01 - Distillation Columns Opeation and Control

Refining-Petrochemicals-Chemicals-Engineering
———
DISTILLATION COLUMNS: OPERATION AND CONTROL
A - ANALYSIS OF DISTILLATION COLUMN OPERATION - BASIC CONTROL SYSTEMS
INTRODUCTION .......................................................................................................................................1
I - GENERAL DESCRIPTION OF A DISTILLATION COLUMN - TERMINOLOGY .........................2
II - MATERIAL BALANCE FOR THE COLUMN..................................................................................4
III - OPERATING PRESSURE FOR A DISTILLATION COLUMN ......................................................8

1 - Pressure profile ..................................................................................................................................8
2 - Tray operation and pressure drop.....................................................................................................9
3 - Pressure control ...............................................................................................................................11
IV - ENERGY BALANCE AND LIQUID-VAPOR CIRCULATION INSIDE AN

INDUSTRIAL DISTILLATION COLUMN......................................................................................14
1 - Energy balance for a distillation column .........................................................................................14
2 - Condensing rate Q C ........................................................................................................................15
3 - Function of the external reflux .........................................................................................................16
4 - Reboiling rate QR.............................................................................................................................18
5 - Function of the vapor produced in the reboiler...............................................................................21
6 - Control of the reboiler duty ..............................................................................................................21
7 - Molar flow rate profiles in a distillation column ...............................................................................23
V- TEMPERATURE AND CONCENTRATION PROFILES IN A DISTILLATION COLUMN..........31

1 - Concentration and temperature profiles in a column processing a binary mixture ......................31
2 - Concentration and temperature profiles in a column processing a complex mixture with more
than two components.......................................................................................................................32
DT BIN - 01312_A_A - Rev. 2 16/02/2009

© 2009 - IFP Training
II
B - OPERATING VARIABLES IN DISTILLATION COLUMNS - CONTROL
I - CONCEPT OF DISTILLATION COLUMN SEPARATING POWER ..........................................43

1 - Number of theoretical separation stages ........................................................................................43
2 - Liquid-vapor circulation ....................................................................................................................43
3 - Feed inlet location ............................................................................................................................45
4 - Separating power to meet a given separation problem .................................................................46
5 - Adapting separating power to separation difficulty .......................................................................48
II - VARIATIONS IN A DISTILLATION COLUMN'S SEPARATING POWER .................................50

1 - Increased reflux and reboiling rate with a constant cut point ........................................................50
2 - Influence of the new separating power on resulting separation ....................................................54
III - VARIATION IN THE MATERIAL BALANCE FOR INDUSTRIAL COLUMNS -

SENSITIVE TRAY TEMPERATURE CONTROL ........................................................................57
1 - Impact of disturbances on distillation column operation ................................................................57
2 - Change in the cut point by increased reboiling ..............................................................................58
3 - Changing the cut point by other types of action .............................................................................61
4 - Concept of sensitive tray .................................................................................................................63
5 - Implementing sensitive tray temperature control ...........................................................................68
6 - Advantages and limits of sensitive tray temperature control .........................................................69
IV - CHANGE IN FEED CHARACTERISTICS ..................................................................................72

1 - Change in feed flow rate ..................................................................................................................72
2 - Change in feed temperature............................................................................................................74
3 - Change in feed composition ............................................................................................................75
V- CHANGE IN A DISTILLATION COLUMN'S OPERATING PRESSURE ....................................78

1 - Modification in operating pressure - Increased pressure...............................................................78
2 - Comparison of column operation at two different pressures .........................................................79
3 - Adapting the column to changes in operating pressure - implementing quality regulators .........81
01312_A_A © 2009 - IFP Training

1
INTRODUCTION
The purpose of most of the courses dealing with the distillation process as it is widely used in the chemical
and oil industries is to describe the engineering methods used to solve problems in designing columns so
that they can meet specified separation requirements. Solving such design problems means choosing the
operating pressure and determining the optimum values of the parameters that define the separating
power of industrial columns:
– the number of trays or height of packing needed,

– the required energy expenditure that governs the column's internal liquid and vapor
circulation,
– the optimum location for feed inlet.
Then in the operational context, distillation problems are examined with a different approach.
Industrial columns are designed to achieve a given separation that may change with production needs. They
are subjected to numerous disturbances of different origins and are operated by a control system that
prioritizes some parameters with respect to others.
The purpose of this paper is to discuss the operational behavior of industrial columns. By this we mean to
analyze the way they operate regarding different types of changes in operating conditions and to show the
possibilities and limitations of the relevant control systems that are implemented.
Consequently, the following study comprises two main parts:
• The first part aims to clarify the significance of the distillation column's operating
parameters: feed, products, pressures, profiles of temperature and composition, molar flow
rates and energy expenditures, etc. It also includes the description of the basic control
systems that apply to the major variables used in operation.
• The second part covers setting parameters and the behavior of columns with respect to
different variations in operating conditions. It winds up with the justification, advantages and
limitations of the various control systems used on industrial columns.

2
A - ANALYSIS OF DISTILLATION COLUMN OPERATION - BASIC

CONTROL SYSTEMS
I- GENERAL DESCRIPTION OF A DISTILLATION COLUMN - TERMINOLOGY

The basic diagram of an industrial distillation column is given below. Countercurrent circulation of liquid and
vapor is achieved inside the column by the external reflux injected at the top and by the reboiler which
generates the vapor stream required by the process. The feed is incorporated in this circulation by delimiting
rectifying and stripping zones located respectively above and below the feed inlet. The liquid-vapor
contacts that allow the feed components to be separated according to their volatility usually take place on
trays. The reboiler, and even the condenser in the event that overhead vapors are not totally condensed,
constitute extra separation stages.
In normal operation in the diagram below, condensation is total and consequently the overhead product or
distillate that comprises the volatile components of the feed is obtained in the liquid state after condensation
and proceeds through the reflux accumulator. The bottom product or residue that contains the nonvolatile or
heavy components is drawn off in the liquid state at the bottom of the column.
Overhead line Cooling

TI fluid
PRC
PI CONDENSER
Reflux
External PI drum
TI reflux
Rectyfying TI LIC
zone REFLUX
FRC
DRUM TI
Feed
FR TR DISTILLATE
TI
or overhead product
AR FR
TI
Stripping
zone
PI
REBOILER FRC TI
LRC Reboiling
medium
TI
TI
D PCD 293 E
RESIDU
or bottom product
FR
AR

3
The instrumentation and control equipment on the column is quite conventional. It includes:
– An overhead pressure controller (PC) that acts first on the cooling ability by the cold fluid
flow rate and then on a reflux drum degassing valve.
– An external reflux flow rate controller (FC) and at the same time a reflux drum level
controller (LC) that acts on the distillate flow rate.
– A reboiler fluid flow rate controller, since the residue draw-off is under the control of the
liquid level at the bottom of the column.
– Flow rate recorders (FR) for the feed, products, reflux and reboiler fluid.
– Temperature measurements with indicators or recorders (TI or TR):
• reflux drum
• overhead column
• rectifying zone
• stripping zone
• bottom of the column
• feed at the column inlet
• hot fluid at the reboiler inlet and outlet
– Two analyzers (AR) used to measure the impurity content in each of the two products.
The control devices equipping the column is relatively simple. Pressure is regulated in most distillation
columns. Control of the external reflux flow rate and control of the heat input to the reboiler through the hot
fluid flow rate is a very common basic setup. As shown later on, this implies leaving the distillate and residue
being leaving the column without any flow control. This is achieved by subordinating them to the liquid levels
in the reflux drum and in the bottom of the column respectively.
The body of data provided by instrumentation (temperatures, pressures, flow rates, analyses, etc.) is used to
assess process operation, which is the subject of the study in the following sections. The study deals mainly
with the points listed below:
– the material balance for the column
– the internal pressure profile and pressure control
– the energy balance and the duty of the condenser and the reboiler
– the concentration and temperature profiles

4
II - MATERIAL BALANCE FOR THE COLUMN

Under stable operating conditions, the amounts of matter that go into the column and the amounts that come
out are equal.
This is true from an overall standpoint, but also for each component of the feed.
If the molar (or mass) flow rates of feed, of distillate and of residue are called A, D and R, the following
equation should hold true:
A=D+R Overall balance
Likewise if the partial flow rates of any component i are called Ai, Di and Ri, the following holds true:
Ai = Di + R i Partial balance for component i
Accordingly, separation involving a mixture of n components will yield n material balance equations that can
be broken down into n-1 partial balances and one overall balance for example.
In practice, the column's operating conditions determine the values of D and R, which in turn define what is
called the feed cut point. This concept is illustrated in the diagram below. The feed going into the column is
represented by a rectangle, with the different components a, b, c, d, e, and f appearing inside it in order of
decreasing volatility. The area of each one is proportional to its concentration in the feed. The distillate-
residue separation performed by the column is represented by a theoretical horizontal line dividing the feed
into two parts: the light or volatile components concentrated in the distillate and the heavy components
in the residue.
Non distributed components a-e-f

Distributed components b-c-d
LRC
a
FRC
b D
D c
FEED Overhead product Cut point
A
d
A
Separation
FRC line
LRC
e R
D PCD 352 J
R Bottom
product f
Overall material balance cut point Light key: the heaviest of the light components c
Separating power separation line Heavy key: the lightest of the heavy components d

5
The feed cut point is also expressed in the form of the ratio D/A. It is located near the borderline between the
two components in the mixture that are the most difficult to separate because their volatility values are so
close. In the example in the illustration, the cut point is located near the borderline between components c and
d. Separating the two is the basic function of distillation. This is why the two components adjacent to the cut
point are often called the key separation substances, with the definition:
- the light or volatile key, (LK), here component c
- the heavy key, (HK), here d
The separation therefore depends on:
– the difficulty of the separation, which can be characterized by the volatility interval
between the two key components or relative volatility,
– the separating power of the distillation process.
As a result, a feed separation line rests horizontally on the cut point on the preceding diagram and delimits
equal areas on either side. This line represents the real composition of the distillate and of the residue and
shows how the impurities are distributed in each of the two products.
These two lines give a synthesis of the result of separation and is very useful in analyzing the changes in
operating situations. It also shows that -- as is often the case -- only some of the components are distributed,
i.e. present at the same time in the distillate and the residue. In the diagram, a, e, f, and g are not
distributed in both of the products and b is present in the residue, but in a very small proportion. The two key
components c and d are obviously found on both sides.
In many instances, these considerations are used to simplify the partial material balances by writing Ai = Di for
the lighter components and Ai = Ri for the heavier ones. If the composition of the feed is known and if the
analyzers provide the concentration in distributed components (mainly the key components), a material
balance table can then be set up for each one.
Figures 1 and 2 on the following two pages show the material balance for an aromatic hydrocarbon
separation column and for a debutanizer:
– The aromatics separation column processes a mixture of benzene, toluene and xylenes. It
is designed to separate the benzene at the top with a good degree of purity. The key
separation components are benzene and toluene.
– The debutanizer processes a mixture containing a little hydrogen and light hydrocarbons
from C1 to C11. It yields C4-gases at the top in the form of a vapor distillate and a liquid
distillate in the reflux drum, with a C5+ gasoline cut at the bottom. The light key is n-butane
here (nC4) and the heavy key is isopentane (iC5).

