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1

Abstract

Liquefaction of air and subsequent rectification of the liquid air is the basis of the Linde-
frankls processon which this project is based . Prof.Linde is credited today with the first man
producing liquid oxygen on a commercial scale. This thesis report is a design of an oxygen
plant of capacity 205 tonnes /day, along with oxygen this plant also produces nitrogen of very
high purity . In it a complete design of a distiallation column and a 1-2 shell and tube condenser
has been done.
The Linde Frankls process is the most important process for the commercial production of
oxygen in this process in which the air stream is divided in two , one is cooled by J-T effect and
the other by incoming pure nitrogen which is the most striking thing about this process and
which makes it more economical .
Results have been obtained with mechanical calculation and then verified by chemical
enggineering software chemsep ,kamlex and chem office. Fianlly a safety and preventions have
been delat with along with breif overview of plant layout and locations of the plant.




2

Contents
Chapter page no.
1.Introduction 1
2. Selection of process 8
3.Mass & Energy balance 19
4. Equipment Design 30
5. Conclusion and discussion 51

3





List of Tables
Table page no.
1. Analysis of air 20
2. Conditions and enthalpy of streams 24
3. Enthalpy chart 27
4. The equilibrium data for lower column 28
5. Excell sheet 37



4

List of figures
Fig. Page no.
1. T-S diagram for cla 10
2. Flowsheet of the linde frankls process 12
3. T-S for linde frankls process 13
4. Typical distillation column 31
5. Condenser flow pattern 43
6. LMTD calculation 44
7. Designed condenser 49
8. Schematic diagram 50



5

List of graphs
Graph page no.
1. Equilibrium data 34
2. McCabe Thiele rough 35
3. McCabe Thiele by chemsep 38
4. Relative volatility vs stage 39
5. Entropy Vs stage 41
6


Chapter 1.



Introduction









7

INTRODUCTION, PROPERTIES AND USES

Oxygen has been known to the scientists from as early as the 3
rd
and 4
th
centuries. The Chinese
were the first to detect its presence as an essential element in the atmosphere without which life
and combustion is not possible.
In 1770, Henry Cavendish, Joseph priestly and Karl withelm Scheele investigated the properties
of oxygen. Later on priestly carried out some experiments and produced it in small quantities.
It combines with hydrogen forming water covering around 70% of earth crust combine with
various metals and nonmetals to be present in around 99% of rocks. Overall oxygen constitutes
49.2%of the mass of the earth and 23.2%of the atmosphere is oxygen.
Oxygen can be produced in the laboratory by heating oxides, peroxides, permanganates and
bicarbonates in the presence of sulphuric acid.
One of the first industrial manufactures of oxygen was Brin process which was based on the
property possessed by the monoxide of barium of absorbing oxygen readily from the air at a
temperature of about 54
0
C forming dioxide, this dioxide at 870
0
C gives up the oxygen absorbed,
barium being restored to monoxide.
Another process is the electrolysis of water using caustic soda solution in distilled water as
electrolyte.

Now coming to the modern process, which is the liquefaction of air and subsequent rectification
of the liquid air. Which will be the main concern in this report; few pioneers who were
responsible in the gradual development are Noothmore, who was the first to produce chlorine in
its liquid form in 1806,


8


Faraday who succeeded in liquefying many gases by the application of pressure. But still gases
such as H
2
, O2, and N2

for many years resisted all attempts to liquefy them and were therefore
called permanent gases.
Investigations in 1863by Andrew revealed that gases could not be liquefied however great the
pressure applied, until the temperature of the gas is below a certain limit, this temperature is
called critical temperature. Further in this field two French scientists Pictat and Caillete in 1877
actually succeeded in liquefying first oxygen and then many other gases.
Pictat merely elaborated the Faraday tube experiment using high pressure and low temp gas
already liquefied as the refrigerant, while Caillete on the other hand obtained this refrigerating
effect by suddenly expanding a gas under high pressure
Rest was for Deval, Linde and Hampson in 1844 to adopt Cailletets method to a practical
continuous process and prof.Linde is credited today with the first man producing liquid oxygen
on a commercial scale.








9


PROPERTIES AND USES

OXYGEN IN SOLID STATE: It is a hard, pale blue, doubly refracting crystalline solid.
Melting point: -218.81
0
C
Density at -252.5
0
C: 1.4256 gm/cc
Specific heat at -256
0
C: 0.078 cal
Heat of fusion at -219
0
C : 313 cal/gm
OXYGEN IN LIQUID STATE : It is a pale steel blue, transparent and very mobile liquid

Boiling point : -182.02
0
C
Density at boiling point: 1.14gm/cc
Surface tension at B.P. : 13074 dynes/cm
It is a non conductor of electricity and strongly magnetic when compared to iron.
OXYGEN IN GASEOUS STATE: It is a colorless, odorless, tasteless, diatomic gas, a volume of
it slightly heavier than equal volume of air. One Litre of oxygen under standard condition weighs
1.42901gm and the corresponding weight of air is 1.2929gm. The oxygen is only slightly soluble
in water at ordinary temperature and pressures
The value of Ostwald coefficient=conc. in liquid phase/conc. in gas phase
=0.308 at 25
0
C and 1atm.
Physiochemical properties:
Atomic mass: 15.9994
10

