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Sequencing Separation Trains
Process Design/Retrofit Steps
Assess Primitive
Problem
Development
of Base-case
Plant-wide
Controllability
Assessment
Detailed Design,
Equipment sizing, Cap.
Cost Estimation,
Profitability Analysis,
Optimization
Detailed Process
Synthesis -
Algorithmic
Methods
PART II
Algorithmic Methods
Lecture 4 – Introduction
• Almost all chemical processes require the separation of
chemical species (components), to:
 Purify a reactor feed
 Recover unreacted species for recycle to a reactor
 Separate and purify the products from a reactor
• Frequently, the major investment and operating costs of a
process will be associated with separation equipment
• For a binary mixture, it may be possible to select a
separation method that can accomplish the separation task
in just one piece of equipment.
• More commonly, the feed mixture involves more than two
components, involving more complex separation systems.
Lecture 4 – Objectives
 Be familiar with the more widely used
industrial separation methods and their
basis for separation.
 Understand the concept of the separation
factor and be able to select appropriate
separation methods for liquid mixtures.
Example: Butenes Recovery
3.31
196.3
36.1
F
n-Pentane
4.02
161.4
3.7
E
cis-2-Butene
4.12
155.4
0.9
D
trans-2-Butene
3.73
152.0
-0.5
C
n-Butane
3.94
146.4
-6.3
B
1-Butene
4.17
97.7
-42.1
A
Propane
Pc, (MPa)
Tc (C)
b.pt.(C)
Species
3.31
196.3
36.1
F
n-Pentane
4.02
161.4
3.7
E
cis-2-Butene
4.12
155.4
0.9
D
trans-2-Butene
3.73
152.0
-0.5
C
n-Butane
3.94
146.4
-6.3
B
1-Butene
4.17
97.7
-42.1
A
Propane
Pc, (MPa)
Tc (C)
b.pt.(C)
Species
Example: Butenes Recovery
100-tray column
C3 & 1-Butene in
distillate
Propane and
1-Butene recovery
Pentane withdrawn
as bottoms n-C4 and 2-C4=s
cannot be
separated by
ordinary distillation
(=1.03), so 96%
furfural is added as
an extractive agent
(  1.17).
n-C4 withdrawn as
distillate.
2-C4=s withdrawn as
distillate. Furfural is
recovered as bottoms
and recycled to C-4
Separation is Energy Intensive
• Unlike the spontaneous mixing of chemical species, the
separation of a mixture of chemicals requires an
expenditure of some form of energy
• Separation of a feed mixture into streams of differing
chemical composition is achieved by forcing the different
species into different spatial locations, by one or a
combination of four common industrial techniques:
 The creation by heat transfer, shaft work, or pressure reduction
of a second phase that is immiscible with the feed phase (ESA –
energy separating agent)
 Introduction into the system of a second fluid phase (MSA –
mass separating agent). This must be subsequently removed.
 Addition of a solid phase upon which adsorption can occur
 Placement of a membrane barrier
Common Separation Methods
difference
in volatility
V and L
Liquid
entrainer and
heat transfer
L and/or V
Azeotropic
Distillation
difference
in volatility
V and L
Liquid solvent
and heat
transfer
L and/or V
Extractive
Distillation
difference
in volatility
V
Vapor stripping
agent
L
Stripping
difference
in volatility
L
Liquid
absorbent
V
Gas
Absorption
difference
in volatility
V or L
Heat transfer
or shaft work
L and/or V
Distillation
difference
in volatility
V or L
Pressure
reduction or
heat transfer
L and/or V
Equilibrium
flash
Separation
principle
Developed or
added phase
Separation
agent
Phase of
the feed
Separation
Method
difference
in volatility
V and L
Liquid
entrainer and
heat transfer
L and/or V
Azeotropic
Distillation
difference
in volatility
V and L
Liquid solvent
and heat
transfer
L and/or V
Extractive
Distillation
difference
in volatility
V
Vapor stripping
agent
L
Stripping
difference
in volatility
L
Liquid
absorbent
V
Gas
Absorption
difference
in volatility
V or L
Heat transfer
or shaft work
L and/or V
Distillation
difference
in volatility
V or L
Pressure
reduction or
heat transfer
L and/or V
Equilibrium
flash
Separation
principle
Developed or
added phase
Separation
agent
Phase of
the feed
Separation
Method
Common Separation Methods
difference in
permeability
and/or
solubility
Membrane
Membrane
L or V
Membranes
difference in
adsorbabililty
Solid
Solid
adsorbent
L
Liquid
adsorption
difference in
adsorbabililty
Solid
Solid
adsorbent
V
Gas
adsorption
Difference in
solubility or
m.p.
