CHE 303: Mass Transfer I
Extraction of Partially Miscible Systems
Dr. Mahbuba Jannat
Assistant Professor
Department of Chemical Engineering, BUET
[email protected] and +8801719068707
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Chapter Objective:
1. Plot extraction equilibria on a triangular diagram.
Find the saturated extract, saturated raffinate, and
conjugate lines.
2. Find the mixing point and solve single-stage and
cross-flow extraction problems.
3. For countercurrent systems, do the external mass
balances, find the difference points, and step off
the equilibrium stages
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Features:
❑ All extraction systems are partially miscible to some extent.
❑ When partial miscibility is very low, as for toluene and water, we can
treat the system as if it were completely immiscible and use McCabe-
Thiele analysis or the Kremser equation.
❑ When partial miscibility becomes appreciable, it can no longer be
ignored, and a calculation procedure that allows for variable flow rates
must be used. In this case a different type of stage-by-stage analysis,
which is very convenient for ternary systems, can be used.
❑ The number of independent variables that can be arbitrarily specified
(i.e., the degrees of freedom) for a system at equilibrium can be
determined from the Gibbs phase rule F = C − P + 2, which for a
ternary extraction is F = 3 − 2 + 2 = 3 degrees of freedom.
In an extraction, temperature and pressure are almost always constant
so only one degree of freedom remains. Thus, if we specify the
composition of one component in either phase, all other compositions
will be set at equilibrium.
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Table: Equilibrium data for the system water chloroform-acetone
at 1 atm and 25°C
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Extraction equilibrium data are easily shown graphically as
either right triangular diagrams or equilateral triangular
diagrams.
Figure: Equilibrium for water-chloroform-acetone at 25°C and 1 atm
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Figure. Construction of tie line using conjugate line
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Figure: Equilateral triangular diagrams
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Partially Miscible Single-Stage and Cross-Flow Systems
Figure. Continuous mixer-settler
Known variables: S, F, yA,S, yD,S, xA,F, xD,F, T, and p.
Desired variables: E, R, yA,E, yD,E, xA,R, and xD,R
The calculation method proceeds as follows:
1) Plot the locations of S and F on the triangular equilibrium
diagram.
2) Draw a straight line between S and F, and use the lever-arm
rule or Eqs. (18.3) to find the location of the mixed stream M.
Now we know that stream M settles into two phases in
equilibrium with each other. Therefore,
3) construct a tie line through point M to find the compositions of
the extract and raffinate streams.
4) Find the ratio E/R using mass balances. We will follow this
method to solve the following example.
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Example 18-1: A solvent stream containing 10% by weight
acetone and 90% by weight chloroform is used to extract acetone
from a feed containing 55 wt % acetone and 5 wt % chloroform
with the remainder being water. The feed rate is 250 kg/h, while
the solvent rate is 400 kg/h. Operation is at 25 °C and atmospheric
pressure. Find the extract and raffinate compositions and flow
rates when one equilibrium stage is used for the separation.
A. S = 400, yA,S = 0.1, yS,S = 0.9, yD,S = 0
F = 250, xA,F = 0.55, xS,F = 0.05, xD,F = 0.40.
Find xA,R, xD,R, yA,E, yD,E, R, and E.
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S = 400, yA,S = 0.1, yS,S = 0.9, yD,S = 0
F = 250, xA,F = 0.55, xS,F = 0.05, xD,F = 0.40.
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✓ From this example it is evident that a single extraction stage is
sufficient to remove a considerable amount of acetone from water.
However, quite a bit of solvent was needed for this operation, the
resulting extract phase is not very concentrated, and the raffinate
phase is not as dilute as it could be.
✓ The separation achieved with one equilibrium stage can easily be
enhanced with a cross-flow system
We found that cross-flow
systems are less efficient than
countercurrent systems. In the
next section the calculations for
countercurrent cascades will be
developed.
Figure: Cross-flow extraction; (A) cascade, (B) solution of triangular diagram
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Countercurrent Extraction Cascades for Partially Miscible Systems
The mass balances around the entire cascade are-
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Countercurrent Extraction Cascades for Partially Miscible Systems
The mass balances around the entire cascade are-
Thus, the difference in flow rates of passing streams is
constant even though both the extract and raffinate flow
rates are varying.
