which is significantly higher than the
minimum profitable IRR% of 12%. The results from performing the sensitivity analysis were
also quite positive as most of the variables does not affect the resulting IRR % largely to be
less than the profitable range. The major thing to control to ensure that the project is
profitable will be the selling price determination of the products, as a 10% decrease in selling
price would lead to the project being non-profitable. Hence, maintenance planning systems
should be implemented to minimize the impact of these variables.
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Chapter 12:
Project Viability
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12.1 Technical Viability Including Safety
The proposed Mono Ethylene Glycol processing plant, is designed to produce a capacity of
128,000 tonnes/year, which is slightly more than 100,000 tonnes/year. This is done to ensure
that the capacity of production would still achieve its goal even during unforeseen
circumstances such as emergency plant shutdown or any other potential disruption which
could lead to a slight drop in the capacity of production. The purity of MEG produced in the
final product is above 99.0% as it is purity required by the market demand. In this study,
MEG is synthesised from Syngas which functions as its main feedstock and other minor
feedstocks such as Nitrogen Oxide and Oxygen.
The manufacturing process can be separated into 7 sections which are, Syngas separation,
Dimethyl Oxalate Synthesis, Methyl Nitrite Synthesis, Dimethyl Oxalate Purification,
Dehydration, Hydrogenation and MEG Purifications. Various existing technologies of each
sections were compared and analysed based on safety, economic parameters, and
environment impacts. The design of all the major equipment was done based on ASM
Pressure Vessel Code (ASME BPVC). The operating conditions of each sections were
determined and controlled precisely in order to produce high purity of Mono Ethylene Glycol
according to the global market demand. Hence, appropriate control system and alarm system
were designed to minimize the potential risks and damage caused by abnormal operation,
uncontrolled reaction or equipment failures. Proper utilities are chosen to provide sufficient
heating and cooling duty to the equipment within the plant to prevent either excessive heating
or cooling. This is due to the fact that excessive heating or cooling could result in higher
potential risk during operation as well as requiring higher operating cost.
Inherent and extrinsic safety were considered during the design stage of each and every
section. Hazard Identification, (HAZID) and Hazard Operability (HAZOP) studies were
conducted to identify all the potential harmful impact during plant start -up, normal
operation, shutdown and maintenance by analysing the potential risks, hazards, errors and
outcomes. Furthermore, preventive and mitigating actions were developed to properly
address all these hazards. Standard Operating Procedure, (SOP), and Maintenance Planning
System (MPS) are established and applied to all the equipment and instrumentation to further
lower the risk poses in the processing plant. An emergency response plan (ERP) has also
been carefully design to cope with critical and emergency situation.
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Layout of the processing plant was designed based on the plant layout guidelines provided by
American Institute of Chemical Engineers (AIChe). A safe distance between each equipment
must be followed and different section of process must be segregated and separated based on
its relative potential hazards. For instance, DMO Synthesis and MN Synthesis are both an
interactive process with flammable and explosive components flowing in between the
sections. Hence these two processes must be located within an appropriate distance between
one another to ensure that it does not violate the minimum safe distance required. The
location of this plant is located at Tanjung Langsat Industrial Estate where both water and
electricity supply is available at a relatively close distance. Furthermore, the location is
appropriately accessible to raw materials by either pipeline transport or by shipping. The
minimum distance of 5km between processing plant and the nearest residential area is falls
within the satisfactory range based on Department of Environment in Malaysia. The plant
layout was designed to ensure total safety and efficiency during operation.
In a nutshell, this project is technically and safety viable based on all the considerations
mentioned above.
12.2 Economic Viability

