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LIQUID-LIQUID
EXTRACTION
An Introduction
45 Eisenhower Drive, Suite 350, Paramus, NJ 07652
| Te l : ( 2 0 1 ) 2 6 7- 8 6 7 0
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| www.modularprocess.com
WHO IS
?
Koch Modular Process Systems (KMPS) is a joint venture with KochGlitsch LP, one of the world's most prominent suppliers of mass
transfer equipment. Koch-Glitsch's parent company is Koch Industries,
one of the largest privately held corporations in the United States.
For over 20 years KMPS has successfully designed and constructed
mass transfer systems for the worldwide Chemical Processing
Industry. Our customer’s rely upon KMPS for our quality products and
technical expertise.
2
Hierarchy of Separation Technologies
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
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Typical Applications
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
When is it prudent to use extraction?
When you want to:
• Remove products and pollutants from dilute aqueous streams
• Wash polar compounds or acids/bases from organic streams
• Separate heat sensitive products
• Purify non-volatile materials
• Process azeotropic and close boiling mixtures
• Avoid a high cost distillation solution
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Industries Using Extraction Technology
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Chemical
•Washing of acids/bases, polar compounds from organics
•Recovery of valuable chemicals from aqueous solutions
Biochemical Processing
• Recovery of carboxylic acid from fermentation broths
• Recovery of valuable “oil” from algae broths
Effluent Treatment
• Recovery of phenol, DMF, DMAC
• Recovery of acetic acid from dilute solutions
Pharmaceuticals
• Recovery of active materials from fermentation broths
• Purification of vitamin products
Polymer Processing
• Recovery of caprolactam for nylon manufacture
• Separation of catalyst from reaction products
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Industries Using Extraction Technology
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Petroleum
• Lube oil quality improvement
• Separation of aromatics/aliphatics (BTX)
Food
• Decaffeination of coffee and tea
• Separation of essential oils (flavors and fragrances)
Metals
• Copper production
• Recovery of rare earth elements
Inorganic Chemicals
• Purification of phosphoric acid
Nuclear
• Purification of uranium
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Removal of Organics From Water:
Distillation vs. Extraction
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
BP [°C]
Water Solu.
[%]
Azeotrope
B.P. [°C]
Azeotrope
Water [%]
40
2.0
38.1
1.5
Acetone
56.2
Infinite
Non Azeotropic
< 50 ppb
Methanol
64.5
Infinite
Non Azeotropic
< 50 ppb
Benzene
80.1
0.18
69.4
8.9
< 50 ppb
Toluene
110.8
0.05
85.0
20.2
< 50 ppb
-21
Infinite
Formic Acid
100.8
Infinite
Acetic Acid
118.0
Infinite
Pyridine
115.5
57
92.6
43
< 10 ppm
Aniline
181.4
3.60
99.0
80.8
< 10 ppm
Phenol
181.4
8.20
99.5
90.8
< 10 ppm
Nitrobenzene
210.9
0.04
98.6
88.0
< 10 ppm
Dimethyl Acetamide
166.1
Infinite
Non Azeotropic
< 10 ppm
n-Methylpyrrolidone
202.0
Infinite
Non Azeotropic
< 10 ppm
Organic
Compound
Distillation
Methylene Chloride
Extraction
Formaldehyde
Non Azeotropic
107.1
Typical Reduction
Level
< 50 ppb
< 1,000 ppm
22.5
Non Azeotropic
< 500 ppm
< 500 ppm
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Simple Extraction Single Stage
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
A–0
Extract (E)
B – 50
C – 0.8
Feed (F)
50.8
A – 99
B–0
A – 99.0
C–1
B–0
100
A–0
C – 0.2
Raffinate (R)
B – 50
Solvent (S)
99.2
C–0
50
Fraction Unextracted
Distribution Coefficient
Extraction Factor
