Liquid-Liquid Extraction

Hierarchy of Separation Technologies

Physical Separations
Decantation, Coalescing, Filtration, Demisting

Easy

Evaporation
Single Effect, Multiple Effect

Distillation
Simple, Azeotropic, Extractive, Reactive

Extraction
Simple, Fractional, Reactive

Difficulty
Of
Separation

Adsorption
Pressure Swing, Temperature Swing

Crystallization
Melt, Solvent

Membranes
MF, UF, NF, RO

Difficult

Typical Applications

Remove products and pollutants from dilute aqueous streams

Wash polar compounds or acids/bases from organic streams
Heat sensitive products
Non-volatile materials
Azeotropic and close boiling mixtures
Alternative to high cost distillations

Extraction is Used in a Wide

Variety of Industries
Chemical

Washing of acids/bases, polar compounds from organics

Pharmaceuticals

Recovery of active materials from fermentation broths

Purification of vitamin products

Effluent Treatment

Recovery of phenol, DMF, DMAC

Recovery of acetic acid from dilute solutions

Polymer Processing

Recovery of caprolactam for nylon manufacture

Separation of catalyst from reaction products

Petroleum

Lube oil quality improvement

Separation of aromatics/aliphatics (BTX)

Petrochemicals

Separation of olefins/parafins
Separation of structural isomers

Food Industry

Decaffeination of coffee and tea

Separation of essential oils (flavors and fragrances)

Metals Industry

Copper production
Recovery of rare earth elements

Inorganic Chemicals

Purification of phosphoric acid

Nuclear Industry

Purification of uranium

Removal of Organics From Water

Distillation vs. Extraction
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

Dinitrotoluene (2,4)

300.0

0.03

99 100

> 90

< 10 ppm

Dimethyl Formamide

153.0

Infinite

Non Azeotropic

< 10 ppm

Dimethyl Acetamide

166.1

Infinite

Non Azeotropic

< 10 ppm

n-Methylpyrrolidone

202.0

Infinite

Non Azeotropic

< 10 ppm

Distillation

Organic Compound
Methylene Chloride

Extraction

Formaldehyde

Non Azeotropic
107.1

22.5

Non Azeotropic

Typical
Reduction Level
< 50 ppb

< 1,000 ppm

< 500 ppm
< 500 ppm

Simple Extraction Single Stage

Extract (E)
A0
B 50

Feed (F)

C 0.8
50.8

A 99
B0
C1
100

A0

Raffinate (R)

B 50

A 99.0
B0
C 0.2

C0

99.2

50

Solvent (S)
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

Cross Flow Extraction

E1

E2
B+C

A+B
F

E3
B+C

R1

B+C

R2

C
F + S = M1

B+C

R3

C
R1 + S = M 2

E4

R4

C
B

R2 + S = M 3

R3 + S = M 4

F
R2

R3
R4

R1

M1
M2
M3
M4

E1

E2

E3
E4

Countercurrent Flow Extraction

E1
B+C
A+B
F

B+C

R1

R2
B+C

E3

R3

E2

R4
B+C

E4

Equations
F+S=M
E1 + R 4 = M
F + S = E1 + R4
F E1 = R4 S =

F
R1
R2

R3
R4

E1

E2
E3

E4

S C

Countercurrent Extraction
B+C

Feed (F)

A+B

Extract (E):
Solute Rich Stream
Primary Interface
Continuous Phase

Dispersed Phase

Solvent (S)

Raffinate (R):
Solute Lean Stream

Bench Scale Test Apparatus

Variable Speed Drive
Baffle

Thermometer

Tempered
Water Out

1 Liter Flask

Tempered
Water In
Drain

Simple Extraction
Solute Free
Basis

S
yAS
yBS
yCS
1.0

SI
R
xAR
xBR
xCR
1.0

YBE
m

XBF = xBF
xAF

YBE = yBE
yAR+ yCE

Sl
op
e

FI

->

xAS
xBF
1.0

yAE
yBE
yCE
1.0

C
ur
ve

EI

Graphical
Solution

YBS = yBF
yAS+ yCS

RI
XBR = xBR
xAR+ xCR

FI=F(xAR)
SI=S(yAS+yCS)
EI=E(yAE+yCE)
RI=R(xAR+xCR)

