Ekstraksi Cair-Cair

Outline

1. Definisi
2. Penerapan di Industri
3. Teoric
4. Perancangan
Ekstraksi Cair-Cair
 Proses yang dilakukan dengan melakukan kontak
antara larutan yang mengandung solut dengan
suatu zat pelarut sehingga solut akan masuk ke
fase solven untuk dapat dipisahkan lebih lanjut.

 Setelah kontak biasanya terdapat dua fase yang

jelas bedanya
 Larutan : solut (A) + diluen (B)
 Solven (umumnya adalah solven murni atau
terkadang mengandung sedikit konsentrasi solut)
: S (terkadang dituliskan sebagai C)
Penerapan
• Pemisahan produk/polutan dalam suatu larutan yang encer
(konsentrasi rendah)
• Pemisahan komponen polar atau asam/basa dari larutan
organik
• Pemisahan produk yang sensitif terhadap panasHeat
• Pemisahan bahan-bahan Non-volatil
• Pemisahan bahan-bahan Azeotropic dan/atau bahan-bahan
yang memiliki titik didih berdekatanand
• Sebagai proses pemisahan alternatif jika dislisai mahal
Teknologi Pemisahan
Pemisahan fisis Mudah
Dekantasi , Sedimentasi, filtrasi, elutriasi

Evaporasi
Single Effect, Multiple Effect

Distilasi
Simple, Azeotropic, Extractive, Reactive

Tingkat
Ekstraksi Kesulitan
Simple, Fractional, Reactive

Adsorpsi
Pressure Swing, Temperature Swing

Kristalisasi
Melt, Solvent

Membran
MF, UF, NF, RO
Sulit
Ekstraksi di Dunia Industri
•Pemurnian larutan organik dari komponen asam/basa/
Industri Kimia polar
• Pemisahan komponen aktif pada efluen larutan hasil
Farmasi fermentasi
• Pemurnian vitamin

• Pemisahan phenol, DMF, DMAC

Effluent Treatment • Pemisahan asam asetat dari larutan encer

• Pemisahan kaprolaktam pada industri nilon

Polymer Processing • Pemisahan katalis dari produk
• Proses peningkatan kualitas minyak pelumas
Petroleum • Pemisahan senyawa aromatis/alifatis(BTX)
• Pemisahan olefin/parafin
Petrochemicals • Pemisahan isomer-isomer
• Dekafeinasi pada produk
Industri Makanan • Pemisahan minyak atsiri
• Industri tembaga
Industri Logam • Pemisahan bahan-bahan loham berharga

Kimia anorganik • Pemurnian asam fosfat

Industri Nuklir • Purification of uranium

Pemisahan Bahan Organik dari Air
Distilasi vs. Ekstraksi
Azeotrop Azeotrope Tingkat
Bahan Organik TD [°C] kelaruta
TD [°C] air [%] kemurnian
n [%]
Distilasi

Methylene Chloride 40 2.0 38.1 1.5 < 50 ppb

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
Formaldehyde -21 Infinite Non Azeotropic < 1,000 ppm
Formic Acid 100.8 Infinite 107.1 22.5 < 500 ppm
Acetic Acid 118.0 Infinite Non Azeotropic < 500 ppm
Ekstraksi

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
Istilah dan Simbol

 Feed (Umpan) 

 Solven 

 Ekstrak

 Rafinat 
Proses Ekstraksi
Ekstrak, yEA (A,C, sedikit sekali B)

Ekstraktor
Umpan: Rafinat, xRA
Solut (A), xfA (A (sedikit), B, S)
Diluen (B)

Solvent, ysA=0 (pure)

Perhitungan: Ekstraksi Cair-Cair
Ekstraksi: Single Stage
Extrac (E)
A–0
B – 50
Feed (F) C – 0.8
50.8
A – 99
B–0
C–1
100 A–0 A – 99.0
B – 50
Rafinat (R) B–0
C–0 C – 0.2
50 99.2

Solven (S)

Fraksi tidak terekstrak U

Solut di Rafinat 0.2
  0.2
Solut di Feed 1.0
0.8
kons.Solut di Ekstrak 50  7.92
Koefisien Distribusi M 
kons.Solut di Rafinat 0.2
99

Faktor ekstraksi E S  
F

50 
M   99 7.92  4.0
Countercurrent Extraction
B+C Ekstrak (E):
Solute Rich Stream

A+B Primary Interface

Feed (F)

