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Abstract
Liquefaction of air and subsequent rectification of the liquid air is the basis of the Linde-
frankl’s procession which this project is based .Prof Linde is credited today with the first man
producing liquid nitrogen on a commercial scale. This thesis report is a design of a nitrogen
plant of capacity 432 tones /day, along with nitrogen this plant also produces oxygen of very
high purity. In it a complete design of a distillation column , 1-2 shell and tube condenser and
a adsorption column has been done.
The Linde Frankl’s process is the most important process for the commercial production of
nitrogen 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 .
Finally a safety and preventions have been dealt with along with brief overview of plant
layout and locations of the plant.
1
Nitrogen
2
Nitrogen
SR PAGE
NO. TITLE NO.
INTRODUCTION 1
1 1.1 PROPERTIES 1
1.2 INDUSTRIAL APPLICATIONS 2
2 LITERATURE SURVEY 5
PROCESS SELECTION AND PROCESS DESCRIPTION 7
3.1 AIR PROPERTIES 7
3.2 AIR SEPARATION TECHNOLOGIES 7
3 3.3 PROCESS SELECTION- CRYOGENICS AIR SEPARATION 9
3.4 PROCESS DESCRIPTION 12
3.5 PROCESS VARIABLES 15
3.6 THERMODYNAMICS OF THE PROCESS 17
MASS AND ENERGY BALANCE 19
4.1 OVERALL MASS BALANCE 20
4 4.2 AIR COMPRESSOR 21
3
Nitrogen
LIST OF FIGURES:
SR PAGE
NO. TITLE NO.
3.1 AIR COMPOSITION 7
3.2 AIR SEPRETION SCHEME 8
3.3 SELECTION DIAGRAM FOR N2 PRODUCTION 9
3.4 T-S DIAGRAM FOR CLAUDE PROCESS 12
3.5 T-S DIAGRAM FOR LINDEFRANKL PROCESS 13
3.6 PROCESS FLOW SHEET 14
5.1 AIR DISTILLATION DOUBLE COLUMN 30
5.2 LOWER DISTILLATION COLUMN 31
5.3 EQUILIBRIUM DIAGRAM 34
4
Nitrogen
LIST OF TABLES:
PAGE
TABLE NO. TITLE NO.
1 PURCHASED EQUIPMENT COST 89
2 RAW MATERIAL COST 94
3 TOTAL ANNUAL FIXED CHARGES 98
4 TOTAL MANUFACTURING COST 98
5 TOTAL GENERAL EXPENSES 100
B PROPERTY ESTIMATION 102
CHAPTER 1 INTRODUCTION
.1 INTRODUCTION [2]:
5
Nitrogen
described sodium salts that did not contain nitrate, and is a cognate of natron.
Nitrogen is a common element in the universe, estimated at about seventh in total abundance
in our galaxy and the Solar System. It is synthesised by fusion of carbon and
hydrogen in supernovas. Due to the volatility of elemental nitrogen and its common
compounds with hydrogen and oxygen, nitrogen is far less common on the rocky planets of
the inner Solar System, and it is a relatively rare element on Earth as a whole. However, as
on Earth, nitrogen and its compounds occur commonly as gases in the atmospheres of planets
and moons that have atmospheres.
Nitrogen is a chemical element with symbol N and atomic number 7. Elemental nitrogen is a
colorless, odorless, tasteless, and mostly inert diatomic gas at standard conditions,
constituting 78.09% by volume of Earth's atmosphere.
1.2 PROPERTIES
1. NITROGEN IN SOLID STATE: It is a hard, pale blue, doubly refracting crystalline
solid.
Molecular weight : 28.0134 g/mol
Melting point : -210 °C
Latent heat of fusion (1,013 bar, at triple point) : 25.73 kJ/kg
2. NITROGEN IN LIQUID STATE: It is a pale steel blue, transparent and very mobile
liquid
Liquid density (1.013 bar at boiling point) : 808.607 kg/m3
Liquid/gas equivalent (1.013 bar and 15 °C ) : 691 vol/vol
Boiling point (1.013 bar) : -195.9 °C
Latent heat of vaporization (1.013 bar at boiling point) : 198.38 kJ/kg
1. NITROGEN IN GASEOUS STATE: It is a colorless, odorless, tasteless, diatomic
gas, a volume of it slightly heavier than equal volume of air.
Gas density (1.013 bar at boiling point) : 4.614 kg/m3
Gas density (1.013 bar and 15 °C ) : 1.185 kg/m3
Compressibility Factor (Z) (1.013 bar and 15 °C ) : 0.9997
Specific gravity (air = 1) (1.013 bar and 21 °C ) : 0.967
Specific volume (1.013 bar and 21 °C ) : 0.862 m3/kg
6
Nitrogen
Heat capacity at constant pressure (Cp) (1.013 bar and 25 °C ) : 0.029 kJ/(mol.K)
Heat capacity at constant volume (Cv) (1.013 bar and 25 °C) : 0.02 kJ/(mol.K)
Ratio of specific heats (Gamma:Cp/Cv) (1.013 bar and 25 °C (77 °F)) : 1.403846
Viscosity (1.013 bar and 0 °C ) : 0.0001657 Poise
Thermal conductivity (1.013 bar and 0 °C ) : 24 mW/(m.K)
Critical point Triple Point:
Critical temperature : -147 °C Temperature : -210.1°C
Critical pressure : 33.999 bar Pressure : 0.125 bar
Critical density : 314.03 kg/m3
[10]
1.3 INDUSTRIAL APPLICATIONS : Following are the applications of Nitrogen in
various industries.
1. Chemicals Industries:
Nitrogen can be used for blanketing
Storage for protecting raw materials or finished products in liquid form from the
formation of peroxides and/or gum, and from contamination by oxygenated
components.
Regeneration of purification beds (alumina and molecular sieve).
Preparation of catalysts and transportation of polymer powders
Medium for the exhaust of emitted heat in fluid bed reactors
Temperature Control in reactors.
2. Pharmaceuticals Industries:
Nitrogen is used for inerting, cryo-grinding, lyophilisation, drying, liquid phase
transfer of products or synthesis intermediates, cryo-condensation of waste gases and
low temperature storage.
3. Food and Beverage
Liquid nitrogen: N2 is the most used cryogenic fluid, to chill, freeze or store food
products.
Gaseous nitrogen: N2 is very commonly used in contact with foodstuffs to avoid
oxidation or micro-organism growth by inerting of liquids. Modified Atmosphere
Packaging (MAP) preserves and protects foods (pure nitrogen or mixed with CO2).
7
Nitrogen
9. Electronics
Nitrogen is used as carrier gas for overall protection against impurities and oxidation
in semiconductor and soldering processes. In its cold and liquid form, N 2 is used as a
cooling medium in the environmental testing of electronic devices.
10. Automotive & transportation
Gas Assisted Injection Molding requires pressures between 10 bar (145 psi) and 200
bar (2900 psi) and a nitrogen content of between 98.0 % and 99.9 %.Tires filling with
nitrogen increases their lifetime and therefore decrease the recycling or treatment of
this waste.
Other industries
Pneumatic transportation of powdered flammable materials (charcoal).
●●●
8
Nitrogen
Nitrogen is a chemical element with symbol N and atomic number 7. Elemental nitrogen is a
colorless, odorless, tasteless, and mostly inert diatomic gas at standard conditions,
constituting 78.09% by volume of Earth's atmosphere. Nitrogen is formally considered to have
been discovered by Scottish physician Daniel Rutherford in 1772,
Nitrogen gas is an industrial gas produced by the fractional distillation of liquid air, or by
mechanical means using gaseous air (i.e., pressurized reverse osmosis membrane or Pressure
swing adsorption). Commercial nitrogen is often a byproduct of air-processing for industrial
concentration of oxygen for steelmaking and other purposes. When supplied compressed in
cylinders it is often called OFN (oxygen-free nitrogen).[5]
9
Nitrogen
Small amounts of impurities NO and HNO 3 are also formed in this reaction. The impurities
can be removed by passing the gas through aqueous sulfuric acid containing potassium
dichromate.[6] Very pure nitrogen can be prepared by the thermal decomposition of barium
azide or sodium azide.[7]
2 NaN3 → 2 Na + 3 N2
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, 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 nitrogen 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 Cailletet’s method to a practical
continuous process and prof.Linde is credited today with the first man producing liquid
nitrogen on a commercial scale.
