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Chapter 1. Separation Processes
2012. 1
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Energy Consumption /.
/.
: enantiomerically pure components
Softenon : (R-enantiomer), (S-enantiomer)
Aspartame : (S, S) , (R, R) Limonen : (S), (R)
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Separations
Separations Enrichment
Concentration
Purification
Refining
Isolation
Separations are important to chemist andchemical engineers Chemist : Small scale (Analytical separation methods)
Chemical Engineers : Economical, large scale methods
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Industrial Chemical Processes
Natural raw material
Plant or animal matter
Chemical intermediate
Chemicals of commerce
Waste products
Feed
Batchwise
Continuous
Semicontinuous
Mode of Operation
Key Operation
Reaction
Separation
Auxiliary Operation
Heat / Work
Mixing, Dividing
Size reduction
Operation
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Hypothetical vs. Industrial Processes
Simple ,hypotheticalprocess is not possible
Impurities in the feed
Side Reactions
Separation processes areimportant in real industrialapplication
5
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Mechanism of Separation
Mixing : Spontaneous, natural process
Separation : Not spontaneous process
Require energy (heat / work)
Question : Why ?
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General Separation Technique
Separation by Phase Creation Energy (heat/work) ,
Separation by Phase Addition 3 (MSA : Mass Separating Agent)
Separation by Barrier Barrier (membrane)
Separation by Solid Agent ,
Separation by Force Field or Gradient ,, ,
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Classification of Separation Techniques
8
Barrier
Force fieldor gradient
Feed
Phase 1
Phase 2
(i) By Phase Creation
Feed
Phase 1
Phase 2
Feed
Phase 1
Phase 2
Feed
Phase 1
Phase 2
Feed
Phase 1
Phase 2
(ii) By Phase Addition
(iii ) By Barrier
(iV) By Solid Agent (Vi) By Force Field or Gradient
MSA
Mass SeparatingAgent
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Driving Force of Separation :Gradient of Concentration
Rate of Separation : how fast ? Governed bymass transfer
Extent of Separation : how far ?
Limited bythermodynamics
Properties of ImportanceMolecular Properties Thermodynamic and Transport Properties
Molecular Weight
Van der Waals Volume
Van der Waals Area
Molecular Shape (Accentric Factor)
Dipole Moment
Polarizability
Dielectric Constant
Electric Charge
Radius of Gyration
Vapor Pressure
Solubility
Adsorptivity
Diffusivity
9
Handbooks
Journals
Electronic Databases
Commercial Process Simulators
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Separation By Phase Addition or Creation -1
1
V/L
V
L
V/L
V
L
Partial Condensation or Vaporization Flash Vaporization
(Heat Transfer) (Pressure Reduction)
ESA
(Energy-Separating Agent)
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Separation By Phase Addition or Creation - 2
1
V/L
L
L
Distillation
(Heat transfer (ESA) or sometimes work transfer)
When the volatility difference
among species are not sufficiently
large
Most widely used industrial
separation technique
Multiple contact between counter
current flow of V/L in trays (stages) .
Rectifying section
Stripping section
Condenser
Reboiler
Reflux
Reboil
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Distillation Tower
1
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Separation By Phase Addition or Creation - 3
13
V/L
L
L
Azeotropic Distillation
Liquid entrainer (MSA)
and Heat Transfer (ESA)
Recycle MSA
Makeup MSA
Recovery of acetic acid from water
using n-butyl acetate
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Separation By Phase Addition or Creation - 4
1
MSA (L)
L1
L2
L1
LiquidLiquid Extraction
Liquid solvent(MSA)
Recovery of Aromatics
MSA2 (L)
L
L
L
Liquid-Liquid Extraction
(Two Solvent)
Use of Propane and Cresylic acid as solvents to separate
paraffins from aromatics and naphthenes
MSA1 (L)
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Separation By Phase Addition or Creation - 5
1
Drying Evaporation Crystallization Desublimation
V (V)
L/(S) S
V
L
(V)
L L
S
V
S
LV
Removal of water from PVCEvaporationof water from
Water + Urea
Crystallization op-Xylenefrom m-Xylene
Recovery ofphthalic anhydride
Heat transfer (ESA)
Heat transfer (ESA) Heat transfer (ESA) Heat transfer (ESA)
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Crystallizer
1
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Separation By Phase Addition or Creation - 6
1
Leaching (Liquid-Solid Extraction) Foam Fractionation
S
MSA (L)
S
L
L
MSA (g)
L (foam)
V
L
Extraction of sugar using hot water
Liquid Solvent
Recovery of detergent from water soln.