BENZENE SEPARATION COLUMN
01312_A_A
91.39 — Materials balance —
1.5
94.9
1 690.9
53.935 % mol
BZ 99.9
% mol 80 1 0.1
TOL
BZ 41.77 EB
TOL 10.54 LC PX
EB 10.15 MX 10
PX 8.02 FC OX
MX 17.62 11
Distillate
OX 11.90 BENZENE
C
(37,458)
Feed 100.00 20
D = 37.455
15 BENZENE
89.676
16 37.455
FEED
O
30
6
122.5
Vaporisation %
— Figure 1 —
21
134 37.455 37.458
22

40
C TOLUENE
(9.452)
46.910
1.78 % mol
733.8 50 ETHYLBENZENE
91.065 BZ 0.075
28 (9.102)
TOL 18.029
EB 17.430 56.012
PX 13.772
R = 52.221
LC PARAXYLENE
MX 30.258 60
OX 20.436
(7?192)
Temperature (°C) FC 63.204
Residue 100.000
Pressure (atm)
METAXYLENE
Flow rate (kmol/h) FC 52.221 (15.801)
D PCD 2458 B
Duty (t/h) AROMATICS 70

155.3
F.G.
Q C = 6536
DEBUTAIZER
01312_A_A
— Material balance —
12,0 36,3
11,65 0
DV Hydrogene
1 36,5 1,85 2 Ethane (1,78)
68,4 (0,11)
2,55
4
6 Propane (6,68) Méthane

e(0,66)
1026 8
7 9,18
87,7 DL 10
i-Butane (4,29)
(20,04)
13,47
rf = 2,39
15
393,2 % C 5 = 0,29 n-Butane (8,59)

1961,6 11
20
7
12 21,89
144,1 22,06
atm. abs. Iso-Pentane (2,98)
— Figure 2 —
Kmoles/h 25

°C
160,9 n-Pentane (7,02)
18 th/h
30
Others C5 (1,00)
35
26 186,6
12,39 Q R = 10535
rb = 0,99
40
R Cut C6 (17,08)
45
% C4 = 22,06 %
mol.
D PCD 2459 B
203,0 1532,1 % nC 4 = 0,28

8
III - OPERATING PRESSURE FOR A DISTILLATION COLUMN

1- PRESSURE PROFILE
The operating pressure for a distillation column is determined by the conditions that arise after
condensation in the condenser or in the reflux drum.
Under design conditions, this reference pressure is the vapor pressure or bubble point pressure of
the liquid distillate. It therefore depends mainly on the distillate's composition and temperature.
• The composition of the liquid distillate is a result of: the nature of the mixture that is being
processed, the separation specifications and the corresponding material balance that can
be deduced.
• The temperature in the reflux drum mainly depends on the temperature of the cooling
fluid that is used in the condenser.
The required separation determines the composition of the liquid distillate and the temperature of the
drum is approximately 30 to 50•C under design conditions in the common setup where water or air is
used as a cooling fluid. The temperature of the drum can be lower when chilled water or refrigerants
are is used. This is necessary when components are distilled whose critical temperatures are lower
than the ambient temperature. On the other hand, it can be higher if the vapor pressure of the distillate
at ambient temperature is lower than atmospheric pressure. Here the temperature of the drum is
usually kept slightly higher than the normal boiling temperature to avoid to operate in vacuum.
Poverhead
CONDENSER
∆Pc
Pressure drop
Pdrum
Pressure drop
on trays
Td
A
D
Pbottom
D PCD 2162 B
Based on the reference pressure Pb prevailing in the reflux drum, a pressure profile is created in the
column which corresponds to the pressure losses that occur because of the vapor stream flowing
from the reboiler to the condenser.
The value of the pressure drop Pc due to the condenser and the overhead line usually ranges from
200 to 500 mbars.

9
2- TRAY OPERATION AND PRESSURE DROP

The pressure drop due to the trays Pp is the sum of the pressure drops caused when the rising
vapors move through each tray. The value can vary from 3 to 20 mbars (design conditions). The figure
below illustrates the circulation of and contact between the two liquid and vapor phases on a one-way
tray. The pressure drop is the result of:
• Making the vapor gain speed in a restricted cross-sectional area in the active part of the
tray (dry tray pressure drop).
• The resistance exerted by the layer of liquid on the tray (pressure drop related to the
vapor passing through the liquid phase).
In an industrial column with fixed geometry, the through-tray pressure drop is therefore variable
according to the flow rates of liquid and vapor circulating in the column. In particular, any increment in
the hydraulic load of the trays causes an increase in the rising velocity of the vapors and a thicker layer
of liquid on the tray as well. These two effects have the same impact, i.e. to increase the through-tray
pressure drop.
Downcomer
ΔP : pressure drop per tray

Weir
hb : weir height
e : height of liquid above the weir
hpL : liquid pressure drop in U-turn
Vapour
hpV : vapour pressure drop
ΔPp H hpV
e hpL
hb
Vapour ACTIVE AREA

D PCD 294 A
Upstream Downstream
downcomer downcomer

10
It should be noted that the differential pressure from one tray to another causes an additional hydraulic
load in the downcomer. The total height of liquid H above the tray level therefore corresponds to the
sum of the following heights:
– weir height (30 to 70 mm determined by design) hb,
– height of liquid above the weir: e which depends on the liquid flow rate,
– height of liquid due to the restricted cross-section for the liquid when it enters the tray
(liquid pressure drop in the U-turn) hpL,
– height of liquid due to the vapor pressure drop hpV.
For nominal operating conditions, the height H reckoned in clear liquid is located approximately at the
halfway point between two trays. The between-tray spacing generally ranges from 40 to 70 cm.
This height H varies depending on operating conditions and may reach the level of the upper tray when
liquid and vapor flow rates are high. This corresponds to the flooding threshold and is detrimental to
the column's operating performance. At high vapor loads, it is also due to carryover of droplets of liquid
by the vapor stream. This occurs when the droplets have not had enough time to settle out between
two trays and are recycled to the upper tray. Recycling this additional liquid overloads the liquid stream
and contributes to flooding of the tray (flooding by vapor).
Another cause of flooding is the liquid flow rate when it is too high. The liquid can no longer flow or
separate properly from the vapor phase and eventually fills the downcomer. The simplified diagrams
below illustrate these two types of flooding. In actual fact, flooding is usually due to both excess liquid
and excess vapor flow rates at the same time.
D PCD 552 A
Normal tray operation Carryover and flooding Flooding

(excess vapour) (excess liquid)
During normal operation under design conditions, a pressure drop of 3 mbars occurs with specially
sized trays, 6 to 10 mbars are the most common values and values of over 15 mbars can be
considered high. In the usual setup, with columns of 20 to 50 real trays, the pressure at the reboiler
is therefore 0.1 to 0.5 bar higher than at the top of the column. This is a very slight relative
variation for columns that operate under pressure, but may be significant in columns operating under
vacuum conditions.

11
Additionally, it is important to point out that the design programs used to size or simulate industrial
columns are generally able to deal with the pressure variations caused by the trays. Since these
programs work on the basis of a theoretical number of trays, an overall efficiency value E is required
for real trays. In this way, each theoretical tray can be assigned the proper pressure drop by using the
following equation:
P real tray
P theoretical tray = E
3- PRESSURE CONTROL
The operating pressure of a distillation column directly influences the operating temperatures, the
fluid characteristics (the vapor volume flow rate in particular), and the heat exchange conditions at the
condenser and at the reboiler.
Variations in pressure are therefore likely to disturbance the operation of the column and may become
very troublesome when a temperature control is implemented to run the column.
Numerous disturbances may cause pressure variations, e.g. temperature and flow rate variations in
the cooling fluid, condenser fouling, and modification in process conditions. As a result, a control
system for the operating pressure is usually provided for.
Since the pressure is variable in the column, a particular pressure is controlled, often the pressure at
the top of the column. The pressure in the reflux drum, on a particular tray or at the bottom of the
column may also be used.
There are a large number of pressure control systems that can be classified into two major types
according to which control variable is used:
- adjusting the condensation duty by acting on the flow rate of cold fluid or by varying the heat
transfer area in the condensation sector (submerged condensers)
- adjusting the reflux drum conditions by gassing: hot bypass, outside gas makeup, or by
degassing
a - Acting on the condenser duty
The duty of the condenser can be regulated by acting on the cooling fluid flow rate or on the heat
transfer area. The diagrams below show the principle of these two systems.
PRC
In the cooling fluid flow rate method, the

pressure controller acts directly on an
automatic valve for liquids or on the fans
(angle of blades or speed) for air
condensers.
D PCD 2161 B

12
When the heat transfer surface area method

PRC is used, the area is made to vary by
submerging a selected number of tube arrays
in the condensates. Here the condensers are
said to be submerged.
Controlling the condensate discharge allows

the area required for condensation to be
D PCD 2153 C
adjusted.
b - Adjusting the reflux drum conditions
In these systems, there is no action on the condenser -- its efficiency is what it is because of the cold
fluid flow rate, the temperatures and any degree of fouling. Depending on its performance, the required
corrective action is taken downstream at the reflux drum:
– by lower pressure conditions (when the condenser is too efficient) a vapor makeup is
brought about by bypassing the condenser or gassing is implemented with outside gas
– by higher pressure conditions, (when the condenser is not efficient enough) degassing is
performed
PRC
Condensation duty:
- too much: hot bypass

- not enough: degassing
D PCD 2153 D
The diagrams below show examples of types of systems that use gassing or degassing:
– gassing by bypassing the condenser or degassing at the reflux drum

13
– gassing by outside gas makeup or degassing
Degassing Gassing
PRC
D PCD 2153 B
It should be noted that in both cases, when the condenser is too efficient, gassing offsets the
inadequate vapor pressure of the drum liquid. The liquid is no longer at liquid-vapor equilibrium, it is
said to be subcooled. Subcooling is variable depending on the operating temperature of the drum and
can be a troublesome cause of perturbances in smooth operation via the reflux.

14
IV - ENERGY BALANCE AND LIQUID-VAPOR CIRCULATION INSIDE AN INDUSTRIAL

DISTILLATION COLUMN
1- ENERGY BALANCE FOR A DISTILLATION COLUMN

Given the following symbols:
A, D, R molar or mass flow rates
HA, hD, hR molar or mass enthalpies of the feed, the liquid distillate and the residue
QC duty of the condenser
QR duty of the reboiler,
the energy balance for a column inside the enclosed area shown in the diagram below can be written
as follows (in coherent units and disregarding heat losses):
Energy balance
QC Inflow Outflow
A • HA + QR = D • hD + R • hR + Q c
A, HA
D,hD
QR
D PCD 553 A
R,hR
Inflow
• Thermal energy input by the feed A . HA. It depends mainly on the degree of vaporization of
the feed.
• Heat input by the heating fluid at the column reboiler QR.
Outflow
• Heat flow rates carried off by the products at the top and at the bottom, i.e. D . hD and
R . h R.
• Heat flow rates removed by the cooling medium at the condenser QC.

15
2- CONDENSING RATE QC
Depending on the physical state of the distillate, two types of condensers can be distinguished: total or
partial. A total condenser implies a liquid distillate, while a partial condenser involves a vapor or mixed
distillate.
Total condenser Partial condenser
DV DV
D PCD 554 B
DL DL
Liquid distillate Mixed distillate Vapor distillate
The function of the condenser is therefore at least to condense the external reflux of the column in all
instances. Total or partial condensation of the distillate may be added.
For a total condenser, the duty QC is defined on the basis of material and energy balances in the
condenser area.
V1 , H 1
Lo
1
QC
D PCD 2154 A
D,h D
- V1 is the molar flow rate of the overhead vapors with enthalpy H 1,
- L0 is the molar flow rate of the external reflux.
Then: V1 = L0 + D (material balance)
V1 . H1 = (L0 D) . hD + QC (energy balance)
i.e.
QC = (L0 + D) . (H1 - hD ).

16
For a total condenser, Q C therefore appears as the condensation heat of the external reflux and of
the distillate. It can be calculated from the flow rates L0 and D and the data required to access the
enthalpies: distillate composition, temperatures at the top of the column and in the drum.
In many columns Q C corresponds to a quantity of waste energy since it is degraded at the ambient
temperature of cooling fluids such as water or air.
The reflux ratio, rf is defined to characterize the condenser duty and the liquid circulation initiated at
the top of the column by the external reflux. It is the ratio between the external reflux flow rate and the
distillate flow rate.
L0
Reflux ratio rf = D
By introducing rf into the expression of QC, we get:
QC = D . (rf + 1) . (H1 - hD)
This equation shows the existing proportionality between QC and rf for a given material balance,
(D = constant).
3- FUNCTION OF THE EXTERNAL REFLUX
OVERHEAD
overhead vapors The external reflux enters the column
LINE in the liquid state on the top tray.
Cooling
External reflux fluid Prior to this, the same amount had to
CONDENSER flow out of the column in the vapor
liquid
Condensation state with the overhead vapors. The
of the external liquid reflux receives a heat rate on the
reflux top tray in the column corresponding to
the amount of heat required to vaporize
it. this phenomenon of extracting heat
Internal
reflux
by vaporization is what gives the term
REFLUX vaporizing reflux that is sometimes
DRUM used to designate the external reflux.
D PCD 038 E
Distillate or overhead product

17
Heat is extracted at the expense of the rising vapors on the top tray, thereby causing them to condense
partially. This gives rise to a new liquid flow called the internal reflux. Vaporization and condensation
then proceed on each tray.
The heat that is taken in this way from the column by the external reflux is later given up to the cooling
fluid used in the condenser.
In summary, the external reflux acts as a device to extract heat from the column and then transmit it to
the cooling fluid in the condenser.

18
4- REBOILING RATE QR
The reboiler serves to partially vaporize the liquid in the bottom of the column in order to initiate a
vapor current.
Industrial columns may be equipped with different types of reboilers, some of which are illustrated
below.
Vertical or horizontal thermosiphon reboiler Vapour separation reboiler

Kettle type
1 1
D PCD 629 C
This reboiler partially vaporizes the liquid from
The liquid from the bottom of the column the bottom of the column and separates the
circulates naturally toward the reboiler where it resulting liquid and vapor phases.
is partially vaporized.
Fired heater
"once-through"reboiler
1
1
D PCD 629 D
The liquid is taken from the last bottom tray and

goes through the reboiler once. The liquid and
vapor phases are separated in the bottom of the The liquid from the bottom of the column is
column. pumped into the pipes of the fired heater
where it is partially vaporized.

