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LIQUID-LIQUID
EXTRACTION
SITI FATIMAH BINTI ABDUL HALIM
FACULTY OF CHEMICAL ENGINEERING
UiTM PULAU PINANG
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LEARNING OUTCOME
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3.1 DEFINITION & APPLICATIONS
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Liquid-liquid Extraction Principle
C - solvent (blue)
A-solute (black)
B-liquid solution(red)
When Liquid-liquid extraction is carried out in a test tube or flask the two
immiscible phases are shaken together to allow molecules to partition
(dissolve) into the preferred solvent phase.
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DEFINITION & APPLICATIONS
Common production processes using LLE i.e:-
i. Food processing
ii. Pharmaceutical separation
iii. Oil purification
.
The difference between LLE and distillation process in the separation of liquid mixture:-
LLE depends on solubilities between the liquid components and produces new
solution which in turn has to be separated later, whereas;
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Table 3.1.1: Industrial Liquid Liquid Extraction (LLE) Processes
b) Separation of mixture which the components have close boiling point (vapor
pressure)
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Work in a group
LLE or DISTILLATION ?
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Solvent is the key point need to consider for optimized LLE separation. The criterias are as follows:
a) Distribution coefficient - the ratio (at equilibrium) of solutes concentration in extract and
raffinate phases. It gives a measure of the affinity of the solute for
the 2 phases.
b) Solubility - the solutes are soluble in solvent but insoluble (low solubility) in the
feed solution. For example, if there is significant solubility of
solvent in the raffinate stream, an additional separation is required
to recover the solvent.
c) Recoverability - necessary to recover the solvent for re-use purposes.
d) Density - A large difference in density between extract and raffinate phases
permits high capacities in equipment. This especially important for
extraction equipments that utilizing gravity for phase separation.
e) Chemical Reactivity - Chemically stable and inert towards other components of th
system & construction
f) Viscosity / P - Low & P for ease in handling & storage. E.g. high leads to
difficulties in pumping, dispersion & mass transfer rate.
g) Availability & cost.
-selectivity :
-interfacial tension: (sept 2014)
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Work in a group
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PROCESS FLOW DIAGRAM LIQUID-LIQUID EXTRACTION
1 2 3 N
Lo Feed LN Raffinate
XAO XAN
XBO XBN
XCO XCN
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Principles of Liquid-Liquid Equilibrium
0.9
0.8
0.7
0.6
xC,yC
0.5
0.4
0.3
M
0.2
0.1
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
xA, yA
(B)
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Figure 3.1.3 Ternary diagram of ethylene water-glycol-furfural (25C)
(b) Right triangular diagram
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
xA, yA
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Tie line
A pair of extract and raffinate coordinate
1
water layer Isopropyl ether layer
0.9
Acetic isopropyl Acetic isopropyl
0.8
acid water ether acid water ether
xC,yC
0.0141 0.971 0.015 0.0037 0.007 0.989 0.5
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SINGLE STAGE OF LLE
- Solvent and feed streams are contacted each other in single stage producing the raffinate
and extract streams which are in equilibrium states.
- Feed stream normally consists of binary solution containing solute (A) dissolved in a
diluent/carrier (B).
- The extracting solvent (C) can be either pure solvent or may content low concentration of
solute (A) (recycle solvent).
- When feed mixed with solvent, an intermediate phase M momentarily forms as the light
liquid moves through heavily liquid in the form of bubbles. These bubbles provide a large
surface area for contact between the feed solution and the solvent that speed up the mass
transfer process
- In most single stage LLE, it is interested to determine the equilibrium composition and
mass flowrates of extract and raffinate by using ternary phase diagram and mass
balance principle.
feed raffinate
% Removal=
= LoXAo-L1XA1 x100%
LoXAo
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Figure 3.2.1.1 Single stage equilibrium LLE
(a) Schematic diagram of LLE (b) Ternary phase diagram
- The material balance for the diagrams boundary in Fig 3.2.1.1 can be written as:-
Overall mass balance : LO + V2 = L1 + V1 = M (3.1)
Mass balance on comp. A : LOxAO + V2yA2 = L1xA1 + V1yA1 = MxAM (3.2)
Mass balance on comp. C : LOxCO + V2yC2 = L1xC1 + V1yC1 = MxCM ...(3.3)
- The points Lo, V2 and M can be plotted as shown in Fig 3.2.1.1 (b).