Atomic number: 8
Isotopes: O
16
99.759%
O
17
0.037%
O
18
0.204%
Thermo physical properties:
Gas at 1 atm:
Density (0): 1.42908gm/lit
Density (21.11): 1.327gm/lit
Density at B.P: 4.467gm/lit
Density at triple point: 0.0108
Viscosity, at 25
0
: 206.39 mili poise

CHEMICAL PROPERTIES:
Action of oxygen with hydrogen: oxygen and hydrogen at an ambient temperature when
activated by a catalyst such as platinum metal, forms water.
2H
2
+O
2
= 2H
2
O
Action of oxygen on metals: all metals react with oxygen, although not with same rate or the
same energy.
Action of metals on non metals: oxygen reacts directly with all the non metals although direct
action often is not the most effective way of producing oxide. Even fluorine forms a compound
with oxygen, OF
2


11



USES
Iron and steel applications:
Around 98%pure oxygen is needed in steel industry for blast furnace to enrich the air from
21%normal oxygen to 26%.
It is required for cutting and welding and for scarfing billets, for this purpose oxygen should be
99.5% pure
Application in chemical industry:
In chemical industry, oxygen is used in the manufacturing of synthetic materials such as
acetylene, ethyline oxide, methanol, acrolein, hydrogen peroxide, titaniumdioxide etc.
Also find its wide application in waste water treatment.
Oxygen for cutting purposes:
oxygen cutting of ferrous metals into shapes for fabrication is practiced on a large scale, in this
technique the metal is heated first by means of a fuel oxygen torch to the point of combustion
&then a narrow, high velocity(1500ft/sec or more)stream of oxygen is introduced through the
center of the flame. It is used that oxygen should be of high purity of 99.55 or better.
Aerospace uses:
Aerospace activities have placed an expanding demand on oxygen production. Oxygen continues
to be the preferred oxidant for large scale& first stage firing because it is readily prepared at
nominal cost and unlike fluorine or the oxides of nitrogen, use does not make an area
uninhabitable or require extensive decontamination.


\
12

Oxygen in life support systems:
The development of high fly commercial aircraft, recent projects to explore both inner and outer
space require oxygen in the life support systems.
Moreover under the sea as well as well above the sea level in the mountains oxygen cylinders are
needed. In the medical applications, oxygen cylinders are employed almost routinely for patients
suffering respiratory function &represent the most frequent contact of the patient with medical
oxygen.
Use of oxygen in pediatrics incubator has been an important factor in increasing the survival rate
of premature infants.
Modern anesthesia routinely uses oxygen as a component of the gaseous mixture, herby
overcoming the diluting effects of gaseous mixture, herby overcoming the diluting effects of
gaseous anesthetics & ensuring an adequate supply for life support.










13

Chapter 2


Selection of
process





14

DIFFERENT PROCESSES AND SELECTION OF PROCESS

DIFFERENT MANUFACTURING PROCESS:
There are four different processes for the manufacture of oxygen from air,they are:
1. Low temp. rectification of liquid air
2. Electrolysis of water.
3. Cyclic chemical absorption& desorption from air by barium oxide at elevated temp. This
is called Brin process.
4. A process similar to Brin process but using cobalt compounds.
Out of these only low temp. Rectification process was found to be the most economical &
feasible.
This process mainly comprises of two steps. One is the liquefaction & then the separation of
liquid air into oxygen & nitrogen. Since the process mainly requires low temp., refrigeration is
necessary. Different cycles are in use to have required refrigerating effect.
For the separation also different types of columns are in use like simple, compund & double.
Taking into consideration the two stages various combinations were proposed.
1. Heylandt liquid oxygen process
2.Le rought process
3. Kellog low pressure process
4. Claude process
5. Linde frankl process
Out of the above processes the Claude process and lindey frankl process are really important
processes for the manufacture of oxygen.
Briefly giving an overview of these two processes.
15

CLAUDE PROCESS:
This process is characterized by the double expansion engine. After passing through the
preliminary heat exchanger, at 60 atm pressure, part of the air traverses the liquefier from top to
bottom & is admitted to the base of the dephlagmetar after expanded to 4 atm.The reset is
expanded like wise to 4 atm,in the first stage of the expansion engine, after which it is again
separated into two portions. One is added to the partially liquid air behind the valve, the other is
warmed by passing up the upper part of the liquefier,& is then expanded to 1 atm.
In the second stage of the engine, the expanded air there upon mixes with the cold nitrogen vapor
emerging from the top of the column & returns through the lower part of the liquefier & through
the preliminary heat exchanger. The oxygen in this air is wasted. The refrigerant between the
tubes of the dephlagmator is liquid oxygen from the column, part of which is withdrawn through
tube.



fig 1 t-s diagram for claud process.
16


LINDE-FRANKL PROCESS:
This is the most important process for the commercial production of oxygen in this process at
first air is filtered & compressed to 6.8 atm in turbo compressor. During the compression cooling
is done to maintain the temp to 35 -40
0
C.
After compression the air is divided into two streams. One is 65% stream & the other is 35%,
now the larger stream is then passed through after cooler and heat exchanger where it is cooled
to -150
0
C to -170
0
C by the incoming pure nitrogen & waste nitrogen streams produced from
rectification columns. The smaller stream is passed through reciprocating compressor to increase
the pressure to about 200atm.Here the air temp is maintained at 4-8
0
C by intermediate cooling
between stages using cold water obtained by ammonia refrigeration. Then the air goes through
high pressure heat exchanger where the temp of air is brought down to about-120 -140
0
C. Now
the air undergoes expansion to about 6.5 atm in the expansion engine .The temperature of air is
brought down to -170 to-174
0
Cby joule Thompson effect. Now the air will be in liquid state
&mixes with the larger stream & changes the whole air stream into saturated liquid state.
This saturation liquid is fed to Linde rectification column. This column may be single, double or
compound depending on requirement. the liquid product coming out will have a purity of about
99.4 -99.99%.This liquid is partially vaporized in condenser, to liquefy the nitrogen vapor &the
rest may be taken as liquid product or it may be obtained in gaseous state if it is used for cooling
of incoming air, the other products that obtained are pure nitrogen of purity above 98% & waste
nitrogen product of purity of about 92-96%.These cold streams are utilized for cooling air, this
process is most economical for tonnage oxygen plants &most widely used in the world.