19
Flow rate L = 140 kmol/h

Flow rate R = 50 kmol/h
Vaporization rate 30% mol
The limitation of admissible vaporization

rates often means that a device to
segregate liquids needs to be installed in
Heating fluid inlet
the bottom of the column. A standard
setup for thermosiphon reboilers is shown
below. A reboiled liquid can be drawn off
LC as a residue that is not mixed with the
Heating fluid outlet
liquid coming from the last tray.
D PCD 362 B
Residue
A simplified diagram with a reboiler considered as a theoretical tray is shown below.
The reboiler is fed by L'1 molar flow rate of liquid

coming from the last theoretical tray with an enthalpy
1'
V' R H' 0 h'1.
h' 1 L' 1
The streams coming from the reboiler V'0 (enthalpy
QR H'0) and R are considered to be in liquid-vapor
equilibrium.
D PCD 561 A
R, hR The material and energy balances can be written:
L'1 = V'0 + R
L'1 . h'1 + QR = V'0 . H'0 + R . hR
i.e.
QR = V'0 . (H'0 - h'1) + R . (hR - h'1)

20
Physically speaking, the duty of the reboiler includes:
– an initial component corresponding to the vaporization of V'0 since the difference H'0- h'1
corresponds to a latent heat of vaporization
– a second component for warming up the residue from the temperature of the last tray to
that of the reboiler. It corresponds to a sensible heat (hR - h'1) for heating a liquid
Generally speaking, the vaporization part is largely dominant and this allows the relation between QR
and V0 to be prioritized.
However, in some cases a significant variation in temperature between the last tray in the column and
the reboiler or a high residue flow rate gives particular importance to the residue heating component.
In actual practice, this formula cannot be used but Q R can, however, be reckoned easily by totaling the
heat input from the external hot fluid that is used for reboiling.
If its flow is M and its enthalpy expressed in coherent units is He at the reboiler inlet and H s at the
outlet, then:
QR = M . (He - Hs)
This is the duty of the reboiler calculated on the basis of the characteristics of the reboiling medium.
In order to characterize the duty of the reboiler and the vapor circulation in the column, we define the
reboiling ratio rb as the ratio between V'0 and R, i.e.:
V'0
Reboiling ratio = rb = R
By introducing rb in the expression for QR we get:
QR = rb . R . (H'0 - h'1 + R . (h R - h'1)
At a given cut point (R = constant), this equation shows the proportional relationship that exists
between the duty of the reboiler QR and the reboiling ratio rb.

21
5- FUNCTION OF THE VAPOR PRODUCED IN THE REBOILER
Flow
vapor Internal reflux
Vapor generated REBOILER

at the reboiler
Reboiling fluid
partial
vaporization
D PCD 038 F
Liquid of the Residue
bottom of the column or bottom product
The vapor flow generated at the reboiler enters the column in the gaseous state, but prior to this an
equivalent amount of liquid is fed into the bottom of the column from the last tray. This vapor flow is
therefore condensed on the bottom tray by giving up an amount of heat which is equal to the amount
that was required to vaporize it.
This heat input causes partial vaporization of the liquid coming down from the next-to-last tray, thereby
generating a new vapor flow. It will proceed toward the tray above where it will in turn be condensed
by vaporizing part of the internal reflux. This process is repeated from tray to tray and explains how
there is a continuous vapor flow from the bottom to the top of the column.
6- CONTROL OF THE REBOILER DUTY

The control systems for distillation column reboiling vary widely depending on the type of reboiler
used and the nature of the reboiling medium.
A distinction can mainly be made between:

• Reboilers that use steam or a gaseous fluid that condenses. Here the heat rate
transmitted to the reboiler is proportional to the vapor flow that is fed into the reboiler. If:
is the heat of condensation of the vapor and
M is its flow,
then:
QR = M .

22
As a result, QR and therefore V'0 are regulated by the vapor flow rate.
FC
Steam
D PCD 506 F
Condensates
• Reboilers with hot liquid where the amount of heat that is transferred depends largely on
the average temperature difference between the reboiling fluid and the reboiled fluid. As a
result, it is not proportional to the flow rate of hot liquid.
Given the possible disturbances, e.g. variations in pressure or temperature in the hot liquid
circuit, it is often advantageous to implement a system to control the transmitted heat rate.
X = QR QRQR= MCΔT
V' O XC
F T
Hot
liquid
D PCD 508 B
• Fired heaters where the amount of transferred heat can be regulated by the flow rate of the
liquid that is fed into the furnace and by its temperature at the furnace outlet.

23
7- MOLAR FLOW RATE PROFILES IN A DISTILLATION COLUMN
a - Theoretical profiles with constant molar flow rates
The standard theoretical profiles of the liquid and vapor molar flow rates in a distillation column are
shown on the diagram below.
QC = Condensation heat
V1 QC
of V1 = (Lo + D) D
External reflux Lo V1 Overhead vapor
Lo
D
D
V L Internal reflux L V
V-L=D
A (LA , VA) LA
VA
R
V' L' L' - V' = R V' L'
QR
V'o
D PCD 354 C
Vaporized flow rate V'
QR = Vaporization R in reboiler o R
of V'o
Molar flow rate
heating of R
These theoretical profiles are based on the Lewis hypotheses which say that the molar flow rates of
saturated liquid and vapor streams remain the same in distillation columns.
In view of the condensation and vaporization that occur on each tray, this assumes that the molar heat
of vaporization remains constant whatever the composition may be.
More simply stated, this means that on a tray the amount of heat released by the condensation of one
mole of vapor is equal to the amount of heat required to vaporize one mole of liquid.

24
The Lewis hypotheses

- constant molar heat of vaporization and condensation;
- each mole vaporized is replaced by a mole that is condensed;
- the molar flow rates of the saturated liquid and vapor phases remain constant.
Starting with the molar flow rate of the external reflux L0, the flow rate of the internal reflux in the
rectifying zone L is, however, a little higher than L0. This corresponds to an amount of condensed
liquid L that is greater than the amount that was vaporized L0.
The external reflux is not in fact injected in the saturated liquid state but as a subcooled liquid. This is
due to the fact that the pressure at the top of the column is higher than the reflux drum pressure. As a
result, even if the external reflux is a saturated liquid in the drum, it is in the subcooled liquid state at
the top of the column.
The consequence is additional condensation of vapors which corresponds to the heating required to
bring the subcooled reflux back to saturation conditions.
The vaporization and condensation process then proceeds on each tray, thereby maintaining the
continuity of the internal reflux all along the column. According to the preceding hypotheses, this yields
a constant internal reflux flow rate L in the rectifying zone.
The contribution by the liquid part of the feed LA gives rise to the constant internal reflux in the
stripping zone L'.
The stream L' obtained at the bottom of the column is fed into the reboiler and is partially vaporized.
This generates the revaporization flow V'0 that returns under the last tray in the column.
The nonvaporized part of L' makes up the residue of the bottom product R.
V'0 then gives rise to V' the molar vapor flow rate which remains constant throughout the stripping
zone.
When the vapor flow goes through the feed inlet tray, it incorporates the vapor part of the feed V A,
which results in V, the molar vapor flow rate in the rectifying zone. The overhead vapor flow V1 is
totally condensed then divided up into external reflux L0 and the overhead product or distillate D.

25
b - Significance of rectifying and stripping zones
The discontinuity of liquid-vapor circulation that appears at the feed inlet level defines two zones in the
column:
• The rectifying zone at the top, characterized by:
L
- a ratio V < 1,
- a difference V - L which is constant at all levels and equal to the distillate flow rate.
• The stripping zone at the bottom where there is:
L'
- a ratio V' > 1,
- a difference L' - V' that is constant and equal to the residue flow rate.
The difference in the names is related to the treatment given to the prevailing stream in each zone: a
vapor is rectified and a liquid is stripped.
c - Validity of theoretical profiles - Real profiles
In actual practice, the Lewis hypotheses are of course never borne out absolutely since the molar heat
of vaporization usually varies with the composition. The hypotheses do, however, give a fairly good
picture of reality in many cases. This is particularly true when the different components of the
processed feed have neighboring volatility values and form a mixture that behaves like an ideal
solution. The preceding condition usually assumes that the components belong to the same chemical
family.
When the volatility values are very different -- which yields quite a wide temperature gradient in the
column -- considerable deviations can be seen from the Lewis hypotheses. By way of an example,
Figures 3 and 4 on the following pages show the profiles of molar flow rates calculated in the aromatics
separation column which was discussed earlier. The hypotheses of constant molar flow rate are fairly
well verified. In contrast, the debutanizer is seen to have quite wide variations in flow rates. The simple
model of the Lewis hypotheses does, however, provide a simple way of assessing the variations in
liquid and vapor circulation inside industrial columns.

BEZENE SEPARATION COLUMN
01312_A_A
MOLAR FLOW RATE PROFILES
1.5 91.39
94.9 Reflux Over head steam
Molar flow rate
Distillate (kmol/h)
1 690.9 Reflux 50 100
53.935 % mol
BZ 99.9 D
% mol 80 1 0.1
TOL
BZ 41.77 EB
TOL 10.54 LRC PX
EB 10.15 MX
PX 8.02 FRC OX L V
MX 17.62 11
Distillate
OX 11.90 C
Internal reflux
Feed 100.00
Steam flow rate
15 BENZENE
89.676
16 37.455
A
FEED
O
122.5
26
Steam %
21
— Figure 3 —
134
22 R

C
V' L'
1.78 % mol
733.8 BZ 0.075
91.065 28
TOL 18.029
EB 17.430
PX 13.772
LC Residue
MX 30.258
D PCD 2460 B
OX 20.436
Temperature (°C) FC 100 150
Résidue 100.000 50
Pressure (atm) Steam from reboiler
flow rate (kmol/h) FC 52.221
Duty (t/h) AROMATICS
155.3
01312_A_A
F.G. DEBUTANIZER LIQUID VAPOR
Q C = 6536
PFLOW RATES PROFILES
Lo V1
12,0 36,3
11,65
1 36,5
68,4
1026
7 L D V
87,7
rf = 2,39
1961,6 393,2 % C 5 = 0,29

11 VA LA
27
12
144,1 atm. abs.
— Figure 4 —
Kmol/h
°C

18 160,9 th/h L'
V' R
26 186,6
12,39 Q R = 10535
rb = 0,99
% C4 = 22,06 V'o
203,0 1532,1 % nC 4 = 0,28
D PCD 2461 B
1000 2000 3000

28
d - Internal reflux
The real profiles and even the theoretical ones show a flow rate discontinuity between L0 external
reflux and L the internal reflux. The discontinuity is because the external reflux is subcooled as
mentioned earlier and can be explained basically by two causes.
• The pressure at the top of the column is greater than the pressure in the reflux drum, except
in special cases. Even if the reflux is at its bubble point under drum conditions, the external
reflux is subcooled at the higher pressure prevailing at the top of the column.
• Some pressure control systems, e.g. submerged condensers, use of gassing, cause the
reflux to be subcooled right from the reflux drum and this intensifies the first cause.
Accordingly, variations in temperature at the reflux drum can cause changes in internal liquid
circulation at a given external reflux flow rate. They can consequently be a source of disturbances that
trouble smooth operation of the column. When this is the case, it may be advantageous to implement
an internal reflux flow rate control system.
Specialists in process control usually employ a simple equation to calculate the internal reflux flow rate
from physical parameters that are easy to measure.
L = L0 (1 + kt)
L internal reflux flow rate

L0 external reflux flow rate
t temperature at the top of the column - temperature of the drum
k constant to be determined depending on process characteristics
An internal reflux flow rate control system is implemented according to a setup of the type shown
below.
TR
L = Lo (1 + KΔT)
XC
V L
FR
X = internal reflux TR
flow rate
D PCD 2500 B

29
It can be noted that when the temperature in the drum decreases, this system normally causes a
reduction in the external reflux flow rate in order to get a constant internal reflux flow rate. In contrast,
since the same behavior is foreseeable when the temperature at the top of the column increases, it is
easy to see that this control system can operate properly only when the temperature at the top of the
column is also regulated.
e - Feed inlet
The profiles show a discontinuity in the vicinity of the feed zone which is materialized in the context of
the Lewis hypotheses by the equations below:
V y n+1
L, xn
VA
V = V' + VA A yA
LA
xA
L' = L + LA ZA
V'
ym
L', xm+1
D PCD 1120 J
m
In actual fact, the profile discontinuities comply with these equations quite well.
Accordingly, the two liquid and vapor streams are seen to increase when they pass by the feed inlet
zone, except when the feed is at its bubble point,
V = V'
L
V = V’ Feed at its
A LA
bubble point
L' = L + A
V'
L' = L + A
D PCD 1120 H
or when it is at its dew point,
V = V' + A L'
V = V' + A Feed at its A

A V'
dew point
L' = L L = L'
D PCD 1120 G

30
It is also necessary to consider the case of feed introduced as a subcooled liquid or as a

superheated vapor in some particular columns. For both, induced streams are generated when the
feed comes back to equilibrium conditions.
• Vapor condensation and generation of an additional induced reflux when the feed is
subcooled.
L
VA
V < V' yA
Subcooled A A
L' > L + A
Liquid feed
V'
D PCD 1120 K
L'
m
• Liquid vaporization (induced vapor) when the feed is a superheated vapor.`
V > V’ + A L

L' < L A
Superheated
vapor feed
V'
L' < L
D PCD 1120 F
The same as for the external reflux-internal reflux relationship, the induced reflux flow rate can be
calculated by the energy balance.