Eq
ui
lib
riu
m

Process
Scheme

YBS
XBR
m = YB*
XB*

g
in
at
r
e
Op

ne
Li

->

e
op
Sl

I
I S
/
F

XBF

Distribution Coefficient
on Solute Free Basis

Extract Composition (Wt Fract., Solute Free)

Typical LLE Equilibrium Curve

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 Fract., Solute Free)

0.020

Graphical Determination of Theoretical Stages

Extract Composition (Wt Fract., Solute Free)

95% Solute Extraction, S/F = 1.0 mass basis

(0.136, 0.114)
0.12

0.10

1
0.08

0.06

0.04

0.02

2
0.00
0.000

0.020

0.040

0.060

0.080

0.100

Raffinate Composition (Wt Fract., Solute Free)

0.120

Graphical Determination of Theoretical Stages

Extract Composition (Wt Fract., Solute Free)

98% Solute Extraction, S/F = 1.0 mass basis

(0.136, 0.118)

0.12

0.10

1
0.08

0.06

0.04

0.02

6
0.00
0.000

2
3
0.020

0.040

0.060

0.080

0.100

Raffinate Composition (Wt Fract., Solute Free)

0.120

Kremser Equation

n
Where: n
xf
xn
ys
m
E

=
=
=
=
=
=

x f s m
1 1
LOG
1

y
E E
xn s

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)

Engineering Calculations
Kremser Type Plot
YBE

E1

1.0
0.8
0.6

F1

E = 0.3

XBF

0.04
0.03
0.02

1.
3

E = Extraction Factor
E = m (S1/F1)

0.1
0.08
0.06

0.01
0.008
0.006
0.004
0.003
0.002

0
E=2

XBR

R1

0.2

YBS

0.3

S1

XBR/XBF = Fraction Unextracted

0.4

0.001
0.0008
0.0006
0.0005

4 5

7 8 10 15 20

Number of Ideal Stages

Typical Extraction System

Feed

B+C+(A)

A+B

Solvent
Recovery

Raffinate
Stripping

C
(A+B)

Extraction

Solvent

C
(A)

A+(B+C)

A (B+C)

B (C)

C
(A+B)

Removal of Phenol from Wastewater

Extract
Wastewater Feed
0.1 8 % Phenol

Solvent
Recovery

Raffinate
Stripping

Extraction

Recycled
Solvent

Raffinate

< 1 ppm Phenol

Biological Treatment
Or
Carbon Adsorption

ppb Phenol

Phenol

Recovery of Acetic Acid from Water

Using a Low Boiling Solvent

Extract
Aqueous Feed
20 - 40 %
Acetic Acid

Solvent
Recovery

Raffinate
Stripping

Extraction

Recycled
Solvent

Typical Solvents:
Ethyl Acetate
Butyl Acetate

Raffinate

Aqueous Raffinate

Acetic Acid

Recovery of Carboxylic Acids from Wastewater

Using a High Boiling Point Solvent
Formic Acid
99%+ Purity

Water

Water Feed
0.1 5 %
Mixed Acids

Acid
Recovery

Solvent
Recovery

Dehydration

Extraction
Raffinate
< 1,000 ppb
Mixed Acids

Recovered Solvent
Clean Up

Acetic Acid
99%+ Purity

Neutralization/Washing of Acid or Base

or Polar Compounds from Organic Stream

Organic
Water

Extraction

Caustic (Mild)**

Feed (Organic + Acid) **

Water + Salts

** Organic Feed could

contain caustic. MidFeed would be mild acid.

Series Extraction

Feed

Extract

Solvent 1

B+C

Solvent 2

A+B

Extractor 1 & 2 May Differ By:

- Temperature
- pH
- Solvent

Extractor #2

Extractor #1
Raffinate
A

Product
B+D

Recovery of Caprolactam
Extract

Lactam Oil Phase

65 70% Caprolactam

Water

Raffinate

AQ Waste
to
Discharge

Re-Extraction

Reaction
Section

Ammonium Sulphate Phase

2 3% Caprolactam

Am. Sulphate Ext.

