1. General points2. Theoretical principles3. Cryogenic separation
1. The distillation flask2. Liquid / vapor equilibrium of a mixture3. Principle of fractional distillation4. Single column model5. Double column model6. Operating conditions
4. Heat Exchange5. Air Purification6. Cold production7. Air and products compression8. Air separation unit process control9. Argon, Xr&Xe, He&Ne extraction
Air Distillation
Hamilton Sept. 2009
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
COMPRESSION
AIR
OXYGEN
NITROGEN
PURIFICATION
COLDPRODUCTION
(option 1)
DISTILLATIONCRYOGENIC
NON-CRYOGENIC
HEAT EXCHANGE
WASTE
COLDPRODUCTION
(option 2)
Distillation in the air separation process
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
The distillation flask
Mixture
water + alcohol
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
The distillation flask
Cooler
water + alcohol
vapor phase
Liquid phase
Distillate
Heater
vapor richerin alcohol
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Partial pressure definition
The partial pressure of a component in a gas mixture is the pressure this component would have if it alone occupied the same volume at the same temperature as the mixture.
P = P « » + P « » P = P « »
In case of red
component alone
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Equilibrium - Partial pressure
0.79bar1bar10079PN2
0.21bar1bar10021PO2
Mixture
Partial pressures:
Total P = 1 bara
N2 = 79 %
O2 = 21 %
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Liquid-Vapor Equilibrium
Composition of the liquid
79% N2 and 21% O2 Temperature: - 183 °C
What are the pressure and the composition of the vapor phase?
Liquid
Vapor
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Determining of the vapor composition At T = -183 °C:
P0O2 = 1 bar abs => PO2 = 0.21 x 1 = 0.21 bar
P0N2 = 3.6 bar abs => PN2 = 0.79 x 3.6 = 2.84 bar
P = PO2 + PN2 = 0.21 + 2.84 = 3.05 bar
Dalton’s law : [O2]vapor = 0.21 / 3.05 = 7 % [N2]vapor = 2.84 / 3.05 = 93 %
Liquid-Vapor Equilibrium: Raoult law
Liquid
Vapor
7% O2
93% N2
21% O2
79% N2
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Equilibrium ratio of a component
K (most volatile component) > 1and
K (less volatile component) < 1
component content in the vapor phaseK = component content in the liquid phase
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Phase diagram of a mixtureO2-N2 diagram under constant pressure
YXYZLiq%
YXZXVap%
% O2
100 %XZ0 % Y
PPV
Q2V
Q2LQ2
Q1
Q3
Q41
Q0T
PL[L] [V]
L
V2
Appearance of the the first gas bubble in the liquid“boiling point curve”
Appearance of the first liquid drop in the vapor“dew point curve”
Q3V
Q3L
Q1V Q1L
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Phase diagram of a mixture O2-N2 diagram under constant pressure
Effect of pressure:
P2 > P1
% O2100 %
T
0 %
P2
P1
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Phase diagram of a mixtureO2-N2 diagram at constant temperature
YXYZLiq%
YXZXVap%
% O2100 %
P
PV
Q2V
Q2L
Q2
Q3
Q1
Q0
1
Q4
P
0 %
PL2 [L]
[V]
X Z Y
L
V
Oxygen content ofthe first liquid drop
Oxygen content ofthe last gas bubble
Q1V
Q1L
Q3V
Q3L
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Phase diagram of a mixtureO2-N2 diagram at constant temperature
Effect of temperature:
T2 > T1
100 %0 % % O2
P
T2
T1
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
1 bar abs
P bars abs
%O2
T °C
5 bar abs
Liquid / vapor equilibrium curve of pure O2
Liquid / vapor
equilibrium curve of pure N2
Phase diagram of a mixture
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Exercise 1
We consider an exchanger made of a pipe fed by a liquid nitrogen flow under 1 bar abs.
This pipe is going through a jacket fed by de-carbonated and dry air maintained at a constant pressure of 1 bar abs.
• What happens to the air ?
