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CENG 3210

Separation Process

CENG 3210_1

Lecture 8: Extraction
Learning Outcomes
By the end of this lecture, you should be able to:

Understand the use of McCabe-Thiele Method


for dilute and immiscable solvent
Understand the Method for cross flow multistage
extraction
Understand the multistage extraction for partially
miscable LLE.

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Liquid-Liquid Extraction

CENG 3210_3

Immiscible solvents

McCabe-Thiel analysis is similar to the analysis for absorption


and stripping
For linear system, Kremsers equation is also applicable
Concentrations are expressed as weight fraction or weight ratio
Flow rates are expressed as mass flow rates
CENG 3210_4

McCabe-Thiele Method
Mass Balance Envelope for Simple Countercurrent Cascade

= diluent flow rate, kg D/hr


= solvent flow rate, kg S/hr

= weight ratio solute in diluent


=weight ratio solute in solvent

=
=

= weight fraction solute in raffinate


= weight fraction solute in extract

raffinate flow rate, kg/hr


extract flow rate, kg/hr

both y and x are liquid


Assumptions:
1. Isothermal
(liquid-liquid absorption)
2. Isobaric

=
3. Negligible heat of mixing
1
4. Diluent and solvent are totally immiscible
CENG 3210_5

solute free basis

=
1

McCabe-Thiele Method
Method 1: use mass fraction (valid for dilute systems).

= 0 = 1 = =
= +1 = = 1 =
Mass balance around the envelope:
+1 + 0 = 1 +

Solving for yj+1 we obtain the


operating line

+1 = + [1 0 ]

CENG 3210_6

McCabe-Thiele Method
Method 2: use weight ratio
Operating line

+1

=
+ [1 0 ]

Note:
Method 1 & 2 will essentially give the
same results for very dilute systems.
Use method 2 if the system is
concentrated (say, x & y > 0.05), and
carrier & solvent are still immiscible.
Kremser equation for stripping (i.e. in
terms of liq. phase composition) can be
used directly for extraction.
Mole fraction becomes mass fraction and
L/V replaced with R/E
Mole fraction becomes mass ratio and
L/V replaced with FD/FS

CENG 3210_7

Kremser Method for Dilute Systems (optional)


Assumptions: 1) dilute system and 2) linear equilibrium relationship

= +

We can use the Kremser equations directly, but we have used different different
symbols for flow rates, replace L/V with R/E.

+1 1
=

1 0

=1

1 1
=

+1 1

=
CENG 3210_8

1
+1
1

ln [ 1

1 = 0 +

+1 1

+
]
1 1

ln (
)

Kremser Type Plot (optional)


YBE

E1

1.0
0.8
0.6

F1

E = 0.3

0.4
0.3

XBF

S1

YBS
XBR

R1

E = Extraction Factor
E = m (S1/F1)

XBR/XBF = Fraction Unextracted

0.2

0.1
0.08
0.06
0.04
0.03
0.02

0.01
0.008
0.006
0.004

0.003
0.002

0.001
0.0008
0.0006
0.0005

4 5

Number of Ideal Stages

CENG 3210_9

7 8 10 15 20

Example 1
A feed of 100.0 kg/minute of a 1.2 wt % mixture of acetic acid in water is to be
extracted with 1-butanol at 1 atm pressure and 26.7. We desire an outlet
concentration of 0.1 wt % acetic acid in the exiting water. We have available
solvent stream 1 that is 44.0 kg/minute of pure 1-butanol and solvent stream 2 that
is 30.0 kg/minute of 1-butanol that contains 0.4 wt of acetic acid. Devise a scheme

to do this separation, find the outlet flow rate and concentration of the exiting 1butanol phase, and find the number of equilibrium contacts needed.
Equilibrium data: = 1.613.

CENG 3210_10

Cross Flow Extraction

E1

E2
B+C

A+B
F

R1

B+C

R2
C

F + S = M1

CENG 3210_17

E3

E4
B+C

R3
C

R1 + S = M 2

B+C

R4
C

R 2 + S = M3

A
C

R3 + S = M 4

Single-stage and cross-flow extraction


One type occasionally used is the cross-flow cascade,

For dilute systems the resulting steady-state mass balance for stage j is
For single-solute systems the same five assumptions made for counter-current cascades are
required for the McCabe Thiele analysis.

1 + , = +
Solving for yj to obtain the operating equation,

= + ( 1 + , )

CENG 3210_18

Multiple stages with cross flow of solvent


If the process liquid stream from the first stages fed into a second

extractor and mixed with more fresh solvent, as shown in the Figure,
we have what is called cross-flow extraction.
The process can be described the same as for a single stage. it is simply
repeated again for each stage, using the raffinate phase from the
upstream stage as the feed to each stage.

CENG 3210_19

Single-stage and cross-flow extraction


Each stage will have a different operating equation. On a McCabe-Thiele diagram
plotted as y vs. x, this is a straight line of slope R/Ej and y intercept (yj, in , xj1)
Designer can specify values of Ej and yj, in as well as x0, R, and either xN or N.

CENG 3210_20

Example 2
We wish to extract a dilute solution of the protein alcohol dehydrogenase from a aqueous solution of
5 wt % poly (ethylene glycol) (PEG) with an aqueous solution that is 10 wt % dextran. Aqueous
two-phase extraction system is a very gentle method of recovering proteins that is unlikely to
denature the protein since both phases are aqueous (Albertsson et al., 1990; Harrison et al., 2003).
The two phases can be considered to be essentially immiscible. The dextran phases is denser and
will be the cross-flow solvent. The entering dextran phases contain no protein. The entering PEG
phase flow rate is 20 kg/hr.

a. If 10 kg/hr of dextran phase is added to a single-stage extractor, find the total recovery fraction of
alcohol dehydrogenase in the dextran solvent phase.

b. If 10 kg/hr of dextran phase is added to each stage of a cross-flow cascade with two stages, find
the total recovery fraction of alcohol dehydrogenase in the dextran solvent phase.
The protein distribution coefficient is (Harrison et al., 2003)

= (wt frac protein in PEG, x)/(wt frac protein in dextran, y) = 0.12

CENG 3210_21

Extraction of Concentrated Solution


Ternary System

Most practical situations involving liquid-liquid equilibrium involve


three or more components.

Our attention is with three component systems. In this process, a


solute is removed from a feed stream by contacting it with a
solvent.

The solute is quite soluble in the solvent, while the other


component in the feed is less soluble.

CENG 3210_28

Extraction of Concentrated Solution


Extraction of Concentrated Solution

CENG 3210_29

Example 3 Single-stage extraction


In an extraction process we have two entering streams (L kg and
V kg). The solvent, as stream V2, enters from one side and the
stream L0 enters from the other side. The two entering streams
are mixed and equilibrated and then exit as streams L1 and V1,

which are in equilibrium with each other. Find the final product
compositions in the two phases

CENG 3210_30

Example 4
Example 4: 30,000 kg/hr of a ternary
mixture of 19 weight percent

isopropyl alcohol (IPA, component 1),


41 weight percent toluene, and 40
weight percent water (component 3)
are fed into a decanter operating at
25C. The figure gives the LLE data
for the system. Determine the
compositions and flow rates of the

two liquid streams leaving the


decanter.

CENG 3210_33

Multistge countercurrent extraction


Multistage

countercurrent

extraction

is

the

most

commonly

encountered liquid-liquid extraction process. The raffinate and


solvent streams travel countercurrent to each other through N
stages. The flow rate of the raffinate leaving the last stage (tray N) is

R.

CENG 3210_36

Multi-stage extraction
E1

B+C
A+B
F

R1
B+C

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B+C

R2

E3

R3
E2

R4
B+C

E4

Multi-stage extraction
The overall balance on all N stages is

0 + +1 = + 1 =
where
M is the total mass (kg/h) and is a constant,
L0 the inlet feed flow rate (kg/h),

VN+1 the inlet solvent flow rate (kg/h),


V1 the exit extract stream, and
LN the exit raffinate stream.

CENG 3210_38

Multi-stage extraction
Material balance on C gives

0 ,0 + +1 ,+1 = , + 1 ,1 = ,
xCM is obtained
,

0 ,0 + +1 ,+1 , + 1 ,1
=
=
0 + +1
+ 1

CENG 3210_39

0 ,0 + +1 ,+1 , + 1 ,1
=
=
0 + +1
+ 1

Multi-stage extraction
So the point M, which ties together the two entering streams (usually known) and the two exit
streams, can be located.
The desired exit composition xAN is
often set, which is on the equilibrium
curve (phase boundary). Then the line
LNM is extended to intersect the phase
boundary of the extract phase to give V1
composition.