17







Fig 2. Flow sheet of linde frankl process



18




Fig 3.T-S diagram for the process





19

PROCESS VARIABLES:

1. Initial temperature: The initial or the entrance temp for air is an independent variable.
Although it varies from 10 to 50
0
C depending on the weather conditions and the type of after
cooler, for most cases, it is assumed as 27-30
0
C.

2. Initial pressure: This is an important variable; it is independent in the case of liquid oxygen
process. The lowest allowable value of pressure is controlled by the saturation temp. Of air
or nitrogen, this must be higher than the boiling point of oxygen at column pressure. In a
double column, the air pressure must be such that the nitrogen will condense at the temp of
boiling point of oxygen in order to produce reflux. This will be in the 4-6.5atm range,
depending on the pressure in the lower pressure column, and on the necessary temperature
difference in the condenser boiler.

3. Temperature approaches: An analysis of the process shows that it is necessary to establish
the minimum temp approaches for heat exchangers. For the exchange of sensible heat, the
minimum approach has to be 3-5
0
C

4. Temperature level of refrigerants: vapor liquid refrigerants may be used at almost any
temp level down to liquid air temperature provided the right material is chosen. The
following is a list of common refrigerants with the temp to which they can cool air.

Refrigerant temperature (
0
K)

Sulphur dioxide 263
Methyl chloride 249
F_12 244
Ammonia 240
Propane 231
Ethane 184
Ethylene 169
20

Methane 111
Nitrogen 77

5. Intake temperature to expander: this variable has the flexibility of being at almost any
value between the room temp and one close to that of air liquefaction, without appreciable
effect on the efficiency of expander. It is so chosen that the exhaust is saturated vapor.

6. Purity of product gases: this is fixed at some value less than 100%,with due regard to
certain limitation that may set a definite upper limit with a single column, the product
nitrogen purity cannot exceed 93%.in case of producing liquid oxygen, the available
refrigeration may set a still lower limit.

7. Heat leak: this is one of the most difficult variables to be selected since it depends on
factors which cannot readily be evaluated in advance. For e.g. the size of the plant is of at
most importance. Although the leak on an hourly basis increases when expressed the basis
increases as plant size increases when expressed the basis of a unit of air treated or oxygen
produced, it decreases and in large plants, is almost negligible.

8. Energy requirement: once the various quantities, temp, pressure are established the work
done by the compressors and expanders, and hence the energy requirements can be easily
calculated.



9. Sizes of equipment units: The thermodynamic analysis plays an important role in this
variable, since it deals with the driving forces in the heat exchangers and in distillation
columns.

The type of column chosen also plays a big role in the operation of the unit. There are
3 types of columns that can be used for rectification namely simple, double and compound.
21

Simple consists of only an exhausting column and liquid feed to it consists only the reflux. It
has an adv of simplicity and economy of distribution and construction, but the disadvantage
is that it suits only moderate yield of oxygen since nitrogen leaving the column can never be
enriched beyond 93%.

The compound column has both exhausting and enriching sections, but it must be provided
with a source of refrigeration at a very low temp, ie below the B.P.of nitrogen at the
operating pressure of the column.

The double column has two rectification columns operated at two different pressures, so
chosen that the nitrogen at high pressure column condenses at a temperature above the
boiling point of oxygen of low pressure column. Usually the pressure in the high pressure
column is 6-7 atm and in the other is 1.5-2 atm. This has the adv of high yield without
auxiliary refrigeration, but it is expensive and complicated to manufacture. But on the
tonnage scale, double column is preferred of high yield and high purity.












22

THEORETICAL MINIMUM ENERGY REQUIREMENT

The computation of absolute minimum work required for air separation and oxygen
liquefaction with the case is possible. It known that this work is given as:
W=H-T
0
.S
In air separation is zero if one neglects the enthalpy of mixing. The valve of S may be shown
that the enthalpy change accompanying the mixing of pure oxygen and pure nitrogen to yield
one mole of a mixture of x mole fraction of O
2
is

S = RX lnX+R(1-X)ln(1-X)
A similar expr may be written for a mix of mole fraction Y
So the entropy of M1 moles of air relative to pure O
2
andN
2
is
0.21Rln0.21+0.79ln0.79
Accordingly if M1 moles of air to be separated into M2 moles of O
2
rich gas of composition
X
2
mole fraction O
2
and M3 moles of oxygen lean gas of X
3
mole fraction of O
2
,the overall
entropy change will be,
S = R [ M2 { (2X
2
lnX
2
)+(1-X
2
)ln(1-X
2
) } + M3{ (X
3
lnX
3
)+(1- X
3
)ln(1-X
3
) }]
-RM1 {0.21ln0.21+0.79ln0.79}
This expr when multiplied by ambient temp., usually taken as 303K yields the theoretical
minimum energy requirement.
Now the material balance equations are:

M1=M2+M3

0.21M1=X
3
M3+X
3
M3
Defining M2 and M3 for chosen values of M1,X
2
and X
2
.
23

SELECTION OF THE PROCESS

Prior to the selection of the process it should be emphasized that there are so many adjustable
variables involved, it is very difficult to put all on a comparable basis. Usually on the smallest
scale, the most important economic factors are capital and labor charges. Thermodynamic
efficiency and hence power charges for compression are of less consequence.
Charges for material such as compressor oil, chemicals for air purification are small in relation
to the other costs. The labor charges also decreases when the scale increases and in this cases the
capital costs and power costs dominate. When the plant produce a liquid product, as in this case
the power requirement to provide necessary refrigeration is considerably increased and
thermodynamic efficiency is of much importance.
The essential requirement on a general scale is a cheap and simple plant, easy to operate for
which a thermodynamic efficiency is not needed. But if the liquid is produced on a large scale,
the thermodynamic efficiency becomes important.
As the purpose of this project is to design large scale oxygen product plant the only process that
seems economical is the LINDE FRANKL PROCESS.
As the most important adv here is the high purity of oxygen (99.5) %, although the work of
liquefaction of air is about 3.5kwh/gallon which is relatively higher than other process. Also the
outgoing streams from the rectification column are used effectively in supplying the required
refrigeration for cooling the incoming air.
In view of all the above cited advantages the process For this project is linde-frankl.





24

Chapter 3


Mass & Energy
balance





25

MASS AND ENERGY BALANCE

CAPACITY of the unit is, 205 T/day of gaseous oxygen of 99.95 purity.
And 10 t/day of liquid oxygen of 99.97% purity.
So total oxygen production = 215 T/day
= (215*1000)/(24*32)
= 281.25 kg moles/hr

At standard temperature and pressure,
1kg.mole occupies 22.4m
3
Oxygen produced in volumetric units =281.25*22.4
=6300Nm
3
/hr



Standard analysis of air:
Component volume%
Nitrogen 78.03
Oxygen 20.99
Argon 0.94
Hydrogen 0.01
Helium 0.0003
Krypton 0.00011
Xenon 0.00009
Carbon dioxide 0.03-0.06
Moisture 0.02-0.05

Table 1.
26

Quantity of intake air:

Capacity of the unit = 6300m
3
/hr of oxygen
Volume % of oxygen in the air =21%
Quantity of air needed =6300/0.21
=30000m
3
/hr
Assuming about 15% less of air due to removal of moisture,CO
2
and from possible leaks.
The quantity needed = 30000+30000 *.15
=34500m
3
/hr
Atmospheric conditions :
Temperature =30
0
C,relative humidity =60%

Now the air passes through elements of the system


Enthalpy of air at 1 atm and 30
0
C=kcal/kgmol.
Enthalpy of air at 6.8 atm and38
0
C=3766.23 kcal/kgmol
Moles of air entering compressor=34500Nm
3
=1540.18 kgmol/hr
Enthalpy of air entering compressor=1540.1883701kcal/hr=5701515.3kcal/hr
Enthalpy of air leaving the compressor=1540.18*3766.23=5800672.1kcal/hr.
So change in enthalpy of air = 5800672.1-5701515.3
99156.8kcal/hr

Now the air is split into two streams one is 65% and the other is 35%. Larger stream passes
through refrigeration cycle and the smaller stream passes through compression cycle and then
expanded in expansion engine.




27

Mass & energy balance for the refrigeration cycle
65% stream
Amount of air passing = 1540.18*0.65 = 1001.117 kg moles /hr
First air passes through water cooler
Water cooler
Inlet 6.8 atm and 38
0
C
Outlet 6.5 atm and 8
0
C

Relative humidity = 60%
So partial pressure of water at 38
0
C=.6*49.692=29.82cm of Hg
Total pressure is 760*6.8 = 5168 mmHg
Now

P = (H
1
*P
t
)/(Mw/Ma+H
1
) from Perrys handbook eq 15.6

Where
P = partial pressure in mm Hg
P
t
= total pressure in mm Hg
Mw = molecular weight of water = 18
Ma = molecular weight of air =29
H
1
= molal absolute humidity in kg moles of water vapor / kg moles of dry air
Substituting the values in the formula,
We get H
1
= 3.6*10
-3

Let us assume air coming out from the cooler is saturated
28

So final humidity = 100%
Vapor pressure of water at 80
0
C =8.045 mm Hg.
Final partial pressure of water = 8.045 mm of Hg
Total pressure = 6.5 *760 =4940 mm of Hg
Using the same eq
We get H
2
= 9.68*10
-4
kg moles of water vapor /kg moles of dry air
Let the amount of dry air be M kg moles
Now M +.0036M=1001.117
So M=997.52
So amount of water contained =997.52(.0036-.000968)
=2.625kg moles /hr
Moles of air coming out of cooler
1001.117 - 2.625 =998.492 kg moles/hr
Coming to energy balance, from enthalpy chart of air

Enthalpy of entering air = 3766.23 kcal/kgmol
Enthalpy of outgoing air = 3573.09 kcal/kgmole
Enthalpy of entering air =1001.117*3766.23 = 37770436.8 kcal/hr
Enthalpy of leaving air = 998.492*3573.09=3567701.7 kcal/hr
Change in enthalpy of air = 202735.1 kcal/hr

29

Heat exchanger
Air entering = 99.2492 kg moles /hr
Volume % of CO
2
in air = 0.045%
Moles of CO2 present in air entering
= 998.492*0.045/100= 0.4493 kg moles/hr
Amount of dry air leaving heat exchanger = 997.52-0.4493 = 997.07kg moles /hr
This is cooled to -168
0
C by circulating pure nitrogen and waste nitrogen streams coming from
distillation column. Total
Amount of pure nitrogen is 361.61 kg moles /hr
It splits into 2 streams one passes through this heat exchanger and other through high pressure
heat exchanger in the compression cycle
Let the amount of pure nitrogen stream passing this exchanger is M kg.
Amount of waste nitrogen 892.69 kg moles /hr

Conditions and enthalpy of streams: from enthalpy chart.



Stream Flow rate
Kg moles/hr
temp
0
C Pressure (atm) Enthalpy(kcal/kg)
Dry air In-997.07 8 6.5 3573.09
30

Out -997.07 -168 6.5 2092.35
Pure N
2
In- M
Out M
-178
4
1.5
1.5
1500
2750
Waste N
2
In 892.69
Out 892.69
-172
6
1.5
1.5
1510
2800
CO
2
In- 0.4493
Out- nil
8
solidifies at -
56.6
Calculated below
Moisture In-.972
Out-nil
8
Solidifies at - 4
Calculated below.

table 2
Heat given up by dry air = 997.07(3573.09-2092.35)=1476401.4 kcal/hr
Heat given up by CO
2
:
CO
2
at first cools from 8 to -56.6
0
C and then solidifies
Specific heat Cp is 10.34 +0.0027T-195500/T in kcal/kg mol

k
T is absolute temp in k
Heat lost by CO
2
on cooling to -56.6
=

T2
M CpdT

T1

= 411.95 kcal/hr
31

Heat of sublimation of CO
2
= 1993.83 kcal/kg mole
Heat lost by CO
2
on freezing
=




0.4498*1993.83 kcal/hr = 896.83 kcal/hr
Total heat lost by CO
2
411.95 +896.83 = 1308.78 kcal/hr
Heat lost by water molecule by cooling to -4= .972 *18(8-(-4))= 209.952 kcal /hr
Heat lost by water molecule on freezing 0.972 *80*18 = 1399.6 kcal/hr
Latent heat of condensation = 80 kcal/hr
So total heat lost by water = 209.52+1399.6=1609.632 kcal /hr
Heat joined by water nitrogen stream 892.67 (2800-1500) = 1160497 kcal /hr
Heat gained by pure nitrogen = M(2750-1510) = 1240M

11160497+1240M = 1476401.4+1308.78+1609.632
Or 1204M=318822.81
M = 257.115 kg moles/hr
The amount of waste nitrogen passing through heat exchanger = 257 kg moles /hr

Amount of air passing
= 34500*.35=12075
1207/22.4=539.063 kg moles/hr
This air passes through compressor

Compressor
Before compression, air is at 6.5 atm and 38 0C
And after it is at 800 atm & 6 0C
Enthalpy of inlet air = 3766.23 kcal/kgmol
Enthalpy of outlet air = 3251.119 kcal/kgmol

So net enthalpy of entrance = 3766.23*539.063 kcal/hr = 2030235.2 kcal/hr
32

And for exit air 539.063*3251.119 kcal/hr
Assuming no condensation of water vapor
The net change in enthalpy of air =
27677.3 kcal/hr

CO
2
absorber: volume % ofCO
2
in air =.045$%

Moles of V present = .045*539.063/100=.2426 kg moles/hr
From the earlier calculations, molar humidity of air + 3.6*10
-3



If G is the amount of dry air in kg mole/hr then G+.0036G=539.063
So G=538.478 kg moles/hr
Moisture present 539.063-538.478 = 0.535kgmoles/hr
In the adsorber most of the moisture and CO
2
is removed


High pressure heat exchanger
No change in mass. Now heat balance, from enthalpy chart in Perrys handbook

Stream Flow rate
Kg
moles/hr
Temp.
0
C
Pressure
atm
Enthalpy
Kcal/kg
Pure
nitrogen
In- 104.495
Out-
104.495
-178
4
1.5
1.5
1500
2750
Oxygen In -267.86 -178.2
2
30
30
2161.6
3328.64
Air In
538.478
Out-
538.478
6
?
200
200
3251.119
?
Table 3.
33

Heat taken by pure nitrogen stream= 104.495(2750-1500)= 130618.75 kcal/hr
Heat taken up by oxygen = 267.86 (3328.64-2161.6) = 312603.33 kcal/hr
Heat lost by air = 538.478(3251.119-H)
Now H=2428.91 kcal/kg mol
Now the corresponding temp of air is -150
0
C
So the air entering the expansion engine is at 200 atm and -150
0
C

Here air is expanded to 6.5 atm the temp. Of air after compression is -174
0
C(liquid state)
Now both the air streams are mixed. And finally the temp. Is at -172
0
C and will be in
saturated liquid state and fed to lower distillation column.

The set up of oxygen plant consists of two linde column:
Upper column (1.5 atm)
Lower column (6.5atm)

The equilibrium data is as follows For lower column.


Temp.
0
C Liquid composition
X%
Vapor composition
Y%
-160.9 0 0
-163 2.5 6.5
-165 17 32.5
-167 27 48.5
-168 32.5 50
-170 45 68
34

-172 60 79.5
-174 79 90
-175 89 95
-176 100 100

Table 4.





