De-carbonatedand dry air
Liquid nitrogen
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
First stacking model
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
First stacking model ISOBARIC SYSTEM :
P1= P2= P3 = P4
TEMPERATURE GRADIENT : T1 > T2 > T3 > T4
P1,T1
P2,T2
P3,T3
P4,T4
TEMPERATURE INCREASES
TEMPERATURE DECREASESEnrichment by morevolatile constituant
Enrichment by lessvolatile constituant
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Second stacking model
P1,T1
P2,T2
P3,T3
P4,T4
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Third stacking model
Condenser
Boiler
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Distillation column
Most volatile element
Less volatile element
CONDENSER
Trays
BOILER
Enric
hmen
t in
Lig
ht
Enric
hmen
t in
Hea
vy
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Distillation tray
vapor V1
vapor V0
vapor V2
liquid L2
liquid L1
liquid L0
Liquid – vaporcontact
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Distillation packing
NITROGEN
OXYGEN
PACKING
Continuous liquid – vapor contact
VAPO
R R
ICH
ER A
ND
RIC
HER
IN N
ITR
OG
EN
LIQ
UID
RIC
HER
AN
D R
ICH
ER
IN O
XYG
EN
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Total reflux column
V
L
Total condenser
Total boiler
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Boiler / condenser column introduction
The more volatile product (N2)
The less volatile product(O2)
Mixture to be treated (O2+N2)
Condenser
Boiler
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Single boiler column
liquide
VAPOR
LIQUID
LIQUID
Mixture to be treated (O2+N2)
Residual product (O2+N2)
Boiler
The less volatile product (O2)
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Single condenser column
VAPOR
LIQUID
LIQUID
Mixture to be treated (O2+N2)
Residual product (O2+N2)
Condenser
The more volatile product (N2)
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Double column model
GOX
LOX
GAN
LIN
Heat exchangeLOX
Waste
Waste
AIR
LIN
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Double column model - Vaporizer
EXCHANGER
GAN
LIN
Upper column
Lower column
LOX
GOX
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Double column – Vaporizer-CondenserP (b abs)
T (°C)
1.0
N2
O2
-196 -183 -179 -177
T= 2°C
1.4
3.5
5.6
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Non-condensable gases
GAN
LIN
T= 2°C
Non condensable gases
GOX
LP column
HP column
-179°C1.4b
-177°C5.6b
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Double column model
LOX
GAN LIN
LP column
HP column
vaporizer-condenser
GOX
Liquid rich in O2
Waste (N2+O2)
Blow-off of theNon-condensable
Gaseous AIR
O2 content ~ 15 %
O2 content ~ 40 %
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Second configuration
LOX
GAN LIN
LP column
HP column
vaporizer-condenser
GOX
Rich Liquid
Lean Liquid
Waste: Impure nitrogen
Gaseous AIR
O2 content < 0.5 %
O2 content ~ 1 %
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Liquid / Vapor ratio
Liquid / Vapor ratio =
Liquid flow (Nm3/h)
Vapor flow V (Nm3/h)
Liquid flow L
Vapor flow V
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Effect of the variation of reflux ratio
Initialstate
Firstmodified
case
Secondmodified
case
L flowNm3/h
1000 1000 1000
V flowNm3/h
1000 1100 900
L / V 1 0.91 1.11
BottomV purity
%O221 21 21
TopV purity
%O210.5 > 10.5 < 10.5
V L
V L
10.5% O2
21% O2
(purities written are only given as an example)
Initial purities
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
L / V
Top product
N2 purity (V)
Bottom product
O2 purity (L)
Effect of the variation of reflux ratio
V L
V L
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Double column model - with top hat
LIN
LOX
HP GAN
LP column
HP column
GOX
Rich liquid
Lower
Impure nitrogen
LP GAN
Top hat
Upperlean liquid
lean liquid
Gaseous AIR
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Material balance
Oxygen balance:
Σ(outlets)Σ(inlets)
2WasteFlow2LOXFlow2GOXFlow2AirFlow OOOOWASTELOXGOXAIR
Total balance:
