Liquid –Liquid Extraction

B+C
B A+C
A+B

A+B+C

A+B+C
 Liquid –Liquid Extraction

Feed Extract AA+Ester

Ester Acetic
Solvent acid+water Raffinate Water+AA

Double solvent method

Water + Chloroform
P-isomer
o-isomer

O and p- nitrobenzoic acid

When to use?

Needs further treatment for getting pure components

When other separation routes are difficult/ineffective

Long chain fatty acid separation from vegetable oils by distillation

needs vacuum
Tantalum –niobium separation difficult by fractional crystallization

Dilute feed

Reduced chemical reagents- Environmental concern

Uranium-vanadium ; Hafnium-zirconium; fission products

Separation of chemically similar compounds

paraffinic and aromatic hydrocarbons of same molecular weight – have

same vapor pressure – Liquid sulfur oxide, DEG
 Experiment
A B C
Analyze the
100 0 0 two phases
80 10 10 formed for all
70 15 15 Mix and the three
allow to components
60 20 20
separate

Phase 1 Phase 2
A B C A B C

Plot in ternary
diagram
https://www.youtube.com/watch?v=J3QFoXRoKEg
 C

A
B
Case 1

One pair partially soluble

A B C
Water Chloroform Acetic acid
benzene water Acetic acid

C dissolves completely in A and B

A and B dissolve to limited extent in each other

A rich and B rich layers

The more A and B insoluble the curve in the ternary

corordinate will move towards the apex
Temperature effect
 Two pairs partially miscible

A B C
Chlorobenzene water MEK

A and C completely soluble

A-B: Limited solubility

B-C: Limited solubility
Solvent selection

Should be greater than 1

Solubility of solvent: The more insoluble, more effective the
separation
Single stage extraction (batch/ continuous)
Multistage crosscurrent extraction
Case 1: 3 stage unit

Step 1
Stage 1: F = 100 kg,
XF = 0.30, Ys = 0 (pure solvent)
Raffinate Extract S1 = Bl = 40 kg.
B x B y
0.012 0.0069 0.993 0.0018
0.015 0.0141 0.989 0.0037
0.016 0.0289 0.984 0.0079
M1 = 100+40= l40kg
0.019 0.0642 0.971 0.0193
0.023 0.133 0.933 0.0482
0.034 0.255 0.847 0.114
0.044 0.367 0.715 0.216
0.106 0.443 0.581 0.311 100(0.30) + 40(0) = 140 xm1
0.165 0.464 0.487 0.362
xM1 = 0.214

22
 F
0.3 0.3
0.25
M1 0.25
xM1
Y and x

0.2 0.2

y
0.15 0.15
0.1 0.1

0.05 0.05

0 S 0
0 0.2 0.4 0.6 0.8 1 0 0.05 0.1 0.15 0.2 0.25 0.3

B wt fraction x

Plot the x vs. B and y vs. B in the same plot

Plot beside x vs. y graph, x and y axis scale should be same. The y axis
scale in both the graphs should be same, as shown..

Locate F, B, M1 and xM1.

Draw tie line by trial and error

23
 F
0.3 0.3
0.25
M1 0.25
xM1
Y and x

0.2 0.2

y
0.15 0.15
0.1 0.1

0.05 0.05

0 S 0
0 0.2 0.4 0.6 0.8 1 0 0.05 0.1 0.15 0.2 0.25 0.3

B wt fraction x

Plot the x vs. B and y vs. B in the same plot

Plot beside x vs. y graph, x and y axis scale should be same. The y axis
scale in both the graphs should be same, as shown..

Locate F, B, M1 and xM1.

Draw tie line by trial and error

24
 F
0.3 0.3
0.25
M1 0.25
xM1
Y and x

0.2 0.2

y
0.15 0.15
0.1 0.1

0.05 0.05

0 S 0
0 0.2 0.4 0.6 0.8 1 0 0.05 0.1 0.15 0.2 0.25 0.3

B wt fraction x

Plot the x vs. B and y vs. B in the same plot

Plot beside x vs. y graph, x and y axis scale should be same. The y axis
scale in both the graphs should be same, as shown..

Locate F, B, M1 and xM1.

Draw tie line by trial and error

It should pass through point Mi
Read the x and y values values for the correct trial 25
 F
0.3 0.3
0.26
0.25 0.25
M1
xM1
0.2 0.2

x and y
0.12
x and y

0.15 0.15

0.1 0.1

0.05 0.05

0 S 0
0 0.2 0.4 0.6 0.8 1 0 0.05 0.1 0.15 0.2 0.25 0.3
B concentration B concentration
Stage 1 Stage 2 S 2 = 40
F = R1 = 94
x1 = 0.26
M 2 = 134
y1 = 0.12
M ( x − x1 ) 140 (0.214 − 0.26)
xM 2 = [96(0.26) + (0)] / [136] = 0.183
E1 = 1 M 1 = = 46
( y1 − x1 ) (0.12 − 0.26)
For stage 2, Raffinate from
R1 = 140 − 46 = 94 stage 1 is feed, and solvent is
fresh
For feed line of stage 2- Join
raffinate point of stage 1, 0.26
to x-axis 1, fresh solvent point 26
 F
0.3 0.3