The components presented in air (Nitrogen, Oxygen, Argon etc.) are very often
applied components in chemical technology. Large quantities of high‐purity air products are
used in several industries, including the steel, chemical, semiconductor, aeronautical,
refining, food processing, and medical industries. Distillation of air is currently the most
commonly used technique for production of pure oxygen, nitrogen and Argon on an
industrial scale. Much has been written concerning the design of air separation processes and
certainly the world wide patent activity for flow sheet and equipment innovation continues.
10
Nitrogen
Advanced control has been practiced in the air separation business for decades.
●●●
11
Nitrogen
12
Nitrogen
Air can be separated into its components by means of distillation in special units. So‐called
air fractionating plants employ a thermal process known as cryogenic rectification to separate
the individual components from one another in order to produce high‐purity nitrogen, oxygen
and argon in liquid and gaseous form. Different type of air separation technologies was
developed:
Cryogenic Air separation
Membrane Air separation
Separation by adsorption
Other
Different technologies are applicable for different requirement on amount and purity of the
products. Figure (2.3) shows the Oxygen production process selection grid. A similar graph
describing the ranges for which the different nitrogen processes are applicable can be seen in
Fig. (2.3)
13
Nitrogen
industrial gas production plants make use of cryogenic technology to produce liquid
products. There are different variations arising from differences in user requirements in the
cryogenic air separation cycles to produce industrial gas products. The cycle of processing
depends on:
How many products are required (whether simply oxygen or nitrogen, both oxygen
and nitrogen, or nitrogen, oxygen and argon).
Required purities of the products.
Gaseous product delivery pressures.
Lastly whether the products need to be stored in Liquid form.
In the cryogenic gas processing, various equipment is used like the distillation columns, heat
exchangers, cold interconnecting piping etc. which operate at very low temperatures and
hence must be well insulated. These items are located inside sealed "cold boxes". Cold boxes
are tall structures with either round or rectangular cross section.
14
Nitrogen
3. Third Step: The third step in the cryogenic air separation is the transfer of additional
heat against product and waste gas so as to bring the air feed to cryogenic
temperature. The cooling is usually done in brazed aluminum heat exchangers. They
let the heat exchange between the incoming air feed and cold product and waste gas
streams leave the air separation process. The very cold temperatures required for
distillation of cryogenic Products are formed by a refrigeration process comprising
expansion of one or more elevated pressure process streams.
4. Fourth Step: This step involves the use of distillation columns to separate the air into
desired products. For example, the distillation system for oxygen has both "high" and
"low" pressure columns. Nitrogen plants can have one or two column. While oxygen
leaves from the bottom of the distillation column, nitrogen leaves from the top. Argon
has a boiling point similar to that of oxygen and it stays with oxygen. If however high
purity oxygen is needed, it is necessary that at an intermediate point argon must be
removed from the distillation system. Impure oxygen produced in the higher pressure
distillation column is further purified in the lower pressure column.
This process mainly comprises of two steps. One is the liquefaction & then the separation of
liquid air into nitrogen & 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, compound &
double. Taking into consideration the two stages various combinations were proposed.
1. Heylandt liquid nitrogen process
2. Le rought process
3. Kellogg low pressure process
4. Claude process
5. Linde frankl process
Out of the above processes the Claude process and Linde frankl process are really important
processes for the manufacture of nitrogen.
Briefly giving an overview of these two processes.
CLAUDE PROCESS:
This process is characterized by the double expansion engine. After passing through the
preliminary heat exchanger, at 60 atm pressures, part of the air traverses the liquefier from
15
Nitrogen
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 nitrogen in this air is wasted. The
refrigerant between the tubes of the dephlagmator is liquid nitrogen from the column, part of
which is withdrawn through tube.
columns. The smaller stream is passed through reciprocating compressor CC 2 to increase the
pressure to about 200atm.Here the air temp is maintained at 4-8 0C by intermediate cooling
between stages using cold water obtained by ammonia refrigeration. Then the air goes
through high pressure heat exchanger HE 2 where the temp of air is brought down to about-
120 -1400C. Now the air undergoes expansion to about 6.5 atm in the expansion engine EE1
The temperature of air is brought down to -170 to-1740Cby 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 DD1. 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 nitrogen
plants &most widely used in the world.
17
Nitrogen
The stream from the lower column is passed to the column DD2.The streams from the
column is passed through heat exchanger 4 HE4 for the heat recovery. These cold streams are
used for refrigeration of inlet feed air.
18
Nitrogen
19
Nitrogen
Ethane 184
Ethylene 169
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 nitrogen, 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 nitrogen 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. 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 nitrogen 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
20
Nitrogen
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
nitrogen 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.
21
Nitrogen
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 nitrogen product plant the only process
that seems economical is the LINDE FRANKL PROCESS.
As the most important adv here is the high purity of nitrogen (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.
●●●
22
Nitrogen
MASS BALANCE:
Before any significant design procedure is carried out, the most important part to be
considered is the material balance. Material balances are the basis of process design. A
material balance taken over complete process will determine the quantities of raw materials
required and products produced. Balances over individual process set the process stream
flows and compositions. Material balance involves calculation of the product formed at the
end of the process and also the loss of the product occurred inherently in the process. Various
assumptions have to be made while carrying material balance, which are clearly stated where
used .The general conservation equation for any process can be written as:
Material out = material in + generation – consumption + accumulation
For a steady state process the accumulation term is zero. If a chemical reaction is taking
place a particular chemical species may be formed or consumed. But if there is no chemical
reaction, the steady state balance reduces to,
Material out = Material in
A balance equation can be written for each separately identifiable species present, elements,
and compounds and for total material.
ENERGY BALANCE:
The first law of the thermodynamics says that energy is conserved in the process.Energy is
converted from one form to another. It can neither be generated nor destroyed.
Energy out = Energy in
23
Nitrogen
24
Nitrogen
=34500m3/hr
= 34500*0.44509
=1535.5605 Kmol/hr
= 1535.5605 – 281.25
= 1254.6126 Kmol/hr
Total Capacity of gaseous nitrogen of 99.95%
= (1255.6126 * 14*24) /1000
= 421.8853 t / day
Total Capacity of nitrogen = 421.8883 + 10
= 431.8853 t /day
EQUIPMENT WISE MASS AND ENERGY BALANCE:
Atmospheric conditions :
Temperature =300C, relative humidity =60%
Now the air passes through elements of the system
4.2 COMPRESSOR CC 1:
AIR INLET OUTLET UNIT
TEMP 30 38 C
PRESSURE 1 6.8 ATM
ENTHALPY 3701.84 3766.23 Kcal/kmol
TOTAL ENTHALPY 5684399.3 5783274 kcal/hr
25
Nitrogen
26
Nitrogen
P = partial pressure in mm Hg
Pt = total pressure in mm Hg
Mw = molecular weight of water = 18
Ma = molecular weight of air =29
H1 = molal absolute humidity in kg moles of water vapor / kg moles of dry air
Substituting the values in the formula, we get
H1 = 3.6*10-3 kmol of water vapor / kmol of dry air
Let us assume air coming out from the cooler is saturated
So final humidity = 100%
Vapor pressure of water at 80 0C =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 equation, we get
H2 = 1*10-4 kmol of water vapor /kmol of dry air
Let the amount of dry air be M kg moles
Now M +.0036M = 998.11
M = (998.1/1.0036)
M =994.539 kmol of dry air
So amount of water contained =994.534(.0036-.000968)
=2.575 kmol /hr
Moles of air coming out of cooler
= 998.114 - 2.575
= 995.539 kmol / hr
Hence water at the inlet
= H1 * M
= 0.0036 * 994.539
=3.581972kmol/hr
Water at Outlet in air
= 0.0001 * 994.534
= 1.00693 kmol / hr
27
Nitrogen
ENERGY BALANCE:
AIR INLET OUTLET UNIT
TEMP 38 8 c
PRESSURE 6.8 6.5 atm
ENTHALPY 3766.23 3573.09 Kcal/kmol
995.5392
MOLES OF AIR 998.114325 9 kmol/hr
3557151.