- Then using trial and error method to find tie line which can be drawn through the point M, that locates the
compositions of L1 and V1
- The amounts of L1 and V1 can be determined by substitution into Eqs. (3.1) - (3.3)
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EXERCISE 3.1
A single stage extraction is performed in which 400kg/h of a solution containing 40 wt% acetic acid in
water is contacted with 400kg/h of pure isopropyl ether. Determine:-
L1
Lo=400kg/h
xAo=0.4
xBo=0.6
xCo=0
M coordinate (0.2,0.3,0.5), make sure this point align with Lo-V2 line 21
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V2 (0,0,1) = (yA2, yA2 yC2)
V1 = (0.14,0.05,0.81) M
L1 = (0.29,0.68,0.03) L0(0.4,0.6,0) = (xA0, xB0, xC0)
Answer (B)
V1 = 480 kg/h
L1 = 320 kg/h
Answer (C)
% Removal=LoXAo-L1XA1 x100%=42%
LoXAo
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3.2.2 MULTIPLE STAGES OF LLE
- The material balance for the diagrams boundary in Fig 3.2.2.1 can be written as:-
Overall mass balance : LO + VN+1 = LN + V1 = M (3.4)
Mass balance on comp. A : LOxAO + VN+1yAN+1 = LNxAN + V1yA1 = MxAM (3.5)
Mass balance on comp. C : LOxCO + VN+1yCN+1 = LNxCN + V1yC1 = MxCM ..(3.6)
- Determination of LN and V1 flowrates will be as follows (Fig. 3.2.2.2-a):-
i. Plot the ternary diagram of the system
ii. Calculate the M coordinate (xAM, xCM) by using eqs (3.2 & 3.3) & locate the M coordinate accordingly on
the ternary diagram
iii. Locate the coordinates of VN+1 (yAN+1, yCN+1); LO (xAO, yCO) & LN (xAN,xCN). Coordinates of VN+1 & LN
must lie on the phase envelope/ boundary. Normally xAN (composition of solute at raffinate) will be
given.
iv. Plot line from LN to M V1( yA1, yC1). V1 coordinate must lie on the phase boundary.
v. Finally calculate the LN and V1 flowrates value by substituting the respective value using eq.( 3.4 3.6)
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- Determination of no of theoretical (graphical method) will be as follows (Fig. 3.2.2.2-b):-
i. Find reference coordinate. It is interception point between 2 operating lines:-
a) LO & V1 - Initial
b) LN & VN+1 - Final
ii. Start iteration from V1 to equilibrium diagram then back to ternary diagram to give L1 coordinate.
iii. Draw tie line from V1 to L1 1 stage
iv. Continue iteration from L1 to reference coordinate to give V2 2nd operating line
v. Continue the same procedure until the tie line intercept the final operating line.
vi. Finally, calculate the quantity of tie line in the diagram which represent the no of theoretical stages.
iv. The amounts of the extract and raffinate (V1: 663.63 kg/h, Ln:136.36 kg/h)
v. Percentage of the acetic acid is being removed from the system 82.9% .
vi. The number of theoretical stages (2.2-2.56)
2. Locate the coordinates of LO, VN+1, & LN (must lie on the equilibrium curve).
4. Plot line from LN to M V1 is located at the intersection of line LN-M with the
phase boundary
5. Line LoV1 and LNVN+1 are drawn and the intersection is the operating line
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C V1 VN+1
1. Plot the ternary diagram of the system Lo 1 N
Vn+1 LN
2. Locate the coordinates of LO, VN+1, &
LN (must lie on the equilibrium curve). V2
V1
3. Plot line from Lo to VN+1
4. Calculate the M coordinate (xAM, xCM), m
where M point located at line Lo VN+1
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3.3 LLE FOR IMMISCIBLE SOLVENT
- For the immiscible LLE, the material balance for the diagrams boundary in Fig 3.3 can be written as:-
OPERATING LINE
Where;
L = kg inert B/ h
V = kg inert C/ h
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- No. of theoretical stages are determine through the graphical method ( Fig. 3.3.2) from:-
i. Equilibrium line
ii. Operating line
yA1
yAN+1
xAN xo
Figure 3.3.2 : Graphical method for immiscible LLE
- Refer to example 12.7- 3 (P796) for further understanding.
Figure 3.4.1 (a) Compartmented mixing Figure 3.4.1(b) Horizontal gravity-settling vessel.
vessel with variable-speed turbine agitators CHE 347/ 251: UNIT OPERATIONS
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(a) Scheibel column-first design (b) Scheibel column-second design