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Difference Points and Stage-by-Stage Calculations:
There are three methods for finding the location of Δ:
1. Graphical construction: Since the points Δ, E0, and R1; and Δ,
EN, and RN+1 are on straight lines, we can draw these two straight
lines. The point of intersection must be the Δ point. For the typical
design problem (see Figure below), points RN+1, E0, and R1 are easily
plotted. EN can be found from the external balances (Figure 13-
21B). Then Δ is found as shown in Figure below.
Figure: Location of difference point for typical design problem
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2. Coordinates. The coordinates of the difference point were found
in Eq. below. These coordinates can be used to find the location of Δ.
It may be convenient to draw one of the straight lines in method 1
(such as line ) and use one of the coordinates (such as xD,Δ) to find
Δ. This procedure is useful since accurate graphical determination of
Δ can be difficult.
3. Lever-arm rule. The general form of the lever-arm rule for two
passing streams is
The lever-arm rule can be used to find the Δ point. For instance, if
flow rates R1 and E0 are known, then Δ can be found on the straight
line through points R1 and E0 at a distance that satisfies Eq. above
with j = 0.
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Figure: Stage-by-stage solution
The stages are counted along the tie lines, which represent extract and
raffinate streams in equilibrium. To obtain an accurate solution, a large
piece of graph paper is needed and care must be exercised in
constructing the diagram.
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Complete Partially Miscible Extraction Problem
Example 18.2: A solution of acetic acid (A) in water (D) is to be
extracted using isopropyl ether as the solvent (S). The feed is 1000
kg/h of a solution containing 35 wt % acid and 65 wt % water. The
solvent used comes from a solvent recovery plant and is essentially
pure isopropyl ether. Inlet solvent flow rate is 1475 kg/h. The exiting
raffinate stream should contain 10 wt % acetic acid. Operation is at
20°C and 1 atm. Find the outlet concentrations and the number of
equilibrium stages required for this separation. The equilibrium data are
given by Treybal (1968) and are reproduced in Table below.
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Find the outlet concentrations and
F = 1000, xA,F = 0.35, xD,F = 0.65,
the number of equilibrium stages
S = 1475, yA,S = 0, yD,S = 0,
required for this separation.
xA,1 = 0.1.
F(0.65, 0.35)
N = 5.8
E5
E4
E3
E2
E1
S(0, 0)
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Problem D9. We are extracting acetic acid from water with isopropyl
ether at 20°C and 1 atm pressure. Equilibrium data are in Table below.
The column has three equilibrium stages. The entering feed rate is 1000
kg/h. The feed is 40 wt % acetic acid and 60 wt % water. The exiting
extract stream has a flow rate of 2500 kg/h and is 20 wt % acetic acid.
The entering extract stream (which is not pure isopropyl ether) contains
no water. Find:
a. The exit raffinate concentration. (xA,1=?)
b. The required entering extract stream concentration. (yA,0=?, yS,0=?)
c. Flow rates of exiting raffinate and entering extract streams (R1, S=E0
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Solution:
F = RN+1= 1000, xA,F = 0.40, xD,F = 0.60,
Eo=S=?, yA,0= ? , yD,o=0
EN = 2500, yA,N = 0.20,
R3 Find:
R2 a. The exit raffinate concentration.
(xA,1=?)
b. The required entering extract stream
concentration. (yA,0=?, yS,0=?)
E2 c. Flow rates of exiting raffinate and
E1
entering extract streams (R1, S=E0
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Two-Feed Extraction Column:
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Problem D1. The equilibrium data for extraction of methylcyclohexane
(A) from n-heptane (D) into aniline (S) are given in Table below. We
have 100 kg/h of a feed that is 60% methylcyclohexane and 40%
nheptane and 50 kg/h of a feed that is 20% methylcyclohexane and
80% n-heptane. These two feeds are mixed with 200 kg/h of pure
aniline in a single equilibrium stage.
a. What are the extract and raffinate compositions leaving the stage?
b. What is the flow rate of the extract product?
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