0.25 0.25
M1
0.24
0.2 M2 0.2
xM2
0.15 0.15
0.095
0.1 0.1

0.05 0.05

0 S 0
0 0.2 0.4 0.6 0.8 1 0 0.05 0.1 0.15 0.2 0.25 0.3

Stage 2 Stage 3
F = R2 = 82.55
x2 = 0.24
y2 = 0.095 S = 40
M 1 ( xM 1 − x1 ) 136 (0.183 − 0.24) M 3 = 122.55
E2 = = = 53.44
( y1 − x1 ) (0.095 − 0.24) xM 3 = [82.55(0.24) + (0)] / [122.65] = 0.16
R2 = 82.55

Similar procedure for stage 2 and 3 tie lines

 F
0.3 0.3

0.25 0.25
M1
0.21
0.2 M2 0.2
x0.15
M3 0.15
0.09
0.1 0.1

0.05 0.05

0 S 0
0 0.2 0.4 0.6 0.8 1 0 0.05 0.1 0.15 0.2 0.25 0.3

Stage 3
x3 = 0.21
y3 = 0.09
M 3 ( xM 3 − x3 ) 122.55 (0.16 − 0.21)
E3 = = = 51.05
( y3 − x3 ) (0.09 − 0.21)
R2 = 71.5

Total E= 150.49 kg, Total acid in E=51.05*0.09+53.44*.0955+46*.12=15.2 kg

R=235.84, total acid= 30-15.2=14.78 kg
 F
0.3 0.3

0.25 0.25

0.2 0.2

0.15 M 0.15

0.1 0.13 0.1

0.05 0.05

0 S 0
0 0.2 0.4 0.6 0.8 1 0 0.05 0.1 0.15 0.2 0.25 0.3

Stage 3
x = 0.21
y = 0.09
xM = 0.13
S xF − xM
= = 100(0.3 − 0.11) / (0.11) = 172kg
F xM − ys
 Raffinate Extract
x FrB y Fr B
0.012 0.0069 0.993 0.0018
0.015 0.0141 0.989 0.0037
0.016 0.0289 0.984 0.0079
0.019 0.0642 0.971 0.0193
0.023 0.133 0.933 0.0482
0.034 0.255 0.847 0.114
0.044 0.367 0.715 0.216
0.106 0.443 0.581 0.311
0.165 0.464 0.487 0.362
 Insoluble solvents
Raffinate only A+C, Extract contains only B and C
x´ and y´ are used

Single stage and multistage cross-current:

A ( y ' S − y 'n ) mass C
− = x 'F =
B ( x ' F − x 'n ) mass A
x 'F = xn −1 in cross current flow mass C
x 'R =
mass A
Slope of operating line: –A/B mass C
y 'E =
In general for cross current mass A
Stage 1 Ax 'F + By 'S = Ax 'n + By 'n
−A ( y '1 − y 's )
=
B ( x '1 − x 'F )
Stage 2
−A ( y '2 − y ' s )
=
B ( x '2 − x '1 )
Stage 3 B is not constant
−A ( y '3 − y 's ) For constant B , slope for all
=
B ( x '3 − x '2 ) stages is same
A 5% solution of acetaldehyde in toluene is to be extracted with water in 3 stage unit. S=100
kg/stage. F= 500 kg. Equilibrium relation is y’= 2.3 x’. y’= kg acetaldehyde/kg water; x’ = kg
acetaldehyde/kg toluene. Insoluble case.

F= 500 kg, xf= 0.05, x’= 0.05/0.95= 0.0526 B=100 kg/stage

A= toluene in feed= 475 kg Slope= -475/100=-4.75

Draw x’ v-y’ curve

x' y'
Locate xf’
0 0
From there draw three lines with slope -4.75 0.01 0.023
Locate the final concentration from third stage 0.02 0.046
operating line as shown in figure. 0.03 0.069
0.04 0.092
0.05 0.115
0.06 0.138
 0.16

0.14

0.12
Y’ 0.1

0.08

0.06

0.04
0.03
0.02

0
0 0.01 0.02 0.03 0.04 0.05 0.06 0.07
Xf’
0.0126 X’
X’=0.0126 kg C/kg A
Y’=0.03 kg C/ kg B

So final raffinate contain

A in raffinate is 475

So C in R is 475 x 0.0126 =5.98 kg

Total R= 5.98+ 475 kg

C extracted = (0.03 + 0.05 + 0.082) = 0.162 x 100 = 16.2

E = 300 + 16.2 = 316.2 kg

% E = 16.2 /25 = 64.8 %

Cascade Unit
Cascade Unit
Sieve tray column

Heavy liquid is
continuous phase
Sieve tray column
Rotating disc contactor