Solid
Heat
transfer
L
Crystalli-
zation
Difference in
solubility
Second
liquid
Liquid
solvent
L
Liquid-liquid
Extraction
Separation
principle
Developed
or added
phase
Separation
agent
Phase of
the feed
Separation
Method
difference in
permeability
and/or
solubility
Membrane
Membrane
L or V
Membranes
difference in
adsorbabililty
Solid
Solid
adsorbent
L
Liquid
adsorption
difference in
adsorbabililty
Solid
Solid
adsorbent
V
Gas
adsorption
Difference in
solubility or
m.p.
Solid
Heat
transfer
L
Crystalli-
zation
Difference in
solubility
Second
liquid
Liquid
solvent
L
Liquid-liquid
Extraction
Separation
principle
Developed
or added
phase
Separation
agent
Phase of
the feed
Separation
Method
Common Separation Methods
Difference
in volatility
V
Heat
transfer
S and L
Drying
Difference
in solubility
L
Liquid
solvent
S
Leaching
Difference
in solubility
Supercritical
fluid
Supercritical
solvent
L or V
Supercritical
extraction
Separation
principle
Developed
or added
phase
Separation
agent
Phase of
the feed
Separation
Method
Difference
in volatility
V
Heat
transfer
S and L
Drying
Difference
in solubility
L
Liquid
solvent
S
Leaching
Difference
in solubility
Supercritical
fluid
Supercritical
solvent
L or V
Supercritical
extraction
Separation
principle
Developed
or added
phase
Separation
agent
Phase of
the feed
Separation
Method
Separation Method Selection
• The development of a separation process requires the
selection of:
 Separation methods
 ESAs and/or MSAs
 Separation equipment
 Optimal arrangement or sequencing of the equipment
 Optimal operating temperature and pressure for the equipment
• Selection of separation method depends on feed condition:
• Vapor Partial condensation, distillation, absorption,
adsorption, gas permeation (membranes)
• Liquid Distillation, stripping, LL extraction, supercritical
extraction, crystallization, adsorption, and dialysis
or reverse osmosis (membranes)
• Solid If wet  drying, if dry  leaching
Separation Method Selection
• The separation factor, SF, defines the degree of separation
achievable between two key components of the feed. This
factor, for separation of component 1 from component 2
between phases I & II, for a single stage of contacting, is:
II
II
I
I
C
C
C
C
SF
2
1
2
1
/
/
 (8.1)
C = composition variable,
I, II = phases rich in
components 1 and 2.
• SF is generally limited by thermodynamic equilibrium. For
example, in the case of distillation, using mole fractions as the
composition variable and letting phase I be the vapor and phase
II be the liquid, the limiting value of SF is given in terms of
vapor-liquid equilibrium ratios (K-values) as:
(8.2), (8.3)
 
    
1 1 1 1
1 2
2 2 2 2
for ideal L and V
s
, s
y / x K P
SF
y / x K P
Separation Method Selection
• For vapor-liquid separation operations that use an MSA that
causes the formation of a non-ideal liquid solution (e.g.
extractive distillation):
(8.5)
s
L
s
L
P
P
SF
2
2
1
1
2
,
1





• If the MSA is used to create two liquid phases, such as in liquid-
liquid extraction, the SF is referred to as the relative selectivity,
β , where:
I
I
II
II
SF
2
1
2
1
2
,
1
/
/






 (8.6)
• In general, MSAs for extractive distillation and liquid-liquid
extraction are selected according to their ease of recovery for
recycle and to achieve relatively large values of SF.