31
V- TEMPERATURE AND CONCENTRATION PROFILES IN A DISTILLATION COLUMN

As soon as the operating pressure has been determined, the temperature profile in a distillation column will
match the variations in circulating stream composition more or less explicitly.
The temperatures that become established are in fact equilibrium temperatures that correspond to saturated
products: vapors at their dew point and liquids at their bubble point. At a specified pressure, the
temperature that prevails at a given point in the column characterizes the overall composition of the mixture
inside the column.
At a given pressure, the variation in temperatures is therefore directly related to the variation in liquid and
vapor stream concentrations on the trays.
The temperature-concentration relationship is simple to assess for binary mixtures. It is a little more
complicated for complex mixtures and may eventually involve draw-offs.
The temperature at any point in a column is related to:

- the composition of the vapor at this point (dew-point temperature of the vapor),
- the composition of the liquid at this point (bubble-point temperature of the liquid),
- the operating pressure.
1- CONCENTRATION AND TEMPERATURE PROFILES IN A COLUMN PROCESSING

A BINARY MIXTURE
It is easy to interpret the variation in component concentrations in the streams circulating inside a
distillation column that processes a binary mixture, since there is only one volatile component and one
heavy one.
If we focus on the mole fraction of the volatile component (a) in the liquid phase, we can see that it
will reach a high value close to 1 in the distillate and in the reflux L0; it will have a value close to zero in
the residue (provided of course that the aim is to separate the two components properly). The mole
fraction of the heavy component (b) is the complement of 1 cited for the other fraction and therefore
varies symmetrically in the opposite direction.
If the pressure is assumed to be constant, the corresponding temperatures are given by the isobaric
liquid (or vapor) composition-temperature equilibrium diagram.
t (°C) P t (°C)
Bottom
temperature Vap
or p
has
e
Liqu
id p
has
e
Overhead
temperature
D TH 079 B
Mole fraction in A
b a

32
When good quality separation is sought, numerous trays will work at each end on a very small
concentration interval. As such, the profiles have an asymptotic shape as shown in the diagrams
below.
t
bp a
L
o
Binary b
mixture
a - b
a
t 0 1 temperature
bp b b Liquid phase top bottom
D PCD 355 B
mole fraction temperature
t t
bp a bp b
An examination of the profiles raises the question of the best position for introducing the feed into the
column. So that the variations in composition are not thrown off, the feed is introduced in such a way
that its liquid fraction composition is close to that of the internal reflux with which it is mixed. For binary
mixtures, this means seeking identical temperatures.
2- CONCENTRATION AND TEMPERATURE PROFILES IN A COLUMN PROCESSING

A COMPLEX MIXTURE (MORE THAN TWO COMPONENTS)
The variations in composition in a column processing a complex mixture are much more complicated.
In a simple practical approach, one can look at the problem from the standpoint of total reflux. This
special case will be used to show the phenomena that are preserved as demonstrated by simulation
studies under normal operating conditions.
a - Study of concentration profiles in a column operating with total reflux
Total reflux operation is illustrated by the figure below.

33
Lo
p
Vp+1
Lp
yip+1 p+1
Xip
Vp+2 Lp+1
yip+2 p+2 Xip+1
D PCD 2209 E
This is a column where a given amount of feed A has been introduced. The feed circulates around
repeatedly and holds the cut point at the required value via the system of retention at the top and
bottom of the column. If tray holdup is disregarded, the amounts retained in the reflux drum and in the
reboiler are D and R.
This type of operation is governed by relatively simple laws. A material balance set up between any
two theoretical trays p and p + 1 including the top of the column gives:
Vp + 1 = Lp
Vp + 1, Lp are the overall molar flow rates that circulate between the two trays.
Likewise, if the mole fractions of i in Lp and Vp + 1 are called xip and yip + 1, a partial balance on
component i gives:
Vp + 1 . yip + 1 = Lp . xip
or:
yip + 1 = x ip (1)
This relationship shows that with total reflux the streams that meet between two trays have the same
composition.
Additionally, the thermodynamic equilibrium at tray p + 1 involves the streams that leave the tray, i.e.
Vp + 1 and Lp + 1. The corresponding compositions yip + 1 and xip + 1 are therefore related by the
equilibrium equation:
yip + 1 = K ip + 1 xip + 1
when Kip + 1 is the K value of component i on tray p + 1.

34
Given equation (1), this leads to:
xip = K ip + 1 xip + 1
As such, two consecutive mole fractions of component i in the liquid phase are related by the K value
of the same component i on the intermediate tray.
If K i > 1 (light) xi increases when rising
If K i < 1 (heavy) xi increases when coming down
So it is of interest to examine the variation in the value of the K factors all along the column. Very
approximately, it can be estimated by using the simplest form of the K value taken from Raoult's law
(liquid: ideal solution, vapor: mixture of ideal gases). If the vapor pressure of component i at a
temperature t and a pressure P is called PSi, then:
S
Pi
Ki = P
In the column:
– the total pressure P can be considered constant in an simplified approach,
– the vapor pressure of component i, PSi, decreases when the temperature drops, and this
causes a general decrease in all the K i from the bottom to the top of the column.
S
It can also be noted that K i is equal to 1 when P i = P, i.e. when the temperature t is equal to the
boiling point temperature of component i (tbpi) at the pressure P.
As a result, for this component i:
at any point where t > tbpi K i > 1, therefore this component will behave as a
light component
at any point where t < tbpi K i < 1, therefore it will behave as a heavy one
This leads to a classification for the components in the processed mixture into several categories
depending on the value of the boiling point temperature in relation to the column's operating
temperature range.
The diagram below shows an example concerning a seven component mixture:
• Light components whose boiling point temperature is lower than the temperature at the top
of the column (components A - B - C).
• Heavy components whose boiling point temperature is higher than the temperature at the
bottom of the column (component G).
• Intermediate components whose boiling point temperature is the same as a temperature

in the column. Among them are the key separation components of course (components LK -
HK -F).
35
t t bottom
top Column Temperature
temperature
tbp A tbp B tbp C tbp CK tbp HK tbp F tbpG
D TH 080 B
Light components Intermediate components Heavy components
From the standpoint of the value of the K factors, we can conclude that:
• Light components have a Ki that is always greater than 1, and therefore their
concentration in the liquid phase increases constantly from bottom to top in the column
(xip > xip + 1).
• Heavy components in contrast decrease in concentration in the liquid phase from bottom
to top in the column (xip < xip + 1).
• Intermediate components behave in two different ways:
- if t > tbpi, then K i > 1 and xip > xip + 1
- if t < tbpi, then Ki < 1 and xip < xip + 1.
Their concentration profile in the liquid phase is therefore always on the increase in the
lower part of the column, but reverses and starts to decrease after the boiling point
temperature has been reached.
Given the relative values of the boiling point temperatures, the reversal generally occurs in
the rectifying zone for the light key and in the stripping zone for the heavy key.
With total reflux, these considerations yield the characteristic profiles represented on the diagram
below involving the components b (light), g (heavy) and the two key components.
It can be noted that the vapor phase profiles are identical but offset by one tray (xip = yip+1).

36
a,b,c,d
b
t = tbp.d
)
LK
d(
a,b,c,d,e,f,g
t = tbp.e
Concentration profiles at
K)
(H
total reflux conditions
e
g
D PCD 2213 B
e,f,g 0 Molar fractions 1
x i or y i
b - Real concentration profiles
The concentration profiles determined for total reflux operation look practically the same for columns
operating under real conditions. The differences involve the absolute value of concentrations and the
position of maximum values of concentrations that are no longer located exactly on the trays where the
Ki values reach 1.
These real profiles can be determined by simulating column operation and figures 5 and 6 on the
following pages show the results obtained for the two examples presented earlier: benzene separation
column and debutanizer.
• For the benzene separation column, a maximum toluene (the heavy separation key)
concentration can be seen in the stripping zone. In contrast, benzene (the light key) shows
no maximum since it is the most volatile component in the mixture that is being processed.
However, it can be noted that the presence of impurities lighter than benzene, even in small
amounts, would cause a maximum concentration on one of the trays near the top of the
column.

01312_A_A
BENZENE SEPARATION
— Concentration profile in the liquid phase —
1,5 91,39
94,9
1 690,9
Top
53,935 % mol
BZ 99,9
% mol 80 1 0,1
TOL
BZ 41,77 EB
TOL 10,54 LRC PX
EB 10,15 MX
PX 8,02 FRC OX
MX 17,62 11
Distillate
OX 11,90 F
Feed 100,00
BZ
15 BENZENE
89,676
16 37,455
FEED Feed
O
37
122,5
% vap. 0
21
— Figure 5 —
134
22

F
TOL
1,78 % mol
733,8 BZ 0,075
91,065 28
TOL 18,029
EB 17,430
PX 13,772 OX
LC
MX 30,258
OX 20,436
D PCD 2462 B
Temperature (°C) FRC Bottom

Residue 100,000 0 0,2 0,4 0,6 0,8 1
Pressure (atm)
Flow rate (kmol/h) FRC 52,221
Thermal duty (t/h) AROMATICS
155,3
F.G.
01312_A_A
Q C = 6536
DEBUTANIZER
12,0 36,3 — Concentration profile in liquid phase —
11,65
1 36,5
68,4
C3
1026
7
87,7
rf = 2,39 nC 4
1961,6 393,2 % C 5 = 0,29

11
38
12
144,1 atm. abs.
Kmol/h
— Figure 6 —

°C
18 160,9 th/h
nC6
26 186,6
12,39 Q R = 10535 iC5
rb = 0,99
coupe
100/105 % mol C3, nC6
cut 100 - 105
2 10 20 30
D PCD 2463 B
% C4 = 22,06
203,0 1532,1 % nC 4 = 0,28 5 25 50 75
% mol nC4, iC5
39
• For the debutanizer, the volatile key, n-butane, shows a maximum concentration in
rectification and the heavy key, isopentane, also shows a maximum at the base of the
rectifying zone. This column operates on a wide range of components, i.e. over a wide
temperature interval and there are other components that a show maximum concentration.
Even for isopentane, a second maximum concentration value can be seen in the stripping
zone. This can be explained by the preferential revaporization of this compound in the
reboiler. There is in fact a considerable volatility interval between the C5 and the other
residue components.
c - Real temperature profiles
The temperature profiles in the columns that process complex mixtures can look extremely different
depending on the type of separation.
Separating a mixture with several components into a pure substance at the top and a mixture at the
bottom (e.g. the benzene separation column, Plate 7) yields an asymptotic profile on the pure
substance side as illustrated below.
Purification of the pure

substance a
abcd
Temperature (°C)
bcd Boling point Buble point

D PCD 570 B
temperature temperature
of the pure of the mixture bc
substance a
Separating a mixture into two mixtures can give widely varied profiles depending on the volatility
intervals of the components in the feed (e.g. the debutanizer, Figure 7).

TEMPERATURE PROILES
01312_A_A
V1
BENZENE SEPARATION V1 DEBUTANIZER
A
40
— Figure 7 —

R
°C °C
R
D PCD 2464 B
90 100 110 120 130 140 150 160 50 100 150 200
41
The influence of the heavy components in the feed on temperature variations can be noted in the
diagram below.
A-I
No heavy components
Backward shift of heavy components
Decrease in the internal

A-Z
volatility due to the feed
Sharp decrease in volatility

at the reboiler
D PCD 2502 C
I-Z Dew temperature Bubble temperature
of distillate of the residue
d - Example: Sidedraws
The maximum concentration values for some intermediate components in a distillation column mean
that it is possible to use sidedraws to get a product with a high concentration in a given intermediate
component.
The following separation can be performed for a mixture of three components A, B, and C whose
volatility decreases from A to C, assuming that the volatility of B is closer to A than to C.
A Side draw
B Stripping
rich in B
column
A, B, C
B
D PCD 1838 A
0 0,5 1
Concentrations in C
liquid phase

42
Here, the major impurity in the product that is drawn off is component A which can be eliminated by
stripping in a further column.
In fact, this use of sidedraws is almost common practice for another problem: separating the most
volatile component from a mixture, such as for the benzene column. Because of processing or storage
prior to distillation, the feed often contains small amounts of impurities that are more volatile than the
target component. Impurities are often inert gases, hydrogen and others which cause a maximum
concentration value to appear for the target component near the top of the column. This is what
justifies recovering the product by sidedraw. The zone located between the sidedraw and the top of the
column, which is designed to eliminate volatile impurities from the sidedraw, is sometimes called the
"pasteurization" zone.
Volatile
impurities
ies
imp tile
urit
a
Vol
A
Volatile
impurities A
+ABCD
0 1
D PCD 1839 A
Molar fraction in liquid phase
This layout is very common in petrochemical plant separations.
In most cases, sidedraws consist in removing part of the internal reflux from the column. However, it
should be pointed out that there are vapor stream sidedraws. This is true particularly in certain
extractive distillation setups where an intermediate component can not be drawn off in the liquid phase,
since this phase is diluted by the solvent. On the other hand, the solvent's very low volatility means that
it is practically absent from the gaseous phase where a high intermediate component concentration
can be found, thereby justifying a sidedraw.