35

Chapter 4


Equipment
design








36

Equipment design

Distillation column

Fig.4.
Typical distillation column with reflux and reboiler

For mass balance, total air entering the column=
997.07+538.478=1535.55 kg moles/hr
From an overall balance of linde column kg moles of oxygen coming out = 6300/22.4
37

=281.25kgmoles/hr
So amount of waste nitrogen issuing out = 1535.55-(361.61+281.25)
=892.69 kg moles/hr

Let the liquid to vapor ratio at the top of both columns to be .58
So L1/V1=L2/V2=.58
Suffix 1 for upper column

Now V2=361.61
L2=.58*361.61=209.734 kg moles /hr

This L2 comes out of condenser in vapor state and fed at the top of upper column as
liquid after passing through expansion valve

.58V1+209.734=V1
.42V1=209.734 so V1=499.366 kg moles/hr
The amount L1 refluxed to the lower column after condensation occurs in the condenser
=.58*499.366
= 289.632 kg moles/hrLet F=amount of feed =1535.55kgmoles/hr
W=bottom product from lower which is refluxed back to the top column ( rich liq)
S=side stream from lower column, which is refluxed back to top column (impure liquid)
Xf=mole fraction of N
2
in feed = .79
Xw=mole fraction of N
2
in rich liquid =.65
Xs= mole fraction of N
2
in IPL=.96
X1= mole fraction of N
2
in top product = .9999

Now, from overall& component balance
F=W+S+L2 (1)
38

FX
F
=WX
w
+SXs + X1L2 (2)
From (1) 1535.55 = W + S +209.734

W +S = 1325.816
From (2) (1535.55 *.079) = (W*.65)+(S*.96)+(209.734*0.9999) (4)

1003.3714 = .65W + .96S
Multiplying (3) by .65

0.65W +0.65S = 0.65 * 1325.816 (5) subtracting 5 from 4
141.591= s (0.96-0.65)
S=456.746 kg moles /hr
From 3
W = 1325.816-456.746 = 869.07 kg moles/hr

Also L1/V1 = .58
L1/V1 = (456.746-289.633)/499.366
= .335
The stream S is taken out as liquid
V1 = V1=V1
L!/V1 = (1535.55+167.112)/499.366=3.4

Using the equilibrium composition data at 6.5 atm, the curve is drawn from XL1=.9999
the operating line is drawn with L1/V1=0.58
The side stream being taken out is impure liquid of 96% of N
2


For this point from which the operating line of slope L1/V1 = 0.335 is drawn will be
Xs1 = [(456.746*.96) + (209.734*0.9999)]/456.746+209.734
= 0.978
These 2 operating lines are seen to be intersecting at X =0.96
39

Now the operating line for exhausting section is drawn from Xw =0.65 with slope
L1/V1 =3.4
Hence from the graph no. of theoretical plates = 17.3





Graph 1.





0
10
20
30
40
50
60
70
80
90
100
0 20 40 60 80 100
equilibrium data
40



Graph 2.




Plate efficiency

Where is the average molal viscosity of the feed in cp
41

Of liquid O
2
= 0.19 Cp
Of liquid N
2
=0.24 Cp
Avg molal of feed = .79*.24 +.21*.19
= .2295 Cp
= .6127
So actual no. of plates = 17.3/.6127= 27.249 =28
So no. of plates =28
From graph, feed enters the 15
th
plate.
Actual plate at which feed enters = 15/.6127 = 23.952 = 24
Feed enter 24
th
plate
From graph, side stream is taken out from 5
th
plate
Actual plate from which side stream is taken out is 5/0.6127=8.16 = 9
th
plate
Height of column :
No. of plates =28
Plate spacing = 12
Spacing at top & bottom = 12each
Spacing for feed = 12
Total height =( 28+2)*12 =360 = 9.146



42

Computer aided design of column
The software CHEMSEP from chem. Office was used, data were fed and the following excel
sheet obtained.
Stream Feed1 Top Bottom

Stage 14 1 28
Pressure (N/m2) 650000 200000 650000
Vapour fraction (-) 1 1 0
Temperature (K) 105 83.686 104.821
Enthalpy (J/kmol) 5624000 6248000 11000000
Entropy (J/kmol/K) 41261.1 42611.3 92166.4

Mole flows (kmol/s)
Oxygen 120 0.390691 119.609
Nitrogen 379 300.729 78.2712

Total molar flow 499 301.12 197.88

Mole fractions (-)
Oxygen 0.240481 0.001297 0.604452
Nitrogen 0.759519 0.998703 0.395548

Mass flows (kg/s)
Oxygen 3839.88 12.5017 3827.38
Nitrogen 10617.3 8424.62 2192.69

Total mass flow 14457.2 8437.13 6020.06

Mass fractions (-)
Oxygen 0.265604 0.001482 0.63577
Nitrogen 0.734396 0.998518 0.36423

Vapour:
Mole weight (kg/kmol) 28.9723 28.0192
Density (kg/m3) 21.5723 8.0542
Viscosity (N/m2.s) 7.7E-06 5.67E-06
Heat capacity (J/kmol/K) 29204.5 29254.8
Thermal cond. (J/s/m/K) 0.010864 0.008368

43

Liquid:
Mole weight (kg/kmol) 30.4227
Density (kg/m3) 889.88
Viscosity (N/m2.s) 0.0001
Heat capacity (J/kmol/K) 60360.7
Thermal cond. (J/s/m/K) 0.112383

Table 6.
With the help of software the mcabe thiele diagram was obtained .