TOTAL ENTHALPY 3759128.11 5 kcal/hr
28
Nitrogen
Calculations:
Heat given up by dry air = 994.534 (3573.09-2092.35)
=1472646 kcal/hr
Heat given up by CO2 :
CO2 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/kmol K
T is absolute temp in k
Sensible Heat lost by CO2 on cooling to -56.6 from 8 C
T1=298 k = inlet temperature
T2=216.4 k= outlet temperature
29
Nitrogen
T1
∫ M CpdT
T2
= 27794.73 Kcal/hr
Heat of sublimation of CO2 = 1993.83 kcal/kg mole
Heat lost by CO2 on freezing = 0.4498*1993.83 kcal/hr
= 896.83 kcal / hr
Total heat lost by CO2 = 27794.73 +896.83
= 28691.56 kcal/hr
WATER:
Heat lost by water molecule by
Cooling to -4 = 1.006 *18(8-(-4))
= 217.4972 kcal /hr
Heat lost by water molecule on freezing
=1.006 *80*18
= 1449.985kcal/hr
Latent heat of condensation = 80 kcal/hr
So total heat lost by water = 217.4972 +1449.985
=1667.483kcal /hr
Heat gained by water nitrogen stream
=892.67 (2800-1500)
= 1151750.7 kcal /hr
Heat gained by pure nitrogen
= M (2750-1510)
= 1240M
1151750.7+1240M = 1476264.4+28691.56+1667.483
1204M = 318822.81
M = 281.0036 kg moles/hr
The amount of pure nitrogen passing through heat exchanger = 281.0036 kmol/hr
Amount of pure nitrogen routed to compression cycle = 361.61 – 281.0036
30
Nitrogen
=80.606 kmol / hr
31
Nitrogen
=0.2426 kmol/hr
Water Balance:
From the earlier calculations, molar humidity of air H1 = 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 = 0.535kmol/hr
4.4.2 HIGH PRESSURE HEAT EXCHANGER HE 2:
No change in mass. Now heat balance, from enthalpy chart in Perry’s
handbook
32
Nitrogen
= 312603.33kcal/hr
Heat lost by air in High press HE = 538.478(3251.119-H)
Heat lost by air = Heat gained by N2 + Heat gained by O2
Hence, 538.478(3251.119-H) = 100757.8827 +312603.33
H = 2481.9979 Kcal / hr
Now the corresponding temp of air is -1500 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.
33
Nitrogen
●●●
34
Nitrogen
Distillation column combined from bottom column (2), condenser and reboiler (3) and upper
column (4). Bottom column work under 5.5‐ 6.5 at pressure and its allocation for preliminary
distillation of air in to nitrogen and mixed of oxygen and air that has 60 – 65% nitrogen and
35 – 40 % oxygen. In upper column that works at 1.3 – 1.4 at for finally distillation of mixed
oxygen and air in to nitrogen and oxygen . The produced Nitrogen, Oxygen and Argon purity
is: Mol fraction of oxygen 98.7%, mol fraction of nitrogen 99.0%, mol fraction of
Argon99.5%.
5.1.1 PROCESS DESIGN OF A DISTILLATION COLUMN:
V1 L2 (REFLUX TO THE UPPER
COLUMN)
SIDE STREAM S
FEED (AIR) F
35
Nitrogen
Let the liquid to vapor ratio at the top of both columns to be 0 .58
So L1’/V1’=L2’/V2’=.58
Suffix 1 for LOWER column
Now V2’=361.61 kmol / hr
L2’= 0.58 * 361.61
=209.734 kmol / 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.
Hence overall balance at the top of the lower column gives,
0.58V1’+209.734 = V1’
0.42V1’ = 209.734
V1’ = 499.366 kmol / hr
The amount L1’ refluxed to the lower column after condensation occurs in the
condenser = 0.58 * 499.366
L1’ = 289.632 kg moles/hr
F = amount of feed =1535.55 kmol/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 N2 in feed = .79
36
Nitrogen
38
Nitrogen
Plate efficiency
39
Nitrogen
COLUMN DIAMETER:
FLV top = (L/V)*(v/L) ^0.5 = 0.58 * (7.564/721.565)^0.5
= 0.0593835
FLV bot = (L/V)*(v/L) ^0.5 = 3.4 * (6.693/805.6)^0.5
= 0.3099
Take tray spacing as 0.5 m
From Figure 11.27(Coulson & Richardson's Chemical Engineering - Volume VI)
Base K1 = 0.070
Top K1 = 0.065
Base Uf = 0.059 *((805.6-6.693)/805.6)) ^0.5
= 0.07082 m/s
Top Uf = 0.065 * ((721.565 – 7.564) / (721.565)) ^0.5
= 0.064658 m/s
Design for 80 per cent flooding at maximum flow rate
Base Uf = 0.80*0.07082
= 0.05612 m/s
Top Uf = 0.8*0.064658
= 0.051726 m/s
Vapor volumetric flow-rate is constant through out the column.
Top = (499.366 * 14) / (3600*14*7.564)
=0.25674 m3/s
40
Nitrogen
Area required
Top area = 0.2567/0.051726
Area (A) = 4.96338 m2
As first trial take down comer area as 12 per cent of total.
Down comer area =0.12 * 4.96338
= 0.59560 m2
Coss sectional area = 4.96338 – 0.59560
= 4.3677 m2
Column diameter = ((4.366 * 4)/3.14)) ^ 0.5
Dc = 2.358 m
Weir length (from Figure 11.31, Coulson & Richardson's Chemical Engineering - Volume
VI)
lw = 0.76 x Dc = 0.76*2.358
= 1.816 m
Take weir height 50 mm
Hole diameter 5 mm
Plate thickness 5 mm
CHECK WEEPING TOP
Max liq. Rate = 289.6323 * 14/3600 = 1.1263 kg/s
Min liq. Rate at 70% turndown = 0.70 * 1.126 = 0.78844 kg/s
Max how = 750 *(1.1263 / (721.56 * 1.816)) ^ (2/3)
= 6.8115 mm liquid
Min how = 750*(0.7884/ (721.56 * 1.816))^(2/3)= 5.372 mm liq
43
Nitrogen
Back-up in downcomer,
hb = (hw + how)+ ht + hdc = (50+5.133)+72.893+0.167 = 129.79 mm
= 0.130 m
44
Nitrogen
= 0.153 m
0.153 < (1/2)*(plat spacing + weir height) so tray spacing is acceptable.
Check residence time
tr = (Ad * hb *L )/ Lwd = (0.05 * 0.153 * 805.6)/6.6206
= 3.5sec > 3 sec satisfactory
CHECK ENTRAINMENT:
Uv = Vol flowrate / net area =0.2564 / 3.7112 = 0.05206 m/s
Percent flooding = (0.05206 /0.64658 )*100 = 79.89%
FLV= 0.060 from fig. 11.29 (Coulson & Richardson's Chemical Engineering - Volume VI)
=0.070 well below 0.1.
As the per cent flooding is well below the design figure of 85, the column diameter could be
reduced, but this would increase the pressure drop.
TRIAL LAYOUT:
Use cartridge-type construction. Allow 50 mm unperforated strip round plate edge; 50 mm
wide calming zones.