Equal Cost Separators
Ref: Souders (1964)
Extractive distillation
should NOT be used
when α for ordinary
distillation is
greater than 2
Liquid-Liquid Extraction
should NOT be used
when α for ordinary
distillation is greater
than 3.2
Summary – Separation Trains
 Be familiar with the more widely used industrial separation
methods and their basis for separation.
 Understand the concept of the separation factor and be
able to select appropriate separation methods for liquid
mixtures.
On completion of this part, you should:

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Sequencing Separation Trains.ppt

  • 2. Process Design/Retrofit Steps Assess Primitive Problem Development of Base-case Plant-wide Controllability Assessment Detailed Design, Equipment sizing, Cap. Cost Estimation, Profitability Analysis, Optimization Detailed Process Synthesis - Algorithmic Methods PART II
  • 4. Lecture 4 – Introduction • Almost all chemical processes require the separation of chemical species (components), to:  Purify a reactor feed  Recover unreacted species for recycle to a reactor  Separate and purify the products from a reactor • Frequently, the major investment and operating costs of a process will be associated with separation equipment • For a binary mixture, it may be possible to select a separation method that can accomplish the separation task in just one piece of equipment. • More commonly, the feed mixture involves more than two components, involving more complex separation systems.
  • 5. Lecture 4 – Objectives  Be familiar with the more widely used industrial separation methods and their basis for separation.  Understand the concept of the separation factor and be able to select appropriate separation methods for liquid mixtures.
  • 6. Example: Butenes Recovery 3.31 196.3 36.1 F n-Pentane 4.02 161.4 3.7 E cis-2-Butene 4.12 155.4 0.9 D trans-2-Butene 3.73 152.0 -0.5 C n-Butane 3.94 146.4 -6.3 B 1-Butene 4.17 97.7 -42.1 A Propane Pc, (MPa) Tc (C) b.pt.(C) Species 3.31 196.3 36.1 F n-Pentane 4.02 161.4 3.7 E cis-2-Butene 4.12 155.4 0.9 D trans-2-Butene 3.73 152.0 -0.5 C n-Butane 3.94 146.4 -6.3 B 1-Butene 4.17 97.7 -42.1 A Propane Pc, (MPa) Tc (C) b.pt.(C) Species
  • 7. Example: Butenes Recovery 100-tray column C3 & 1-Butene in distillate Propane and 1-Butene recovery Pentane withdrawn as bottoms n-C4 and 2-C4=s cannot be separated by ordinary distillation (=1.03), so 96% furfural is added as an extractive agent (  1.17). n-C4 withdrawn as distillate. 2-C4=s withdrawn as distillate. Furfural is recovered as bottoms and recycled to C-4
  • 8. Separation is Energy Intensive • Unlike the spontaneous mixing of chemical species, the separation of a mixture of chemicals requires an expenditure of some form of energy • Separation of a feed mixture into streams of differing chemical composition is achieved by forcing the different species into different spatial locations, by one or a combination of four common industrial techniques:  The creation by heat transfer, shaft work, or pressure reduction of a second phase that is immiscible with the feed phase (ESA – energy separating agent)  Introduction into the system of a second fluid phase (MSA – mass separating agent). This must be subsequently removed.  Addition of a solid phase upon which adsorption can occur  Placement of a membrane barrier
  • 9. Common Separation Methods difference in volatility V and L Liquid entrainer and heat transfer L and/or V Azeotropic Distillation difference in volatility V and L Liquid solvent and heat transfer L and/or V Extractive Distillation difference in volatility V Vapor stripping agent L Stripping difference in volatility L Liquid absorbent V Gas Absorption difference in volatility V or L Heat transfer or shaft work L and/or V Distillation difference in volatility V or L Pressure reduction or heat transfer L and/or V Equilibrium flash Separation principle Developed or added phase Separation agent Phase of the feed Separation Method difference in volatility V and L Liquid entrainer and heat transfer L and/or V Azeotropic Distillation difference in volatility V and L Liquid solvent and heat transfer L and/or V Extractive Distillation difference in volatility V Vapor stripping agent L Stripping difference in volatility L Liquid absorbent V Gas Absorption difference in volatility V or L Heat transfer or shaft work L and/or V Distillation difference in volatility V or L Pressure reduction or heat transfer L and/or V Equilibrium flash Separation principle Developed or added phase Separation agent Phase of the feed Separation Method