Solute in Raffinate 0.2

 0.2
Solute in Feed
1.0
0.8
Conc. Solute in Extract
50  7.92
M

Conc. Solute in Raffinate 0.2
99
E  S M   50 7.92  4.0
F
99
U
 


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Cross Flow Extraction
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
E1
E2
Feed
E3
R1
E4
R2
R3
F + S = M1
R1 + S = M2
R2 + S = M3
C
C
C
R4
R3 + S = M4
A+B
Solvent
Solvent
Solvent
C
B
Solvent
LEGEND
A, B
Components in feed
C
Component in solvent
Rx
Raffinate from stage x
Ex
Extract (made up of components B & C)
Mx
Composition of two phase mixture
F
R2
A
R3
R4
R1
M1
M2
M3
M4
E1
E2
E3
E4
C
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Countercurrent Flow Extraction
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
NOTE: Extract is made up
of components B and C
E1
E3
R2
R1
Feed
Solvent
C
R3
R4
A+B
E2
E4
B
A
Equations
F+S=M
E1 + R4 = M
F + S = E1 + R4
F – E1 = R4 – S = Δ
F
R1
A
E1
M
R2
R3
R4
E2
E E3
4
C
Δ
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Countercurrent Extraction
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
B+C
Feed (F)
Extract (E):
Solute Rich Stream
Primary Interface
A+B
Continuous Phase
Dispersed Phase
Solvent (S)
C
Raffinate (R):
Solute Lean Stream
A
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Bench Scale Test Apparatus
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Variable Speed Drive
Baffle
Thermometer
Tempered
Water Out
1 – Liter Flask
Tempered
Water In
Drain
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Simple Extraction
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Solute Free Basis
Graphical Solution
E’
𝑌𝐵𝐸
F’
𝑋𝐵𝐹 =
𝑋𝐵𝐹
𝑋𝐴𝐹
S’
𝑌𝐵𝑆 =
𝑦𝐵𝐹
𝑦𝐴𝑆 + 𝑦𝐶𝑆
𝑦𝐵𝐸
=
𝑦𝐴𝑅 + 𝑦𝐶𝐸
𝑋𝐵𝑅 =
R’
YBE
𝑥𝐵𝑅
𝑥𝐴𝑅 + 𝑥𝐶𝑅
Y
YBS
𝐹 ′ = 𝐹 𝑥𝐴𝑅
𝑆 ′ = 𝑆 𝑦𝐴𝑆 𝑦𝐶𝑆
𝐸 ′ = 𝐸 𝑦𝐴𝐸 𝑦𝐶𝐸
𝑅′ = 𝑅(𝑥𝐴𝑅 𝑥𝐶𝑅 )
XBR
𝑚=
𝑌𝐵 ∗
𝑋𝐵 ∗
X
XBF
Distribution Coefficient
on Solute Free Basis
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Typical LLE Equilibrium Curve
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Extract Comp. (Wt. Frac., Solute Free)
0.09
0.08
0.07
0.06
0.05
0.04
0.03
0.02
0.01
0.00
0.000
0.005
0.010
0.015
Raffinate Composition (Wt. Frac., Solute Free)
0.020
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Graphical Determination of Theoretical Stages
95% Solute Extraction, S/F = 1.0 mass basis
Extract Comp (Wt Frac., Solute Free)
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
(0.136, 0.114)
0.12
0.10
1
0.08
0.06
0.04
0.02
0.00
3
0.000
2
0.020
0.040
0.060
0.080
0.100
0.120
Raffinate Composition (Wt Frac., Solute Free)
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Graphical Determination of Theoretical Stages
98% Solute Extraction, S/F = 1.0 mass basis
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
(0.136, 0.118)
Extract Comp (Wt Frac., Solute Free)
0.12
0.10
1
0.08
0.06
0.04
0.02
6
5
0.00
0.000
4
2
3
0.020
0.040
0.060
0.080
0.100
Raffinate Composition (Wt Frac., Solute Free)
0.120
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Kremser Equation
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
n
Where: n
xf
xn
ys
m
E
=
=
=
=
=
=
ys 


x




m 1 1   1 
LOG  f
ys   E  E 
 xn  m 


LOG E
Number of theoretical stages required
Conc. of solute in feed on solute free basis
Conc. of solute in raffinate on solute free basis
Conc. of solute in solvent on solute free basis
Distribution coefficient
Extraction factor = (m)(S/F)
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Engineering Calculations
Kremser Type Plot
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
YBE
1.0
0.8
0.6
E’
E = 0.3
0.4
0.3
F’
XBR/XBF = Fraction Unextracted
0.2
XBF
S’
YBS
R’
XB
E: Extraction Factor
E = m (S’/F’)
0.1
0.08
0.06
0.04
0.03
0.02
0.01
0.008
0.006
0.004
0.003
0.002
0.001
0.0008
0.0006
0.0005
1
18
2
3 4 5
6 7 8 10 15 20