PERFORATED AREA:
From Figure 11.32 (Coulson & Richardson's Chemical Engineering - Volume VI)
at lw/Dc = 0.76
c = 99°
45
Nitrogen
47
Nitrogen
= (100*10-3*575*2.386)*X/(8.2*10-3*2.376)
= 7.04*103 X N /m2
48
Nitrogen
Vw =44.7m/s
pw = 1197 N /m2( from table)
fwx = 1.4* pw *X2 /π Do ( ts – c)
= 27.46*103*X2
To determine the value of X
ft max = 118 *106 N/m2
ftmax = fwx + fap – fdx
118 * 106 (0.85) = (27.46*103X2 +49.837*106) – (266776.19 X +743065.18)
X = 48.3139 m >>9.04 m
49
Nitrogen
Am2 = Wm2 / fb
Am1= 4006*103/58.7*106
= 0.0682 m2
Am2 = 0.0899 m2
Number of bolts = mean diameter /bo x 2.5
=244 bolts
To determine the size of bolts, the larger of above two areas should be considered
Diameter of bolts = [(Am2 /Number of bolts) x (4/π)]1/2
= [(0.0899/244)*(4/π)]1/2 = 2.166 cm
FLANGE THICKNESS
Thickness of flange tf= [G√(p/K f) ] + c
Where,
K=1/[ 0.3 + ( 1.5 Wm hG)/H x G]
Hydrostatic end force = H = (π /4) G2 P
=(π/4)*(3.05)2*6.8*105
50
Nitrogen
=4.8*106 N
hG is radial distance from gasket load reaction to bolt circle,
hG = ( B – G )/ 2
= 3.11-3.05/2 = 0.03m
B = outside diameter of gasket + 2 x diameter of bolt +12mm =
3.08 +2*0.90*10-2 +12*10-3
= 3.11 m
Wm = 90*105 N
K= 1/(0.3+(1.5*90*105*0.03/4.8*106*3.05))
K= 3.05
Hence the thickness of flange = 60 mm
NOZZLE THICKNESS
Material Cu
Considering diameter of nozzle = Dn =0.5 m
51
Nitrogen
52
Nitrogen
H=9.142 m
plw = k P1 h1 Do
= 10598.
Bending moment due to wind at the base of the vessel is determined by
Mw = Plw*H/2
=48446.595 N- m
fwb = 4 x Mw / πDo tsk
=4*48446.595 /π*2.366*tsk
=26084.2804/tsk
53
Nitrogen
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.
ΔTm = Ft ΔTm
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
54
Nitrogen
The overall heat transfer coefficient U is the sum of several individual resistances as follows
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.
55
Nitrogen
Figure5.5 Condenser
56
Nitrogen
fig.6
Tha is inlet temp of nitrogen vapor = -176.50 C
Thb is outlet temp of nitrogen = -178.20 C
Tca is inlet oxygen liquid =-179.50 C
Tcb is outlet oxygen vapour =-178.20 C
∆Tl = 1.491
Taking overall heat transfer coefficient as 100 Btu/hrft 2F0=567W/m2 0
C
Now Q = UA∆Tl
From this A comes around 460 m2
Let N is the no. of tubes so total heat transfer area =N*π*D* L
Where D is tube OD
And L is the length
We are choosing 1 inch OD. and 14 BWG cu tubes of 20 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 460.5m2
So using this value of heat transfer area the U becomes 560.6W/m2 0C
Inside and outside coefficient calculations:
Nitrogen in tube side
Flow area for the given tube is 3.52cm2
57
Nitrogen
58
Nitrogen
59
Nitrogen
60
Nitrogen
RK = 6% Rc
W =1/4*(3+ (RC/RK) 1/2) = 1.77
th = 0.1575*1676 * 1.77/2*95
=2.4590 mm
Use thickness same as for shell , i.e. 10mm including corrosion allowance.
TIE RODS AND SPACERS
Tie Rods and Spacers shall be provided to retain all cross baffles and tube support heater
accurately.
Diameter of rod=15mm
No. of the rod =6mm
Following is from bhattacharya
FLANGES
Design Pressure =0.1575MN/m2
Flange material =IS:2004 ------1962
class2 Bolting Steel = 5% Cr Mo Steel
Gasket material = Asbestos composition
Shell diameter =1676mm
Shell thickness =10mm
Outside diameter = 1686mm
Allowable stress of flange material =100MN/m2
Allowable stress for bolting material =138 MN/m2
dO / di =(y-Pm)/( y-pm)
where
m =gasket factor
y = min design seating stress MN/m2assuming gasket thickness of 1.6mm
y =25.5
m= 2.75…………… from IS 2825-1969
do/di = [(25.5-0.1575*2.75)/(25.5-0.1575(2.75 +1)]1/2
do/di =1.002
Let dI of the gasket equal to 1696mm , 10mm greater than Shell dia
61
Nitrogen
Therefore
do =1.002*di
=1.002*1696
=1699.4mm
Minimum gasket width =do –di /2 = (1699.4-1696)*10-3/2
=0.0034m =3.4mm
Taking Gasket width = 0.012m
Diameter of location of gasket load reaction is
G = di +N
= 1.696 +0.010
=1.706 m
Estimation of bolt loads
Load due to design pressure
H= ∏*G2*P/4
=∏ (1.706)2*0.1575/4
=0.359 MN
Load to keep joint tight under operation
HP=∏*G*(2*b)*m*p
= ∏*(1.707)2*2*5*10-3*2.75*0.1575
=0.0396 MN
62
Nitrogen
Therefore
Controlling load =0.6829MN
Minimum bolting area =Am = Wg/Sg
= 0.6829/138
=4.94*10-3 m2
Sg =138 from bhattacharya pg no.10
Calculation for optimum boltsize Let
us choose Bolt as M 18X12 Min no.
Of bolts = 44
Also
R=0.027 We have
G1= B + 2(g1+R) G1
= 1.686 + 2[g1 +R]
g1 = go/0.707 =1.415go for weld leg
G1 = 1.686 +2 (1.415*10*10-3 +0.027)
G1 = 1.7683
Using 75 mm bolt spacing C1 = 44*0.075/∏
=1.05m
From the above calculation the minimum bolt circle is 1.424 m when M18 Bolt 44
bolts of 18 mm diameter on 1.424 m bolt circle are specified.
63
Nitrogen
64
Nitrogen
where
k= A/B =1.46/1.087 =1.34
Assuming Cf = 1
Y = 6 from graph
t2 = 0.108*1*6/1.087*100
t = 0.0792 m
Actual bolt spacing
BS = ∏*C/n = ∏*1.42/44 = 0.101
Bolt correction factor
Cf = (BS/2*d + t)1/2
Cf = [(0.101)/ (2*0.018 +0.101)]1/2
Cf = (0.737)1/2 = 0.858
Actual Bolt thickness = (C) 1/2 *t
= 0.93* 0.0792
= 0.0796 = 73.66 mm = 75mm
Tube Sheet Thickness
tts = f*G*(0.25*P/f)1/2
tts = 1*1.107* (0.25*0.11/95)1/2 = 0.0188m
tts = 18.83 +3 = 22 mm (Includes corrosion allowance )
65
Nitrogen
=
H = 290.205 mm
Weight of vessel & contents, W = 12000 kg.
Distance of saddle center line from shell end,
A = 0.5 x R = 419 mm
Longitudianl bending moments:
= 20619.42 Kg
66
Nitrogen
M1 = 4054.16 kg m
M2 = 7154.13 kg m
Stresses in shell at the saddle
1. At the topmost fibre of the cross section.
f2 = 18.38 kg/cm2
Stresses are well within the permissible values.
Stresses in the shell at mid – span: The stress at the span is ,
F3 = 32.44 kg /cm2
fp = 285.30 Kg / cm2
Total stress = 285.30 + 32.44
= 317.745 kg/cm2
Stresses are well within the permissible values.
