Table of Contents

Introduction....................................................................................................... 2
Process Description........................................................................................... 3
Block Diagram................................................................................................... 4
Process Design Basis......................................................................................... 5
Overall Material Balance................................................................................... 6
Design of column, reboiler and condenser......................................................7
Equipment List................................................................................................. 15
PFD, Piping and Instrumentation Diagram and Plot plan..............................16
Line Sizing....................................................................................................... 17
Pump Hydraulic Calculations..........................................................................19

Introduction
The instructions given in the following pages are for the design of 100 MT/day Liquid N2O4
plant.

Process Description
Raw liquid N2O4 containing a small amount of Nitric acid is branched off from
the discharge of N2O4 pump P-1 and fed to N2O4 distillation column T-1
through a flow control valve.
The distillation column is provides with stripping and rectification sections
and has beds of intalox saddles.
The heat required for the vaporization of N2O4 is supplied by indirect steam
in the thermosyphon reboiler E-1. Saturated LP steam at 3 kg/cm2 g pressure
will be utilized for this purpose. The temperature at the bottom of the column
is maintained at approx. 25 degC.
Pure N2O4 vapors leaving the top of the column at approx 21 degC are
condensed and sub cooled to 0 degC in condenser E-2 using brine. A
controlled quantity of condensed N2O4 is fed back to the column as reflux for
proper rectification. The quantity of reflux required depends upon the purity
of product obtained.
The bottom product containing N2O4 and nitric acid is returned to tank D-2
by gravity.
Excess N2O4 from the condenser is drawn off as product and is led to
collecting tank D-3 from where it can be transferred to the main storage
tanks using transfer pumps. If there is no draw-off from D-3 to main storage,
the product overflows into D-1.

Block Diagram

Feed
TPD
95 % (w/w)
N2O4
Temperature 0
degC

Distillatio
n

Distillate
100 TPD
99.9 % (w/w)
N2O4
Temperature
0 degC

Bottoms
84 % (w/w)
N2O4
Temperature
25 degC

Process Design Basis

Plant Capacity
The plant has been designed to produce 100 MT/day of pure N2O4
Product Quality
Liquid N2O4

Concentration 99.9% (w/w)

Temperature 0 degC

Feedstock and Utilities

Raw N2O4

Temperature 0 degC
Quality 95% (w/w)

LP Steam

Pressure 3 Kg/cm2 g
Temperature Saturated

Brine

Pressure 4 Kg/cm2 g
Temperature -13 degC

Inst Air

Pressure More than 4 Kg/cm2 g

Temperature Ambient
Dew Point -40 degC

Overall Material Balance

Product Distillate flow rate = 100 TPD
Product concentration = 99.9% (w/w) N2O4
Bottom concentration = 84% (w/w) N2O4
Feed concentration = 95% (w/w) N2O4
Let feed, distillate and bottom mass flow is identified by F, D and W
respectively.
Also let feed, distillate and bottom mass fraction of component N2O4 is
identified by Xf, Xd and Xw respectively.
Therefore at steady state taking material continuity balance,
F=D+W
Xf.F = Xd.D + Xw.W
Therefore,
F = 100 + W
.95F = .999*100 + .84W
Solving above two linear equations in two unknowns,
F = 144.5455TPD = 6022.7273 kg/hr
W = 44.5455 TPD = 1856.0606 kg/hr

Design of column, reboiler and condenser

Taking material balance across the distillation column
Distillate product rate =
External reflux ratio =
Hence,
Reflux rate to column =

100 TPD
4
400 TPD

The reflux is cooled to 0 deg C and top temp is 21 deg

C.
Taking material balance across condenser,
Vapor in to condenser = Distillate product + Reflux
flow
Therefore,
Vapor to
condenser=

400+10
0=

500 TPD

Above vapor value is the vapor leaving the enriching section. But the vapor flow
through the
enriching section will be more than above value because cold reflux is
used.
Taking material and energy balance at top end of enriching section to find the
vapor flow in
enriching section,
Vapor in enriching section - Vapor flow out of enriching section = Vapor condensed
Also,
Heat of vaporisation at 21 degC X Vapor condensed = Sensible heat rise of reflux
(i.e 400 TPD)
from 0 to 21
degC
Heat of vaporisation of n2o4 and hno3 at 21 degC is 75.04828 and 148.4839
Kcal/Kg respectively
Taking weighted average,
Heat of vaporisation of vapor mixture at 21 degC is
equal to
Now heat capacity of distillate at 0 deg C is
equal to
Now heat capacity of distillate at 21 deg C is
equal to
Avg heat capacity is
equal to