WNFlowGANFlowLINFlowLOXFlowGOXFlowAirFlow
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Material balance
GOXQ
LOXQ
AIRQ
With: = Gaseous oxygen production flow
= Liquid oxygen production flow
= Air feed flow
0.2096 = Mole fraction of oxygen in air
O2η = Oxygen extraction ratio
AIR
LOXGOXO2 0.2096Q
QQ100η
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Material balance
WNFlow
NFlowAIRFlow0.782
WNFlowOFlowAIRFlow0.21
2
NFlowOFlowAirFlowWNFlow
2
waste
2
waste
22
N
O
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Cold balance
Liquid production(Cold output)
Cold production(Cold input)
Cold losses(Delta T exchangers,radiation losses…)
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Losses of cold: Losses by radiation
Losses by the gap at the warm end of the main exchanger
Losses by liquid production
Cold balance
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Cold balance
Cold production or cold inputs: Expansion through a turbine
Liquid assist
Free gas expansion
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Pressure chart
vapo ΔT
Air HP
waste
Atm P
top LP P
vapo P
cond P
purification ΔP
exchanger ΔP
LP column ΔP
O2 bubble T
N2 dew T
HP column
ΔP
bottom HP P
compressor P
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
P out / P in
Q air
Pressure drops
Compressor curves
Cold Box operating curves
Pressure chart
ANTI S
URGE
SURGE
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Pressure chart
1.013 abs bar
1.463 abs bar
1.513 abs bar
6.6 abs bar 150 mbars
300 mbars
50 mbars
-178 °C
-175 °C3°C
100 mbars
6.7 abs bar
7 abs bar 300 mbars
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Adjusting the L/V ratio 600
LOX
GAN LIN
GOX
RL
LL
Impure nitrogen
1000
L/V = 0.450
L/V = 0.800
L/V = 1.333
L/V = 0.583
450
200
0
800
200
600 350
600 800
1000 800
1000 450
450
350
0
350
Gaseous AIR
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Adjusting the L/V ratio600
LOX
GAN LIN
GOX
RL
LL
Impure nitrogen
1000
L/V = 0.500
L/V = 0.800
L/V = 1.333
L/V = 0.500
500
200
0
800
200
600 300
600 800
1000 800
1000 500
500
300
0
300
Gaseous AIR
Increase in the oxygen contained
Drop of reflux ratio
Rise of reflux ratio
Decrease in the oxygen contained
Decrease in lean liquid
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Adjusting the L/V ratio
LOX
GAN LIN
GOX
RL
LL
Impure nitrogen
800
L/V = 0.450
L/V = 0.800
L/V = 1.333
L/V = 0.583
360
160
0
640
160
480 280
480 640
800 640
800 360
480
360
280
0
280
Gaseous AIR
Conservation of the rates of reflux
Decrease in air flow
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Liquid draw off
LOX
GaN LiN
GOX
RL
LL
Impure nitrogen
1000
L/V = 0.450
L/V = 0.800
L/V = 1.333
L/V = 0.583
450
200
200
800
0
600 350
600 800
1000 800
1000 450
600
450
350
0
350
Gaseous AIR
Liquid falling into the vaporizer = 800 Nm3/h
Liquid vaporized + drawn off = 1000
Nm3/h
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Liquid draw off
LOX
GN
LIN
GOX
RL
LL
Impure nitrogen
1000
L/V = 0.450
L/V = 0.800
L/V = 1.333
L/V = 0.583
450
400
200
600
0
600 350
600 800
1000 800
1000 450
600
450
350
0
350
Gaseous AIR
Liquefier
200
LIN
200
450
LOX
GN LIN
GOX
RL
LL
800L/V = 0.312
L/V = 0.750
200
200
600
0
800 600
800 250
0
350
Gaseous AIR200
Liquid AIR
Impure nitrogen
L/V = 1.333
L/V = 0.583 600 350
600 800
450
350
800 250
600
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Content profile
LIN
GOX
RL
LL
Impure nitrogen
Gaseous AIR
Content of the LL
%O2
Decrease of the GOX draw off
Increase of the GOX draw off
Content of the GOX
20 40 60 80 1000
Number of
tray
GAN
LP
RL
LOX
Content n of the GAN or tthe LIN
Content of the RL AIR
Content of the impure nitrogen
52This document is the property of the AIR LIQUIDE Group and may not be communicated to any party without its formal authorization – This is an uncontrolled copy, the only controlled copy is kept in Alexandria data base
Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Exercise
a HPN is fed by an air flow of 1000 Nm3/h at 6 bar a.