The total capital cost that needs to be invested is calculated to be RM 529.006 million. By
investing this amount of money, the payback period estimated is to be 7.4 years. The
cumulative cash flow after tax of RM 1044.99 after 15 operating years is found to be RM
1044.99. By implementing a real discount rate of 10% for the project, the Net Present Value
(NPV) of the project after 17 years is calculated to be RM 186.98 million. The Internal Rate
of Return (IRR) is also estimated to be 15.8% for this proposed project. The IRR value
obtained was higher than the real discount rate used of 10%, therefore the project is deemed
to be economically viable to operate.
Sensitivity analysis were also performed for project viability study. Scenarios such as
decrease in sales volume, decrease in selling price, increase in capital expenditure, and
increase raw material cost were considered to obtain a different IRR value for comparison
purpose. Based on the sensitivity analysis, the decrease in selling price is shown to have the
biggest impact on the IRR of project as a 10% decrease in selling price will lead to 8.2%
decrease in the IRR value. This decrease in IRR value results in the new IRR value to be
around 7.8% which is lower than the real discount rate of 10% and the minimum profitable
IRR% of 12%. The project would also have a NPV of RM -68.67 million with this change.
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This shows that when a 10% decrease in selling price occurs, the project will no longer be
profitable. The second major variation that would lead to a large fluctuation of IRR value will
be the raw material cost as a 10% increase in raw material cost will result in a newly IRR
value of 12.1% obtained. This value is just above the minimum profitable IRR% of 12% and
therefore will not lead to the project being non-profitable.
Other factors such as 10% decrease in sales volume and 10% increase in capital expenditure
will result in IRR values of 14% and 13% respectively which is considerably bigger than the
minimum profitable IRR value of 12%. Hence, these variables are not as significant as the
two other variables compared above. To minimize the occurrence of these variables that can
affect the project’s profitability, proper training for the operator as well proper maintenance
planning systems should be implemented into the operation of the plant.
12.3 Environmental Viability

The environmental viability of the project is determined via life cycle assessment (LCA) and
environmental assessment to investigate the environmental sustainability and potential risks
in the plant. The LCA in this report focuses mainly on the major impact categories which are
global warming potential (GWP) and resource depletion (RD). From the LCA conducted, it is
observed that the total impact score for GWP and RD is 14670.97 kg CO2-eq and 8.25 ×
10−12 kg respectively where syngas separation contributes to the highest GWP and RD,
followed by DMO synthesis.
The Environmental aspect and impact register is also conducted in the environmental
assessment in the report. The activities that can lead to different environmental impacts are
listed in the environmental aspect and impact register matrix with the indication of their
respective likelihood and significance tabulated. Most of the risk existing in the plant consists
of scores within the range of 11-15 which is categorized under High significance. However,
after mitigation measures are implemented, the significance is greatly reduced to the
Moderate ranges. It is also to note that there were no risks in the plant which are extreme. The
risks are therefore tolerable and acceptable by society and impacted victims. Wastewater
generated by different processes in the plant will be sent to a wastewater treatment plant to be
treated before discharging it to the environment according to standards set by the Department
of Environmental (DOE).
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The scheduled waste generated from the plant such as solid wastes from spent catalyst and
sludge from wastewater treatment will be handled with care and provided with proper storage
to avoid any land or water source contamination. The purpose of the storage is to minimize
further contamination to the environment before sending the wastes to a scheduled waste
treatment facility. The plant is also located at an industrial area in Johor and will not be near
enough to any residential area or natural habitat for endangered species to cause significant
impacts. Air emissions from the plant that does not comply with the standards set by DOE
will also be sent to a flare tower to reduce its concentration of discharge to the atmosphere.
In conclusion for the environment aspect of the plant, the plant is deemed to be
environmentally viable to operate and the environmental performance can still be further
improved by implementing more environment friendly based approach in operation for
coming operating years.
12.4 Strategic and Technology Impacts

