Extraction Technology

Extraction Process

Figure 8.1 Typical liquid-liquid extraction process.

 Typical Extractor
Light Phase Light Phase
Out Heavy Phase Out
In
Heavy Phase
In

Light Phase
In
Light Phase
In

Heavy Phase Heavy Phase

Out Out

Light Phase Dispersed Heavy Phase Dispersed

 Typical Extractor
Extract
Out

Feed
In

Solvent
In

Raffinate
Out

Light Phase Dispersed

Liquid-liquid Equilibrium
f i I  f i II

x P
i i  i   xi Pi  i 
vap I vap II
Phase I

xi i I  xi i II

Phase II

xiI  iII
II
 I
xi i
 Design Methods
Theoretical Trays
Hunter – Nash graphical method
Aspen

Packed Tower Height

Seibert et al.

Sieve Tray Efficiency

Seibert et al.
Hunter – Nash Graphical Method

Blender Material Balance

M = F + S = RNp+ E1

M xM = F xF + S yS = RNp xNp + E1y1

Hunter – Nash Graphical Method

Figure 8.14 Location of product point.

  “P” Point
100 lbs 181 lbs  = 81 lbs
10 lbs

90 lbs 171 lbs  = 81 lbs

12 lbs

78 lbs 159 lbs  = 81 lbs

9 lbs

69 lbs 150 lbs  = 81 lbs

Hunter – Nash Graphical Method

Figure 8.15 Location of operating point.

Hunter – Nash Graphical Method

Figure 8.18 Determination of minimum solvent to feed ratio.

Hunter – Nash Graphical Method

Figure 8.17 Determination of the number of equilibrium stages.

 Graphical Method Example
In a continuous counter-current train of mixer settlers, 100 kg/hr of a 40 wt % acetone / 60 wt % water
solution is to be reduced to 10 wt % acetone by extraction with pure 1,1,2 trichloroethane (TCE) at 25 C.

Find:
1. The minimum solvent rate
2. At 1.8 times the minimum solvent rate, find the number of mixer settlers required.

Water Phase ( wt %) TCE Phase ( wt %)

C2H3Cl3 Water Acetone C2H3Cl3 Water Acetone
0.73 82.23 17.04 73.76 1.10 25.14
1.02 72.06 26.92 59.21 2.27 38.52
1.17 67.95 30.88 53.92 3.11 42.97
1.60 62.67 35.73 47.53 4.26 48.21
2.10 57.00 40.90 40.00 6.05 53.95
3.75 50.20 46.05 33.70 8.90 57.40
6.52 41.70 51.78 26.26 13.40 60.34
 Acetone

E1min

Mmin

RNp

s Water
TCE
 Acetone

E1
F

RNp

TCE
s Water
 10 Minute Problem
A feed stream “C” of 100 kg/min containing 30 mass percent solute “A” is
being contacted in a single stage stirred contactor with 50 kg/min of pure
solvent “S” (equilibrium figure below). Determine the composition and
amount of the resulting raffinate and extract streams.
Extractor Sieve Tray

Photo of Sieve tray

Trayed Extractor Efficiency
(Treybal Empirical Model)

0.42
3.12 H t 0.5
Ud 
Eo   
  Uc 

Where: Ht = tray spacing (ft)

Ud = superficial dispersed
phase velocity
Uc = superficial continuous
phase velocity
 = interfacial tension (dyne/cm)
Interfacial Tension
 Trayed Extractor Efficiency
(Seibert Model)

 4.4 K od , f   dVS  6 K od ,r d z  h 
    
ln 1  EMD   1  U d dVS U d U d mdc
Eo  EMD   o  o  
 0.4 K od , f   dVS  3 K od ,r d z  h 
2
ln  Uc
1      
 U o  o d dVS U d

Kod,r

Kod,f

Seibert, A.F. and Fair, J.R., “Mass-Transfer Efficiency

of a Large-scale Sieve Tray Extractor,” Ind. Eng. Chem.
Res., 32 (10): 2213-19 (1993).
 Trayed Extractor Efficiency

1 D   c U S dVS c
K od ,r  kc ,r  0.698  AB  Re0c .5 Scc0.4 1  d  Rec  Scc 
1 m  dVS  c  c DAB
 dc
k d ,r kc ,r

k d ,r  0.023 U S Scd 
 0.5
 6 k d ,r 
0.00375U S
 6 
Scd 
0. 5

 d
1 d 1
c c

Correction of k d,r from Seibert Table VI Equation 16

 Trayed Extractor Efficiency

 
1/ 2 1/ 2 N o   dVS3
1 D  D  6 Qd
K od , f  k c , f  1.3  AB,c  k d , f  1.3  AB, d  f  Uo 
1 mdc     Qd N o  d o2
  f   f 
kd , f kc , f 4