CENG 3210_40

Example 5
Example 5: Pure solvent isopropyl ether (C) at the rate of +1 = 600 kg/h is being used to
extract an aqueous solution of 0 = 200 kg/h containing 30 wt % acetic acid (A) and 70 wt %
water (B) by countercurrent multistage extraction. The desired exit acetic acid concentration

in the aqueous phase is 4%. Calculate the compositions and amounts of the ether extract 1
and the aqueous raffinate . The equilibrium data at 20oC, 1 atm, are given and plotted
below.
isopropyl ether phase (mass fraction)

Water phase
(mass fraction)
acetic acid
(xA)

Water (xB)

isopropyl ether (xC)

acetic acid
(yA)

Water (yB)

isopropyl ether (yC)

6.9e-3

0.9810

0.0120

1.8e-3

5.0e-3

0.9930

0.0141

0.9710

0.0150

3.7e-3

7.0e-3

0.9890

0.0289

0.9550

0.0160

7.9e-3

8.0e-3

0.9840

0.0642

0.9170

0.0190

0.0193

0.0100

0.9710

0.1330

0.8440

0.0230

0.0482

0.0190

0.9330

0.2550

0.7110

0.0340

0.1140

0.0390

0.8470

0.3670

0.5890

0.0440

0.2160

0.0690

0.7150

0.4430

0.4510

0.1060

0.3110

0.1080

0.5810

0.4640

0.3710

0.1650

0.3620

0.1510

0.4870

CENG 3210_41

Single stage Extraction


1. Calculate M.
2. Calculate xAM and xCM.
3. Locate the point M using xAM and xCM .
4. Find the LLE tie-line that passes through the
point M.
5. The points at the two ends of the LLE tie-line
give the compositions of the two phases
leaving the system.
6. 6. Calculate the flow rates

CENG 3210_46

Multi-stage extraction
The next step is to go stage by stage to determine the concentrations at each stage
and the total number of stages N needed to reach LN in the process.

Making a total balance on stage 1


0 + 2 = 1 + 1
on stage n

1 + +1 = +

The above equations can be rearranged as


0 1 = 1 2 = = +1 = +1 =
CENG 3210_47

Multi-stage extraction
The mass balances for the first stage, the definition of can be
combined to give

0 1 = 1 2 = = +1 = +1 =

The two streams L1 and V2 that pass each other between the first and
second stages are related to each other by the point. Hence, if

we know L1 we can determine V2 by using the straight line that


connects L1 and .

CENG 3210_48

Multi-stage extraction
The coordinates of the operating point

can be obtained by

material balances on A, B or C:
0 0 1 1 = = +1 ,+1 = xA
0 0 1 1 = = +1 ,+1 = xC

(0 0 1 1 ) , +1 ,+1
=
=
0 1
+1

CENG 3210_49

Multi-stage extraction
The pseudo composition , is entirely fictitious and, therefore, can
be less than zero or greater than unity.
We see that

0 1 = 1 2 = = +1 = +1 =
Therefore, the point must lie on two straight lines, one through the
points LN and VN+1 and the other through the points L0 and V1.

CENG 3210_50

Multi-stage extraction
can lie either to the left or to the right of the phase diagram.

V1
LN
V0

V1

LN
V0

CENG 3210_51

Multi-stage extraction
This point

is located

either by its coordinates as


calculated or graphically as
the intersection of lines

L0V1 and LNVN+1. All the


operating lines (L0V1,
L1V2, LnVn+1, ... , LNVN+1)

must pass through the


common point .

CENG 3210_52

Example 6
Example 6: Number of stages in countercurrent extraction
Pure isopropyl ether (C) of 450 kg/h is being used to extract
an aqueous solution of 150 kg/h with 30 wt % acetic acid
(A) and 70 wt % water (B) by countercurrent multistage

extraction. The exit acid concentration in the aqueous phase


is 10 wt %. Calculate the number of stages required.

CENG 3210_53

Multi-stage extraction
To graphically determine the number of stages, follow the
procedures below.
(1)
locate L0, VN+1 and LN by their compositions.
(2)
draw a line L0VN+1, and locate the mixture point M
(3)
draw a line from LN through M & extend it until it
intersects the phase boundary, where is V1.
(3)
extend lines L0V1, and LNVN+1, which will intersect at
the common operating point .
(4)
start at L0 and draw a line L0 which intersects the
phase boundary at V1.
(5)
draw an equilibrium tie line through V1 to locate L1.
(6)
draw a line L1 to give V2 at the phase boundary.
(7)
a tie line from V2 gives L2. This is continued until the
desired LN is reached.
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Take home message


Understand the calculation of single stage
extraction.
Understand the graphical method of multistage
cross flow extraction.
Understand the graphical method of multistage
countercurrent extraction.

CENG 3210_60

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