The technology and economic impacts of the projects are the two major factors that could
decrease the profitability of the project to the point in which it becomes non-profitable. New
technologies are being discovered and implemented every day in this digital era at an
extremely fast rate, which results in old and inefficient technologies to be eliminated fairly
easily. Therefore, technology updates from time to time will be beneficial to the operation of
the plant in order for the process yield and efficiency of production to increase.
Implementation of new technologies needs to be decided by the management to ensure that
the Project remains in a competitive position in the MEG market. It is also important to
understand the market for the product purity that the plant is producing to tackle the sales
volume and revenue that the company is trying to achieve. Generally, a higher purity product
production will be less common and will result in a higher selling price per tonne of products
sold but the demand for the higher purity product might not be as large as a lower purity
product. Producing a high purity product will lead to high energy cost, therefore to ensure the
energy efficiency is high, heat integration is performed on process streams to maintain high
energy efficiency operation of the plant by reducing the required amount of fresh utilities.
To reduce the negative economic impacts towards the profitability of the plant operation,
different economic strategies should be adopted. One of the direction to focus on will be
based on the fact that the global demand of MEG is on a steady increase for the past recent
years. Therefore, the plant could produce more MEG to be sold in order to increase revenue
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from operation. Another strategy is to obtain a lower price for raw material cost from
suppliers as the plant requires constant supply of these materials throughout its operating
years. Contracts can be made between suppliers and the plant to decrease the raw material
cost of the plant. The raw material cost is also the biggest factor affecting the IRR % of the
plant, therefore a decrease in raw material cost will undoubtedly increase the profitability of
the MEG plant. Other strategies should also be discovered and developed by the management
throughout operation years to maintain profitability of the project.
12.5 Other Factors Affecting Project Viability

Although the plant has been determined to be viable, it is however still affected by some risks
which could affect the viability of the whole project. First and foremost, there is a
geopolitical risk regarding the availability of utilities. However, this risk will only pose
minimal affect since the selected area which is Tanjung Langsat Industrial Park is considered
to be a well-developed area. The next factor to be considered is the potential political risk.
The potential risk is present based the price cartel policy where the price of a certain product
is fixed to a certain range by people of the same business to ensure that there is no
competition against each other. This policy might not affect organisations which are already
existing. However, for new plants, this policy will cause a huge problem for the viability of
the project as the prices for raw materials and selling prices can be controlled by
organizations which are involved in the cartel.
Another factor which will affect the viability of this project is the exchange rate. As the final
product of the plant will be sold mostly in Malaysia and Asia region, hence the difference in
the exchange rate will not have much effect on buyers. The part where exchange rate will
cause the most effect will be the fixed capital investment of the plant. This is because the
equipment purchased for the plant is calculated based on USD. Hence, the equipment price
will depend on the current exchange rate of MYR to USD. However, the exchange rate will
not cause much effect on the viability as this cost is only for the construction phase of the
plant which has been plan to be completed in 2 years.
12.6 Recommendations
Based on the analysis of potential factors that could negatively affect the viability of the
project, it is concluded that the project is viable enough as the potential factors does not post
a huge threat to the viability of the project. However, a few improvements can be
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recommended in order to achieve greater viability in various aspects such as technical,
economics and environmental aspects.
In term of technical aspect, a more advanced technology can be employed to improve the
inefficiencies in the current plant technology. Equipment such as absorption columns, pumps,
compressors and heat exchangers can also be improved in efficiency. Even though the capital
costs would increase, eliminating the inefficiencies would result in other positive manner as
wastes such as material and energy could be minimized, hence increasing the yield and
production rate. Strategies for water and wastewater reduction could also be carried out in
order to reduce utilities usage.
Even though the project is economically viable, based on the sensitivity analysis carried out,
a slight decrease in selling price will cause the project to become infeasible. To enhance the
economic viability, alternatives for cheaper raw materials can be used to substitute the current
highly priced raw materials. The utilities costs such as electricity and water costs could also
be reduced as the efficiency in equipment is increased, as discussed in the aforementioned
technical aspect. This could reduce the operating costs as the current operating costs are made
up of 70 % of variable costs, i.e. raw materials and utilities. Besides, unreacted materials
could also be sold to other plants instead of being sent to flares, to generate side incomes for
the plant. Furthermore, further expansion of the reserved space in the plant could also be
carried out to maximise production capacity, generating higher sales revenue for the plant.
In term of environmental aspect, in order to reduce emissions and increase environmental