67
Nitrogen
5.3ADSORPTION COLUMN:
Adsorption is the adhesion of atoms, ions, or molecules from a gas, liquid, or dissolved solid
to a surface.[1] This process creates a film of the adsorbate on the surface of the adsorbent.
This process differs from absorption, in which a fluid (the absorbate) permeates or
is dissolved by a liquid or solid (the absorbent).[2] Note that adsorption is a surface-based
process while absorption involves the whole volume of the material. The term sorption
encompasses both processes, while desorption is the reverse of adsorption. It is a surface
phenomenon.
Design of a column for adsorption starts with laboratory testing to establish the breakthrough
curve. At time intervals, the effluent from a column is sampled. Time zero is when the
solution is applied to the column.At first, the adsorbent (usually activated carbon) is fresh
with all its adsorption sites. Essentially none of the material to be removed escapes from the
column. As time passes, some of the adsorption sites are used up, and concentration in the
effluent rises.The shape of the graph may vary considerably for different situations. Usually
there is a long time before the effluent concentration rises sharply and then levels off. If all
the sites were occupied, we would expect the inlet concentration and the outlet
concentrations to become the same.
68
Nitrogen
Note the lines in blue. The breakthrough concentration is determined by the process
specifications. This is the allowable concentration. If a pollutant is being removed, the
breakthrough concentration might be the government regulation for what your plant can
discharge. For a commercial product where the column is removing color, the break through
concentration is determined by your specification for product quality. The point is that
breakthrough concentration is not some fundamental number but depends on how you decide
to operate your process.The exhaustion concentration also depends on process
considerations. If there are not enough workers on the night shift, the column may have to be
removed in time for regeneration by the day shift so that it can ready in time the next day to
become the t rail column. Note that the column could still adsorb some more material.
However, you get little benefit by running for a longer time. You pay for labor, for
electricity, for plant costs, etc. When the benefits are not worth the costs, the column is
considered exhausted.
CO2 Removal
H20
Air
69
Nitrogen
70
Nitrogen
1
0.666666
Ye 0.0024 0.0023 10000 9.304 1.000 7 0.33333 0.096
Table 1: Equilibrium data
The table shows the equilibrium data. Data is used in designing of the adsorption column.
Equilibrium relationship is obtained from Treybal.
Y=0.0025X
Assuming unit cross sectional area of the tower.
Hence, diameter of the column
D = (1*4/3.14) ^ 0.5
D = 1.12m2
Adsorbent used is silica gel.
At breakthrough point the fractional ability of the adsorbent to adsorb is
f=
72
Nitrogen
Substituting D we get,
Height of bed Z = 2.1465158 m3 adsorbent/m2 of cross section
Bed density = 690 kg / m3 from Perry
The mass of the adsorbent = 2.1456 * 690
=1330.84 kg / m2
M =1330.84 kg
At 90% of equilibrium with air the gel contains = 0.90 * M *X
= 0.90 * 1330.84 * 0.152
=192.173 kg H2O/m2 cross section
The air introduces with water = 0.0036 * 4.329
= 0.015585 kg H2O/m2 s
Break point occurs at =192.173/0.015585
= 12330.638 sec
Break point =3.425 hrs
Break point occurs after 3.425 hrs after introducing air in an adsorber.
Total height = Height of bed + Disengaging space
H = 2.146 + 2*(0.5)
H = 3.146 m
THICKNESS OF SHELL
Thickness of shell =
ts = [p D / 2f J – p] + c
Where,
Inner Diameter of vessel = Di = 1.12 m
Working Pressure = 6.58 *105 N/m2
Design Pressure = p = 1.05 * 6.58 x105 N/ m2
= 6.9 x 105
Permissible Stress = 118 *106 N/m2
J= Joint Efficiency = 0.85
Corrosion allowance =2mm
Hence, ts =5.640mm
Support Design:
73
Nitrogen
Bracket:
(a)Base plate: Suitable base plate size, a = 140 mm
74
Nitrogen
B = 150 mm
Average pressure on the plate,
Pav = P/(aB)
Pav=(3463)/(14x15) = 16.5 Kg/cm2
Maximum stress in a rectangular plate subjected to a pressure Pav and fixed at the edges
is given by
f = 0.7 Pav *
= 1290/T2
F= 1575 /Kg cm 2
T1 = 8.7 mm
Use a 9 mm thick plate
(b) Web plate.
Bending moment of each plate =
For f = 1575, T2 = 7 mm
Column support for bracket:
It is proposed to use a channel section as column.
The size chosen is ISMC 150.
75
Nitrogen
Size – 150 x 75
Area of cross section – 20 .88 cm2
Modulus of section – 19.4 cm3
Radius of gyration , r– 2.21 cm
Weight – 16.4 Kg/m
Height from foundation, l=1.8m
Equivalent length for fixed ends le=1/2
= 0.9 m
Slenderness ratio=
For the load acting accentric on a short column, the maximum combined bending and
direct stress is given by,
w = Load on column
A – Area of cross section
E – Eccentricity
Z – Modulus of section of cross – section
N – Number of columns
76
Nitrogen
Process control is such an important topic in the design of increasingly complex chemical
77
Nitrogen
plants. Instruments which can monitor the important process variables during plant operation
must be specified. These instruments must be capable of measuring the variables and should
have an acceptable accuracy and repeatability of measurement, usually the latter attribute is
more important than the former on chemical plant measurements. The instruments may be
used for manual measurements or included in automatic control loops. Automatic alarms
may also be required to indicate deviations outside acceptable limits. If possible, direct
measurement of the process variable should be made, however it is often easier to measure a
dependent variable, e.g. temperature measured as an indication of composition for distillation
column top product.
The specification of a control scheme and the associated instrumentation for a chemical plant
should satisfy several main objectives. First, the plant should operate at all times in a safe
manner. Dangerous situations should be detected as early as possible and appropriate action
initiated, also the process variables should be maintained within safe operating limits.
Second, the plant should operate at the lowest cost of production. Finally, the production rate
and the product quality must be maintained within specified operating limits.
The P & ID is used to prepare the preliminary instrumentation and control scheme. Control
loops are identified for level, flow, pressure and temperature controls to ensure steady plant
operation. The first steps in the design of a good control system are to define which variables
need to be measured and which need to be controlled. To specify pressure, temperature, flow
and level controllers on all units at different locations, and to assume that the measurements
will provide the basis for adequate control is unrealistic.It is necessary to specify:
(a) The variables that need to be measured;
(b) The location of these measurements;
(c) The variables that need to be controlled;
(d) How the desired control can be achieved.
The process and instrumentation (P&I) diagram provides a graphical representation of the
control configuration for the process. The P&I diagrams illustrate the measurement devices
that provide inputs to the control strategy, the actuators that will implement the results of the
control calculations, and the function blocks that provide the control
logic.
78
Nitrogen
79
Nitrogen
variables through controllers and other mathematical functions with widely differing degrees
of effectiveness. Columns also differ from each other, so that no single rule of configuring
control loops can be applied successfully to all.
Here in distillation at cryogenics , temperature and pressure are the most important
parameters. The minute disturbance in the temperature and pressure may change the purity of
products.The temperature controller (TC) in the loop are used to control the temperatures of
the top and bottom column for steady state operation of the column.The manipulated variable
to control the temperature of both upper and lower column is the flowrate of liquid oxygen to
the condenser and flowrate of liquid nitrogen to lower column from the condenser. The flow
rate controllers will give signal to the valves (main controlling element).The valve opening
will be adjusted to contol the flow and thereby controlling the temperature. Pressure is
controlled by manipulating the heat-transfer surface in the condenser through flooding. If the
condenser should become overloaded, pressure will rise above set point, but this has no
significant effect on the other control loops.The PC is placed in the vapor line of nitrogen to
ensure high pressure in the lower column.
Hence contol system of each equipment of process is necessary and important part of the
designing.A good Process control system of the process will give most economic and stable
performance of the plant .
●●●
80
Nitrogen
7.1 SAFETY:
In recent years there has been an increased emphasis on process safety. Process safety differs
from the traditional approach to accident prevention in a number of ways
• There is more concern with accidents that arise out of the technology.
• There is more emphasis on foreseeing hazards and taking action before accidents occur.
There is more emphasis on a systematic rather than a trial-and error approach, particularly
on systematic methods of identifying hazards and of estimating the probability that they will
occur, and their consequences.
• There is concern with accidents that cause damage to plants and loss of profit but do not
injure anyone, as well as those that do cause injury.
• Traditional practices and standards are looked at more critically
Process safety can be applied in any industry, but the term and the approach have been
particularly widely used in the process industries, where it usually means the same as loss
prevention.
Two studies are suggested: one at the conceptual or business analysis stage when the process
is being chosen, and another at the flowsheet stage. For the latter, the usual hazard and
operability (HAZOP) study questions may be suitable but with one difference. Having
specified the detailed design , the Hazard and Operability Study (HAZOP) can now be
performed. This study is used to determine the process control requirements and also to gain
an appreciation of the difficulties that may occur during operation of plant. The HAZOP
study comprises a detailed examination of each of the streams flowing into and out of the
various equipments. All significant aspects of deviation for each of these streams are then
considered under ‘Key Word’ headings. The HAZOP approach used here follows that
suggested by the Institute for the Prevention of Accidents in their HAZOP publication. The
HAZOP study was instrumental in determining the need for an adequate alarm system on
each of the specified controllers.
81
Nitrogen
cold. Nitrogen makes up the major portion of the atmosphere (78% by volume). Nitrogen is
inert and will not support combustion; however, it is not life supporting. When nitrogen is
converted toliquid form it becomes a cryogenic liquid. Cryogenic liquids are liquefied gases
that have a normal boiling point below -150oC (-238oF).Liquid nitrogen has a boiling point of
-195.8oC (-320.5oF). All cryogenic liquids produce large amounts of gas when they vaporize.
HEALTH EFFECTS:
Extensive tissue damage or burns can result from exposure to liquid nitrogen or cold nitrogen
vapors. Being odorless, colorless, tasteless, and nonirritating, nitrogen has no warning
properties. Humans possess no senses that can detect the presence of nitrogen. Although
nitrogen is nontoxic and inert, it can act as a simple asphyxiant by displacing oxygen in air to
levels below that required to support life. Inhalation of nitrogen in excessive amounts can
cause dizziness, nausea, vomiting, loss of consciousness, and death. Death may result from
errors in judgment, confusion, or loss of consciousness that prevents self-rescue. At low
oxygen concentration, unconsciousness and death may occur in seconds and without
warning. Personnel including rescue workers should not enter areas where the oxygen
concentration is below 19.5%, unless provided with a self-contained breathing apparatus or
air-line respirator.
Containers
Liquid nitrogen is stored, shipped, and handled in several types of containers, depending
upon the quantity required by the user. The types of containers in use are the dewar,
cryogenic liquid cylinder, and cryogenic storage tank.
Cryogenic Liquid Cylinders
Cryogenic liquid cylinders are insulated, vacuum-jacketed pressure vessels. They come
equipped with safety relief valves and rupture discs to protect the cylinders from pressure
build up. These containers operate at pressures up to 350 psig and have capacities between 80
and 450 liters of liquid.
Cryogenic Storage Tanks
Tanks may be spherical or cylindrical in shape. They are mounted in fixed locations as
Stationary vessels. Tanks are designed to ASME specifications for the pressures and
temperatures involved. Use only suitable vessels for the handling and/or transport of
cryogenic liquids. Do not store liquid nitrogen in any container with a tight fitting lid; a loose
82
Nitrogen
fitting lid helps preventing air and moisture from entering the container and at the same time
allows pressure to escape.
7.1.2Safety Considerations
Cold contact burns
Liquid or low-temperature gas from any of the specified cryogenic substances will produce
effects on the skin similar to a burn. The extremely low temperature of the liquid can cause
severe frostbite or eye damage upon contact. Symptoms of frostbite include change in skin
color to white or grayish yellow and the pain after contact with liquid nitrogen may quickly
subside. Items in contact with liquid nitrogen become extremely cold. Touching these items
may result in torn flesh.
Asphyxiation
Liquid nitrogen gas released in a confined space can displace sufficient oxygen to make the
atmosphere incapable of sustaining life and cause asphyxiation without warning. Degrees of
asphyxia will occur when the oxygen content of the working environment is less than 20.9%
by volume. Effects from oxygen deficiency become noticeable at levels below ~ 18% and
sudden death may occur at ~ 6% oxygen content by volume. This decrease in oxygen content
can be caused by a failure/leak of the cryogenic vessel or transfer line and subsequent
vaporization of the cryogen.
Explosion – Pressure
Heat flux into the cryogen from the environment will vaporize the liquid and potentially
cause pressure buildup in cryogenic containment vessels and transfer lines. On vaporization
liquid nitrogen expands by a factor of 696; one liter of liquid nitrogen becomes 24.6 cubic
feet of nitrogen gas. Adequate pressure relief must be provided to all parts of a system to
permit this routine out gassing and prevent explosion.
Explosions – Chemical
Cryogenic fluids with a boiling point below that of liquid oxygen are able to condense
oxygen from the atmosphere. Repeated replenishment of the system can thereby cause
oxygen to accumulate as an unwanted contaminant. Similar oxygen enrichment may occur
where condensed air accumulates on the exterior of cryogenic piping. Violent reactions, e.g.
rapid combustions or explosion, may occur if the materials which make contact with the
oxygen are combustible.
83
Nitrogen
Buildings
Because of the large expansion ratio of liquid to gas (1:696), it is important to provide
adequate ventilation in areas using liquid nitrogen. A minimum of six air changes per hour is
required in these areas.
Oxygen level monitoring should be provided for areas where oxygen displacement may
occur. OSHA has established 19.5% oxygen concentration as the minimum for working
without supplied air.
7.1.3 Storage and Handling
Store and use liquid nitrogen containers with adequate ventilation. Do not store containers in
confined areas or in areas unprotected from the extremes of weather. Cryogenic containers
are equipped with pressure relief devices designed to control the internal pressure. Under
normal condition these containers will periodically vent product. Do not plug, remove or
tamper with any pressure relief device.
Cryogenic containers must be stored, handled, and transported in the upright position. When
moving never tip, slide, or roll containers on their side. Use a suitable hand truck for moving
smaller containers. Move larger container by pushing, not pulling. Use freight elevators
whenever possible to transport liquid nitrogen. Do not ride in the elevator with the liquid
nitrogen. Make arrangements for someone to send the elevator to a receiving person waiting
on the desired floor. Avoid mechanical and thermal shock. Never leave the vessel unattended
while transferring liquid nitrogen. Ensure that the delivery of the liquid nitrogen is directly
below the mouth of the receiving vessel. Always fill warm dewars slowly to reduce
temperature shock effects and to minimize splashing. Do not fill cylinders and dewars to
more than 80% of capacity. Never allow any unprotected part of the body to come in contact
with uninsulated pipes or equipment containing cryogenic product. The extreme cold will
cause flesh to stick fast and potentially tear on withdrawal.
If there is any difficulty in operating the container valve or container connections discontinue
use and contact the vendor.
Do not remove or interchange connections. Use only the properly assigned connections. Do
not use adapters. Use only transfer lines and equipment designed for use with cryogenic
liquids. Some elastomer sand metals, such as carbon steel, may become brittle at extremely
low temperatures and may easily fracture. These materials must be avoided in cryogenic
84
Nitrogen
service.
On gas withdrawal systems use check valves or other protective apparatus to prevent reverse
flow in the containers. On liquid systems pressure relief devices must be used in lines where
there is the potential to trap liquid between valves. It is recommended that all vents be piped
to the exterior of the building.