43
B - OPERATING VARIABLES IN DISTILLATION COLUMNS -

CONTROL
I- CONCEPT OF DISTILLATION COLUMN SEPARATING POWER

The parameters that determine the separation capability of a distillation column are determined during
engineering design. There are three main divisions:
– the number of theoretical stages (or trays),
– the magnitude of internal liquid-vapor circulation related to the energy expended,
– the feed inlet level location
1- NUMBER OF THEORETICAL SEPARATION STAGES

It is obvious that the larger the number of theoretical separation stages, the greater the separating
power of a column is.
In an industrial distillation column, the number of theoretical stages depends on:
– the real number of trays, which is a given construction parameter,

– the efficiency of the trays, which depends on the type of tray, the nature of the mixture that
is processed and the operating conditions: pressure, temperature and hydraulic load.
In an simplified approach, it can be assumed that the number of theoretical stages is constant in an
existing column that always operates under roughly similar conditions. This approach is usually
adopted in simulation studies. However, it should be noted that this hypothesis loses its validity in the
event of substandard operation, e.g. trays with poor performance or damaged, flooding, loses its
volatility, etc.
Industrial columns have a constant number of real trays corresponding to a number of theoretical
stages that may be variable.
2- LIQUID-VAPOR CIRCULATION
The impact of liquid-vapor circulation on the separating power of the column is characterized by:
L
– the ratio V of liquid and vapor flow rates in the rectifying zone,
L'
– the ratio V in the stripping zone.
Despite the variations in flow rate, these ratios are relatively constant in each zone. The highest flow
rates are for vapor in the rectifying zone and for liquid in the stripping zone, i.e.:
L L'
V <1 and V' > 1

44
L L'
Distillation theory shows that the separating power of the contact stages increases if V and V'
approach the value 1.
With a given material balance (D and R = constant) this occurs when:
L
– L and V increase by the same amount, i.e. V increases and approaches 1,
L'
– L' and V' increase by the same amount, i.e. V' decreases and approaches 1.
The limit value 1 corresponds to the case termed total reflux when the liquid-vapor circulation in the
column becomes infinite.
Clearly, it is not always easy to handle L/V ratios since liquid and vapor flow rates are not accessible.
This explains why an attempt is made to define parameters that are easier to assess but have the
same significance. This is the function of the reflux ratio rf and the reboiling ratio rb, which are
defined below.
Lo
Lo
reflux ratio rf = D
FC LC
V L
A
D
V' L' V'o
reboiling ratio rb = R
V'o FC
LC
D PCD 2468 B
It can be noted that the reflux ratio is directly accessible by measuring the reflux and distillate flow
rates. This does not hold true for the reboiling ratio, since the value of V'o can only be estimated on the
basis of the heat flow transmitted to the reboiler Q R.
This largely explains why particular importance is given to the reflux ratio in assessing distillation
column operation.
The relationship between the L/V ratios and the reflux and reboiling ratios for a given material balance
is as follows:
– in rectification, if rf increases, then the liquid-vapor circulation grows and the L/V ratio
approaches 1;
– in stripping, if rb increases, then the liquid-vapor circulation varies in the same way and
L'/V' approaches 1.
As a result, the separating power of a distillation column increases when the reflux and reboiling ratios
go up.

45
Lastly, it should be noted that the preceding definitions of rf and rb are valid only for a simple column
with two products comprising a total condenser. When the setup is different the definitions used must
be in relation to the |L/V ratios.
If the column has a gaseous distillate G, for example, the corresponding definition with the same
significance is:
Lo
rf = D + G
In a rectifying column with sidedraws on the internal reflux, a reflux ratio must be defined for each zone
in order to take account of the discontinuity that occurs in the liquid circulation.
In the example shown in the diagram below the equivalent definitions of the reflux ratio are as follows:
Lo
overhead reflux ratio rf0 = D
L0
reflux ratio at
D
L1
S1 the first sidedraw rf1 = D + S
1
L1
reflux ratio at
D PCD 2469 A
S2
L2 L2
the second sidedraw rf2 = D + S + S
1 2
3- FEED INLET LOCATION

If the feed is improperly incorporated into the circulating streams in the column, it may be detrimental to
the separating power. As mentioned earlier in the simple instance of binary mixtures, an attempt is
made to introduce the feed in such a way that the composition of the feed is close to the composition of
the streams that it is mixed with in the column.
When this rule is not complied with, the impact of the feed inlet can throw off the variations in
composition, thereby hampering the column's overall performance. As a result, there is an ideal
position for the feed inlet for each column and for given feed and product specifications. This is called
the right feed position. When a column processes different feeds with variable separation objectives,
several positions must be anticipated for the feed inlet.

46
4- SEPARATING POWER TO MEET A GIVEN SEPARATION PROBLEM

Distillation column design shows that the series of technical solutions corresponding to the separating
power for a specified separation is illustrated by the curve below where the number of stages N vs. the
rf-rb couple is plotted.
N Minimum
(number of reflux
trays)
N Inproper feed position

Optimum Total
solution reflux
R ig
ht fe
N min e d pos
i ti o n
rf opt rf - rb
D PCD 566 A
rf min
rb min
This curve shows the effect of each of the different separating power parameters.
We can consider that a specified separation requires a given separating power that can be broken
down into:
– A larger number of stages N so as to operate with smaller liquid-vapor circulation values
and therefore less energy expended.
However, separation can not be achieved if the reflux and reboiling ratios drop below a
boundary value generally called the minimum reflux ratio (rf min). For this reflux ratio:
• energy consumption is at its lowest,
• liquid-vapor circulation values are at a minimum,
• the number of theoretical trays is infinite.
– Very high liquid-vapor circulation rates when rf and rb approach infinity. For these
conditions, often called total reflux, the number of trays N takes on a minimum value
Nmin.
– A position for the feed inlet into the column that is right (hyperbola-shaped curve) or wrong
(located in the cross-hatched area). In this context, improper feed inlet means:
• additional energy expended for a given number of stages,
• an increased number of trays required for a given reflux ratio.

47
The selection of optimum conditions is dictated by economic considerations that include:
– the investment cost (IC) of the column and its accessories,
– the operating cost (OC) which is mainly due to energy consumption by the condenser and
the reboiler.
The curves below show the characteristic shape of cost variations.
– The investment cost is infinite when rf = rf min and when rf •
– The operating cost is roughly proportional to the reflux ratio, since the relative magnitude of
this cost is directly related to the energy cost.
Costs Total cost
Minimum Depreciation cost

total
cost
Operating cost
D PCD 567 A
rfmin rf opt rf
The sum of the IC and the OC is materialized by a curve showing a minimum which defines the
optimum reflux ratio for the separation. Experience has situated this optimum in relation to the
boundary cases rf min and total reflux.
1.05 x rf min< rf optimum < 1.4 x rf min

N = 2 x N min

48
5- ADAPTING SEPARATING POWER TO SEPARATION DIFFICULTY

For comparable specifications, separation difficulty depends basically on the volatility interval between
the key components. The interval is usually characterized by the relative volatility of the volatile key in
relation to the heavy key, LK-HK.
In ideal solutions, this parameter can in fact be considered as approximately constant for all of a
distillation column's operating conditions. The definition of the relative volatility:
KLK
LK-HK = K
HK
shows that its value is greater than 1 and corresponds to the ratio of the vapor pressures at a mean
temperature in the column when the K values can be taken from Raoult's law.
PSLK
LK-HK = S
PHK taverage
It should be pointed out that when hydrocarbon mixtures are processed, the relative volatility depends
not only on the nature of the two key components, but also on the column's operating pressure. Higher
pressure means higher mean temperature and this causes the volatility interval to tighten up.
In summary, if the relative volatility of the volatile key in relation to the heavy key is greater than 2.5,
the separation can be considered fairly easy. It is more troublesome between 2.5 and 1.5 and below
this limit separations are termed difficult.
The required separating power can be prohibitively expensive when the relative volatility approaches
1.
The variations in corresponding column characteristics are illustrated by the figure below. It shows that
as the separation becomes more difficult, the number of theoretical stages required and the rf-rb
couple also increase at the same time. This means columns that are both higher and wider.

49
Number of stages
α LK-HK decreasing
um
it m ions
op lut
so
D PCD 2571 B
Couple rf
rb
The limits on the distillation process are generally considered to be reached when the relative volatility
of the volatile key in relation to the heavy key becomes equal to 1.1.
Under this value there is a solution that can be used without changing the process, however. It consists
in having distillation operate in the presence of a solvent. The solvent must be miscible with the mixture
which is being separated. It has also to be able to throw off the natural volatility scale through different
interactions in the liquid phase between the two key components and the solvent itself. In this way,
separation is made easier. This process is called extractive distillation.

50
II - VARIATIONS IN A DISTILLATION COLUMN'S SEPARATING POWER

Adapting the separating power of an industrial distillation column usually means modifying the liquid and
vapor circulation. The possibility of acting on the other two variables, i.e. number of theoretical stages and
position of the feed inlet, is in fact restricted:
• The number of theoretical stages is considered in an initial approximation as being

constant, but can vary considerably given the changes in efficiency due to the variations in
the hydraulic load of real trays. A simulation study of an industrial column with different
operating conditions corresponding to various liquid and vapor circulation values can be
used to define these variations.
In addition, it is sometimes possible to modify the number of theoretical stages in a

distillation column by replacing the existing trays with more efficient liquid-vapor contact
material.
• The feed inlet position is often located in only one place and must be accepted as is. The
question of the right or wrong position should, however, be raised when there are several
possible inlet levels and when the feed itself varies significantly in composition and in
thermal state.
The essential operational variable is therefore the liquid and vapor circulation. We discuss a change in the
separating power at a constant cut point in the following section. The cases we consider assume that the feed
characteristics and the operating pressure remain constant for the column.
1- INCREASED REFLUX AND REBOILING RATE WITH A CONSTANT CUT POINT

a - Implementation
Given the control layout presented earlier, the procedure consists in:
– increasing the set point of the external reflux flow rate L0 controller,
– increasing the duty of the reboiler in order to generate more vapor flow V'0 .
These two adjustments -- the first one direct and the second via an intermediate heat transmission
mechanism -- must be made in such a way that the cut point remains unchanged, i.e. so that D and R
remain constant.
This implies that the variation L0 in the reflux takes place at the same time as a variation V1 in the
overhead vapor flow rate such that:
L0 = V1
If the heat of condensation of the overhead vapors is called , it is easy to show that
QR = V1 .
or
QR = L0 .
Depending on the type of exchange at the reboiler, the required additional heat transfer can be
implemented.
51
b - Variations in liquid and vapor circulation in the column
The diagram below shows the modification in circulation.
QC + ΔQC
V1 + ΔV1
ΔV1 = ΔLo
Lo + ΔLo
LC
FC
ΔV = ΔL
V + ΔV L + ΔL
D constant
A
V' + ΔV' L' + ΔL'
ΔV' = ΔL'
V'o + ΔV'o
FC
LC
QR + ΔQR
TI
D PCD 293 C
R constant
The increase in external reflux flow rate L0 causes a rise in the internal refluxes L and L'. Since R is
constant, this extra liquid is vaporized in the reboiler, thereby causing a parallel increase in the flow
rates V'0, V', V and V1.
As a result, there is a rise in the liquid and vapor flows circulating in the column. A material balance set
up between any two trays shows that at all levels L = V or L' = V'.
The liquid and vapor flow rate profiles are therefore shifted by an equal value.