sustainability, the emissions should be treated before being discharged to the environment.
Equipment such as air scrubbers and cyclone dust separator can be employed to improve air
emission whereas water treatment plant can be incorporated in the plant to minimize the
pollution caused by water emission. Last but not least, operators should also ensure that the
air, water and land emissions are within the standard limits set by DOE.
12.7 Conclusion
In conclusion, the proposed MEG plant by G6 Engineering Sdn. Bhd is feasible in terms of
all viabilities assessed in the project. In terms of technical and safety viability, the
implementation of good SOPs and MPS is achieved whereas HAZID and HAZOP are also
conducted. The project is also found to be both economically and environmentally viable.
The IRR of 15.8 % is achieved, as opposed to the minimum required IRR of 12 %. As for
358
environmental viability, LCA and risk assessment is conducted and mitigation measures are
carried out to reduce the risk significance to Moderate range.
359
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CHE 4170 Design Project

Production of Ethylene glycol from various feedstocks:

G6 Engineering Sdn Bhd.

G6 Engineering Sdn Bhd declares the following:

Signed on: 25th October 2017

 Prof. Chan Eng Seng

2.4.3 MN synthesis .............................................................................................. 25

4.1.4 Major Equipment in Hydrogenation ............................................................ 80

5.5 Specification sheets (by Wong Yoong Chin) .................................................... 117

6.4.2 Basis of Performance ................................................................................ 155

7.3.1 Control philosophy .................................................................................... 206

8.2.2 DMO Synthesis ......................................................................................... 257

10.5.15 Tank Farm ............................................................................................. 333

12.5 Other Factors Affecting Project Viability ....................................................... 357

1.1 Background Information

Figure 1.1.1.1: World Consumption of

The industrial process of MEG

1.1.2 Objectives of the Project

 Choosing the process route to synthesis EG.

 Providing a construction plan by choosing a suitable location to construct the

1.2 Process Information

1.2.2 Feedstock and product specifications

Table 1.2.2.1.3: Methanol specification

Table 1.2.2.1.4: Nitric oxide specification

Table 1.2.2.1.5: Nitrogen specification (The Linde Group, 2013)

Table 1.2.2.2.1: Quality needed for Ethylene Glycol

1.2.3 Feedstock Availability

1.2.4 Plant Availability and Capacity

1.2.5 Scope of Design

1.2.5.1 Technical Aspect

1.2.5.2 Social and Environmental Aspect

1.2.5.3 Economic Aspect

1.2.6 Definition of Terminal Points

Table 1.2.6.1: Definition of terminal points across system boundary

1.2.7 Site Location

1.2.8 Utilities and Storage

2.1 Market for products and by-products

Figure 2.1.1.1: Market segmentation of

2.1.2 Market demand of MEG

Figure 2.1.2.3: Biomass-based syngas Figure 2.1.2.4: Oxygen availability as

Figure 2.1.2.5: Nitrogen availability as feedstock (Jones, 2017)

2.1.3 Market price

2.1.4 Market of byproducts: Nitric acid and DMC

2.2 Feedstocks characteristics

Lastly, methanol is required in a few sections as a reactant and stabilization medium. As

2.3 Preliminary Economics

 Inflation index for chemical plants in Malaysia in year 2017 is estimated to be

2.3.2 Operating Costs

 The plant is operating at 100% capacity.

 Insurance and Property Taxes are fixed at 1% of the fixed capital

 Book Depreciation is fixed at 7.5% of the fixed capital.

 Plant Overhead is fixed at 50% of the fixed labor.

 Operating supplies is fixed at 10% of the fixed labor.

 Corporate Administration cost is fixed at 3% of production cost.

 Research and Development cost is fixed at 2% of production cost.

 Selling expenses cost is fixed at 5% of production cost.

2.3.3 Working Capital

 Work in progress inventory is negligible

 Since the MEG produced will be exported overseas, a period of 6 weeks of