  • 10. Common Separation Methods difference in permeability and/or solubility Membrane Membrane L or V Membranes difference in adsorbabililty Solid Solid adsorbent L Liquid adsorption difference in adsorbabililty Solid Solid adsorbent V Gas adsorption Difference in solubility or m.p. Solid Heat transfer L Crystalli- zation Difference in solubility Second liquid Liquid solvent L Liquid-liquid Extraction Separation principle Developed or added phase Separation agent Phase of the feed Separation Method difference in permeability and/or solubility Membrane Membrane L or V Membranes difference in adsorbabililty Solid Solid adsorbent L Liquid adsorption difference in adsorbabililty Solid Solid adsorbent V Gas adsorption Difference in solubility or m.p. Solid Heat transfer L Crystalli- zation Difference in solubility Second liquid Liquid solvent L Liquid-liquid Extraction Separation principle Developed or added phase Separation agent Phase of the feed Separation Method
  • 11. Common Separation Methods Difference in volatility V Heat transfer S and L Drying Difference in solubility L Liquid solvent S Leaching Difference in solubility Supercritical fluid Supercritical solvent L or V Supercritical extraction Separation principle Developed or added phase Separation agent Phase of the feed Separation Method Difference in volatility V Heat transfer S and L Drying Difference in solubility L Liquid solvent S Leaching Difference in solubility Supercritical fluid Supercritical solvent L or V Supercritical extraction Separation principle Developed or added phase Separation agent Phase of the feed Separation Method
  • 12. Separation Method Selection • The development of a separation process requires the selection of:  Separation methods  ESAs and/or MSAs  Separation equipment  Optimal arrangement or sequencing of the equipment  Optimal operating temperature and pressure for the equipment • Selection of separation method depends on feed condition: • Vapor Partial condensation, distillation, absorption, adsorption, gas permeation (membranes) • Liquid Distillation, stripping, LL extraction, supercritical extraction, crystallization, adsorption, and dialysis or reverse osmosis (membranes) • Solid If wet  drying, if dry  leaching
  • 13. Separation Method Selection • The separation factor, SF, defines the degree of separation achievable between two key components of the feed. This factor, for separation of component 1 from component 2 between phases I & II, for a single stage of contacting, is: II II I I C C C C SF 2 1 2 1 / /  (8.1) C = composition variable, I, II = phases rich in components 1 and 2. • SF is generally limited by thermodynamic equilibrium. For example, in the case of distillation, using mole fractions as the composition variable and letting phase I be the vapor and phase II be the liquid, the limiting value of SF is given in terms of vapor-liquid equilibrium ratios (K-values) as: (8.2), (8.3)        1 1 1 1 1 2 2 2 2 2 for ideal L and V s , s y / x K P SF y / x K P
  • 14. Separation Method Selection • For vapor-liquid separation operations that use an MSA that causes the formation of a non-ideal liquid solution (e.g. extractive distillation): (8.5) s L s L P P SF 2 2 1 1 2 , 1      • If the MSA is used to create two liquid phases, such as in liquid- liquid extraction, the SF is referred to as the relative selectivity, β , where: I I II II SF 2 1 2 1 2 , 1 / /        (8.6) • In general, MSAs for extractive distillation and liquid-liquid extraction are selected according to their ease of recovery for recycle and to achieve relatively large values of SF.
  • 15. Equal Cost Separators Ref: Souders (1964) Extractive distillation should NOT be used when α for ordinary distillation is greater than 2 Liquid-Liquid Extraction should NOT be used when α for ordinary distillation is greater than 3.2
  • 16. Summary – Separation Trains  Be familiar with the more widely used industrial separation methods and their basis for separation.  Understand the concept of the separation factor and be able to select appropriate separation methods for liquid mixtures. On completion of this part, you should: