Liquid - Liquid extraction_4

Counter current extraction 2

• Say for total N stages, cascade is represented in figure

• Feed and solvent entering from two opposite ends of cascade

• Raffinate and Extract emerging again from two opposite ends

• Raffinate from previous stage act as feed for next stage

• Extract from previous stage act as solvent for next stage

Counter current extraction 3
• Concentration and flow rates of feed and solvent are usually given

• For given permissible concentration of solute in raffinate

• Determination of number of Ideal contact stages required

Final
given Raffinate

given

given

Final
Extract
Counter current extraction 4

Two Envelops are considered

• Envelop 1 : for all 1 to N stages
• Envelop II : for n to N stages

Final
Raffinate

Final
Extract
Counter current extraction 5
For Envelope 1 (for 1 to N stages)

• Total mass balance

F  S  E1  RN  M (8.11)

• Corresponding solute balance

FxF  S ys  E1 y1  RN xN  MxM (8.12)

Final
Raffinate

Final
Extract
Counter current extraction 6
Envelop II (for n to N stages)

• Total mass balance Rn 1  S  E n  RN (8.13)

Feed

• Corresponding solute balance Rn1 xn1  S ys  En yn  RN xN (8.14)

Counter current extraction 7
• Equilibrium curve is drawn from given data

• From known composition of feed, solvent, and

Final Raffinate, points F, S, and RN, located on
diagram

xC , yC
• Point M representing mixture of F and S is also
located on line FS

xB , yB
Counter current extraction For Envelope 1 8
• point M lies also on line joining points F  S  E1  RN  M (8.11)
RN and E1

• RN is given

• RN & M are joined

xC , yC
• RNM line extended to meet equilibrium
curve

• Intersection should point gives

equilibrium point E1

• RNE1 is the corresponding tie line

xB , yB
Counter current extraction 9
For Envelope 1 (for 1 to N stages)
• Total mass balance equation 8.11 may be rearranged as : F  S  E1  RN  M (8.11)
E1  F  S  RN   (8.15)

For Envelop II (for n to N stages)

• Total mass balance equation 8.13 may be rearranged as : Rn1  S  E n  RN (8.13)
En  Rn 1  S  Rn

or En  Rn 1  S  Rn   (8.16)
Feed
Counter current extraction 10

• Δ is difference point

• Δ considered as fictitious stream obtained by ‘removing’

• mass F of feed from first phase extract E1

• or mass RN, of end raffinate from solvent S

E1  F  S  RN   (8.15) For Envelop I

En  Rn 1  S  Rn   (8.16) For Envelop II

Feed
Counter current extraction 11
• Δ , the difference point, lies on line
• FE1 extended
• and also on RNS extended
• it is point of intersection of FE1 and RNS extended

For Envelop I

E1  F  S  RN   (8.15)
Counter current extraction 12
• Also for Envelop 2 from Eq. 8.16
• if line Rn-1En is extended, it has to pass through difference point Δ

• Here Rn-1 would be any point on Raffinate arm

• So from any point of raffinate arm, the extension meeting Δ, would intersect Extract arm at
corresponding En ( Where En is the extract from that stage)

For Envelop II

En  Rn1  S  Rn   (8.16)
Feed
Counter current extraction 13
• Since stages are ideal, streams En and Rn leaving stage
n at equilibrium

• Then for n =1 ,
• E1 and R1 should be at equilibrium
• tie line through point E1 meets equilibrium curve at
R1
• E1R1 tie line for stage 1

Tie line R1E1

Counter current extraction 14
• for n=2, From Equation 8.16,

En  Rn 1  S  Rn   (8.16)
Feed

E2  R1  S  R2   For stage n = 2

For stage n=2 , R1 = Feed ; E2=extract

• line joining R1 and Δ meets

equilibrium curve at E2
Counter current extraction 15
E2  R1  S  R2  
• For E2, corresponding equilibrium point is R2
R1  S  E2  R2
• tie line through E2 meets equilibrium curve at point R2

• procedure is repeated till point RN representing final raffinate is reached

• Each tie line represents a stage

• Number of tie lines drawn in process to reach point RN , is number of
Ideal stages R1 and E1 at equilibrium
R2 and E2 at equilibrium

Tie line R2E2

Counter current extraction : EXAMPLE 16

It is planned to extract diphenyl hexane (DPH) from a solution in a docosane (A) using ‘pure’ furfural (B) as
the solvent. The feed enters extractor cascade at a rate of 2000 kg/h with 45% DPH (C) that has to be
reduced to 4% in final raffinate. The solvent rate is 2500 kg/h. Determine number of theoretical stages
required. Extraction is to be carried out at 45℃. Several compositions on the extract and the raffinate arms
and the tie-line data in mass% of components at 45℃ are given below.
Equilibrium data
A: 96.0 84.0 67.0 52.5 32.6 21.3 13.2 7.7 4.4 2.6 1.5 1.0 0.7
B: 4.0 5.0 7.0 10.0 20.0 30.0 40.0 50.0 60.0 70.0 80.0 90.0 99.3
C: 0 11.0 26.0 37.5 47.4 48.7 46.8 42.3 35.6 27.4 18.5 9.0 0.0

Tie-line data
• Raffinate (Docosane) phase, mass% Extract (Furfural) phase, mass%
A B C A B C
85.2 4.8 10.0 1.1 89.1 9.8
69.0 6.5 24.5 2.2 73.6 24.2
43.9 13.3 42.6 6.8 52.3 40.9
Solution 17

• Feed rate = 2000 kg/h

• Mass fraction of DPH in feed = xCF=0.45

• Solvent rate = 2500 kg/h

• Mass fraction of DPH in solvent = yCS= 0.0 (solvent is pure)

• Mass fraction of DPH in raffinate is xCR= 0.04

• From equation 8.5

FxCF  SyCS 2000  0.45  2500  0

xCM    0.2 (8.5)
FS 2000  2500
Solution 18

• Locate : points F (0,0.45), S (1.0,0), M (on line FS at xCM = 0.2) , RN (xC = 0.04 on raffinate arm)

• RN and M are joined and extended to meet the equilibrium curve at E1

• Lines FE1 and RNS extended to meet at ‘difference point’ Δ

• Draw tie line from E1 to meet raffinate arm at point R1 19
• Join R1Δ to get E2 at point of intersection with extract arm
• R1E2 is operating line for second stage of cascade
(operating line relates concentration of streams entering or leaving a stage)
• Draw tie line through point E2 to meets raffinate arm at R2 20
• Proceeding in same way, successive stages are obtained till the point RN (xC = 0.04 ) is reached
• Total number of stages required for given separation is 4
Alternate technique 21
• Line emanating from difference
point Δ, intersects
• extract arm at point En+1
[yC=(yC)n+1]
• raffinate arm at point Rn [ xC =
(xC)n]

• such lines are shown by broken lines

figure A
• Locus of points (xn , yn+1) is
operating line on xC-yC plane

• From Fig A several lines are drawn

from point Δ
• From corresponding intersection
points on raffinate and extract arms,
the operating points are generated.
• Set of (xn, yn+1) values obtained from figure A : 22

xC n 0.04 0.1 0.14 0.17 0.22 0.26 0.30 0.33 0.38 0.415
yC n+1 0.03 0.051 0.018 0.09 0.125 0.15 0.178 0.20 0.252 0.280

• Above data used to draw operating line on figure B

figure B
• Equilibrium line drawn using given data ( xC, yC)

• Operating line drawn from generated (xCn , yCn+1) data from

Fig A

• Stages are constructed by drawing stages between

equilibrium line and operating line

• Number of stages is 4.8

Minimum solvent rate 23
• At minimum solvent rate :
• infinite number of contact stages required

• For a line from difference point Δ (operating line) to coincide with a tie line (equilibrium line),
infinite number of stages will be required

• This corresponds to minimum solvent/feed ratio which can be used for the specified system

• Difference point Δm corresponding to infinite number of stages is located

• minimum solvent rate Sm calculated by using Lever arm rule

Minimum solvent rate 24
• Once minimum solvent rate is obtained, actual solvent rate is selected on basis of economic
consideration

• Higher solvent rate

• reduces fixed cost because of less number of stages required
• but operating cost becomes higher because of
• handling larger quantity of liquids
• Large equipment size
• Higher cost of separation of solvent
Determination of minimum solvent rate 25
Steps
1. Equilibrium curve is drawn
2. Points F, S, and RN are located from given compositions of feed, solvent and raffinate
3. Points ​RN and S are joined and extended
4. Tie line through point F and a few others below it are drawn
Determination of minimum solvent rate 26
Steps
6. All tie lines are extended to meet line RNS , producing number of Δ points (Δ1 , Δ2 , Δ3 …….)
7. meeting point closest to S is Δm
8. From figure

Sm length of line segment RN  m

 (8.17)
RN length of line segment S  m

• Here tie lines are inclined towards

point S for particular LLE system
Determination of minimum solvent rate 27
• When tie lines slope away from point S (as shown in figure)
• extended tie lines intersect line S-RN extended on left side of diagram
• yielding a set of Δ points

• minimum solvent rate corresponds to Δm point

• farthest from S

Δm Δ1 Δ2 Δ3
Determination of minimum solvent rate 28
• Minimum solvent rate corresponds to Δm point
• farthest from S, if it lies on left
• nearest to S, if it lies on right

• Actual position of Δ must be farther from S (if on left) or nearer to S (if on right) for a finite
number of stages
• larger amount of solvent, fewer number of stages

• Tie line through F extended will locate Δm, (for minimum solvent) at intersection point with RnS.
Example 29

• An aqueous solution of acetic acid (35% acid, rest water) is to be extracted with ‘pure’ di-iso-
propyl ether in a counter current cascade at a rate of 2000 kg/h. The raffinate stream must not
contain more than 10% of acid in it. Determine the minimum solvent rate required for this
extraction.

Water layer (raffinate), mass% Ether layer (extract), mass%

xA xB xC yA yB yC
0.981 0.012 0.0069 0.005 0.993 0.0018
0.971 0.015 0.0141 0.007 0.989 0.0037
0.955 0.016 0.0289 0.008 0.984 0.0079
0.917 0.019 0.0642 0.01 0.971 0.0193
0.844 0.023 0.133 0.019 0.933 0.0482
0.711 0.034 0.255 0.039 0.847 0.114
0.589 0.044 0.367 0.069 0.715 0.216
0.451 0.106 0.443 0.108 0.581 0.311
0.371 0.165 0.464 0.151 0.487 0.362
 30
• Locate on diagram
• Point F (feed F = 2000 kg/h, xB,F = 0 ; xC,F= 0.35)
• Point S (solvent is pure yB,S = 1 ; yC,S = 0.0)

• Raffinate has 10% of acid ,

• point RN, xC,RN = 0.1

• Point RN and S are joined and line RNS is extended

 31
• Tie line from point F extended to intersect RNS line at Δm

• Em obtained at intersect of F Δm line with extract arm

(Em correspond to extract composition if minimum solvent is used)

• join Em and RN ( desired raffinate point)

• Mm is the intersect point of FS and EmRN
 32

• From lever arm rule F M S

 m m
Sm FM m

• From Figure : FMm = 5.6 and MmSm = 5.55

2000 5.55
  0.99
Sm 5.6
Sm  2018 kg