Continuous Phase

Dispersed Phase

C
Solven (S)

Rafinat (R):
A Solute Lean Stream
Ekstraksi Skala
Laboratorium
Variable Speed Drive

Baffle
Thermometer
Air
pendingin
Out

1 – Liter Flask

Air
pendingin
In Sumbat
Keluar
Simple Extraction
Process Solute Free Graphical
Scheme Basis Solution

E EI
F yAE FI
YBE
yBE YBE = yBE
xAS
xBF N yCE XBF = xBF
xAF
N yAR+ yCE
1.0
1.0
S SI Y
yAS YBS = yBF
YBS
yBS R yAS+ yCS RI
yCS xAR XBR = xBR
1.0 xBR xAR+ xCR XBR XBF
xCR
FI=F(xAR)
X
1.0
SI=S(yAS+yCS) m = YB* Distribution Coefficient
EI=E(yAE+yCE) on Solute Free Basis
XB*
RI=R(xAR+xCR)
Kurva kesetimbangan
Komposisi Ekstrak (fraksi berat, 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 0.020

Komposisi rafinate (fraksi berat., Solute Free)

Persamaan Kremser

 ys  
  x  
LOG f m 1 1   1 
ys   E  E 
 xn  m  
n 
LOG E

Dengan: n = Jumlah stage idela

xf = konsentrasi massa solut di feed (solute free basis)
xn = konsentrasi massa solut di rafinat (solute free basis)
ys = Konsentrasi massa solut di solven (solute free basis)
m = koefisien Distribution
E = faktor ekstraksi = (m)(S/F)
Engineering Calculations
Kremser Type Plot
YBE
E1 1.0
0.8 E = 0.3
0.6

F1 0.4
0.3

XBR/XBF = Fraction Unextracted

XBF
0.2

0.1
0.08
0.06

0.04
0.03

0.02

S1 0.01
0.008

YBS
0.006

0.004

R1 0.003

XB 0.002

R Factor
E = Extraction 0.001
0.0008
E = m (S1/F1) 0.0006
0.0005
1 2 3 4 5 6 7 8 10 15 20

Number of Ideal Stages

Typical Extraction System

Feed B+C+(A)
A+B
Extraction

Stripping
Raffinate

Recovery
Solvent
C C
Solvent (A) (A+B)
C
(A+B)

A+(B+C)

A (B+C) B (C)
Removal of Phenol from
Wastewater

Extract

Wastewater Feed
0.1 – 8 % Phenol

Extraction

Stripping
Raffinate

Recovery
Solvent
Recycled
Solvent

Raffinate
< 1 ppm Phenol
Biological Treatment Phenol
Or
Carbon Adsorption

ppb Phenol
Recovery of Acetic Acid from
Water
Using a Low Boiling Solvent

Extract

Aqueous Feed
20 - 40 %
Acetic Acid

Extraction

Stripping
Raffinate

Recovery
Solvent
Recycled
Solvent

Typical Solvents:
Ethyl Acetate Raffinate
Butyl Acetate

Aqueous Raffinate Acetic Acid

Recovery of Carboxylic Acids from
Wastewater
Using a High Boiling Point Solvent
Formic Acid
Water 99%+ Purity

Water Feed

0.1 – 5 %
Mixed Acids

Dehydration
Extraction

Recovery

Recovery
Solvent

Acid
Raffinate
< 1,000 ppb
Mixed Acids

Recovered Solvent Acetic Acid

99%+ Purity
Clean Up
Neutralization/Washing of Acid or
Base
or Polar Compounds from Organic
Stream

Organic
Water

** Organic Feed could

Extraction
Caustic (Mild)**
contain caustic. Mid-
Feed would be mild acid.

Feed (Organic + Acid) **

Water + Salts
Series Extraction
Extract Solvent 1
Feed Solvent 2
B+C C

A+B D

Extractor #1

Extractor #2
Raffinate Product
A B+D

Extractor 1 & 2 May Differ By:

- Temperature
- pH
- Solvent
Recovery of Caprolactam
Extract

Lactam Oil Phase

65 – 70% Caprolactam Water

Am. Sulphate Ext.

Lactam Oil Ext.

Re-Extraction
Feed From

Reaction
Section

Ammonium Sulphate Phase Solvent

2 – 3% Caprolactam Raffinate

AQ Waste Am. Sulph. Lactam Oil

to Waste to to
Discharge Discharge Recovery
Phosphoric Acid Purification via
Extraction

Recycle Water

Scrub Extraction

Re-Extraction
Phosphate

Extraction
Feed
HCL Rock
Digester

Scrub Solv.

Solvent
Raffinate Phosphoric
to Disposal Acid to
Recovery
Organo-Metallic Catalyst Recovery
Organic
Cobalt

Catalyst
Preparation

Feed
Extraction Organo-Metallic
Catalyst

Reactor

Slipstream
Separator

Makeup
Water Effluent
Organic
(200 ppm Cobalt)
Product
Water Effluent
(1 ppm Cobalt)
Fractional Extraction
Process Scheme

EI
(A-Rich)

SI2 YAE,YBE

XAS2,XBS
2
NR
F1I
XAF,XBF
NS
S1I
XAS1,XBS1

RI
(B-Rich)
XAR,XBR
Extraction of Flavors and Typical Products:
Orange Oil

Aromas Lemon Oil

Peppermint Oil
Cinnamon Oil

Aqueous Alcohol

Extraction

Distillation

Distillation
Essential Oil

Solvent 1

Solvent 2
Hydrocarbon

Oil Essential Extract

Separation of Structural
Typical Applications:
m. p. - Cresol

Isomers Xylenols
2 , 6 - Lutidine
3 , 4 - Picoline
pH Adjust Solvent 1 Recycle Solvent 2 Recycle
(Optional)
pH Adjust
(Optional)

Aqueous
Recycle

Distillation
Distillation
Extraction

Extraction

Solvent 2
Solvent 1
Mixed

Isomer
Feed

Aqueous
Raffinate

Reflux

Isomer 1 Isomer 2
Major Types of Extraction
Equipment
Mixer Column
Centrifugal
Settlers Contactors

Used primarily in the metals Used primarily in the

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

Spray Packed Tray Pulsed Rotary

Reciprocating

Rarely used Used in: Used in: Used in: Used in:
- Refining - Refining - Nuclear - Chemicals
- Petrochemicals - Petrochemicals - Inorganics - Petrochemicals
- Chemicals - Refining
- Pharmaceutical

Example: Example: Example: Example: Example:

- Random - Sieve - Packed - RDC - Karr
- Structured - Tray - Scheibel
- SMVPTM - Disc & Donut
Tangki Decantasi
Karakteristik
Feed Inlet
• Pemisahan fase
• Hanya proses batch
• Perlu penambahan solven berulangkali
(crossflow operation)
• Untuk industri berkapasitas rendah

Sight Glass

Outlet
Mixer / Settlers
Karakteristik
• Laju alir besar
• Cocok untuk proses yang
Light Phase In
memerlukan waktu tinggal
• Ada pengadukan 
meningkatkan transfer
massa
• Perlu ruangan yang luas
• Tepat : multistage
• Perlu solven yang banyak
Heavy Phase Out
Centrifugal Extractor
Karakteristik
• Aliran Countercurrent
• Waktu tinggal cepat
• Tepat untuk industri farmasi
• Jika beda densitas rendah
• Multistage
• Biaya maintenance tinggi
• Mudah tersumbat  larutan tidak
bersih
Packed Column
Karakteristik
Extract (E)
• Kapasitas tinggi:
Feed (F)
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)
• Efisiensi rendah
• Turndown terbatas
• Tidak bagus untuk bahan-bahan yang
rentan terhadap fouling

Solvent (S)

Raffinate (R)
Sieve Tray Column
Karakteristik
Extract (E)
Feed (F)
• Kapasitas tinggi: 30-50 M3/M2-hr
750-1,250 gal/ft2-hr
Primary
Interface • Efisinsi tinggi
• turndown terbatas

Solvent (S)

Raffinate (R)
RDC Extractor
Karakteristik Drive Motor Gearbox

• Kapasitas medium:
20-30 M3/M2-hr Light
Phase Out
• Efisiensi rendah Heavy
Phase In
• Cocok untuk bahan vikositas
tinggi Vessel Shaft
Walls
• Cocok untuk bahan yang
bisa fouling
• Sensitif untuk emulsi
• turndown (40%)

Stators Rotors
Light
Phase In

Interface Interface
Control

Heavy
Phase Out
Scheibel Column
Characteristics Gearbox Variable Speed
Drive
• Reasonable
capacity:
Light
15-25 M3/M2-hr Phase Out
Heavy
350-600 gal/ft2-hr Phase In
Rotating
• High efficiency due Shaft
to internal baffling Horizontal Vessel
Outer Baffle Walls
• Good turndown
capability (4:1) and
high flexibility
• Best suited when
many stages are
required Turbine Horizontal
Light
Phase In Impeller Inner Baffle
• Not recommended
for highly fouling Interface Interface
systems or systems Control
that tend to emulsify
Heavy
Phase Out
Scheibel Column Internal Assembly
Karr Reciprocating Column
Drive
Characteristics Assembly
Seal Light
• Highest capacity: Phase Out
30-60 M3/M2-hr
750-1,500 gal/ft2-hr
Heavy
Spider Plate
• Good efficiency Phase Inlet

Sparger
• Good turndown capability (4:1) Center Shaft
& Spacers
• Uniform shear mixing Metal Baffle
Plate Tie Rods
• Best suited for systems that Perforated & Spacers
emulsify Plate
Teflon
Light
Baffle Plate
Phase Inlet

Sparger

Interface Interface
Control

Heavy
Phase Out
Karr Column Plate Stack Assembly
Pulsed Extractor
Characteristics
Compressed
Light
• Reasonable capacity: Air
Phase Out
Heavy
20-30 M3/M2-hr Phase In
• Best suited for nuclear Timer
applications due to lack of seal
Solenoid
• Also suited for corrosive Valves
applications since can be
Air
constructed out or non-metals
• Limited stages due to
Exhaust
backmixing Liquid
Light
• Limited diameter/height due Phase In
Pulse
Leg
to pulse energy required
Interface Interface
Control

Heavy
Phase Out
Comparison Plot of Various
Commercial Extractors
20
Scheibel
Efficiency / Stages per Meter

10 RZE
Kuhni Key
6
Graesser Karr Graesser = Raining Bucket
4 PFK MS = Mixer Settler
RDC PSE SE = Sieve Plate
FK = Random Packed
2 FK PFK = Pulsed Packed
MS PSE = Pulsed Sieve Plate
SE
1 RDC = Rotating Disc Contactor
RZE = Agitated Cell
.06 Karr = Karr Recipr. Plate
0.4 Kuhni = Kuhni Column
Scheibel = Scheibel Column

0.2
1 2 4 6 10 20 40 60 100
Capacity M3/(M2 HR)
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 Meaningful Accurate

Selection Pilot Tests Scale-Up
Selection Based on: Testing Based on: Scale-Up Based on:

• Sound thermodynamic • Actual feed stocks • Proven techniques

principles
• Full process including • Proper safety factors
• Sound economic solvent recovery
principles
• Availability • Wide range of operating
• Recoverability conditions

• Sound environmental
principles
• Toxicity
• Safety
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” 1’ to 3’ per TS
Scheibel 3” 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
Possible Extraction Column
Configurations
Solvent is Light Phase
B+C E B+C E
F F
A+B Primary A+B
Interface
Solvent Solvent
Primary
Dispersed Continuous Interface

S S
C C
R R
A A
Solvent is Heavy Phase A A
R R
S S
C C
Primary
Solvent Solvent Interface
Dispersed Primary Continuous
Interface
F F
A+B E A+B E
B+C 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. Droplets retain shape.
Interfacial area lost. 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
[m] [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

C Mass Transfer Direction

A+B A+B
Dispersed Continuous
(d c)
• Droplets tend to coalesce
A • Must be counteracted by additional energy

C C Continuous Dispersed
(c d)
A+B
• Droplets tend to repel each other
C+B C+B
• Less energy required to maintain dispersion
Interface Behavior
Actions to control unstable interface Light Phase Heavy Phase
Dispersed Dispersed
As extraction proceeds, interface normally
grows in thickness and forms a “rag” layer
that stabilizes at some thickness
Rag
If rag layer continues to grow, some action Layer
must be taken
1. Rag Draw
Continuously withdraw a portion of the Growing
interface and pass through a filter to Uncontrolled
remove interfacial contamination Interface
2. Reverse Phases Filter
Often a stable interface can be controlled
by reversing which phase is dispersed
1 2
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
E E
E

F F F F

1 OR 2 OR 3
S S S S

R
R
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
F2 > F1
f f
Primary Interface Primary Interface

E E

F1 F2

Second
Interface

S S

R 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

f2 > f 1
f1 f
Primary Interface Primary Interface 2

E E

F1 F2

Second
Interface

S S

R R
Pilot Tests
Static Columns Agitated Columns
(Packed, Tray) (Scheibel, Karr)
N, S/F Process Factors N, S/F
D, H Column Variable D, H
(F+S) Variable (F+S),f
f
F

F
H

S D H

Flood S D
HETS
F+S
F+S
HETS MIN
HETS

f F+S
Extractor Flow Patterns
Ideal Plug Flow Actual Flow

Y Y

X 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
f1 f2

Q1
Q2
Feed Rate
Feed Rate
H1

H2

D1

Basic Scale-up Relationships:

D2/D1 = K1(Q2/Q1 )^M1
D2
H2/H1 = K2(D2/D1 )^M2
f2/f1 = K3(D2/D1)^M3 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
Variable
Speed Drive
Interface

Hot Oil

Organic
Extract

Aqueous
Spent Acid MCB Raffinate
Feed Solvent
Scheibel Column Pilot Plant Test
Results
Nitrated Organics Extraction
Run # of Acid Feed MCB Feed Column Agitation Raffinate - Nit.
Stages [cc/min] [cc/min] Temp [°C] Speed Org. Conc.
[RPM] [PPM]
1 18 300 185 82 400 856
2 18 300 185 80 500 776
3 18 300 185 84 600 328
4 18 380 235 43 500 963
5 18 380 235 91 600 159
6 18 380 235 73 500 563
7 18 380 235 74 700 148
8 36 380 235 78 500 16
9 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

600 14” Dia. = 430 GPH/FT2

Rate in Commercial Column

530

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

[GPH/FT2]
300

100
157
5 10 15 20

[GPH/FT2] [IN]
Rate in 3” Dia. Pilot Scheibel Scheibel Column
Column Diameter
Scheibel Column Pilot Plant Scale-
up
Nitrated Organics Extraction
• Diameter = 14” (D1)
• Expanded Head Diameter = 20” (D2)
D1
• Bed Height = 9’-6” (A)
• Overall Height = 16’-4” (B)

A B

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 Variable
Speed Drive
1” Dia. x 8’ Plate Stack
Plate Spacing from Top:
6’ of 2”
1’ of 4”
1’ of 6”
316SS Shaft, Plates
& Spacers
Hot Oil

Raffinate
(Acrylate Phase)

Extract
Water Acrylate Feed (H2O + Alcohol)
Feed (methyl or ethyl)

Interface
Karr Column Pilot Plant Test Results
Methanol Extraction from Acrylate
Run Plate Feed Rate Water Feed Agitator Interface Raffinate Raffinate
Stack [cc/min] Rate Speed Conc. Conc.
[cc/min] [SPM] Alcohol Water
1 1 150 45 100 Bottom 0.124 2.55
2 1 150 45 75 Bottom 0.165 2.83
3 2 150 45 110 Bottom 0.169 2.78
4 2 150 45 140 Bottom 0.112 2.72
5 2 180 54 100 Bottom 0.203 2.90
6 2 180 54 125 Bottom 0.146 3.08
7 2 180 54 150 Bottom 0.118 2.66
8 2 180 54 200 Bottom 0.078 2.73
9 2 210 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 = ƒ (H)PILOT
* Agitation Speed – SPMCOMM = ƒ (SPM)PILOT
Karr Column Pilot Plant Scale-up
Procedure
Methanol Extraction from Acrylate
• HCOMM = (DCOMM / DPILOT)0.38 x HPILOT
• HCOMM = (45/1)0.38 x (6 feet) = 26 feet
• SPMCOMM = (DPILOT / DCOMM)0.14 x SPMPILOT
• SPMCOMM = (1/45)0.14 x (200 SPM) = 117 SPM
• Where:
* 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” (D1)
• Expanded Head Diameter = 68” (D2)
• Plate Stack = 26’-0” (A)
• Overall Height = 36’-8” (B)

A D1 B

D2
Extraction in industry
Conclusions:

1. Extraction process  F + S = E + R

2. Industrial applications  purification

processes (not a final step of
purification)

3. Choose best solvent

4. Theoretical calculations  designing

the best and suitable equipment
(economical)