1/ 2
  
dVS  1.5    where :   1.0 cd   1.4 d c
  g 

dVS
 Trayed Extractor Efficiency

0.14
2
  3
 4 dVS
2
g    W 
P c
H    P 0.149 W  0.9 cP
C4 g   3   c 

N Re 0.757 N Re 0.441
0.149
 0. 94 H  0.857 H  59.3 0.149
 3. 42 H  0.857 H  59.3
P P

dVS  c U so Ud
N Re  d  U s  U so exp  1.92 d 
c U
U so exp 1.92d   c
1  d
 Trayed Extractor Hydraulics
2
 
  0.2
U 2
0.71  2
 c U down  d 02  g    
h  0.50 d o 1   2.47  3.2    
 g   do U o d    g     d o  g 
log 
 
  d 

h
 Packed Liquid-liquid Extraction

IMTP

Pall Rings

Structured
Packed Extractor Design (Hydraulics)

1/ 2
  
dVS  1.15    where :   1.0 cd   1 .4 d c
  g 

0.14
 c2  3  4 dVS
2
g    W 
P 4 H    P 0.149 W  0.9 cP
 C g   3   c 

N Re N Re
0.149
 0.94 H 0.757  0.857 H  59.3 0.149
 3.42 H 0.441  0.857 H  59.3
P P

Seibert, A.F., Reeves, B.E., and Fair, J.R., “Performance of a

Large-scale Packed Liquid-Liquid Extractor,” Ind. Eng. Chem. Res.
29 (9); 1901-07 (1990).
Packed Extractor Design (Hydraulics)

2
  a p dVS 
U d cos  
N Re 
dVS  c U so
d   8 
c Uc
 U so exp 1.92d  
1  d

  a p dVS     a p dVS   Uc 
U s  U so exp 1.92d cos   1  cos 

   
  1    
 8    8   d 

 
2
 
1

5.63 1  0.925  U d , flood  cos 
 a p dVS 
  
U c , flood  U so  U   8 
  c , flood     
 Packed Extractor Design
(Mass Transfer)

Uc 6  d
Z  HTU oc * NTU oc HTU oc  where aw 
K oc aw dVS

1 1 1 D   c U S dVS c
  kc  0.698  AB  Re 0c.5 Scc0.4 1  d  Re c  Scc 
K oc mdc k d k c  dVS  c  c DAB

k d  0.023 U S Scd 
 0.5
 6 k d ,r 
0.00375 U S
 6 
Scd 
0.5

 d
1 d 1
c c
Extraction Equipment Selection

Depends on:

- solvent recovery economics

- viscosities, interfacial tension, solids
- product/solvent value
- flowrates
- risk assessment
- operation experience
 Static Columns
Lig h t liq uid ou t Lig h t liq u id o ut

He a vy liq u id in

Colum n in te rfa c e
In te r fa c e
Ra g
r e m ova l He a vy liq u id in
La r g e -d ia m e te r
Elg in h e a d

Re d is tr ib u to r

Spray Tower P a c kin g

Packed Tower
Lig h t-p ha s e d is trib u to r Lig h t liq u id in

(a) He a vy liq u id o u t

He a vy liq u id o u t

Lig h t liq u id in
 Static Columns
Light liquid out

Operating
interface

Heavy liquid in

Perforated
plate
Sieve Tray
Downcomer

Coalesced
dispersed

Light liquid in

Heavy liquid out

 Oldshue-Rushston Column
• Develop in 1950s Lig h t liq u id o ut

• Many commercial
installations In te r fa c e

• Solids handling
• Viscosities to 500 cP He a vy liq u id in

• Differential contactor S ta to r Rin g

S tir r e r

Lig h t liq u id in

He a vy liq u id o u t
 Reciprocating Plate Extractor (Karr)

• Developed in 1959
• Many commercial installations Lig h t liq u id o u t
• V. High Volumetric Efficiency
He a vy liq u id in
• Vary tray amplitude and frequency
• Caution at low interfacial tensions
• Tray movement can clean walls
• Differential contactor
• Scale-up to the 0.38 power on diameter
• Other variations (e.g. VPE)

Lig h t liq u id in In te r fa c e

He a vy liq u id o u t
 Podbielniak
• Horizontal centrifugal extractor
• High efficiency
• Short residence time
• Minimum inventory
Light phase out
Light phase in

Heavy phase in

Heavy phase out

Mixer-Settler

• Wide range of designs

• Handle wide range of flow ratios
• Easy start-up
• Easy to clean/inspect
• Batch operations
• Larger equipment
• Handles solids
• Low headroom
• Occupy much floor space
• Can add stages
• Interstage pumping often required
• High solvent inventory
 Hollow Fiber Extractor
Solvent Out Solvent In

Feed In Feed Out

• Developed in 1980s
• Modified in 1990s
• Stage contactor
• Low organic solvent to aqueous feed ratios
• Few commercial extraction applications
• Many commercial gas/liquid applications
 QVF-RZE
RTL (agitated cell)
Pulsed:
packed plate
Kühni

Karr

RDC

Stichlmair (1980)
Packed

M/S
Sieve
Tray