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