Liquid containers should not be left open to the atmosphere for extended periods. Keep all
valves closed and outlet caps in place when not in use. If restriction results from freezing
moisture or foreign material present in openings and vents contact the vendor for
instructions. Restrictions and blockages may result in dangerous over-pressurization. Do not
attempt to remove the restriction without proper instructions. If possible move the cylinder to
a remote location.
7.1.4Personal Protective Equipment (PPE)
Personnel must be thoroughly familiar with properties and safety considerations before being
allowed to handle liquid nitrogen and/or its associated equipment.
Eyes are most sensitive to the extreme cold of liquid nitrogen and its vapors. The
recommended personal protective equipment when handling or using liquid nitrogen is a full
face shield over safety glasses/goggles; loose-fitting thermal insulated gloves; and long-
sleeved shirts and pants without cuffs. In addition, safety shoes are recommended for those
involved with the handling of liquid nitrogen containers.
First Aid
In the event a person is injured by liquid nitrogen, the following first aid treatment should be
given pending the care of a physician ONLY if there is no risk to you.
For skin contact with cryogenic liquid nitrogen, remove any clothing that may restrict
circulationto the frozen area. Do not rub frozen parts, as tissue damage may result. People
with frostbitten feet should not walk on them. As soon as practical place the affected area in a
warm water bath that has a temperature not in excess of 105oF (40oC). Never use dry heat.
Frozen tissue is painless and appears waxy with a possible yellow color. It will become
swollen, painful, and prone to infection when thawed. If the frozen part of the body has been
thawed, cover the area with a dry sterile dressing with a large bulky protective covering,
pending medical care. In case of massive exposure, remove clothing while showering the
victim with warm water. Do not use hot water. Call a physician immediately. If the eyes are
85
Nitrogen
exposed to the extreme cold of the liquid nitrogen or its vapors, immediately warm the
frostbite area with warm water not exceeding 105 oF (40oC) and seek immediate medical
attention.
7.2 Environmental Impact Analysis
This topic needs to be considered at an early stage in the design, in relation to the site
considerations, and reassessed during the detailed design stage . The effect of the operation
of the chemical plant upon the environment and the population must be considered during
the feasibility study and during subsequent design stages. The formal environmental impact
analysis (EIA) has two parts, these relate to:
(a) The treatment of unwanted chemicals (by-products) and the concentrations of liquid
discharges and gaseous emissions during normal operation;
(b) The handling of a major chemical accident, including all chemicals within the plant and
any subsequent reaction products, and containment and clean up.
The environmental impact analysis is specific to the plant under consideration, the
comments/suggestions made here are of a general The concentrations of all chemicals to be
discharged, including gaseous emissions, must be determined and measures taken to ensure
that these levels conform to allowable legislative standards. The cost of clean-up can be high,
e.g. scrubbing systems, filters, etc., and may affect the economic analysis of the plant
operation . It is prudent to ensure that not only are present emission standards observed, but
also that the plant could conform to any subsequent legislative reductions in these emission
levels (while still operating economically). The effects of all emissions on the environment,
and upon company employees and the population must be assessed..Noise levels from the
plant need to be considered, and finally its aesthetic acceptability.
The second part of the environmental impact analysis (EIA) relates to the effects of a major
accident or spill within the plant. The safety aspects of an explosive gas discharge (for
example) should be considered in stored within the plant, prevailing wind direction, location
of plant personnel and the general public, access to the plant and to particular high-risk areas.
There is a large amount of information available concerning chemical discharges,
environmental protection, clean-up and the applicable legislation. The Environmental
Protection Agency in the USA has produced a prodigious number of reports concerning a
wide range of chemical plants. Much of the available information is specific to particular
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chemicals and process routes, however so much information has been published that locating
a relevant source is usually the main problem. Most countries now require a company to file
an environmental impact assessment with any proposal for a new chemical plant. This
document is usually open to public scrutiny and can be a source of much useful information.
Copies of the relevant legislation are readily available and advice can be obtained from
appropriate government departments conjunction with the loss prevention studies for the
plant . However, proposals for containment, clean-up, and discharge of major chemical spills
should be part of the EIA report. Any proposals should ensure the safety of personnel,
minimize the discharge and its effect on the environment, and preserve the integrity of the
plant..
●●●
Introduction
A suitable site must be found for a new project, and the site and equipment layout planned.
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Provision must be made for the ancillary buildings and services needed for plant operation;
and for the environmentally acceptable disposal of effluent.
9.1 PLANT LOCATION AND SITE
The location of the plant can have a crucial effect on the profitability of a project, and the
scope for future expansion. Many factors must be considered when selecting a suitable site,
and only a brief review of the principle factors are given below. The principle factors to
consider are:
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8.1.3 Transport
The transport of materials and products to and from the plant will be an overriding
consideration in site selection. If practicable, a site should be selected that is close to at least
two major forms of transport: road, rail, waterway (canal or river), or a sea port. Road
transport is being increasingly used, and is suitable for long- distance transport of bulk
chemicals. Air transport is convenient and efficient for the movement personnel and essential
equipment and supplies, and the proximity of the site to a major air port should be
considered.
8.1.4 Availability of labour
Labor will be needed for construction of the plant and its operation. Skilled construction
workers will usually be brought in from outside the site area, but there should be an adequate
pool of unskilled labour availability locally; and labour suitable for training to operate the
plant. Skilled tradesmen will be needed for plant maintenance. Local trade union customs
and restrictive practices will have to be considered when assessing the availability and
suitability of the local labour for recruitment and training.
8.1.5 Utilities (Services)
Chemical processes invariably require large quantities of water for cooling and general
process use, and the plant must be located near a source of water of suitable quality. Process
water may be drawn from a river, from wells, or purchased from a local authority.
At some sites, the cooling water required can be taken from a river or lake, or from the sea; at
other locations cooling towers will be needed.
Electrical power will be needed at all sites. Electrochemical processes that require large
quantities of power; need to be located close to a cheap source of power.A competitively
priced fuel must be available on site for steam and power generation.
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An environmental impact assessment should be made for each new project or major
modification or addition or an existing process.
8.1.7 Local community considerations
The proposed plant must be fit in with and be acceptable to the local community. Full
consideration must be given to the safe location of the plant so that it does not impose a
significant additional risk to the community.
On a new site, the local community must be able to provide adequate facilities for the plant
personnel: schools, banks, housing, and recreational and cultural facilities.
8.1.8 Land (site considerations)
Sufficient suitable land must be available for the proposed plant and for future expansion.
The land should ideally be flat, well drained and have suitable load-bearing characteristics. A
full site evaluation would be made to determine the need for piling or other special
foundations.
8.1.9 Climate
Adverse climatic conditions at a site will increase costs. Abnormally low temperatures will
require the provision of additional insulation and special heating for equipment and pipe
runs. Stronger structures will be needed at locations subject to high winds
(cyclone/hurricane) or earthquakes.
8.1.10 Political and strategic considerations
Capital grants, tax concessions, and other inducements are often given by governments to
direct new investment to preferred locations; such as areas of high unemployment. The
overriding of such grants can be the overriding considerations in site selection.
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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.
Following figure shows the plant layout of the nitrogen plant.
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Sr. Quantit
No. Equipment Name y Price in USD.
1 Compressor 2 4326600.00
2 Heat exchagers 3 883800.00
3 Distillation column 1 5181300.00
4 Distillation column 2 5516800.00
5 Adsorption tower 2 901400.00
6 Film type heat exch. 2 749400.00
7 Condensers 1 572400.00
8 Reflux Pump 2 104400.00
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= Rs. 989,855,508.00
= Rs 227,666,766.84
5. BUILDING INSTALLATION:
The cost for building including services consists of expense for labor, material & supply
involved in the erection of all building connected with the plant. In this cost of plumbing,
heating, lighting, ventilation & similar services are included.
