Liquid Liquid Extraction
Liquid Liquid Extraction
Extraction
Introduction
• Liquid-liquid extraction (solvent extraction): is the separation of the
constituents of a liquid solution by contact with another insoluble
liquid.
• It is a mass transfer operation in which a liquid solution (feed) is
contacted with an immiscible or nearly immiscible liquid (solvent)
that exhibits preferential affinity or selectivity towards one or more
of the components in the feed.
Important terms
• The solution which is to be extracted is called the feed,
• the liquid with which the feed is contacted is called the solvent.
• The solvent rich product of the operation is called the extract,
the residual liquid from which the solute has been removed is
the raffinate.
Working Principles of Liquid-liquid
extraction
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.
C
SOLVENT C+A+B
EXTRACT
RAFFINATE
B+A+C
A+B
FEED
• In liquid-liquid extraction, a soluble component (the
solute) moves from one liquid phase to another.
• The two liquid phases must be either immiscible, or
partially miscible.
Extract (C+A+B)
Acetic acid (A) Organic layer contains most of
in Water (B) acetic acid in ethyl acetate with a
small amount of water.
+
Ethyl acetate Raffinate (B+C+A)
(C) Aqueous layer contains a weak
acetic acid solution with a small
amount of ethyl acetate.
Advantages Disadvantages
Reliable scale up techniques. Large amounts of floor space
required.
Can handle high flow rates. Only systems with a few stages
are economical.
Advantages Disadvantages
It has no internal parts except for Inefficient.
the spray nozzles and hence
eliminate the scale buildup and
plugging problem.
Low cost
Typical liquid-liquid extraction
equipment
Packed Extraction Tower
Advantages Disadvantages
Highly efficient when only a few Suffer from solids plugging
stages are needed.
Light
Heavy Phase Out
Phase In
Vessel Shaft
Walls
Stators Rotors
Light
Phase In
rotating-disk contactor
a. agitator; b. stator disk
Interface Interface
Control
Mixer-settlers operate with a purely stage-wise contact.
After every mixer there is a settler. Mixer-settlers can be
Heavy
Phase Out operated in a multistage, co- or countercurrent fashion.
Typical liquid-liquid extraction
equipment
Mechanically agitated extraction tower
Advantages Disadvantages
Mechanical parts result in good Repair of internal mechanical
dispersion. parts can cause process delays.
• The more insoluble the liquid A and B , the nearer the apexes of the
triangle will points L and K be located.
• Curve LPK is a bimodal solubility
curve indicating the change in solubility
of the A-and B-rich phases upon addition
of C.
Any ternary mixture underneath the curve, such as M, will form two
insoluble saturated liquid phase of equilibrium compositions indicated
by a (A-rich) and b (B-rich).
•
water content (xA) : 0.19
Ethylene glycol content (xB): 0.20
Furfural content (xC): 0.61
check: xA + xB + xC = 1
• •
Solution:
L y A − x AM
= (5.5)
V x AM − x A
V
• Similarly combining Eqs (5.2) and (5.4) M
L mixer
L yC − xC M
=
V xC M − xC
(5.6)
xC − xC M xC M − y C
= (5.7)
x A − x AM x AM − y A
Eqn. 5.7 shows that points L, M, and V must lie on a straight line.
By using the properties of similar right triangles,
L( kg ) VM (5.8)
=
V ( kg ) LM
L( kg ) VM
= (5.9)
M ( kg ) LV L
•
M
•
V similar triangles
•
Example 5.4
The compositions of the two equilibrium layers in Example 5.1 are
for the extract layer (V1) yA = 0.04, yB = 0.02, and yC = 0.94, and for
the raffinate layer (L1) xA = 0.12, xB = 0.86, and xC = 0.02. The original
mixture contained 100 kg and xAM = 0.10. Determine the amounts of
V1 and L1.
V2
Given: M= 100 kg, xAM = 0.10
V1
Solution:
Substituting into eq. 5.2
𝑉1 + 𝐿1 = 𝑀 = 100 (a)
A balance on A: L0 x A0 + V2 y A2 = L1 x A1 + V1 y A1 = Mx AM 5.11
L0 L1
L0 x A0 + V2 y A2 = MxAM
x AM = 0.157
Similarly
xc 0 = 1 − x A0 − xB 0 = 1.0 − 0.235 − 0.765 = 0
L0 xC 0 + V2 yC 2 = MxC M
(1000 )(0) + (500)(1) = (1500 ) xC M
xCM = 0.33
V2 (0,1) = (yA2, yC2)
V1 (0.1,0.89) = (yA1, yC1)
L1 xA1 + V1 y A1 = MxAM
L0 x A0 + V2 y A2 = MxAM
L0 xC 0 + V2 yC 2 = MxC M
xCM = 0.5
Draw the equilibrium diagram and Locate point,
L0, V1 and M
• Using trial and error, the tie V2 (0,1) = (yA2, yC2)
V1 (0.12,0.87) = (yA1, yC1)
line is drawn through point
M that determines the
M(0.175,0.5) = (xAM, xCM)
composition of LN and V1
L1(0.22,0.03) = (xA1, xC1)
• From the graph: M
xA1 = 0.22 and
L0(0.35,0) = (xA0,
yA1 = 0.12;
L1 xA1 + V1 y A1 = MxAM
L0 xC 0 + V N +1 y CN +1 LN xCN + V1 y C1 5.15
Combining 5.13 and 5.14 x CM = =
L0 + V N +1 LN + V1
L0 x A0 + VN +1 y AN +1 LN x AN + V1 y A1
Balance on component A gives x AM = = 5.16
L0 + VN +1 LN + V1
Countercurrent process and overall balance
1. Usually, L0 and VN+1 are known and the
desired exit composition xAN is set.