Gas Bubbles (MSA)
Detergent tend torise with gas bubble
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Separation by barrier
Use of microporous / nonporousmembrane as semipermeable
barriers
Membranes Natural fibers
Synthetic polymers Ceramics
Metals
Liquid films
Fabrications Flat sheets
Hollow fibers Spiral-wound sheets
18
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Separation by barrier - 2
2
Microfiltration Ultrafilration Pervaporation
L
L
L
L
V
Microporous membrane Microporous membrane Nonporous membrane
Pressure gradient Pressure Gradient Pressure Gradient
Separation of whey from
cheese
Separation of azeotropic
mixtures
L
L
L
Removal of bacterial
From drinking water
L
0.02-10 mm 1 20 nm
solventsolvent gas (evaporation)
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Separation by barrier - 3
2
Gas permeationLiquid Membrane
V
V
V
V/L
V/L
Nonporous membraneLiquid membrane
Pressure Gradient Pressure Gradient
Hydrogen enrichment Removal of hydrogen sulfide
V/L
gas
Gas mixture
Liquid layer
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Liquid Membrane
2
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Separation by solid agent
Solid mass separating agent
Granular material or packing
Saturation Periodical regeneration required
Batchwise or semicontinuous operation
23
Molecular sieve Silica gel
pore
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Separation by solid agent
2
Adsorption Chromatography Ion Exchange
Solid Adsorbent Solid adsorbent or liquid
Adsorbent on solid support
Resin with ion-active sites
Separation of xylene isomers
and ethylbenzene
Demineralization of water
Purification of
p-xylene
V/L
V/L
V/L V/L
V/L
L
L
L
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Separation by solid agent
Adsorption Adsorbent
Activated carbon
Aluminum oxide
Silica gel
Zeolite adsorbents (Molecularsieve)
Adsorption / Regeneration
Regeneration methods Thermal Swing (TSA)
Pressure Swing (PSA)
Inert purge stripping Displacement desorption
25
Hydrogen PSA Units
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Separation by external field or gradient
Separation operation Initial or Feed Phase Force field or gradient Industrial Example
Centrifugation Vapor Centrifugal force Separation of Uranium
isotope
Thermal diffusion Vapor or liquid Thermal gradient Separation of chlorine
isotope
Electrolysis Liquid Electrical force field Concentration of
heavy water
Electrodialysis Liquid Electrical force field
and membrane
Desalinization of sea
water
Electrophoresis Liquid Electrical force field Recovery of
hemicelluose
Field-flow
fractionaltion
Liquid Laminar flow in force
field
26
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Centrifugation
27
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Electrodialysis
2
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Electrophoresis ()
2
Using different migration velocities of charged colloidal orsuspended species in a electrical field
Application : Biochemicals
Fi ld Fl S ti
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Field Flow SeparationField Flow Fractionation (FFF)
3
Micromolecular andcolloidal materials
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Component Recoveries and Product Purity
Separation process
No reaction
Continuous and steady state
i : 1 ~ C Number of Components
p : 1~ NProduct phases
F : feed
)()1()3()2()1(
1
)()(
...N
i
N
iiii
N
p
p
i
F
i nnnnnnn
31
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Example Hydrocarbon Recovery Plant
3
Purpose :Production of polymers
- PP- PB.
S li F i d S li R i
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Split Fraction and Split Ratio
Split fraction ( 0 1)
Split ratio ( 0 very large value)
)(
,
)1(
,
, F
ki
ki
ki
n
nSF
)1( ,
,
)2(
,
)1(,
,
ki
ki
ki
ki
ki
SF
SF
n
nSR
33
i : component
k : separator
(F) : feed
(1) : f ir st product (ex: top product)
(2) : second product (ex : bottom product)
i product /feed
i top / bottom
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Separation Power
)1/()1(
/
/
/)2()1(
)2()1(
,
ji
ji
j
i
jj
iiji
SFSF
SFSF
SR
SR
CC
CCSP
Key-component split Column SP
Separation Power
nC4H10 / iC5H12 C1 137.1
C3H8/iC4H10 C2 7103
iC4H10/nC4H10 C3 377.6
34
S l i f ibl S i
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Selection of Feasible Separation
Selection of a best separation processes Selection among a number of feasible candidates
Two or more operations may be the best
Important Factors that influence the selectionof feasible separation operations
Feed conditions
Product conditions
Property differences
Characteristics of separation3
F h I fl h S l i f F ibl
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Factors that Influence the Selection of FeasibleSeparation Operation
Feed condition Compositions
Flow rate
Temperature
Pressure
Phase state
Product conditions Required purities of products
Temperatures
Pressures
Phase states
Property differences Molecular
Thermodynamic
Transport
Characteristics of separationoperation
Ease of scale-upEase of staging
T, P, Phase-state requirements
Physical size limiation
Energy requirement
36
Most important
Can be altered by pump,
Compressor, heat exchangers,
Technological and Use Maturity of Separation
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Technological and Use Maturity of SeparationProcesses
3
SeparationBy Barrier
Separation bySolid agent
Creation of Addition ofSecond Phase Cheap
Expensive
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