75.12 Kcal/K
172 g

0.198
728 Kcal/Kg.degK
0.200
991 Kcal/Kg.degK
0.199
86 Kcal/Kg.degK

Putting above values in the equation for calculating condensed vapor

amount
75.12172 X Vapor condensed = 400000 X 0.19986 X
(21-0)
Therefore, Vapor condensed
=
=

22348
.01 Kg per day
22.34
801 TPD

Therfore liquid flow rate in enriching section is equal to

=
Since vapor was condensed from vapor in enriching
section
the vapor flow rate in enriching section is equal to =

422.3
48 TPD
522.3
48 TPD

Taking material balance at feed point,

From the observed value of q for feed it can be predicted that the increase in
liquid flow rate
in stripping section due to subcooled feed is negligible. Hence it can be neglected
safely.
Liquid flow in enriching
422.3
section =
48 TPD
Feed
144.5
flow =
455 TPD
Liquid flow in stripping
section =
Vapor flow in stripping section
is same as in enriching
section =
Therfore, bottom flow rate,
= 566.8935522.348 =

566.8
935 TPD
522.3
48 TPD

44.54
549 TPD

The maximum L/G ratio is obtained at bottom of column. Also maximum gas and
liquid flows
are at bottom of column
Vapor and Liquid densities at 25 degC and prevailing pressure are as
follows

Compnt
n2o4
hno3
Comp

Liquid
Vapor
Unit
89.6476 0.23242
2
2 lb per cuft
94.2580
4
0.1614 lb per cuft

n2o4

0.84

hno3

0.16

0.98549
8
0.01450
2

0.00937
0.00169
7
90.3547
4
52074.4
7

4.24012
0.08985
2
0.23094
8
47982.5
5

Den
mix
Flow

lb per
cuft
lb per
hr

90.12
379
1.002
563
1.001
28

1.086
669

For above value of function the corresponding value of ordinate from graph for a
pressure drop
of .05 inH2O per ft of packing is .003
For 25mm ceramic intalox saddle
packing, Cf =
J=
Liquid
viscosit
y

1.54E08

gc=

98
1.502
4.18E
+08

0.395
977 cP
3.141
593

Gas flow square

=

19453
1
441.0
567 lb/sqrft.hr

Gas flow=
Therfore column cross
108.7
section =
9 sqft
10.10
=
7 sqmtr

Plate dimensions

Therfo
re

Dia=

1.772
454 meter

pi X diameter =

5.56832
8 meter
18.2687
9 feet

Following plate dimensions are available at leading indian alluminium plate manfg
Hindalco
Al
Alloys

Temper

1050
1060
1070
1080 F and O
1100
1200
3003
3105
8011

Thickne
ss
mm
6-200

Lengt
h
mm
10007000

Width
mm
5001550

Design of Vertical Thermosyphon

Vapor flow in stripping
section =

522.3
48 TPD
47990 Lb per
=
.72 hr
A circulation ratio of 4:1 shall be used because Alluminium alloy MOC is used and
alluminium
nitrate salt will get deposited on tubes for smaller
ratios.
3/4 in OD tubes 16 BWG on a triangular pitch of 1 inch shall be
used.
Let initial guess of tube length as 6
feet.
Heat of vaporisation of n2o4 and hno3 at 25 degC is 75.04828 and 148.4839
Kcal/Kg respectively
Weigthed average Heat of vaporisation for wt fraction of n2o4 =
.84 is
Heat of
vaporisation =
84.0 Kcal/Kg
Therefore, Heat of Duty, Q = 84 X
522.348 =

18282 Kcal/h
18 r

The maxium allowable heat flux will be 12000

Btu/hr.sqft =
Therefore, Heat transfer area
=

56.12 sq.mtr
972 =

32571
.3 Kcal/hr.m2
603.9
558 sq.ft

Heat transfer area for 3/4 in OD tube per unit length is 0.1963 sq.ft per
ft of length
Therefore, No of 6ft tube
512.7
lengths =
829
Nearest tube count for 1-Pass, 3/4 in OD tube on 1 in triangular
pitch is,
Shell ID, 27 inch; Total tube count 559
Check for pressure drop,
Static pressure of

z3.rhoavg =
2.3L
. log vo
144
144(vo - vi)
vi

psi

reboiler

Vapor density =
Liquid density =

0.23094
8 lb per cuft
90.3547
4 lb per cuft

Substuting above,
Static pressure of reboiler leg
=

Specific volum
=
Specific volum
=

4.329
972
0.011
067

0.057
524 psi

Frictional resistance through reboiler :

Flow are :
Total tube flow area Tube flow area per tube X No of total
=
tubes
168.8 sq.inc
= 0.302 X 559 =
18 h
1.172
=
347 sq.ft
Mass velocity,G = Total mass flow rate/ Total tube flow
area
= 5 X 47990.73 / 20468 lb per hr per
1.1723 =
6.2 sq.ft

At 25 deg C,
viscos,
nu =
ID of
tube =
Nre=DG/
nu
friction
fac
Avg.sp.v
olm

delta P
=

0.03 lb/hr.ft
0.0517 ft
352742.
6
0.00011 sq.ft per sq.in
2.17052

0.00472
1 psi

Total resistance = 0.0575 +

0.0047 =

0.062
245 psi

Driving force, Liquid leg X Density of

liquid =

3.764
781 psi

Since Driving force is much more than Total resistance a circulation ratio of 4:1 is
assured.

At Nre
=
352742
Coulborn factor, jH
=
Thermal condu, k=
sp heat capacity,
Cp=
k(Cp.nu/k)^1/3 =

700
0.16268
5
0.21058
8
0.05509
1

hi = (jH.k/D)(Cp.nu/k)^1/3 =

Btu per hr per ft per

degF
Btu per lb per
degF

745.9
165

This exceeds the maximum. Use 300

300 X 0.62/0.75
hio = hi X ID/OD = = 248

Btu per hr per sq.ft per

degF

ho for condensing steam = 1500

Btu per hr per sq.ft per

degF

Clean overall coefficient Uc:

Uc =hio.ho/(hio + ho) =1500 X 248/
(1500+248) =

Btu per hr per sq.ft per

213 degF

Assuming steam chest pressure to be just above atmospheric so as to keep temp

driving force
below critical temp difference. Therefore steam temperature is 100 degC
Due to above steam control valve can be designed for enough pressure
drop.
LMTD =
75 degC
40.3609 Btu per hr per sq.ft per
UD =
7 degF
Dirt factor Rd:
Rd = Uc -Ud/Uc.Ud
=

0.02008 hr.sqft.degF/Bt
2 u

Design of Total Condenser with subcooling

3/4 inch OD, 16 BWG tubes on 1 inch triangular pitch shall be
used.
The condensation shall be in tube
side.
According to Nusselt's theory the transition from laminar to turbulent shall occur
for Re=1400
The length of tube at which this transition shall take place from top is
given by,

where,
lambda = heat of vaporisation, Btu/lb

nu = viscosity of condensing film, lb/hr.perft

rho = density of film, lb/cu.ft

k = thermal conductivity of film, Btu/hr.ft.F

g = acceleration due to gravity = 4.18E+8
ft/sq.hr
Tv = Condesing temperature, degF
tw = Temperature of wall, degF

specific heat capacity,Btu/lb.degF

Therefore,
4.70384
xc =
4 feet

=
=
=
=

135.0
869
1.000
964
90.02
211
0.083
496
4.18E
+08
69.8
8.6
0.200
991

6 feet tube length shall be

satisfactory.
Condensing load of condenser = 500 TPD =
Condensing heat load = 45930 X 135.0869 =

45930 lb/hr
62045
41 Btu/hr

Condesing film coefficient can be obtained from Colburn's semiempirical

condensation curve,
Re = 4G'/nu
where,
G' = Loading per tube perimeter,
lb/hr.ft
Inside perimeter for 3/4 inch OD, 16 BWG
0.162
tubes =
316 feet
Assume 27 inch Shell ID, 1-P. Total number of tubes =

559

G' =

506.202
5 lb/hr.ft

2022.
Re = 4 X 506.2025/1.001 =
86
This is the lowest value of Re on Colburns curve. So any change in loading from
above value will
only increase Re and shall increase condensing
coefficient.
Ordinate from Colburns curve for above Re is
0.15

Therefor, condensing
coefficient =

187.9
769 Btu/hr.sqft.F

Condesing area = Condensing heat duty/(Condensing coeff X

(Tv-tw)) =

539.3
291 sq.ft

Heat transfer area sqft per

0.162
linear ft =
3 sq.ft
Length of tubes required for to accommodate above heat load from above heat
transfer area is
5.94461
=
2 feet
Therefore length remaining for subcooling is 6 - 5.9446
=
Heat transfer area corresponding to this remaining
tube length =

Subcooling from 21 degC to 0 degC heating

duty =

According to McAdams heat transfer coeff for

subcooling is,

0.055
388 feet
5.025 sq.fee
098 t

19386
1.8 Btu/hr

Therefore,
Subcooling film coefficient =

LMTD =

21.8428
9 =

4739.
914 Btu/hr.sqft.F
71.31
721 degF

Therefore, area for

0.573
subcooling =
492 sq.ft
The availabe area for subcooling 5.02 sq.ft is much more than required value.
Hence the heat
exchanger is suitable for condensation and subcooling.

Equipment List
EQUIPMENT LIST FOR
PLANT SECTION
ITE
M

DESIGNATION

T-1

N2O4
PRODUCTION
TOWER

E-1

CONDENSER

E-2

REBOILER

NUM
BER
a b

MEDIU
M

TECHNICAL
DATA

1 -

N2O4,
HNO3

H = 5000
MM
D = 1780
MM

N2O4,
BRINE

N2O4,
HNO3
STEAM

D-1

N2O4 FEED
TANK

P-1
A,B

N2O4 FEED
PUMP

1 N2O4

P-2
A,B

REFLUX PUMP

1 N2O4

N2O4

MATERI
AL

DRIV
E

REM
ARKS

AL 99.5

A = 61.2
SQ.MTR
Q=
1.6E+6
KCAL/HR

SHELL :
AL 99.5

A = 61.2
SQ.MTR
Q=
1.8E+6
KCAL/HR

SHELL :
AL 99.8

AL 99.5

F = 5.1
CU.MTR/HR
H = 21
mLC

SS 304
L

E.MO
TOR

F = 14.7
CU.MTR/HR
H = 8 mLC

SS 304
L

E.MO
TOR

V = 210
CU.MTR
D = 4100
MM
L = 16000
MM

TUBE :
AL 99.5

TUBE :
AL 99.8

PFD, Piping and Instrumentation Diagram and Plot plan

Line Sizing
Line sizing:
The Feed pump suction:
From pump rated flow equal to 5.1 cu.mtr per hr
Selecting velocity as 0.6 m/s,
The diameter is equal to 54.88 mm.
Select DN 50 Sch 40 pipe.
The Feed pump discharge:
From pump rated flow equal to 5.1 cu.mtr per hr
Selecting velocity as 1.6 m/s,
The diameter is equal to 33.6 mm.
Select DN 40 Sch 40 pipe.
For vapor line from column to condenser:
Vapor flow from material balance = 500 TPD = 20833 kg per hr
At top temperature vapor density = 3.6 kg per cu.mtr
Therefore, volumetric flow rate = 5787 cu.mtr per hr
Selecting vapor velocity = 15 m/s
Diameter = 370 mm
Select DN 400 Sch 40 pipe.
For condenser outlet line as reflux pump suction:
Condensate mass flow = 20833 kg per hr
Condensate density = 1470 kg per cu.mtr
Therefore, volumetric flow rate = 14.7 cu.mtr per hr
Selecting velocity = 0.6 m/s
Diameter = 94 mm
Select DN 90 Sch 40 pipe.
For reflux pump discharge:
For volumetric flow rate = 14.7 cu.mtr per hr

Selecting velocity = 1.6 m/s

Diameter = 57 mm
Select DN 50 Sch 40 pipe.
For column to reboiler line:
Mass Flow = 108900 kg per hr
Volumetric flow = 75 cu.mtr per hr
Selecting velocity = 0.3 m/s
Diameter = 296 mm
Select DN 300 Sch 40 pipe
For reboiler to column vapor line:
For circulation ratio of 4:1 density of mixture does not change appreciably.
Hence for the same velocity select a DN 350 Sch 40 pipe.

Pump Hydraulic Calculations

Pump hydraulics:
Feed pumps:
Rated flow through pump = 5.1 cu.mtr per hr
The elevation of feed point from grade is 8.5 mtr. But for ease of maintenance
the feed control valve will be located on second floor at elevation of 11 mtr from
grade.
The pump head will be calculated for 11 mtr discharge elevation.
The available positive suction head shall be avoided for this calculation.
Calculating total discharge head,
Selected discharge velocity = 1.6 m/s
The fittings in discharge line can be estimated by following,
Selecting straight length of pipe as 20 meters,
Le/L = 1 + (0.347d^0.5 + 0.216) Fc
Where d = pipe NB inches.
Fc = Correction factor = 1.0
Selected discharge pipe is DN 32 i.e NB 1.1/4
Therefore,
Le/L = 1.61
Le = 32.2 meters
Hence, Total equivalent length = 52.2 meters
Adding 30 % of above value for pressure drop across feed control valve,
Therefore, Final total equivalent length = 1.3 X 60 = 67.9 mtr
Calculation of friction factor,
ID of pipe = 35.048 mm
Velocity = 1.6 m/s
Density = 1470 kg/cu.mtr
Viscosity = 0.4 cP = 0.0004 Pa.s
Nre = 206083