Graph 3. With chem. sep

44






Chem. Sep data sheet


45



Graph 4. The above graph gives the variation of relative volatility with stage no.






Following the similar pattern design of upper column can be done in the same fashion.

46



Graph 5.This is entropy vs stage graph.as obtained by the chemsep,from chemoffice








47

CONDENSER DESI GN

Basic Theory

The fundamental equations for heat transfer across a surface are given by:

Where w is tube side flow and W is shell side flow and CPt is specific heat fr tube side and CPs
is for shell side

In design, a correction factor is applied to the LMTD to allow for the departure from true
countercurrent flow
to determine the true temperature difference.
Tm = Ft Tm
The correction factor is a function of the fluid temperatures and the number of tube and shell
passes and is correlated as a function of two dimensionless temperature ratios


The overall heat transfer coefficient U is the sum of several individual resistances as follows





48

Continuing with our problem .Nitrogen vapors enter counter currently through the tubes of the
condenser, where it meets the liquid oxygen coming out on the bottom product of the top
column. for this purpose, a 1-2 shell and tube condenser is chosen. It is a vertical type condenser.

fig 5.diagram indicating the flow pattern


Enthalpy of N
2
vapor at 96.5K is 238.35 J/gm=1595.16 cal/kgmol
=1595.16 Kcal/kgmol.
Enthalpy of N
2
vapor at 94.8 K is1592.05 cal/kgmol
Enthalpy of N
2
liquid at 94.8K is 443.52 cal/kg mol
So total enthalpy change of stream= (499.367*1595.16) (209.734*1592.02+289.633*443.52)
= 1399009.42KJ/hr
49

LMTD calculations:
fig.6
Tha is inlet temp of nitrogen vapor = -176.5
0
C
Thb is outlet temp of nitrogen = -178.2
0
C
Tca is inlet oxygen liquid =-179.5
0
C
Tcb is outlet oxygen =-178.2
0
C
T
l
= 1.491
Taking overall heat transfer coefficient as 100 Btu/hrft
2
F
0
567W/m
2

0
C
now Q = UAT
l

From this A comes around 460 m
2
Let N is the no. of tubes so total heat transfer area =N*DL
Where D is tube OD
And L is the length
50

We are choosing 1 inch OD. and 14 BWG cu tubes of 8 inch length and calculating the no. of
tubes obtained is 2360
Also taking a triangular pitch of 1.25 inch that ,nearest no of tubes found from TEMA
regulations is 2362 and shell dia as 1.67 meters
Now the corrected area becomes 460.5m
2

So using this value of heat transfer area the U becomes 560.6W/m
2

0
C
Inside and outside coefficient calculations:
a. Nitrogen in tube side
Flow area for the given tube is 3.52cm
2

Gas mass velocity = 499.367*28/(3.52*2362/10000*2)=33634.52kg/m
2
hr
Density of nitrogen =802.6kg/m3
So velocity = .01155 m/sec
So Nre = 822
Condensate loading per linear foot is G = W/DN = 88.955 kg /m hr
From graph in kern we get the value of hi = 240 btu/hr ft
2

0
F
Also ho = hi*id/od= 22.16 btu/hr ft
2 0
F

Oxygen on shell side
Density = 1140 kg/m3
Thermal conductivity =k= 0.07 btu/ft.hr.
0
F
Here flow area = As = ID*C*B/144pt
C is clearance taken as 0.25 inch B = baffle spacing = 1 inch i.d. =66 inch Pt =1.25 inch so
As = 1.1 ft
2
=11.84m
2

51

Gas mass velocity Gs = W/As = 1535.55*32/11.84=4150.135kg/m
2
hr
From this NRE can be calculated by DeGs/
We get it as 72824
Now from the graph of jH Vs Nre
jH =175
now ho = jHk/De*(c/k)^-1/3
solving ho= 223.61 btu/hr ft
2
F
=1267.8w/m
2 0
C

Clean overall coefficient
Uc=hio*ho/(hio+ho)=598.865 w/m
2 0
C
Dirt factor :
Rd = Uc-Ud/(Uc*Ud)= 0.0000952m
2 0
C/w

Pressure drop:
Shell side
No. of crosses = N+1 =8 so no. of baffles =8-1 = 7
For Nre 72824
Friction factor =0001.4 (graph)
Sp gravity of oxygen = .00624
Ds= inside diameter in ft and n is the no. of tube passes
52

So Ps=fGs
2
Ds(N+1)/(5.22*10^10De*S)
So Ps =1.522psi

For tube side:
Pt= fGt
2
Ln/(5.22*10^10*DS) ,psi
= 0.155*10^-3 psi
Return losses: Pr = 4nV
2
/2Sg = 2.2 *10 ^-4 psi
So PT = Pt+Pr = 3.75*10 ^-4

Design summary: no. of tubes =2362
Shell ID = 66 inch
Clean overall H.T.C. = Uc =598.865 w/m
2 0
C
Design overall = 560.6W/m
2

0
C
Dirt factor Rd=) 0.0000952m
2 0
C/w
Pressure drop for tube side = 0.000375 psi
Pressure drop for shell side = 1.522 psi





53



Computer aided design of condenser Used KAMLEX heat
exchanger software to design and test my results obtained from my design

54

Results and diagram.