Number of Ideal Stages
Typical Extraction System
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
B+C+(A)
Feed
A+B
Solvent
Recovery
Raffinate
Stripping
Extraction
C
(A)
Solvent
C
(A+B)
A+(B+C)
A (B+C)
19
B (C)
C
(A+B)
Removal of Phenol from Wastewater
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Extract
Wastewater Feed
0.1 – 8 % Phenol
Solvent
Recovery
Raffinate
Stripping
Extraction
Recycled
Solvent
Steam
Raffinate
< 1 ppm Phenol
Biological Treatment
Or
Carbon Adsorption
ppb Phenol
Phenol
Recovery of Acetic Acid from Water
Using a Low Boiling Solvent
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Extract
Aqueous Feed
1 - 30 %
Acetic Acid
Solvent
Recovery
Raffinate
Stripping
Extraction
Recycled
Solvent
Typical Solvents:
Ethyl Acetate
MTBE
Steam
Raffinate
Acetic Acid
Aqueous Raffinate
21
Neutralization/Washing of Acid or Base
or Polar Compounds from Organic Stream
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Organic
Water
Extraction
Caustic (Mild)**
**Organic Feed could contain caustic.
Mid-Feed would be mild acid.
Feed (Organic + Acid) **
Water + Salts
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Series Extraction
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Feed
Extract
Solvent 1
B+C
C
Solvent 2
A+B
D
Extractor #2
Extractor #1
Raffinate
A
Extractor 1 & 2 May Differ In:
• Temperature
• pH
• Solvent
Product
B+D
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Recovery of Caprolactam
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Extract
Lactam Oil Phase
65 – 70% Caprolactam
Water
Re-Extraction
Reaction
Section
Ammonium Sulphate Phase
2 – 3% Caprolactam
Am. Sulphate Ext.
Lactam Oil Ext.
Feed From
Solvent
Raffinate
AQ Waste to
Discharge
24
Am. Sulph. Waste
to Discharge
Lactam Oil to
Recovery
Phosphoric Acid Extraction
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Recycle
Re-Extraction
Feed
Scrub Extraction
Phosphate Rock
Digester
Extraction
HCL
Water
Scrub Solv.
Solvent
Raffinate to
Disposal
25
Phosphoric Acid to
Recovery
Organo-Metallic Catalyst Recovery
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Organic
Cobalt
Catalyst
Preparation
Extraction
Slipstream
Feed
Organo-Metallic
Catalyst
Reactor
Separator
Water Effluent
(200 ppm Cobalt)
Makeup Organic
Water Effluent
(1 ppm Cobalt)
Product
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Fractional Extraction
Process Scheme
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
EI
YAE,YBE
S I2
XAS2,XBS
2
(A-Rich)
NR
F1I
XAF,XBF
NS
S 1I
XAS1,XBS1
RI
(B-Rich)
XAR,XBR
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Extraction of Flavors and Aromas
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Typical Products:
Orange Oil
Lemon Oil
Peppermint Oil
Cinnamon Oil
Aqueous Alcohol
Solvent 2
Distillation
Solvent 1
Distillation
Extraction
Essential Oil
Hydrocarbon
Oil
Essential
Extract
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Fractional LLE – Mixed Polymer Feed
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
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Major Types of Extraction Equipment
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Column
Contactors
Mixer Settlers
Used primarily in the metals
industry due to:
- Large flows
- Intense mixing
- Long Residence time
- Corrosive fluids
- History
Spray
Rarely used
Packed
Static
Tray
Centrifugal
Agitated
Pulsed
Used in:
- Refining
- Petrochemicals
Used in:
- Refining
- Petrochemicals
Used in:
- Nuclear
- Inorganics
- Chemicals
Example:
- Random
- Structured
- SMVPTM
Example:
- Sieve
Example:
- Packed
- Tray
- Disc & Donut
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
Used primarily in the
pharmaceutical industry due to:
- Low Volume
- Short Residence time
- Handles Small Gravity Diff.
- History
Rotary
Reciprocating
Used in:
- Chemicals
- Petrochemicals
- Refining
- Pharmaceutical
Example:
- RDC
- SCHEIBEL®
Example:
- KARR®
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Mix / Decant Tank
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Characteristics
• Mix – Settle – Phase separate in
a single tank
• Batch Processing only
• Requires multiple solvent
additions for more than one
stage (crossflow operation)
• Typically used for small capacity
operations or intermittent
processing
Feed Inlet
Sight Glass
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Outlet
31
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Mixer / Settlers
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Characteristics
•
•
Light Phase In
•
•
•
Heavy Phase Out
•
Handle very high flowrates
Good for processes with
relatively slow reactions
(residence time required)
Provide intense mixing to
promote mass transfer
Require large amount of floor
space
Suitable when few
theoretical stages required
Large solvent inventory (and
losses)
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Centrifugal Extractor
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Characteristics
•
•
•
•
•
•
Countercurrent flow via centrifugal
force
Low residence time ideally suited for
some pharmaceutical applications
Handles low density difference
between phases
Provide up to several theoretical
stages per unit
High speed device requires
maintenance
Susceptible to fouling and plugging
due to small clearances
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Packed Column
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Extract (E)
Characteristics
•
Feed (F)
•
•
•
•
•
Solvent (S)
Raffinate (R)
•
High capacity:
20-30 M3/M2-hr (Random)
500-750 gal/ft2-hr (Random)
40-80 M3/M2-hr (Structured)
1,000-2,000 gal/ft2-hr (Structured)
Poor efficiency due to backmixing and
wetting
Limited turndown flexibility
Affected by changes in wetting
characteristics
Limited as to which phase can be dispersed
Requires low interfacial tension for
economic usefulness
Not good for fouling service
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Sieve Tray Column
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Feed (F)
Extract (E)
Primary
Interface
Characteristics
• High capacity: 30-50 M3/M2-hr
750-1,250 gal/ft2-hr
• Good efficiency due to minimum backmixing
• Multiple interfaces can be a problem
• Limited turndown flexibility
• Affected by changes in wetting
characteristics
• Limited as to which phase can be
dispersed
Solvent (S)
Raffinate (R)
• Not effective for high interfacial tension
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RDC Extractor
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Characteristics
• Reasonable capacity:
20-30 M3/M2-hr
Drive Motor
Gearbox
Light
Phase Out
Heavy
Phase In
• Limited efficiency due to
axial backmixing
• Suitable for viscous
materials
Vessel
Walls
Shaft
Stators
Rotors
• Suitable for fouling
materials
• Sensitive to emulsions due
to high shear mixing
Light
Phase In
Interface
• Reasonable turndown
(40%)
36
Heavy
Phase Out
Interface
Control
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SCHEIBEL® Column
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Characteristics
• Reasonable capacity:
15-25 M3/M2-hr
350-600 gal/ft2-hr
Variable Speed
Drive
Light
Phase Out
Heavy
Phase In
Rotating
Shaft
Horizontal
Vessel
Outer Baffle
Walls
• High efficiency due to
internal baffling
• Good turndown capability
(4:1) and high flexibility
• Best suited when many
stages are required
• Not recommended for
highly fouling systems or
systems that tend to
emulsify
Light
Phase In
Turbine
Impeller
Interface
Horizontal
Inner Baffle
Interface
Control
Heavy
Phase Out
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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Telephone: (201) 267-8670
SCHEIBEL® Column Internal Assembly
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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KARR® Reciprocating Column
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Drive
Assembly
Light
Phase Out
Characteristics
Heavy
Phase Inlet
• Highest capacity:
30-60 M3/M2-hr
750-1,500 gal/ft2-hr
Sparger
• Good efficiency
• Good turndown capability (4:1)
Perforated
Plate
Light
Phase Inlet
Tie Rods
& Spacers
• Uniform shear mixing
Baffle Plate
• Best suited for systems that emulsify
Sparger
Interface
Control
Interface
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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Heavy
Phase Out
39
Telephone: (201) 267-8670
KARR® Column Plate Stack Assembly
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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Telephone: (201) 267-8670
Comparing Commercial Extractors
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
20
SCHEIBEL
Efficiency / Stages per Meter
10
6
RZE
Graesser
KARR
PFK
4
PSE
RDC
2
1
Key
Kuhni
FK
MS
SE
.06
0.4
Graesser = Raining Bucket
MS = Mixer Settler
SE = Sieve Plate
FK = Random Packed
PFK = Pulsed Packed
PSE = Pulsed Sieve Plate
RDC = Rotating Disc Contactor
RZE = Agitated Cell
KARR = KARR® Recipr. Plate
Kuhni = Kuhni Column
SCHEIBEL = SCHEIBEL® Col.
0.2
1
2
4 6 10
Capacity M3/(M2 HR)
20
40 60 100
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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Telephone: (201) 267-8670
Column Selection Criteria
Static Column
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
A static column design may be appropriate when:
• Interfacial tension is low to medium: up to 1015 dynes/cm
• Only a few theoretical stages are required, and
reduction in S/F is not an economic benefit
• No operational flexibility required
• There is a large difference in solvent to feed
rates
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Telephone: (201) 267-8670
Column Selection Criteria
Agitated Column
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Agitated columns are generally more economical
when:
• More than 2-3 theoretical stages are required
• Interfacial tension is moderate to high, although
low interfacial tensions may also be economical
• A reduction in solvent usage is beneficial to the
process economics
• The process requires a wide turndown as well as
the ability to handle a range of S/F ratios
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Telephone: (201) 267-8670
Column Selection Criteria
SCHEIBEL® Column
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
•
•
•
Systems that require a large number of stages
due to either theoretical stage requirements or
low mass transfer rates
Low volume applications in which a relatively
small column is required
Systems that process relatively easily, without a
tendency to emulsify and/or flood
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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Telephone: (201) 267-8670
Column Selection Criteria
KARR® Reciprocation Plate Column
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
•
•
•
•
Difficult systems that tend to emulsify and/or
flood easily
Systems in which the hydraulic behavior varies
significantly through length of the column
Sometimes requiring non-metallic internals,
such as Teflon due to wetting characteristics or
corrosive materials
Fouling applications that may have tars
formations and/or solids precipitation
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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Telephone: (201) 267-8670
3 Cornerstones of Successful Extraction
Applications
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Successful
Application
Proper Solvent
Selection
Meaningful
Pilot Tests
Accurate
Scale-Up
Scale-Up Based on:
Selection Based on:
Testing Based on:
• Sound thermodynamic principles
• Sound economic principles
• Availability
• Recoverability
• Sound environmental principles
• Toxicity
• Safety
• Actual feed stocks
• Full process including
solvent recovery
• Wide range of operating
conditions
• Proven techniques
• Proper safety factors
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Telephone: (201) 267-8670
Solvent Selection
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
•
Literature – DECHEMA, Perry’s
Chemical Engineers Handbook
•
•
Internet search
•
Experience – consulting with
experts
•
Laboratory Experiments:
Understanding the chemistry of
the process
1.
Quickly screen solvents
2.
Generate equilibrium data
3.
Observe phase behavior
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Liquid-Liquid Extraction Scale-Up
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Theoretical scale-up is difficult due to
Complex processes occurring in an extractor
• Coalescing / Wetting Characteristics
• Interfacial and Drop Turbulence Effects
• Axial and Radial Mixing
• Tendency to Emulsify
• Phase Ratio Variability and Density Gradients
• Effects of Impurities or Solids
• Mass Transfer Rate
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Liquid-Liquid Extraction Scale-Up
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Best method of design:
Pilot testing followed by empirical scale-up
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Pilot Plant Configuration
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Determine type of column to be used based on process considerations
Use the same kind of equipment for the production unit
Determine diameter and height of pilot column based on experience
Table 1: Smallest Possible Column for Testing
Type of Column
Packed
Tray
Diameter
3” to 4”
≥ 6”
Height
3’ to 6’ per Theoretical Stage (TS)
4 to 5 Trays per TS
KARR®
1”
1’ to 3’ per TS
SCHEIBEL®
3”
3 to 6 Actual Stages per TS (Approx. 3” to 6”)
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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Telephone: (201) 267-8670
Continuous Extraction Pilot Plant
Arrangement
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Extract
Hot Oil
Raffinate
Feed
Solvent
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Telephone: (201) 267-8670
KMPS Pilot Plant Services Group
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
KMPS maintains a pilot plant dedicated to
extraction R & D and applications testing
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Which Phase is Continuous?
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Solvent is Light Phase
B+C
E
F
F
Primary
Interface
A+B
Solvent
Dispersed
S
Solvent is Heavy Phase
A+B
Solvent
Continuous
S
C
A
A
S
E
B+C
R
Primary
Interface
F
A+B
R
A
A
S
Solvent
Dispersed
C
R
C
Primary
Interface
R
C
Primary
Interface
Solvent
Continuous
F
A+B
E
B+C
E
B+C
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Determining the Dispersed Phase
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Flow Rate (Phase Ratio)
• For Sieve Tray and Packed Columns – disperse the higher flowing phase
• For Agitated Columns – disperse lower flowing phase
Viscosity
• For efficiency – disperse less viscous phase
Viscous drop
Diffusion rate inside the drop is
inhibited by viscosity
• For capacity – disperse more viscous phase
Viscous continuous phase
Drop rise or fall will
be inhibited
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Telephone: (201) 267-8670
Determining the Dispersed Phase
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Surface Wetting
• Want the continuous phase to preferentially wet the internals – this
minimizes coalescence and therefore maximizes interfacial area.
Droplets coalesce.
Interfacial area lost.
Droplets retain shape.
Maximizes interfacial area.
Importance of maintaining droplets
Assume – 30% holdup of dispersed phase in 1 M3 of solution
Droplet
Droplet
Diameter [m] Volume [M3]
Number
Droplets
Droplet SA
[M2]
Interfacial Area
[M2/M3]
100
0.3
7.16x1010
1.26x10-7
9022
300
0.3
2.65x109
1.13x10-6
2995
500
0.3
5.73x108
3.14x10-6
1796
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Determining the Dispersed Phase
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Marangoni Effect
• Coalescence is enhanced by mass transfer from
droplets
continuous phase
Mass Transfer Direction
C
A+B
A+B
C
A+B
C+B
Continuous
c)
• Droplets tend to coalesce
• Must be counteracted by additional energy
A
C
Dispersed
(d
C+B
Continuous
(c
Dispersed
d)
• Droplets tend to repel each other
• Less energy required to maintain dispersion
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Interface Behavior
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Solids build up at the interface =
Rag Layer
Rag
Layer
Emulsion band builds up at interface
due to slow phase separation
Rag
Layer
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Rag Layer or Emulsion Band
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Corrective Action
1. Reverse Phases
2. For Emulsion Band: slow down capacity or reduce agitation speed
3. For Rag Layer: circulate liquid through an external filter
Filter
Feed
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Entrainment
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Entrainment refers to removing a small portion of one phase out of the wrong end of the
column i.e. where the other phase exits. Entrainment is controlled by:
1.) Increased settling time inside the column
2.) Coalescer inside the column
3.) Coalescer external to the column
E
E
E
E
F
1
S
F
F
F
OR
2
OR
S
S
S
3
R
R
R
R
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Flooding
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Flooding – the point where the upward or downward flow of the dispersed phase ceases
and a second interface is formed in the column
Flooding can be caused by:
• Increased continuous phase flow rate which increases drag on droplets
f
Primary Interface
F2 > F1
f
Primary Interface
E
E
F1
F2
Second
Interface
S
S
R
R
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Flooding
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Flooding can be caused by:
• Increased agitation speed which forms smaller droplets which cannot overcome
flow of the continuous phase
• Decreased interfacial tension – forms smaller drops – same effect as increased
agitation
f1
Primary Interface
f2 > f1
f2
Primary Interface
E
E
F1
F2
Second
Interface
S
S
R
R
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Telephone: (201) 267-8670
Pilot Plant Testing
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Column Selection Based Upon:
1.
Process Criteria
2.
Physical/Chemical Properties
3.
Laboratory Work
4.
Experience
Test Method
1.
Experimental Design
2.
Step-by-Step Optimization
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Agitated Column Testing
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
•
•
Set-up column (multiple inlets)
•
Select initial operating conditions
(capacity – S/F – No. Stages)
•
Operate at increasing agitation
speed (flooding)
•
Based on results, vary:
Select continuous and dispersed
phases
1.
Continuous phase
2.
S/F vs No. Stages
3.
Capacity
4.
Other Variables
(temp, pH, etc.)
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Static Column Testing
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
•
•
Set-up column (multiple inlets)
•
Select initial operating conditions
(capacity – S/F – height)
•
•
Operate 3 different capacities
Select continuous and dispersed
phases
Based on results, vary:
1.
Continuous phase
2.
S/F vs Column Height
3.
Other Variables
(temp, pH, etc.)
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Extractor Flow Patterns
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Ideal Plug Flow
Y
Actual Flow
Y
X
X
This “axial” or “back” mixing causes concentration gradients that
decrease driving force and therefore increase HETS
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Generalized Scale-up Procedure
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Pilot Scale
f2
f1
Q2
Q1
Feed Rate
Feed Rate
H1
D1
Basic Scale-up Relationships:
D2/D1 = K1(Q2/Q1 )^M1
H2/H1 = K2(D2/D1 )^M2
f2/f1 = K3(D2/D1)^M3
D2
Where:
K1, M1 = Capacity Scale-up Factors
K2, M2 = Efficiency Scale-up Factors
K3, M3 = Power Scale-up Factors
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Application – SCHEIBEL® Column
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
• Extraction of nitrated organics from spent acid stream
using an organic solvent
• Reduce nitrated organic compounds from 3.9% to less
than 50 ppm
• S/F ratio fixed by process at 3.9
• Equilibrium data indicated that 4.5 theoretical stages
required
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
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SCHEIBEL® Column Pilot Plant Setup
Nitrated Organics Extraction
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Interface
Variable Speed
Drive
Hot Oil
Organic
Extract
Spent Acid
Feed
Aqueous
Raffinate
MCB
Solvent
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KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
68
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SCHEIBEL® Column
Nitrated Organics Extraction
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Column designed based upon results from the
pilot plant tests:
D1
A
B
•Diameter = 14” (D1)
• Expanded Head Diameter = 20” (D2)
• Bed Height = 9’-6” (A)
• Overall Height = 16’-4” (B)
D2
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Application 2 - Recovery of Carboxylic Acids
from Fermentation Broth
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Broth generated from cellulosic materials – approx. 5% acids
LLE Goal: To achieve >95% recovery (high purity) and minimize solvent usage
Ethyl acetate selected solvent – but emulsified easily
Preliminary Data in RDC Columns
Difficult operation due to emulsification
< 90% acid recovery
High S/F ratio – 2.0
KARR® Column Required
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Pilot KARR® Column for Carboxylic Acids
1” diameter x 12’ Plate Stack
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
Variable Speed Drive
Organic Out (Extract Phase)
Hot Oil
Aqueous Out
(Raffinate)
Whole Broth Feed
Ethyl Acetate
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Results from Extraction Testing
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
• Process successfully tested in KARR® Column and data generated for
scale-up
• KARR® Column is the correct design for this process which failed in RDC
column
• S/F ratio improved to 1.5 (client expected 2)
• 96-97% recovery at room temperature and 98-99% recovery at 40-45 C
• Complete system (LLE + distillations) designed, fabricated, and installed
• LLE testing identified “unknown” component
www.modularprocess.com
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
72
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KARR® Column Design
Carboxylic Acid Extraction from Broth
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
• Diameter = 22” (D1)
• Expanded Ends
Diameter = 44” (D2)
• Plate Stack = 38’-0” (A)
• Overall Height = 50’-6” (B)
D1
A
B
D2
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Application - Aromatic Purification by
Fractional Liquid-Liquid Extraction
MO D U L A R P R O C E SS S Y S T EMS | D I S T I L L ATI O N | L I Q U I D E XT R A C T I O N | E N G I N EER I NG | P I L O T T E S T I NG
•Light tar feed with polar aromatics (product) and non-aromatic impurities
•>90% recovery; 1% impurities
•Polar solvent for aromatics
•Alkane for non-polar impurities
•Preliminary Data in RDC Columns
Many extraction stages
High ratio of non-polar to polar solvent
Significantly more non-polar solvent stages required
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PFD - Pilot Plant Setup: Aromatic
Purification by Fractional Extraction
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Stage 99
Stage 77
Stage 65
Stage 53
Stage 42
Mixed
Polar
Solvent
Organic
Feed
Non-Polar
Solvent
(Alkane)
Stage 0
Extract Raffinate
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Telephone: (201) 267-8670
Fraction Extraction Test Variables
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65-99 agitated stages
12-34 stages above feed
42-65 stages below feed
Capacity 21 – 25.5 m3/m2 hr
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Polar solvent to feed ranged between 0.5: 1 and 1.4 : 1
Non-polar solvent to feed ranged between 1.1:1 and 3:1
Agitation speed 400-850 RPM
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Telephone: (201) 267-8670
Aromatic Purification
Final Results – Design Basis
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Scale-up design:
Diameter 1778 mm (70”)
Height
65 Agitated stages
Feed
Stage 13 from top
Polar solvent: Feed 0.7: 1.0
Non-Polar: Feed 1.8: 1.0
Internals = Variable Impeller Diameters
94% recovery with <1.0% impurities
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Telephone: (201) 267-8670
www.modularprocess.com
Telephone: (201) 267-8670
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Alcohol Extraction from Acrylates
Extraction of methanol from an acrylate stream using water
as the solvent
Reduce methanol from 2.5% to less than 0.1%
S/F ratio specified by client as 0.32 wt. basis
Equilibrium data: distribution coefficient generated by
KMPS, with average value of 5.3
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KARR® Column Pilot Plant Setup
Alcohol Extraction from Acrylates
KARR® Column
1” Dia. x 8’ Plate Stack
Variable
Speed Drive
Variable Plate Spacing
Hot Oil
Raffinate
(Acrylate Phase)
Water
Feed
Extraction Technology Group
www.modularprocess.com
Extract
(H2O + Alcohol)
Acrylate Feed
(methyl or ethyl)
Interface
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
KARR® Column Pilot Plant Scale-up
Methanol Extraction from Acrylate
• Diameter = 45” (D1)
• Expanded Head Diameter = 68” (D2)
• Plate Stack = 26’-0” (A)
• Overall Height = 36’-8” (B)
D1
A
B
D2
Extraction Technology Group
www.modularprocess.com
KARR® and SCHEIBEL® are registered trademarks of Koch-Glitsch, LP.
Extraction Experience
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KMPS has supplied over 300
commercial extraction columns
KMPS has also supplied hundreds of
pilot scale extraction columns
We have tested more than 200
different processes in the pilot plant
QUESTIONS?
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Telephone: (201) 267-8670