1. It produces 200 Nm3/h of pure nitrogen. What is the oxygen content of the rich liquid?
2. What is the maximum nitrogen production of such a plant? (assume the oxygen content of the liquid in equilibrium with the air at 6 bar is 40% O2)
GANAIR
RL
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Annular trays AT
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Weired trays WT
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Packing
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Packing manufacturing
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Liquid distributor
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Assembly of a column in workshop
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Air Separation Unit in Europe
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
ASU in South Africa
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Packing columns
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
O2/N2 concomitant phases diagram
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
McCabe - Thiele Diagram
1
1
0
Tray number : n
LV
Vn-1
VnLn+1
Ln
xn
yn
xn
ynY (fraction in vapor phase)
X (fraction in liquid phase)
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
McCabe - Thiele Diagram
Tray 1
Tray 2
Tray 3
Tray 4
Tray 5
V1
V2
V3
V4
V5
L2
L3
L4
L5
L6
x1 x2 x3
y3
1
1
0
y1
y2
Total condenser
Total boiler
y N2 fraction in vapor phase
x N2 fraction in liquid phase
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
P = constant
% O2
T (°C)
V
L + V
L
1000
O2-N2 Mixture phase diagram
Dew point curve
Boiling point curve
P = 1 atm-183
-196
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Hamilton Sept. 2009 Air Distillation – Cryogenic separation
O2-N2 Mixture phase diagram
% O2
T (°C)
V
zL5
100x
vL
L
y0
V1
P = constant
2
4
3
67This document is the property of the AIR LIQUIDE Group and may not be communicated to any party without its formal authorization – This is an uncontrolled copy, the only controlled copy is kept in Alexandria data base
Hamilton Sept. 2009 Air Distillation – Cryogenic separation
P = constant = P1
P = constant = P2
P2 > P1
% O2
T (°C)
1000
O2-N2 Mixture phase diagram
68This document is the property of the AIR LIQUIDE Group and may not be communicated to any party without its formal authorization – This is an uncontrolled copy, the only controlled copy is kept in Alexandria data base
Hamilton Sept. 2009 Air Distillation – Cryogenic separation
O2-N2 Mixture phase diagram
% O2
P(bar)
L
L+V
V
1000
Dew point curve
Boiling point curve
T = constant
T = - 183 °C3.5
1.013
69This document is the property of the AIR LIQUIDE Group and may not be communicated to any party without its formal authorization – This is an uncontrolled copy, the only controlled copy is kept in Alexandria data base
Hamilton Sept. 2009 Air Distillation – Cryogenic separation
O2-N2 Mixture phase diagram
P (bar)
% O21000
L5
V1
V
z x
VL
L
y
T = constant
2
34
70This document is the property of the AIR LIQUIDE Group and may not be communicated to any party without its formal authorization – This is an uncontrolled copy, the only controlled copy is kept in Alexandria data base
Hamilton Sept. 2009 Air Distillation – Cryogenic separation
% O2
P (bar) T = constant = T1
T = constant = T2
T2 > T1
1000
O2-N2 Mixture phase diagram
71This document is the property of the AIR LIQUIDE Group and may not be communicated to any party without its formal authorization – This is an uncontrolled copy, the only controlled copy is kept in Alexandria data base
Hamilton Sept. 2009 Air Distillation – Cryogenic separation
O2-N2 Mixture phase diagram
% O2
T°C
1000
Li+1
Li
Vi
Vi-1
yi-1 z xi+1 xiyi
V yi-1 + L xi+1
= V yi + L xi
= (V+L) z
P = constant
72This document is the property of the AIR LIQUIDE Group and may not be communicated to any party without its formal authorization – This is an uncontrolled copy, the only controlled copy is kept in Alexandria data base
Hamilton Sept. 2009 Air Distillation – Cryogenic separation
O2-N2 Mixture phase diagram
yO2
xO2
1
1
Li+1
Li
Vi
Vi-1
V yi-1 + L xi+1
= V yi + L xi
= (V+L) z00
xi+1
yi-1
z
zyi
xi
operating straight line of - V / L slope
P = constant
73This document is the property of the AIR LIQUIDE Group and may not be communicated to any party without its formal authorization – This is an uncontrolled copy, the only controlled copy is kept in Alexandria data base
Hamilton Sept. 2009 Air Distillation – Cryogenic separation
O2-N2 Mixture phase diagram
Ln+1
Q
Vn
LiVi-1
Vaporizer
V = Q + L
V yi-1 = Q yn + L xi
yO2
xO2
1
1
00
xi
yi-1
z
yi
xi-1
operating straight line of V / L slope passing through
(yn,yn)
P = constant
74This document is the property of the AIR LIQUIDE Group and may not be communicated to any party without its formal authorization – This is an uncontrolled copy, the only controlled copy is kept in Alexandria data base
Hamilton Sept. 2009 Air Distillation – Cryogenic separation
Safety at Work – how not to do it
4th place
75This document is the property of the AIR LIQUIDE Group and may not be communicated to any party without its formal authorization – This is an uncontrolled copy, the only controlled copy is kept in Alexandria data base
Hamilton Sept. 2009 Air Distillation – Cryogenic separation
This concludes the Section on Distillation
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