52
c - Variations in separating power and product purity
The reflux ratio rf = L0/D and the reboiling ratio rb = V'0/R both increase since L0 and V'0 are larger
and the cut point is unchanged. As a result, the overall separating power is greater for the column,
provided that all possible effects of the number of theoretical stages and the feed inlet position are
disregarded (as is often justified). It can also be noted that the same conclusion, i.e. improved
separating power, can be drawn by examining the variations in L/V ratios.
– In rectification (L/V < 1)
L = V
L + L L
and V + V > V therefore closer to 1
– In stripping (L'/V'> 1)
L' = V'
L' + L' L'

V' + V' < V' therefore closer to 1
With a constant cut point, improved separating power leads to better separation as illustrated on the
diagram below.
b D
c
Base case
After increasing
d of L & V traffics
e R
D PCD 569 A
Greater separating power with a constant material balance

D is purer and therefore lighter
R is purer and therefore heavier

53
d - Variations in temperature
At constant pressure, the changes in composition of the products and of the streams that circulate in
the column cause changes in temperature.
— Top and bottom temperatures
Given the improved product quality:

• The overhead temperature, which is the distillate dew point temperature, tends to
decrease.
It decreases in fact if D is relatively impure to begin with. In contrast, it remains
roughly constant if the overhead product is initially obtained with a high degree of
purity. In this case, the fact that the product is lighter does not cause any significant
drop in its dew point temperature.
• The bottom temperature tends to rise, but this likewise depends on the initial
purity.
Generally speaking, the temperature is sensitive to a change in composition only
when the change is significant. This parameter can represent the product
composition accurately when the impurity values amount to a few percent.
In contrast, it becomes less sensitive, then insensitive to changes in composition
when they amount to less than one percent and even less (thousands and hundreds
of ppm). The concentration expressed in ppm values is common in petrochemical
processes.
– Temperature profile in the column

Improvements in the amounts of impurities obtained at the top and at the bottom cause variations
in composition inside the column. Products with fewer heavy impurities are found on the trays in
the rectifying zone. Likewise, products containing fewer light impurities are found in the stripping
zone.
At first glance then, the temperatures in the rectifying zone tend to decrease and those in the
stripping zone tend to increase. The new temperature profile cuts through the former one and can
look like the profile in the following diagram.
abc
After increased reflux and

reboiling with a constant cut point
Reference
case
D PCD 570 A
t t Temperature (°C)
def top bottom

54
It should be pointed out, however, that a particular reaction is observed for each column. Even though
it complies with the remarks made above, it can yield variations in temperature that are rather different
from the ones depicted in the diagram. The point where the two profiles intersect -- and there is no
general rule governing this -- is sometimes shifted toward one end of the column or the other. In
addition, the presence of a mixed distillate (liquid and gaseous) can cause reverse variations in
temperature at the same time in the rectifying zone.
It is difficult to draw any general rules from the foregoing considerations. However, when the profiles
are examined, they show that with a constant cut point the temperatures inside the column have
some, though not very much, sensitivity to the new separating power that is implemented.
e - Energy aspect
The energy balance is modified little with respect to the products. Therefore, in the case under study,
an equivalent increase in thermal load is seen in the condenser and the reboiler.
QR = Q C
The additional energy expenditure can furthermore be affected by possible reductions in exchange
temperature potentials in the condenser and the reboiler.
This increase in thermal loads is the result of a general correlation in distillation between
better separation . more energy expended
f - Tray operation
The increased hydraulic load in the column causes a thicker layer of liquid to form on the tray and
makes the vapor rise faster. The results are a greater pressure drop and more mechanical carryover of
liquid that may lead to flooding due to liquid backing up in the downcomer.
At high loads, the pressure drop of the vapor flow going through a valve tray corresponds to what is
called the dry tray pressure drop. It increases as the square of the vapor volume flow rate. The
pressure of the height of liquid on the tray, which of course increases with the liquid flow rate, must be
added as well.
2- INFLUENCE OF THE NEW SEPARATING POWER ON RESULTING SEPARATION

It is obvious that opposite action, i.e. decrease in reflux and reboiling flow rate with a constant cut
point, will logically lead to an opposite outcome.
Accordingly, it is possible to adapt the separating power around a given cut point. This means variable
fractionation quality as illustrated on the diagram below.

55
a
SP2
b D
SP0
c SP1
e R
D PCD 571 A
SP : separating power SP1 > SP0 > SP2
The improvement (or deterioration) in purity is not symmetrical for each of the two products, distillate
and residue. It depends on the D/R ratio to the extent that for the same transfer of impurities, the
smaller flow rate undergoes the greater variation in concentration and in cut point position. With an
infinitely greater separating power, it is clear that the fractionation that is achieved corresponds to the
horizontal line determined by the cut point. If the cut point is not located exactly on the intersection of
the two key components, one of the two products -- this is the case of the residue in the example in the
diagram above -- has an impurity content that approaches a finite value different from zero.
Figure 8 on the following page shows the variations in separation with reflux and reboiling ratios for the
debutanizer that was presented earlier. It also gives the corresponding energy consumption.

Debutanizer
01312_A_A
INFLUENCE OF VARIATION IN REFLUX 12400
1.5 3.0 AND REBOILING WITH A CONSTANT CUT POINT QR 12200
12000
11800
% (i + n)C4
% (i + n)C5
Q R (th/h)
% (i
11600
% (i +
+ n)
11400
C4
n) C 5
1.0 2.0 11200
11000
10800
56
10600
— Figure 8 —
10400

0.5 1.0 10200
0.4 0.8 10000
0.3 0.6 9800
0.2 0.4 9600
0.1 0.2 9400
0 0
1.72 1.80 1.89 1.87 2.05 2.14 2.22 2.30 2.39 2.47 2.56 2.64 2.72 2.89 3.06 rf 3.39
D PCD 2499 B
0.85 0.87 0.89 0.91 0.93 0.94 0.96 0.98 0.99 1.01 1.03 1.04 1.06 1.09 1.12 rb 1.19
57
III - VARIATION IN THE MATERIAL BALANCE FOR INDUSTRIAL COLUMNS -SENSITIVE

TRAY TEMPERATURE CONTROL
1- IMPACT OF DISTURBANCES ON DISTILLATION COLUMN OPERATION
The chief causes of disturbances that can cause disadjustments in industrial columns are listed below:
- Variation in feed characteristics: flow rate, composition, thermal state.

- Change in condenser efficiency and particularly in the reflux temperature. This point is
directly related with the system controlling the operating pressure in the column.
- Modification in reboiling conditions: temperature and pressure of the reboiling medium
reboiler operating problems, etc.
These disturbances are usually propagated inside the process by a modification in the liquid and vapor
circulation in the column. For example, an increase in feed temperature causes a higher vapor flow
rate in the rectifying zone and a reduction in liquid flow rate in the stripping zone. Given the reference
control setup presented earlier, this results in a modification in the distillate and residue flow rates,
i.e. a change in the cut point.
Generally speaking, the other disturbances mentioned result in the same type of consequences.
with the reference control setup
Disturbances modification in L-V change in material

circulation balance
With a view to installing more efficient control, it is of interest to study the behavior of distillation
columns when their material balance is modified. It can be modified in a simple way:
- either by changing only the reflux flow rate,
- or by changing only the hot fluid flow rate at the reboiler.
The feed characteristics and the operating pressure of the column are assumed to be unchanged in
the following discussion. It involves modifications in operating conditions when the cut point is changed
either by reboiling or by reflux.

58
2- CHANGE IN THE CUT POINT BY INCREASED REBOILING

As stated earlier, the feed cut point is determined by the reflux flow rate L0 and by the reboiler duty QR.
Any action on one of the two parameters will modify the cut point.
The consequences of increased Q R are analyzed below.
a - Implementation
The action consists in increasing the flow rate of reboiling medium:
– if it is hot oil (pump-around type), there is a change from:
m hot oil flow rate

QR = m . c . T c specific heat
t temperature drop of hot fluid in the reboiler
to: Q'R = m' . c . t'

with m' > m
and t < t' for the same inlet temperature, the outlet temperature of the hot fluid
rises
The amount of heat transferred Q'R is greater than QR, since the mean temperature
potential has grown while at the same time the exchange coefficient has slightly improved.
- If the steam is condensed (not overly superheated):
QR = M . M steam flow rate

heat of condensation of the steam
and this becomes:
Q'R = M' . with M' > M
b - Variations in liquid and vapor circulation in the column
The increase QR of QR causes additional vapor to be generated V'0 in the reboiler and in general
more vapor circulation in the column.
At the same time, the liquid circulation remains roughly constant as shown in the diagram below, since
the external reflux flow rate has not changed and the feed has not been modified.

59
V 1+ Δ V 1
Lo constant
FC
LC
V increases L
Constant
feed More or D+ΔD
less constant
L'
V' increases
V'o + ΔV'o Δ R = ΔD
FC
LC
Q R + ΔQ R
TI
R - ΔR
D PCD 568 B
The first consequence of such a modification is that the cut point is changed with an increased
distillate flow rate and a reduced residue flow rate here.
The adjustment in the balance at the top of the column is such that D grows by D = V1, since V1
is of the same order of magnitude as V'0. At the bottom of the column, the reduced residue flow rate
corresponds in the same way to the excess vaporization of the liquid that is fed into the reboiler. This of
course gives:
D = R

60
c - Variations in separating power and product purity
The separation that is achieved is not only the result of the variation in cut point, but also of the change
in separating power.
The action is usually considered to be small in scale since it has a significant effect. In that case, the
separating power can be deemed to be roughly constant. There is compensation between the reflux
ratio rf = L0/D which decreases and the reboiling ratio rb =V'0/R which increases. Likewise, the two
ratios L/V and L'/V' vary in the same way and both decrease.
Given these considerations, the new separation that is achieved is deduced from the initial separation
by a shift in the dividing line that corresponds to the change in cut point.
a
b D
c
Cut point
ΔD = Δ R d
A
e R
D PCD 572 A
The downward shift in the cut point yields the following variation in purity:
Distillate is less pure, therefore heavier

Residue is purer, therefore heavier
It can be noted in the diagram that the amount of product corresponding to the interval between the
two dividing lines has been transferred from the residue to the distillate.
Additionally, this case underscores the compromise between purity and yield at a given separating
power. An improvement in residue purity is achieved at the expense of its output.

61
d - Variations in temperatures in the column
The change in cut point by increased reboiling causes heavier products to be present at the top and at
the bottom of the column, but also on all the trays by continuity.
Heavier products
- at the top higher temperatures on all trays
- at the bottom
- on all trays
The diagrams below are but two examples among many that show the type of variation that can be
expected.
Top Top
D PCD 2496 B
Bottom Bottom
°C °C
In the left-hand diagram, the temperatures can be seen to undergo widely variable modifications on the
different trays. The reboiler and the overhead temperature are hardly modified.
In the right-hand diagram in contrast, the trays and the reboiler can be seen to receive about the same
temperature increment.
Each column reacts to this type of disturbance in its own specific way. In addition, the variations in
temperature that occur depend on the initial situation of a given column.
3- CHANGING THE CUT POINT BY OTHER TYPES OF ACTION

The previous change in cut point corresponding to an increase in distillate flow rate and a reduction in
residue flow rate was achieved by increasing reboiling. The same result could have been
accomplished by decreasing the reflux flow rate, with all other parameters remaining unchanged.
For small variations, the column would have behaved roughly in the same way.

62
Inversely, the change in cut point corresponding to a decrease in the distillate flow rate and an
increase in the residue flow rate can be achieved:
– either by increasing the reflux flow rate,

– or by reducing the duty of the reboiler.
The result is approximately the same in both cases and from an overall standpoint results in:
– a separating power that remains just about constant,

– a higher degree of purity for the distillate that becomes lighter, but less purity for the residue
that also becomes lighter,
– a general reduction in temperatures in the column that materializes the presence of lighter
products all throughout the column.
Generally speaking, a modification in liquid and vapor circulation that leads to a change in cut point
causes a homogeneous trend in the column:
– either toward heavier products all throughout and higher temperatures when D increases,
– or toward lighter products throughout and lower temperatures when D decreases.
The diagram below summarizes the behavior of product purity and temperature with the different types
of action.
D b
lighter
c Lo t
QR
QR
L o t
d heavier
A
e
R
D PCD 573 A

63
4- CONCEPT OF SENSITIVE TRAY

In conclusion, a change in liquid-vapor circulation corresponding to a change in material balance or cut
point results in a greater or lesser degree of variation in temperatures. Since this parameter is
particularly easy to measure, it is a handy way of characterizing the variations in liquid-vapor circulation
and therefore in the material balance.
The most useful temperatures in the column now remain to be selected to fulfill this function, and this
leads directly into the concept of sensitive tray.
The diagram below shows the static response of the benzene separation column presented earlier
when several variations are made in the external reflux flow rate (+2%, +6%, -2%, -6%) with respect to
the reference case.
90 100 110 120 130 140 150 160

1 Top
5
Reference
case
10
Increase in D
15
Feed
20
Decrease in D
(reflux + 2% et + 6%)
25
Bottom
D PCD 2498 B
Temperatures
90 100 110 120 130 140 150 °C 160
It shows that tray temperatures vary in extremely different ways in the different zones in the column.

64
The differences in tray behavior in comparison with the reference case are shown in the following
diagram for a variation in reflux flow rate of plus or minus 2% in moles.
Top 1
10
Feed 15
20
25
D PCD 2478 B
Δ t (°C) 29 Bottom Δ t (°C)
20 10 10 20
+
REFLUX + 2 % REFLUX - 2 %
All the trays in this column are sensitive to the change in cut point. However, the static process
response shows a great, almost symmetrical, sensitivity to the disturbance around tray 20 in the
stripping zone.

65
In contrast, the trays in the rectifying zone that are sensitive to an increase in distillate flow rate (drop in
reflux or rise in reboiling rate) react very little to the reverse disturbance.
Meanwhile, the lower trays in the column are very sensitive to a reduction in distillate flow rate (rise in
reflux or drop in reboiling rate), but in contrast undergo only a small temperature increase in the
opposite case.
The sensitivity of column temperatures to the feed cut point dictates that it should be kept the same by
using the temperature controller of one of the trays in the column. This controller, whose function is to
maintain the same material balance when any disturbances occur, must be able to act on the liquid-
vapor circulation and therefore adjusts either the reflux flow rate or reboiling. The tray selected is
usually the one that is the most sensitive to conditions on both sides of the reference conditions and it
is generally termed the sensitive tray.
However, it is not easy to select the ideal tray for two basic reasons:
– Each column or rather each separation has reactions that are specific to it and so there are
no general rules as to the position of the sensitive tray.
– In the same column, but for different reference conditions -- in particular variable product
quality -- significant differences can be observed in the trays' temperature reactions. The
sensitive tray in one case is no longer necessarily ideal in another one.
The first point regarding the differences in column behavior is illustrated by the variations in
temperature in the debutanizer. The cut point is changed by reflux in Figure 9 or by reboiling in
Figure 10 on the following pages. The different cases presented are distinguished by the relative
distillate values, with D0 corresponding to the reference case.
They show two sensitivity zones in rectification and in stripping. The rectifying zone is usually preferred
for this type of column because the temperatures are very sensitive to the increase in distillate, i.e. to
the fact that products become heavier. Here, this corresponds to a greater amount of C5 present in the
overhead LPG.
In addition, the conditions in the stripping zone, which are variable depending on the end point of the
gasoline that is processed, seem to be less favorable for implementing this type of control.

Variation in the
01312_A_A
cut point by
the reboiling VARIATION IN THE CUT POINT BY THE REFLUX
B
1
1
D = 1.064 x Do
D = 1.020 x Do
Do
D = 0.982 x Do
D = 0.936 x Do
11
11
12
12
66
— Figure 9 —

26
R en °C
D PCD 2480 B
50 100 150 200

Variation in the
01312_A_A
cut point by VARIATION IN THE CUT POINT BY THE REBOILING
B the reboiling
1
1
D = 1.055 x Do
D = 1.020 x Do
Do
D = 0.982 x Do
D = 0.945 x Do
11
12 11
12
67
— Figure 10 —

26
R en °C
D PCD 2479 B
30 50 80 100 130 150 180 200

68
5- IMPLEMENTING SENSITIVE TRAY TEMPERATURE CONTROL

The diagrams below show two types of control system layouts. They are not the only ones possible
and it may be advantageous for example to control the temperature of a sensitive tray in the rectifying
zone by reboiling.
LC LC
FC FC
TC
TC
FC FC
LC LC
D PCD 2481 D
The control schemes can be seen to modify the significance of action on adjustment parameters:
– Modifying the temperature of the sensitive tray means changing the material balance, and
causes all the products either to become heavier (higher temperature set point) or lighter
(lower temperature set point).
– Changing the set point of the controller that is not involved in temperature control means
changing the liquid-vapor circulation in the column, i.e. the separating power.
• Sensitive tray TRC cut point

(material balance)
• Other controller separating power

(energy balance)
cascade on reflux (right-hand diagram)
cascade on reboiling (left-hand diagram)

69
6- ADVANTAGES AND LIMITS OF SENSITIVE TRAY TEMPERATURE CONTROL

The ideal control system for a distillation column is the one that would hold products to required quality
specifications whatever the process disturbances.
In dealing with the different disturbances, the possibilities of sensitive tray temperature control should
be examined. The example presented below corresponds to a relatively simple case where the feed
undergoes a change in thermal state without any modification in composition.
The consequences of an increase in feed temperature are analyzed below in three control
configurations:
– The reference system presented earlier with an independent reflux and reboiling control.
– Sensitive tray temperature control in rectification governing the reflux.
– Sensitive tray temperature control in stripping governing reboiling.
a - Reference system
The increase in feed temperature causes more vapor to circulate in rectification V and less liquid in the
stripping zone L'. With constant reflux and reboiling, the results are:
– A change in cut point with an increase in D and a reverse variation in R without any
significant change in the separating power.
– D, R and all the products in the column become heavier, along with the corresponding rise
in temperatures.
– If the initial products complied with specifications, the residue is now too pure and the
distillate is now off-grade.
FC LC
V L=
Feed
t Alim.
D
V'= L'
FC
LC
D PCD 2482 B

70
b - Sensitive tray cascade on reflux
To offset the increased vapor circulation and prevent a corresponding rise in temperature, the
controller acts by increasing the external reflux flow rate.
If we assume that this action is performed in such a way that the feed cut point is kept the same, the
situation winds up approximately as follows:
– Constant flow rate of products D and R,

– Increase in L, V and consequently in the reflux ratio,
– V' is constant (constant reboiling) and so L' and the reboiling ratio are also constant.
PC
LC
FC
TC
A D
FC
D PCD 2481 E
LC
On the whole, the separating power of the column is therefore enhanced, and this causes
overfractionation of products at a constant cut point.
It is therefore necessary to lower reboiling to come back to a separating power equivalent to the initial
value.
In the end, the column achieves the same separation with a higher load on the rectifying zone and on
the contrary the stripping zone operating with less liquid-vapor circulation. As a result, the temperature
of the sensitive tray may have to be slightly modified to come back to the original cut point.

71
c - Sensitive tray cascade on reboiling
– The cut point is kept roughly the same in this instance by lowering reboiling, thereby
causing a decrease in V' and in the reboiling ratio as well.
– L and therefore V and the reflux ratio remain constant.
Contrary to the preceding example, there is a poorer separating power which means
products that are inadequately separated. As a result, the reflux flow rate must be increased
(and consequently reboiling as well via the TRC) in order to come back to the original
separating power.
PC
LC
FC
A D
TC
FC
D PCD 2481 F
LC
These three operating cases emphasize the advantages of this type of regulation, which is
mainly characterized by:
- Attenuation of the disturbance and approximately the same material balance and cut
point.
- Implementation of a separating power that is either excessively high or low, but in any
case different from what is required.
The temperature controller therefore keeps the column working under conditions that are not
overly degraded, but it can in no way ensure constant separation quality with this type of
disturbance.

72
IV - CHANGE IN FEED CHARACTERISTICS
1- CHANGE IN FEED FLOW RATE

a - Consequences of a change in feed flow rate
This disturbance naturally causes a modification in the liquid-vapor circulation inside the column and a
change in the distillate and residue flow rates, usually along with a modification in the cut point.
Generally speaking, when the feed flow rate increases: A A'>A:
– Highly vaporized feed causes an increase in D, D such that:
D+ D D
A' > A
and therefore a change in the cut point to the benefit of D, and so all the products in the
column become heavier.
- Slightly vaporized feed causes a small increment in D such that:
D+ D D
A' < A
and therefore a change in cut point at the expense of D, and so all the products in the
column become lighter.
In some cases, the state of feed vaporization can be such that D/A remains constant when the feed
flow rate is increased. Though the cut point remains the same, the separating power is modified since
rf and rb decrease. L0, V'0 are approximately constant and D and R increase with reduced product
purity as a consequence.
b - Operation with a different feed flow rate
When the feed flow rate is changed in a distillation column, the conditions that help preserve product
quality are those that help maintain the separating power.
If a possible variation in tray efficiency is disregarded (a point that is not automatically justified),
maintaining the separating power means keeping the reflux ratio and the reboiling ratio constant or
keeping the L/V or L'/V' ratios identical.
If we examine a variation in feed flow rate that becomes kA for example, manufacturing products of
constant quality implies the following homothetic operation with respect to the original conditions:
– constant cut point: D becomes kD and R, kR,
– constant separating power, which means multiplying L0 and V'0 by the same k factor to
keep rf and rb the same.
The duty of the condenser and the reboiler is modified in the same proportion along with the hydraulic
load on the trays.

73
It can therefore be seen that an industrial distillation column has a capacity limit which corresponds
either to maximum heat exchange equipment performance or to tray flooding.
Homothetic operation
Material Balance Separating power
A k.A Lo kLo
D k.D QR kQR
R k.R QC kQC
c - Implementing control to deal with variations in feed flow rate
A sensitive tray temperature control on a distillation column is capable of modifying the distillate and
residue flow rates when the feed flow rate varies, so that the cut point remains constant.
Disturbance TRC action

Cut point
Variation in maintained
sensitive tray
feed flow rate constant
If the control variable of the sensitive tray TRC is the reflux flow rate, the required separating power
correction is made on reboiling.
On the contrary, if the TRC cascades the reboiling medium flow rate, the separating power is adjusted
by the reflux.
Here it may be of interest to implement a control working on predictive compensation of variations in

feed flow rate (feed forward control). This means that feed flow rate variations must be taken into
account for action designed either to:
– maintain a constant reflux ratio (TRC on reboiling),
QR
– or maintain a constant reboiling ratio (TRC on the reflux) via the ratio A.
The diagram below shows implementation in the second instance.

74
PC
TC LC
FC
A D
FT
QR
QR A
TT FT
QR LC
X =
A
XC
TT
D PCD 2486 B
R
Since it is a hot oil reboiler, the developed variable QR is first calculated, then QR/A and this ratio is
kept constant by acting on the hot oil flow rate.
2- CHANGE IN FEED TEMPERATURE

The consequences of a change in temperature, and therefore in the state of vaporization of the feed,
have already been analyzed in different control configurations to show the possibilities of sensitive tray
temperature control.
The operating conditions that help maintain product quality have only been mentioned.
Analysis of the way the separating power varies can be used to define these conditions in the case
where there is an increase in feed temperature, for example.
This disturbance causes more vapor circulation and less liquid circulation in the column. This means a
change in cut point to the benefit of the distillate flow rate.
There are two solutions for getting back to the original cut point by acting on only one parameter:
– Increase the reflux flow rate, but as we saw earlier the separating power was too high after
the cut point was reached:
rf is greater than the original reflux ratio

rb is equal to the original reboiling ratio.

75
- Decrease reboiling, but on the contrary the separating power is inadequate:
rf is equal to the original reflux ratio
rb is lower than the original reboiling ratio.
Generally speaking, the additional heat input by the feed allows the reboiling rate to be reduced but
increases the condenser duty QC.
The column's energy balance
AHA + QR = QC = DhD + Rh R
shows that the heat input term AHA + QR increases and consequently the process starts consuming
more energy. This means that the reduction in QR is less significant than the increase in AHA. The
heat energy input from the feed does not have the same value as the heat energy that goes into the
reboiler.
In summary, increased feed temperature when product specifications remain constant causes:
- A drop in reboiling duty QR, an increase in the condenser duty Q C and overall energy
expenditure that is greater for the process.
- Increased liquid-vapor circulation in the rectifying zone and therefore a higher load on
the trays.
- Decreased liquid and vapor flow rates in the stripping zone.
If the feed temperature were to be lower, the consequences would be just the opposite.
3- CHANGE IN FEED COMPOSITION

It is relatively complex to analyze the disturbances brought about by a change in feed composition and
the search for operating conditions that can be used in this situation to restore product quality. This is
because several parameters can vary simultaneously: composition, degree of vaporization, possibly
temperature and even flow rate.
Given modifications in feed characteristics, the separating power that can preserve product quality is
basically maintained by:
– The change in cut point, i.e. at constant feed flow rate by the change in flow rates D and
R.
Lighter feed results in an increase in D (D) and an equivalent decrease in R (R), for
example.

76
The change in feed composition roughly corresponds to the variation in distillate flow rate
D. The following diagram illustrates the change in cut point.
a a
b D D'
b
c
c
ΔD
d
A d
e R e R'
D PCD 574 A
f
f
It should be pointed out that heavier feed would, of course, have just the opposite
consequences.
– The change in values for the duo rf-rb (or the L/V ratios). The same separating power
corresponds in fact to a change in the values of rf and rb which is the result of two factors:
• Modification in D and R (rf = L0 /D and rb = V'0/R).
• Modification in the reflux and reboiling medium flow rate due to an almost inevitable
change in the vaporization rate of the feed when it enters the column.
The impact of the change in feed composition on the feed vaporization rate is absolutely fundamental
for the new operating conditions that need to be found to maintain separation and for the disturbances
that affect the column's operation as well. It depends on the characteristics of the feed circuit which
can bring about some widely varied situations: constant temperature if the feed temperature is
controlled, constant enthalpy, constant percentage vaporized, and in actual practice mainly all sorts of
intermediate situations.
In the following section, two specific examples of lighter feed are considered: with a constant
temperature and with a constant percent vaporized (without any change in the feed flow rate).
a - Lighter feed at constant temperature
At constant temperature, feed that is richer in volatile components (or less rich in heavy components) is
obviously vaporized to a greater degree provided the pressure remains constant.