Roughness factor for pipe, episilon = 0.025

Darcy Friction factor,f = 0.0198
Pressure drop = f. (L/ID).(V2/2g) = 0.0198 X (68/0.03505) X (sqr1.6/2X9.8)
=5.1 mLC
=72278 Pa
=0.74 Kg per sq.cm
Therefore total discharge head = Static head + Discharge losses = 11 + 5.1 =
16.1 mLC
Calculating Head loss through suction line:
Distance between feed pump suction and tank outlet = 3.5 meters
Selected suction velocity = 0.6 m/s
The fittings in suction line can be estimated by following,
Selecting straight length of pipe as 3.5 meters,
Le/L = 1 + (0.347d^0.5 + 0.216) Fc
Where d = pipe NB inches.
Fc = Correction factor = 1.0
Selected suction pipe is DN 50 i.e NB 2
Therefore,
Le/L = 1.71
Le = 5.985 meters
Hence, Total equivalent length = 9.485 meters
Calculation of friction factor,
ID of pipe = 52.506 mm
Velocity = 0.6 m/s
Density = 1470 kg/cu.mtr
Viscosity = 0.4 cP = 0.0004 Pa.s
Nre = 115776
Roughness factor for pipe, episilon = 0.025
Darcy Friction factor,f = 0.0198

Pressure drop = f. (L/ID).(V2/2g) = 0.0198 X (9.485/0.0525) X (sqr0.6/2X9.8)

=0.066 mLC
Total Head = 16.1 + 0.066 = 16.2 mLC
Pump shutoff head can be estimated as 30% plus above value.
Therefore, Pump shutoff head = 16.2 X 1.3 = 21.06 meters.
Pump shutoff pressure = Pump Shutoff head X Density X g = 21.06 X 1470 X 9.8
= 303390.4 Pa
=3.09 Kg per sq.cm (abs)

Reflux pumps:
Condensate mass flow = 20833 kg per hr
Condensate density = 1470 kg per cu.mtr
Therefore, volumetric flow rate = 14.7 cu.mtr per hr
Selecting velocity = 1.6 m/s
Diameter = 94 mm
Select DN 50 Sch 40 pipe.
Rated flow through pump = 14.7 cu.mtr per hr
For ease of maintenance and operation reflux pumps shall be located on first
floor at elevation of 5 mtr from grade.
The elevation of reflux point from grade is 12 mtr.
The pump head will be calculated for 12-5 = 7 mtr discharge elevation.
The available positive suction head shall be avoided for this calculation.
Calculating total discharge head,
Selected discharge velocity = 1.6 m/s
The fittings in discharge line can be estimated by following,
Selecting straight length of pipe as 7 meters,
Le/L = 1 + (0.347d^0.5 + 0.216) Fc
Where d = pipe NB inches.
Fc = Correction factor = 1.0

Selected discharge pipe is DN 50 i.e NB 2

Therefore,
Le/L = 1.71
Le = 11.97 meters
Hence, Total equivalent length = 19 meters
Calculation of friction factor,
ID of pipe = 52.506 mm
Velocity = 1.6 m/s
Density = 1470 kg/cu.mtr
Viscosity = 0.4 cP = 0.0004 Pa.s
Nre = 308736
Roughness factor for pipe, episilon = 0.025
Darcy Friction factor,f = 0.018
Pressure drop = f. (L/ID).(V2/2g) = 0.018 X (19/0.0525) X (sqr1.6/2X9.8)
=0.851 mLC
Total Head = 7+0.851 = 8 mLC
Neglecting the losses in suction line and positive suction head,
Pump shutoff head can be estimated as 30% plus above value.
Therefore, Pump shutoff head = 8 X 1.3 = 10.4 meters.
Pump shutoff pressure = Pump Shutoff head X Density X g = 10.4 X 1470 X 9.8
= 149822.4 Pa
=1.53 Kg per sq.cm (abs)