Lactam Oil Ext.

Feed From

Solvent

Am. Sulph.
Waste to
Discharge

Lactam Oil
to
Recovery

Phosphoric Acid Purification via Extraction

Recycle

Re-Extraction

Scrub Extraction

Feed

Extraction

HCL

Phosphate
Rock
Digester

Water

Scrub Solv.

Raffinate
to Disposal

Solvent

Phosphoric
Acid to
Recovery

Organo-Metallic Catalyst Recovery

Organic
Cobalt

Catalyst
Preparation

Extraction

Feed
Organo-Metallic
Catalyst

Reactor

Slipstream

Makeup
Organic

Separator
Water Effluent
(200 ppm Cobalt)
Product
Water Effluent
(1 ppm Cobalt)

Fractional Extraction
Process Scheme

EI
YAE,YBE

SI2
XAS2,XBS2

F1I

(A-Rich)

NR

XAF,XBF

S1I

NS

XAS1,XBS1

RI
(B-Rich)
XAR,XBR

Extraction of Flavors and

Aromas

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

Separation of Structural
Isomers
pH Adjust
(Optional)

Solvent 1 Recycle

Typical Applications:
m. p. - Cresol
Xylenols
2 , 6 - Lutidine
3 , 4 - Picoline

Solvent 2 Recycle

pH Adjust
(Optional)

Aqueous
Recycle

Solvent 2
Distillation

Extraction

Isomer
Feed

Solvent 1
Distillation

Extraction

Mixed

Aqueous
Raffinate

Reflux

Isomer 1

Isomer 2

Major Types of Extraction Equipment

Mixer
Settlers

Column
Contactors

Used primarily in the metals

industry due to:
- Large flows
- Intense mixing
- Long Residence time
- Corrosive fluids
- History

Spray

Packed

Static

Tray

Agitated

Pulsed

Centrifugal
Used primarily in the
pharmaceutical industry due to:
- Large flows
- Intense mixing
- Long Residence time
- Corrosive fluids
- History

Rotary
Reciprocating

Rarely used

Used in:
Used in:
Used in:
- Refining
- Refining
- Nuclear
- Petrochemicals
- Petrochemicals
- Inorganics
- Chemicals
Example:
- Random
- Structured
- SMVPTM

Example:
- Sieve

Example:
- Packed
- Tray
- Disc & Donut

Used in:
- Chemicals
- Petrochemicals
- Refining
- Pharmaceutical
Example:
- RDC
- Scheibel

Example:
- Karr

Mix / Decant Tank

Characteristics

Feed Inlet

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

Sight Glass

Outlet

Mixer / Settlers
Characteristics
Handle very high flowrates
Light Phase In

Good for processes with

relatively slow reactions
(residence time required)
Provide intense mixing to
promote mass transfer
Require large amount of
floor space

Heavy Phase Out

Suitable when few theoretical

stages required
Large solvent inventory (and
losses)

Centrifugal Extractor
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

Packed Column
Extract (E)
Feed (F)

Characteristics
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

Solvent (S)

Limited as to which phase can be

dispersed
Raffinate (R)

Requires low interfacial tension for

economic usefulness
Not good for fouling service

Sieve Tray Column

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)

RDC Extractor
Characteristics

Drive Motor

Gearbox

Reasonable capacity:
20-30 M3/M2-hr
Limited efficiency due to
axial backmixing

Light
Phase Out

Heavy
Phase In

Suitable for viscous materials

Vessel
Walls

Suitable for fouling materials

Shaft

Sensitive to emulsions due to

high shear mixing
Reasonable turndown (40%)
Stators

Light
Phase In
Interface

Heavy
Phase Out

Interface
Control

Rotors

Scheibel Column
Characteristics
Reasonable
capacity:
15-25 M3/M2-hr
350-600 gal/ft2-hr

Gearbox

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

Turbine
Impeller

Light
Phase In
Interface

Heavy
Phase Out

Interface
Control

Horizontal
Inner Baffle

Scheibel Column Internal Assembly

Karr Reciprocating Column

Drive
Assembly
Seal

Characteristics
Highest capacity:
30-60 M3/M2-hr
750-1,500 gal/ft2-hr

Heavy
Phase Inlet

Good efficiency
Good turndown capability (4:1)
Uniform shear mixing
Best suited for systems that
emulsify

Light
Phase Out

Spider Plate

Sparger
Center Shaft
& Spacers

Metal Baffle
Plate

Tie Rods
& Spacers

Perforated
Plate

Teflon
Baffle Plate

Light
Phase Inlet
Sparger
Interface

Heavy
Phase Out

Interface
Control

Karr Column Plate Stack Assembly

Pulsed Extractor
Characteristics
Reasonable capacity:
20-30 M3/M2-hr

Light
Phase Out

Heavy
Phase In

Best suited for nuclear

applications due to lack of seal

Timer
Solenoid
Valves

Also suited for corrosive

applications since can be
constructed out or non-metals

Air

Limited stages due to

backmixing
Limited diameter/height due
to pulse energy required

Compressed
Air

Exhaust

Liquid
Light
Phase In

Pulse
Leg
Interface

Heavy
Phase Out

Interface
Control

Comparison Plot of Various

Commercial Extractors
20
Efficiency / Stages per Meter

Scheibel

10
6

RZE

Kuhni
Graesser

Key
Karr

PFK
PSE

RDC

FK
MS

SE

.06
0.4
0.2
1

4 6 10
20
40 60 100
Capacity M3/(M2 HR)

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 Column

Column Selection Criteria

Static Column
A static column design may be appropriate when:

Interfacial tension is low to medium: up to 10-15

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

Column Selection Criteria

Agitated Column
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

Column Selection Criteria

Rotating Disc Contactor (RDC)

Systems with moderate to high viscosity, i.e. >

100 cps

Systems that are residence time controlled, for

example, slow mass transfer rate with few
theoretical stages required

Systems with a high tendency towards fouling

Column Selection Criteria

Scheibel Column

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

Column Selection Criteria

Karr Reciprocation Plate Column

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

The Three Cornerstones of Successful

Extraction Applications
Successful
Application

Proper Solvent
Selection

Meaningful
Pilot Tests

Accurate
Scale-Up

Selection Based on:

Testing Based on:

Scale-Up Based on:

Actual feed stocks

Proven techniques

Full process including

solvent recovery

Proper safety factors

Wide range of operating

conditions

Sound thermodynamic
principles
Sound economic
principles
Availability
Recoverability
Sound environmental
principles
Toxicity
Safety

Organic Group Interactions

Solvent Class
Solute Class

10

11

12

Phenol

Acid, thiol

Alcohol, water

Active H on multihalogen

Ketone, amide with no H on N,

sulfone, phosphine oxide

Tertiary amine

Secondary amine

Primary amine, ammonia, amide,

with 2H on N

Ether, oxide, sulfoxide

10

Ester, aldehyde, carbonate,

phosphate, nitrate, nitrite, nitrile

11

Aromatic, olefin, halogen, aromatic

multihalogen, paraffin without
active H, manahalogen paraffin

Paraffin, carbon disulfide

12

1 - 4 = H donor groups
5 12 = H acceptor groups
12 = Non-H bonding groups

Liquid-Liquid Extraction Scale-Up

Theoretical scale-up is difficult

Complexity of processes taking place within an extractor
Droplet Breakup
Coalescence
Mass Transfer
Axial and radial mixing
Effects of impurities

Best method of design:

Pilot testing followed by empirical scale-up

Pilot Plant Configuration

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

Type of Column

Diameter

Height

Packed

3 to 4

3 to 6 per Theoretical Stage (TS)

Tray

4 to 6

4 to 5 Trays per TS

Karr

1 to 3 per TS

Scheibel

3 to 6 Actual Stages per TS (Approx. 3 to 6)

Continuous Extraction Pilot Plant

Arrangement
Variable Speed Drive
Extract

Hot Oil

Raffinate
Feed

Solvent

KMPS Pilot Plant Services Group

KMPS maintains a pilot
plant dedicated to extraction
R & D and applications
testing

Possible Extraction Column

Configurations
Solvent is Light Phase

B+C

F
Primary
Interface

A+B
Solvent
Dispersed

Solvent is Heavy Phase

A+B
Solvent
Continuous

C
A

B+C

A
A

Solvent
Dispersed

C
Primary
Interface

Primary
Interface

R
R
Primary
Interface

Solvent
Continuous

F
A+B

E
B+C

A+B

E
B+C

Factors Effecting which Phase is

Dispersed
Flow Rate

For Sieve Tray and Packed Columns disperse the higher flowing phase
For all other 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

Factors Effecting which Phase is

Dispersed
Surface Wetting

Want the continuous phase to preferentially set 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 Number
Droplet
Interfacial
Diameter Volume Droplets
SA [M2]
Area
[M3]
[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

Factors Effecting which Phase is

Dispersed
Marangoni Effect

Coalescence is enhanced by mass transfer from

droplets
continuous phase
A+B

Mass Transfer Direction

A+B

C
A+B

C+B

Continuous
c)

Droplets tend to coalesce

Must be counteracted by additional energy

Dispersed
(d

C+B

Continuous
(c

Dispersed
d)

Droplets tend to repel each other

Less energy required to maintain dispersion

Interface Behavior
Actions to control unstable
interface

Light Phase
Dispersed

As extraction proceeds, interface normally

grows in thickness and forms a rag layer
that stabilizes at some thickness

Heavy Phase
Dispersed

Rag
Layer

If rag layer continues to grow, some action

must Rag
be taken
1.
Draw
Continuously withdraw a portion of the
interface and pass through a filter to
remove interfacial contamination
2.

Reverse Phases
Often a stable interface can be controlled
by reversing which phase is dispersed

Growing
Uncontrolled
Interface
Filter

Entrainment
Entrainment involves carrying over a small portion of one phase out the wrong
end of the column.
Entrainment is controlled by:
1.) Increased settling time inside the column
2.) Coalescer inside the column
3.) Coalescer external to the column

E
F

1
S

E
F

OR

OR

R
R

Flooding
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

Primary Interface

E
F1

E
F2
Second
Interface

S
R

Flooding
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
F1

E
F2
Second
Interface

S
R

Pilot Tests
Static Columns

Agitated Columns

(Packed, Tray)

(Scheibel, Karr)
Process Factors
Column Variable
Variable

N, S/F
D, H
(F+S)

N, S/F
D, H
(F+S),f
f

F
H
S

D
Flood

HETS

D
F+S

F+S

MIN
HETS

HETS
f

F+S

Extractor Flow Patterns

Ideal Plug Flow

Actual Flow

X
This axial or back mixing causes
concentration gradients that decrease driving
force and therefore increase HETS

Generalized Scale-up Procedure

Pilot Scale

Commercial Scale
f2

f1

Q1

Q2

Feed Rate

Feed Rate
H1
H2
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

Application Scheibel Column

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

Commercial design: 3,900 lb/hr (270 GPH) spent acid

feed

Scheibel Column Pilot Plant Setup

Nitrated Organics Extraction
Interface

Variable
Speed Drive

Hot Oil
Organic
Extract
Spent Acid
Feed

MCB
Solvent

Aqueous
Raffinate

Scheibel Column Pilot Plant Test Results

Nitrated Organics Extraction
Run

# of
Acid Feed MCB Feed
Stages [cc/min]
[cc/min]

Column
Temp [C]

Agitation
Speed
[RPM]

Raffinate - Nit.
Org. Conc.
[PPM]

18

300

185

82

400

856

18

300

185

80

500

776

18

300

185

84

600

328

18

380

235

43

500

963

18

380

235

91

600

159

18

380

235

73

500

563

18

380

235

74

700

148

36

380

235

78

500

16

36

380

235

78

600

11

10

36

300

185

70

600

15

11

36

300

185

83

650

13

12

36

240

150

54

600

47

Scheibel Column Scale-up Procedure

Nitrated Organics Extraction

530

Column Capacity
For Dia. < 18
[GPH/FT2]

Rate in Commercial Column

For Dia. 18
[GPH/FT2]

600

157
[GPH/FT2]
Rate in 3 Dia. Pilot Scheibel
Column

14 Dia. = 430 GPH/FT2

300

100
5

10

15

[IN]
Scheibel Column
Diameter

20

Scheibel Column Pilot Plant Scale-up

Nitrated Organics Extraction

Diameter = 14 (D )
Expanded Head Diameter = 20 (D )
Bed Height = 9-6 (A)
Overall Height = 16-4 (B)
1

D1

D2

Application Karr Column

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

Commercial design: 36,900 lb/hr (4,660 GPH) acrylate

feed

Karr Column Pilot Plant Setup

Alcohol Extraction from Acrylates
Karr Column
1 Dia. x 8 Plate Stack
Plate Spacing from Top:
6 of 2
1 of 4
1 of 6
316SS Shaft, Plates
& Spacers

Variable
Speed Drive

Hot Oil
Raffinate
(Acrylate Phase)

Water
Feed

Extract
(H2O + Alcohol)

Acrylate Feed
(methyl or ethyl)

Interface

Karr Column Pilot Plant Test Results

Methanol Extraction from Acrylate
Run

Plate
Stack

Feed Rate Water Feed

[cc/min]
Rate
[cc/min]

Agitator
Speed
[SPM]

Interface

Raffinate
Conc.
Alcohol

Raffinate
Conc.
Water

150

45

100

Bottom

0.124

2.55

150

45

75

Bottom

0.165

2.83

150

45

110

Bottom

0.169

2.78

150

45

140

Bottom

0.112

2.72

180

54

100

Bottom

0.203

2.90

180

54

125

Bottom

0.146

3.08

180

54

150

Bottom

0.118

2.66

180

54

200

Bottom

0.078

2.73

210

63

175

Bottom

0.084

2.65

Notes:
Karr column with 1 dia. X 6 plate stack height.
Plate stack #1 is constant 2 plate spacing.
Plate stack #2 has variable spacing, from top: 4 of 2, 1 of 4, 1 of 6 spacing.
Feed is acrylate with approximately 2.5% methanol

Karr Column Pilot Plant Scale-up Procedure

Methanol Extraction from Acrylate

Select optimal run from test results

* Run 8:

Feed Rate = 150 cc/min

Solvent Rate = 45 cc/min
Specific Throughput (Q) = 560 GPH/FT2

Production column design

* Diameter direct scale-up based on specific throughput

* Height HCOMM = (H)PILOT
* Agitation Speed SPMCOMM = (SPM)PILOT

Karr Column Pilot Plant Scale-up Procedure

Methanol Extraction from Acrylate

H = (D / D ) x H
H = (45/1) x (6 feet) = 26 feet
SPM = (D / D ) x SPM
SPM = (1/45) x (200 SPM) = 117 SPM
Where:
COMM

COMM

PILOT

0.38

PILOT

0.38

COMM

COMM
COMM

PILOT

COMM

0.14

PILOT

0.14

* HCOMM = Height Commercial Column

* HPILOT = Height Pilot Column
* DCOMM = Diameter Commercial Column
* DPILOT = Diameter Pilot Column
* SPMCOMM = Commercial Strokes Per Minute
* SPMPILOT = Pilot Strokes Per Minute

Karr Column Pilot Plant Scale-up

Methanol Extraction from Acrylate

Diameter = 45 (D )
Expanded Head Diameter = 68 (D )
Plate Stack = 26-0 (A)
Overall Height = 36-8 (B)
1

D1

D2

Extraction Experience
KMPS has supplied over
300 extraction columns.

Questions?