mixing line 2. Eqs (5.15) and (5.16) can be used to
calculate the coordinates of point M and
phase diagram, which ties together the
tie-line two entering streams Lo and VN+1 and
the two exit streams V1 and LN.
3. Plot points L0, VN+1, and M as in the
figure, a straight line called mixing line
must connect these three points (points
are collinear).
4. LN, M, and V1 must lie on one line
called tie line. Also, LN and V1 must also
lie on the phase envelope.
Flow rates of LN and V1 are related by mass balance. Compositions of LN and
V1 are also related by equilibrium.
Example 5.6
L0 + V2 = L1 + V1 5.17
Total mass balance on stage 1
Ln −1 + Vn +1 = Ln + Vn 5.18
Total mass balance on stage n
L0 − V1 = L1 − V2 = 5.19
From 5.16 obtain difference Δ in flows
Δ in kg/h is constant and for all stages
= L0 − V1 = Ln − Vn+1 = LN − VN +1 = ....
5.20
L0 x0 − V1 y1 Ln xn − Vn+1 y n+1 LN x N − VN +1 y N +1
x = = = 5.22
L0 − V1 Ln − Vn+1 LN − VN +1
Eqns (5.19) and (5.20) can be written as
L0 = + V1 Ln = + Vn+1 LN = + V N +1 5.23
Stage-to-stage calculations for countercurrent
extraction.
1. Δ is a point common to all streams
passing each other, such as L0 and V1,
Ln and Vn+1, Ln and Vn+1, LN and
VN+1, and so on.
2. This coordinates to locate this Δ
operating point are given for xcΔ and
xAΔ in eqn. 5.21. Since the end points
VN+1, LN or V1, and L0 are known, xΔ
can be calculated and point Δ located.
3. Alternatively, the Δ point is located
graphically in the figure as the
intersection of lines L0V1 and
LN VN+1.
4. In order to step off the number of stages
using eqn. 5.23 we start at L0 and draw
the line L0Δ, which locates V1 on the
phase boundary.
V3
5. Next a tie line through V1 locates L1,
V2 which is in equilibrium with V1.
6. Then line L1Δ is drawn giving V2. The
tie line V2L2 is drawn. This stepwise
procedure is repeated until the
desired raffinate composition LN is
reached. The number of stages N is
obtained to perform the extraction.
N1
N2
Example 5.7
Pure isopropyl ether of 450 kg/h is being used to extract an
aqueous solution of 150 kg/h with 30 wt% acetic acid (A) by
countercurrent multistage extraction. The exit acid
concentration in the aqueous phase is 10 wt%. Calculate the
number of stages required.
Assignment (2 people/1 person)
Pure isopropyl ether of 500 kg/h is being used to extract an
aqueous solution of 250 kg/h with 30 wt% acetic acid (A) by
countercurrent multistage extraction. The exit acid
concentration in the aqueous phase is 10 wt%. Calculate the
number of stages required, and amount of LN and V1.
Solution:
(yA1, yB1, yC1) (yA,N+1, yB,N+1, yC,N+1)
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Solution (Cont.)
71
Continuous multistage countercurrent extraction
x y x y 5.24
L 0 + V n +1 = L n + V 1
1 − x0 1 − y n +1 1 − xn 1 − y1
Where L’ = kg inert B/h, V’ = kg inert C/h, y = mass fraction A in V stream, and
x = mass fraction A in L stream. Eq.(5.24) is an operating-line equation whose
slope ≈ L’/V’. If y and x are quite dilute, the line will be straight when plotted on an
xy diagram.
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Ex ample 5.8
An inlet water solution of 100 kg/h containing 0.010 wt fraction nicotine
(A) in water is stripped with a kerosene stream of 200 kg/h containing
0.0005 wt fraction nicotine in a countercurrent stage tower. The water and
kerosene are essentially immiscible in each other. It is desired to reduce
the concentration of the exit water to 0.0010 wt fraction nicotine.
Determine the theoretical number of stages needed. The equilibrium data
are as follows (C5), with x the weight fraction of nicotine in the water
solution and y in the kerosene.
x y x y
0.00101 0 0.000806 0.00746 0.00682
0.00246 0.001959 0.00988 0.00904
0.00500 0.00454 0.0202 0.0185
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Solution:
The given values are
L0 = 100 kg/h, x0 = 0.010,
VN+1 = 200 kg/h, yN+1 = 0.0005,
xN = 0.0010.
The inert streams are
The equilibrium line is also shown. The number of stages are stepped off,
giving N = 3.8 theoretical stages.
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