77
If the additional amount of feed vaporized is called VA, the study of the influence of composition
changes on vaporization rates in liquid-vapor equilibriums at constant temperature and pressure shows
that:
VA > D
This means that the additional amount vaporized is much greater than the change in composition.
Consequently, the column naturally moves toward a change in cut point D' that is greater than
necessary, with all the consequences that this implies: heavier products, increased temperatures, etc.
At the same time as there is a change in composition, there is also a greater degree of feed
vaporization similar to that which occurs with an increase in feed temperature. In addition, as
mentioned earlier, the reflux flow rate must be increased and reboiling decreased here in order to
maintain the same separating power. This conclusion can be adopted here in an initial approach
contingent on possible additional degradation of the separating power due to the feed inlet position.
In this context, maintaining the same separation results in the following:
– An increased distillate flow rate along with a higher reflux flow rate, yielding an unanticipated
change in the reflux ratio.
– A lower residue flow rate along with reduced reboiling and therefore a change in the
reboiling ratio that can not be quantified.
It can be seen in this case that operating the column at a constant reflux ratio should not cause the
separating power to drift too far.
b - Lighter feed with a constant percent vaporized
The lighter feed must be offset by a decrease in its temperature in order to maintain the same percent
vaporized when it enters the column.
Since the amount of feed vaporized does not vary, it can be assumed that the same separating power
can be achieved without any change in the liquid and vapor circulation in the column, i.e. without
modifying the reflux and reboiling. This can be approximately true only if the feed inlet position does
not cause too much of an disturbance in the separating power, given the change in composition. Here
maintaining product quality leads to the following changes in the column's operating conditions:
– A higher distillate flow rate without any noticeable change in the reflux flow rate. This means
a lower reflux ratio.
– A lower residue flow rate without any noticeable change in reboiling. This means a higher
reboiling ratio.
It should be noted, however, that the change in cut point must be materialized by a modification in the
liquid and vapor circulation. This modification is brought about by adjusting the reflux and reboiling and
by the feed itself.

78
V- CHANGE IN A DISTILLATION COLUMN'S OPERATING PRESSURE

Pressure is known to be a particularly important parameter in distillation columns to the extent that it
determines the operating temperatures for a specified product quality. A change in pressure modifies the
volatility intervals between the components that are being separated, since relative volatilities decrease
when the pressure increases.
The following section deals with the consequences of a modification in the set point of the pressure controller
and the comparison between the way a column operates at two different pressures.
1- MODIFICATION IN OPERATING PRESSURE - INCREASED PRESSURE

Depending on the type of control system in use, the pressure controller acts on the condenser or on
the reflux drum conditions to get the required rise in pressure.
Higher pressure quickly modifies the liquid and vapor circulation in the column, since it means:
– A decrease in the vaporized fraction of the feed, to a greater or lesser extent depending
on whether the feed has a temperature regulation on entering the column or is inlet with
constant enthalpy. The two corresponding paths are shown on the pressure-temperature
diagram below.
Pressure
Constant enthalpy curves
Constant vaporized
fraction curves
P2
P1 Increasing %
3
D TH 1171 A
t Temperature

79
Starting at point 1, the path from 1 to 2 is such that the temperature is kept constant by regulation
when the pressure goes from P1 to P2, and the most significant decrease in percent vaporized
corresponds to it. The path from 1 to 3 follows an isoenthalpy curve leading to less of a decrease in the
percent vaporized and an increase in the feed temperature.
– An instantaneous drop in reboiler efficiency, since the equilibrium temperatures rise with the
pressure.
– A change in the equilibrium conditions on each tray, which means a smaller vapor flow to
the benefit of the liquid at constant enthalpy.
The overall result of the increased pressure is therefore to raise the liquid flow rate in the column at the
expense of the vapor flow rate. The consequences of this action are roughly the same as those
resulting from an increase in the reflux flow rate and a decrease in reboiling:
– A change in the cut point: less distillate, more residue,
– All of the products in the column become lighter.
Generally speaking, when the feed has no temperature regulator, the liquid-vapor circulation
undergoes modifications which -- at constant enthalpy -- correspond to the variation in the vaporized
fraction in the different liquid-vapor equilibriums when the pressure is changed. The variation is usually
small and the effect is not very significant. In contrast, it occurs very quickly since the dynamics are
very fast when the new pressure is established. If the feed temperature is kept constant, the effect on
the liquid and vapor circulation is much more significant, but in this case it is largely due to the variation
in feed enthalpy.
A decrease in pressure gives just the opposite consequences, i.e. less liquid circulation to the benefit
of the vapor flow and a change in the cut point corresponding to more distillate and heavier products.
2- COMPARISON OF COLUMN OPERATION AT TWO DIFFERENT PRESSURES

It is of interest to compare the way a column operates at two different pressures, but with the same
product quality and feed enthalpy value. This second point assumes that the feed provides a
constant heat input to the column and that consequently its vaporized fraction and temperature change
with the pressure via enthalpic flash.
If a decrease in operating pressure is considered, basically the following effects are observed:
– Less separating power must be implemented to achieve the same separation. This is due
to the increased volatility intervals between the components that are being separated and
causes a modification in the liquid and vapor circulation in the column.
Since a larger fraction of the feed is vaporized, the adjustment of the rf-rb duo means a
clear-cut drop in rb and therefore in QR, as well as in the reflux ratio by a much less
significant variation. Accordingly, the decrease in liquid and vapor circulation mainly affects
the stripping zone in the column.
Meanwhile, the condenser thermal load is not modified much, while the reboiler thermal
load decreases significantly, with a resulting energy saving.

80
– A drop in operating temperatures which corresponds to an approximately parallel shift in

the temperature profile in the column.
The temperature variation observed depends on the difference between the new and old
pressures but also on the initial pressure and on the nature of the mixture that is being
processed.
For a given mixture, the curve below shows the variation in equilibrium temperatures with
pressure.
P
P2
ΔP2
Δ P1 = Δ P2 Δt 1 > Δt2
ΔP1
P1 Δ t1 Δt2
D PCD 2490 A
t°C
t 1 t'1 t 2 t' 2
Given the exponential shape of this curve, the temperature variation for an equal pressure
variation is much greater at low pressure (t1 - t'1) than at high pressure (t'2 - t2).
In actual practice, a valid approach to the relationship between temperatures and pressure
is to note that the liquid-vapor equilibrium curves are included in the network of the
linearized hydrocarbon vapor pressure curves on the Cox chart. By placing a mean column
operating point on this diagram (point 1 - P1, t1) and by interpolating in the network, the new
temperature t2 and therefore the foreseeable temperature difference can be determined for
pressure P2.
This process is illustrated on the diagram below.
Pressure COX CHART
P2
2
P1
ΔP 1
D PCD 2491 B
Δt
t1 t2 Temperature

81
– A change in heat exchange conditions due to the modification in temperature potentials

at the condenser and at the reboiler. If, as we saw earlier, the duty of the condenser is
maintained approximately the same, the exchange possibilities at this level become
degraded and the pressure decrease maneuver can correspond only to a situation of
excess condensation capacity.
In contrast, reboiling is made easier: smaller duty and greater temperature potential.
– A modification in fluid characteristics particularly in the vapor flow. The vapor volume
flow rate increases, and this causes a faster rising space velocity with the same flow rate as
is approximately the case here in the rectifying zone. As a result, through-tray pressure
drops are higher. As shown by the laws governing gases, this effect is related to the ratio of
absolute pressures and moderated by the decrease in temperatures.
For the same pressure variation, the lower the original pressure is, the greater the increase
in volume of the vapors.
The same study can be contemplated by maintaining the same percent of feed vaporized on inlet
rather than the same feed enthalpy. This assumes that when a less efficient separating power is
implemented, there is a symmetrical decrease in the reflux and reboiling ratios, along with a reduction
in QC and QR as well.
3- ADAPTING THE COLUMN TO CHANGES IN OPERATING PRESSURE -

IMPLEMENTING QUALITY REGULATORS
The use of a regulation system based on the parameter temperature causes rapid degradation in the
degree of control when the pressure varies. The pressure influences the liquid-vapor equilibrium
temperatures and, as a result, the significance of a temperature being held constant changes with
pressure. Additionally, the pressure can be a disturbance, but it can also be an optimization variable.
This is because it is possible to reduce the pressure when the condenser so allows and make
separation easier and thereby save energy.
Mainly for this reason, but also to better protect against overfractionation which induces unnecessary
energy expenditures, it is advantageous to equip distillation columns with product quality regulators.
This involves installing on-line analyzers, usually chromatographs that can quickly detect the impurity
content in each of the products.
Given the advantages of the control system that was presented earlier, incorporating quality regulators
in the column's control setup consists in "topping off" the previous system as shown in the diagram
below.

82
FC LC
TC
Feed
AC
FC
LC
AC
D PCD 2492 B
– The quality of the overhead product is maintained by action on the temperature setting of
the sensitive tray, which is in turn regulated by the reflux. It is a double AC - TC - FC
cascade. The overhead quality is said to be maintained by the cut point.
– The quality of the bottom product is regulated by the thermal power of the reboiler. The
bottom product quality is said to be maintained by the separating power.
Another example is illustrated by the next diagram.

83
FR LC
Feed FR AC
FFC
TC
FC
LC
D PCD 2493 B
AC
– The overhead product quality is maintained by the separating power, here the reflux ratio
L0
rf = D
– The bottom product quality is regulated by the cut point via the temperature of a sensitive
tray in the stripping zone which governs reboiling.
The advantage in "cascading" the preceding system with the analyzers is that in the event of
disturbances on liquid-vapor circulation (except for pressure), the sensitive tray temperature
regulator prevents excessive degradation in operating conditions.
Degradations in quality are therefore theoretically limited, and this makes the work of quality
regulators easier.

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Refining-Petrochemicals-Chemicals-Engineering

DISTILLATION COLUMNS: OPERATION AND CONTROL

A - ANALYSIS OF DISTILLATION COLUMN OPERATION - BASIC CONTROL SYSTEMS

I - GENERAL DESCRIPTION OF A DISTILLATION COLUMN - TERMINOLOGY .........................2

II - MATERIAL BALANCE FOR THE COLUMN..................................................................................4

III - OPERATING PRESSURE FOR A DISTILLATION COLUMN ......................................................8

IV - ENERGY BALANCE AND LIQUID-VAPOR CIRCULATION INSIDE AN

V- TEMPERATURE AND CONCENTRATION PROFILES IN A DISTILLATION COLUMN..........31

DT BIN - 01312_A_A - Rev. 2 16/02/2009

B - OPERATING VARIABLES IN DISTILLATION COLUMNS - CONTROL

I - CONCEPT OF DISTILLATION COLUMN SEPARATING POWER ..........................................43

II - VARIATIONS IN A DISTILLATION COLUMN'S SEPARATING POWER .................................50

III - VARIATION IN THE MATERIAL BALANCE FOR INDUSTRIAL COLUMNS -

IV - CHANGE IN FEED CHARACTERISTICS ..................................................................................72

V- CHANGE IN A DISTILLATION COLUMN'S OPERATING PRESSURE ....................................78

01312_A_A © 2009 - IFP Training

– the number of trays or height of packing needed,

Consequently, the following study comprises two main parts:

01312_A_A © 2009 - IFP Training

A - ANALYSIS OF DISTILLATION COLUMN OPERATION - BASIC

I- GENERAL DESCRIPTION OF A DISTILLATION COLUMN - TERMINOLOGY

Overhead line Cooling

01312_A_A © 2009 - IFP Training

– Temperature measurements with indicators or recorders (TI or TR):

– the material balance for the column

– the internal pressure profile and pressure control

– the concentration and temperature profiles

01312_A_A © 2009 - IFP Training

II - MATERIAL BALANCE FOR THE COLUMN

A=D+R Overall balance

Ai = Di + R i Partial balance for component i

Non distributed components a-e-f

01312_A_A © 2009 - IFP Training

- the light or volatile key, (LK), here component c

- the heavy key, (HK), here d

The separation therefore depends on:

– the separating power of the distillation process.

01312_A_A © 2009 - IFP Training

© 2009 - IFP Training

Duty (t/h) AROMATICS 70

6 Propane (6,68) Méthane

393,2 % C 5 = 0,29 n-Butane (8,59)

© 2009 - IFP Training

203,0 1532,1 % nC 4 = 0,28

III - OPERATING PRESSURE FOR A DISTILLATION COLUMN

01312_A_A © 2009 - IFP Training

2- TRAY OPERATION AND PRESSURE DROP

ΔP : pressure drop per tray

Vapour ACTIVE AREA

01312_A_A © 2009 - IFP Training

– weir height (30 to 70 mm determined by design) hb,

– height of liquid due to the vapor pressure drop hpV.

Normal tray operation Carryover and flooding Flooding

01312_A_A © 2009 - IFP Training

a - Acting on the condenser duty

In the cooling fluid flow rate method, the

01312_A_A © 2009 - IFP Training

When the heat transfer surface area method

Controlling the condensate discharge allows