Fig 7.Condenser with geometry







55

Schematic diagram

Fig 8.


Results from kamlex.:
No of tubes = 2362
Overall heat transfer coefficient:
Heat exchanged = 563.2 W/m
2

0
C
Heat exchanged =1406504.1KJ/hr
Pressure drop for shell side: 11574.35 P
Pressure drop for tube side: 30.2Pascal
56

Chapter 5

Conclusion
and discussion






57

CONCLUSION AND DISCUSSION
On the basis of above calculations, I propose an oxygen plant with a capacity of 205 T/day with
the above design specifications. This plant can be actually called as an oxygen cum nitrogen
plant as it is producing pure nitrogen along side the oxygen.
Apart from equipment design there are certain other factors which have to kept in mind before
designing and finally establishing a plant., like location analysis and a plant layout .
Plant lay out and location
But before making such a choice, he has to go through the detailed locational analysis
considering various factors, which influence his decision. It is a long-term strategic decision,
which cannot be changed once taken. An optimum location can reduce the cost of production and
distribution to a great extent. Thus great care and appropriate planning is required to select the
most appropriate location.

The efficiency of production depends on how well the various machines;
production facilities and amenities are located in a plant. An ideal plant layout
should provide the optimum relationship among the output, floor area and
manufacturing process. An efficient plant layout is one that aims at achieving various objectives
like efficient utilization of available floor space, minimizes cost, allows flexibility of operation,
provides for employees convenience, improves productivity etc. The entrepreneurs must possess
the expertise to lay down a proper layout for new or
existing plants. It differs from one plant to another. But basic principles to be followed are more
or less same.
Plant layout is applicable to all types of industries or plants. At the end, the layout
should be conducive to health and safety of employees. It should ensure free and
efficient flow of men and materials. Future expansion and diversification may
also be considered while planning factory layout
Safety precaution
All personnel being employed for work in connection with oxygen/rich air should be cautioned
concerning the hazards involved and precautions to be observed. Oil grease or similar substances
58

must not be allowed to come into contact with compressed oxygen or liquid oxygen. Contact of
this substance with oxygen may result in an explosion. Personnel working in an area of possible
oxygen concentration, such as near an oxygen vent or a liquid oxygen spillage, or in a trench
where oxygen seepage and concentration might occur, must ensure that their clothing is free
from contaminations of oxygen before lighting a cigarette or approaching a naked flames. It is
essential that the clothes be dries for at least 15 minutes before approaching a flame after any
such contamination.

The following precautions must be strictly observed at all times:

1. Thoroughly wash all oxygen fittings, valves and parts with clean Tricolor Ethylene / carbon
tetra chloride (CTC) before installation. Never use petrol, kerosene or other hydrocarbon
solvents for this purpose. All tubing, lines valves etc. to be used in oxygen service, must be of an
approved type and must be thoroughly degreased and blown out with clean oil-free compressed
air or Nitrogen before being placed in service.

2. Do not permit the release of Acetylene or other flammable gases in the vicinity of the plant air
intake. A concentration of Acetylene exceeding 5 parts per million in liquid oxygen may explode
with extreme violence. Strict supervision is essential to minimize the possibility of
contamination.

3. The plant and the plant vicinity must be kept clean and free from abstractions at all times. Any
oil leak within the plant surrounding must be rectified without delay. Oil spillage must be
cleaned up immediately using rag and carbon Tetra Chloride.

4. Do not lubricate oxygen valves, regulators, gauges or fitting with oil or any other substance.

5. Ensure that insulation removed from the Air Separator jacket is not contaminated with oil or
other inflammable materials. Personnel carrying out maintenance on the Air Separation Plant
equipment must wear clean overalls and their hands and tools must be free of oil. This ensures
that the insulation and equipment within the jacket is not contaminated with oil. Should
59

contamination take place the affected materials must be discarded and replaced by clean new
material?

6. Do not fasten electric conduits to the plant or its pipelines.

7. Do not use oxygen as a substitute for compressed air, spark present in an atmosphere of
oxygen will immediately burst into flame.

8. Do not fill any container or pipe line with oxygen unless it has been thoroughly degreased
with clean CTC or TCE.

9. When discharging liquid oxygen or rich liquid from drains, valves or pipe lines, open valves
slowly to avoid the possibility of being splashed. In particular ensure that liquid does not run into
shoes or gloves. Contact with liquid oxygen rich liquid will cause frostbite evidenced by
whiteness and numbness of the skin. The affected parts must be batched at once in cold (not box)
water and seek medical attention immediately.

10. Do not breathe cold oxygen vapor. The temperature of the vapor rising from liquid oxygen is
approximately - 181 Deg C. A deep breath of vapor at this temperature can result in frost-bitten
lungs with resultant serious illness and permanent disability or death.











60

References


Basic Theoretical Physics ,Springer new York ,part 4 ,pages 313-325
Cryogenic Engineering, Springer new York ,part 1,pages 3-27 and 146-160
US Patent 4072023 - Air-rectification process and apparatus
Chemical and Petroleum Engineering journal, Air separation in plants with an external
source of refrigeration ,,volume 4 ,pages 825-829
American Chemical society journal , some aspects of gas separation at low temperatures
by W. H. Granville

air liquefaction: distillation
encyclopedia of separation science, 2007, pages 1895-1910,science direct
R. agrawal, D.M. herron

Cryogenic Process Engineering
Encyclopedia of Physical Science and Technology, 2004, Pages 13-36
Klaus D. Timmerhaus