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6. YARD IMPROVEMENT:
Cost of fencing, grading, roads, sidewalk, railroad siding, landscaping & similar item
constitute the portion of yard improvement.
This cost is always 2-5 % of purchased equipment cost
For our convenience we take it as 3% of purchased equipment cost
Therefore,
Cost of yard improvement = 0.03 x 989,855,508.00
= Rs 547,083.00 ------------ (F)
7. SERVICE FACILITIES:
Utilities for supplying steam, water, power, compressed air & fuel lies in the service
facilities. Waste disposal, fire protection & miscellaneous service item such as first aid &
cafeteria equipment are included in this.
This cost is always 8-20 % of purchased equipment cost
But For our convenience we take it as 9% of purchased equipment cost
Therefore,
Cost of service facility = 0.09 x 989,855,508.00
= Rs. 1,641,249.00------------- (G)
8. LAND:
The cost of land & the accompanying surveys & fees depends on the location of property &
may vary by cost factor.
This cost is always 1-2 % of purchased equipment cost
For our convenience we take it as 2% of fixed capital investment.
Therefore,
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Direct Cost = (A) + (B) + (C) + (D) + (E) + (F) + (G) + (H)
= Rs. 1,225,546,158.84 ------------------------- (A#)
= Rs 134,810,077.47-------- (A)
2. CONSTRUCTION EXPENSE:
This includes temporary construction & operation, construction tool & rental office,home
office at construction site etc.
This cost is always 4-16 % of Total direct cost.
For our convenience we take it as 7% of Total direct cost
Therefore,
Construction expense = 0.07 x 1,225,546,158.84
3. CONTRACTOR’S FEES:
The contractor’s fee varies for different situation but it is always 2-6 % of Total direct cost.
For our convenience we take it as 5% of Total direct cost.
Therefore,
Contractor’s fees = 0.05 x 1,225,546,158.84
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4. CONTINGENCIES:
A contingency factor is usually included in an estimate of capital investment to compensate
for unpredictable events such as storms, floods, strikes, price change, small design change
etc.
This is always 5-15 % of Total direct cost. For our convenience we take it as 7% of Total
direct cost Therefore,
Contingencies = 0.07 x 1,225,546,158.84
= Rs 85,788,231.12 --------------- (D)
Now,
Total indirect cost = (A) + (B) +(C) + (D)
= Rs. 379,919,309.24------------------ (B#)
Therefore,
Fixed Capital Investment = Direct Cost + Indirect Cost
= (A#) + (B#)
= Rs 1,605,465,468.08
= Rs 1,888,782,903.62
Therefore,
Working capital =0.15 x 1,888,782,903.62
= Rs 283,317,435.54
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3. OPERATING SUPERVISION
It is most commonly 10 -50% of operating labour
For our convenience we take it as 15% of operating labour
Therefore,
Operating labour cost = 0.15 x 24,818,015.17
= Rs. 3,722,702.28--------- (c)
4. UTILITIES:
The cost for utilities such as steam, electricity, process & cooling water, compressed
air varies depending on the amount of consumption.
As a rough approximation it is always 10-20% of total product cost.
For our convenience we take it as 10% of total product cost.
Therefore,
Utility cost = Rs 400000.00------------ (d)
6. OPERATING SUPPLIES:
In any manufacturing operation, many miscellaneous supplies are needed to keep the
process functioning efficiently & it is not included in the raw material cost.
It is always 15% of maintenance & repair cost.
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Therefore,
Operating supplies cost = 0.15 x 29,695,665.24
= Rs. 4,454,349.79----------- (f)
7. LABORATORY CHARGES:
The cost of laboratory test for control of operation & for product quality is covered in
this cost.
For quick estimates, this is always 2-10% of operating labour cost.
For our convenience we take it as 2% of operating labour cost.
Therefore,
Laboratory charges = 0.2 x 24,818,015.17
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2. LOCAL TAXES:
The magnitude of local property taxes depends on the particular locality of the plant &
regional laws.
This is always 1-4% of fixed capital investment.
For our convenience we take it as 1% of fixed capital investment.
Therefore,
Local taxes = 0.01 * 1,605,465,468.08
= Rs. 16,054,654.68 --------- (i)
3. INSURANCE:
Insurance rate depends on the type of process being carried out in the manufacturing
operation & on the extent of available protection facilities.
It is always 1% of fixed capital investment.
Therefore,
Insurance = 0.01 x 1,605,465,468.08
= Rs. 16,054,654.68 ----------- (j)
4. Annual cost of Depreciation for buildings is taken as 3% of the Initial Cost of
buildings
Annual cost of depreciation = 0.03 x 3,100,137.00
= Rs 93,004.11----------- (k)
= Rs 80,273,273.40---------- (l)
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Therefore
Fixed charges = (h) + (i) + (l)
S.
No. Description Total Annual cost in Rs.
1.00 Depreciation 96,420,932.19
2.00 Taxes 16,054,654.68
3.00 Insurance 16,054,654.68
4.00 Rent 0.00
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= Rs 116,753,884.98---------- (l)
This includes salaries & wages for all personnel directly connected with this type of work.
In chemical industry this cost amount is about 2% of total product cost.
Therefore,
Research & development cost = 0.02 * 233,507,769
4. INTEREST:
Interest is considered to be compensation paid for the use of borrowed capital.
For rough approximation this is 0-10% of total product cost.
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S.
No. Description Total Annual cost in Rs.
Therefore,
Total product cost = Manufacturing cost + General expenses
= (F#) + (G#)
= Rs. 503,414,768.22 --------- (H#).
= 2,683,193,866.08--------- (I#)
Now,
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= (I#) – (H#)
= 2,683,193,866.08 - 503,414,768.22
= Rs 762922684-------------- (K#)
= 1.05 years
= 89.60 %
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APPENDIX
PROPERTY ESTIMATION:
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
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He a l t h
0
F i re
0
Re a c t i v i t y
0
P e rs o n a l
A
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SOLVENT SOLUBILITY:
Soluble: liquid ammonia
Slightly Soluble: alcohol
10. STABILITY AND REACTIVITY
REACTIVITY: Stable at normal temperatures and pressure.
CONDITIONS TO AVOID: Protect from physical damage and heat. Containers
may rupture or explode if Exposed to heat.
INCOMPATIBILITIES: metals, oxidizing materials
HAZARDOUS DECOMPOSITION: Thermal decomposition products: oxides of
nitrogen
POLYMERIZATION: Will not polymerize.
11. TOXICOLOGICAL INFORMATION
Not available
12. ECOLOGICAL INFORMATION
Not available
The information above is believed to be accurate and represents the best information currently available to us.
However, we make no warranty of merchantability or any other warranty, express or implied, with respect to
such information, and we assume no liability resulting from its use. Users should make their own investigations
to determine the suitability of the information for their particular purposes. In no event shall ScienceLab.com
be liable for any claims, losses, or damages of any third party or for lost profits or any special, indirect,
incidental, consequential or exemplary damages, howsoever arising, even if ScienceLab.com has been advised
of the possibility of such damages
●●●
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BE. Kirk and D.F. Othmer (Eds), Encyclopedia of Chemical Technology,
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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
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Air liquefaction: distillation encyclopedia of separation science, 2007, pages 1895-
1910, science direct R. Agrawal, D.M. herron Cryogenic Process Engineering
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Dr.‐Carl‐von‐Linde‐Strasse6‐14, 82049Pullach, Germany, 1/11/2010
http://www.linde‐engineering.com/en/process_plants/airseparation_history/index.html
Site Designed and Maintained by Industrialgasplants.com , 24/11/2010
http://www.industrialgasplants.com/cryogenic‐air‐separation.html
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http://www.matche.com/EquipCost/index.htm
House, F.F., An Engineers Guide to Process-Plant Layout, ChemicalEngineering, 28
July,pp.120-128 (1968).
Cavaseno, V. (Ed), Industrial Air Pollution Engineering, reprints of papers from
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