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Mass Transfer Operations Robert Treybal

Sample Problems

1. If 100 kg of a solution of acetic acid (C) and water (A) containing 30% acid is to be
extracted three times with isopropyl ether (B) at 20C, using 40kg of solvent in each
stage, determine the quantities and compositions of the various streams. How much
solvent would be required if the same final raffinate concentration were to be obtained
with one stage?

Solution. The equilibrium data at 20C are listed below [Trans. AIChE, 36, 628 (1940),
with permission]. The horizontal rows give the concentrations in equilibrium solutions.
The system is of the type shown in Fig 10.9, except that the tie lines slope downward
toward the B apex. The rectangular coordinates of Fig. 10.9a will be used, but only for
acid concentrations up to x=0.30. These are plotted in Fig. 10.15.
Stage 1 F=100 kg, xF=0.30, yS=0, S1=B1=40 kg

OMB:

M1=100+40=140 kg

x bal:

100(0.30)+40(0)=140xM1 => xM1=0.214

Point M1 is located on line FB. With the help of a distribution curve, the tie line passing through
M1 is located as shown, and x1=0.258, y1=0.117 wt fraction acetic acid.
140(0.2140.258)
1 = = 43.6
0.1170.258

R1=140-43.6=96.4 kg

Stage 2 S2=B2=40 kg

M2=R1+B2=96.4+40=136.4 kg

Point M2 is located on line R1B and the tie line R2E2 through M2.x2=0.227, y2=0.095 become
2 (2 2 ) 136.4(0.18220.227)
2 = = = 46.3
2 2 0.0950.227

R2=M2-E2=136.4-46.3=90.1 kg

Stage 3. In a similar manner, B3=40, M3=130.1, xM3=0.1572, x3=0.20, y3=0.078, E3=45.7 and
R3=84.4. The acid content of the final raffinate is 0.20(84.4)=16.88 kg.
The composited extract is E1+E2+E3=43.6+46.3+45.7=135.6 kg and its acid content =
E1y1+E2y2+E3y3=13.12 kg.

If an extraction to give the same final raffinate concentration, x=0.20, were to be done in
one stage, the point M would be at the intersection of tie line R3E3 and line BF or at xM=0.12.
The solvent required would then be, by, S1=100(0.30-0.12)/(0.12-0)= 150 kg, instead of the total
of 120 required in the three-stage extraction.

2. Nicotine (C) in a water (A) solution containing 1% nicotine is to be extracted with


kerosene (B) at 20C. Water and kerosene are essentially insoluble. (a) Determine the
percentage extraction of nicotine if 100 kg of feed solution is extracted once with 150 kg
solvent. (b) Repeat for three theoretical extractions using 50 kg solvent each.

Solution. Equilibrium data are provided by Claffey et al., Ind. Eng. Chem., 42, 166
(1950), and expressed as kg nicotine/kg liquid, they are as follows:

(a) xF= 0.01 wt fraction nicotine, xF= 0.01/(1-0.01)= 0.0101 kg nicotine/ kg


water. F= 100 kg. A= 100(1-0.01)= 99 kg water, A/B= 99/150 = 0.66.
Refer to the figure which shows the equilibrium data and the point F
representing the composition of the feed. From F, line FD is drawn of slope -
0.66, intersecting the equilibrium curve at D where x1=0.00425 and
y1=0.00380 kg nicotine/kg liquid. The nicotine removed from the water is
therefore 99(0.0101-0.00425)= 0.580 kg, or 58% of that in the feed.
(b) For each stage, A/B=99/50= 1.98. The construction is started at F, with
operating lines of slope -1.98. The final raffinate composition is x3=0.0034
and the nicotine extracted is 99(0.0101-0.0034)= 0.663 kg or 66.3% of that in
the feed.

3. If 8000 kg/h of an acetic acid (C)- water (A) solution, containing 30% acid is to be
counter currently extracted with isopropyl ether (B) to reduce the acid concentration to
2% in the solvent-free raffinate product, determine (a) the minimum amount of solvent
which can be used and (b) the number of theoretical stages if 20 000 kg/h of solvent is
used.

Solution. The equilibrium data are plotted on triangular coordinates in the figure. The tie
lines have been omitted for clarity.

(a) F= 8000 kg/h; xF=0.30 wt fraction acetic acid, corresponding to point F on the figure RN,
as shown. In this case the tie line J, which when extended passes through F, provides the
conditions for minimum solvent, and this intersects line RNB on the right of the figure
nearer B than any other lower tie line. Tie line J provides the minimum E1 as shown at
y1=0.143. Line E1mRN, intersects line FB at Mm, for which xM=0.114 with ys=0 and S=B:

8000(0.30)
=
= 0.114
8000 = 13 040 kg/h, min solvent rate
(b) For B= 20 000 kg solvent/h with yS=0 and S=B
8000(0.30)
= = = 0.0857
+ 8000 + 20 000
and point M is located as shown on line FB. Line extended provides E1 at y1=0.10. Line
FE1 is extended to intersect line RNB at R. Random lines such as OKL are drawn to provide yS+1
at K and xS at Ls as follows:

These are plotted on the figure as the operating curve, along with the tie-line data as the
equilibrium curve. There are required 7.6 theoretical stages. The weight of extract can be

Obtained by an acid balance,


( ) 28 000(0.0857 0.02)
1 = = = 23 000 /
1 0.10 0.02

= 1 = 28 000 23 000 = 5000 /

4. If 1000 kg/h of a nicotine (C)-water (A) solution containing 1% nicotine is to be counter


currently extracted with kerosene at 20C to reduce the nicotine content to 0.1%,
determine (a) the minimum kerosene rate and (b) the number of theoretical stages
required if 1150 kg of kerosene is used per hour.

Solution. The equilibrium data of number 2 are plotted in the figure below

(a) F=1000 kg/h, xF=0.01, A=1000(1-0.01)= 990 kg water/h, ys=0


0.01
= = 0.0101
1 0.01
0.001
= 0.001 = = 0.001 001
1 .001

The operating line starts at point L (y=0, x=0.001 001) and for infinite stages passes through K
on the equilibrium curve at xF. Since yK=0.0093,
0.00930
= 0.01010.001001 = 1.021

Bm=A/1.021= 990/1.021= 969 kg kerosene/h

(b) B=1150 kg/h, A/B=990/1150= 0.860


1 1
= = 0.860
0.0101 0.001001
y1=0.00782 kg nicotine/kg kerosene

The operating line is drawn through (y1,xF) and 8.3 theoretical stages are determine graphically.

Alternatively, at the dilute end of the system, m=dy*/dx=0.798, and


0.798(1150)
= = 0.928
990

At the concentrated end, m=0.953, and mB/A=0.953(1150)/990=1.110. The average is


0.001001
[0.928(1.110)]]0.5=1.01. = = 0.099 and the figure indicates 8.4 theoretical stages.
0.0101

Illustration 10.9 Determine the number of transfer units NTU for the extraction of illustration
10.3 if 20,000kg/h of solvent is used.

Solution: Define x and y in terms of weight fractions acetic acid, x1=xF=0.30; y2=0; x2=0.02;
y1=0.10. The operating diagram is already plotted in Fig. 10.2. From this plot, values of x and x*
are taken from the operating line and equilibrium curve at various values of y, as follows:

x 0.30 0.35 0.30 0.15 0.10 0.05 0.02

x* 0.230 0.192 0.154 0.114 0.075 0.030 0

1 14.30 17.25 20.75 27.8 40.0 50.0 50.0



1
The area under a curve of x as abscissa against as ordinate (not shown) between x=
0.30 and x = 0.02 is determined to be 8.40. In these solutions, the mutual solubility ofwater and
18
isopropyl ether is very small, so that r can be taken as 60 = 0.30. Eq.(10.110):

1 10.02 1 0.02(0.31)+1
= 8.40 + ln 10.30 + 2 ln 0.30(0.31)+1 = .
2

Illustration 10.10 Determine the number of transfer units NTU for the extraction of illustration
10.4 if 1150 kg/h of kerosene are used.

Solution: Use weight-ratio concentration as in Illustration 10.4. x1=xF=0.0101; y2=0;


x2=0.001001; y1=0.0782. The calculation can be done through Eq.(10.116) of the equivalent,
Fig. 8.20

2 2
= 0.001001 = 0.0909
1 2 0.0101


The average mE/R = mB/A = 1.01 (Illustration 10.4) From fig. 8.20, NTU = 8.8

Mc Cabe

23.5. In a continuous countercurrent train of mixer-settlers, 100 kg/h of a 40:60 acetone water
solution is to be reduced to 10 percent acetone by extraction with pure 1,1,2-trichloroethane at
25. (a) Find the minimum solvent rate. (b) At 1.8 times the minimum (solvent rate)/(feed rate),
find the number of stages required. (c) For conditions of part (b) find the mass flowrats of all
streams. Data are given in Table 23.6

Solution:
(a) Basis: 100 kg feed solution

Let x,y refer to the wt. fraction of acetone: xw, yw to water, xT,yT to trichloroethane.

Plot the equilibrium line xe, ye

Establish the ends of the operating line from overall material balances.

Balances:

Overall: Lb + Va = Vb +100

Acetone: 0.1 Lb + yaVa = xaLa =40

At minimum solvent rate, ya is found from the equilibrium curve at xa = 0.40 to be 0.53

Hence 0.1Lb + 0.53Va = xaLa = 40

Water: ywaVa + xwbLb = 60

When xb = 0.10, from the first part of Table 23.6, xTb = 0.0061

From these, Vb = 26.46, Va = 63.61

Lb = 62.85

The minimum solvent rate is 26.46

(b) Vb = 1.8 times the minimum


= 1.8 x 26.46 = 47.63

As before, from a water balance:

YwaVa + xwbLb = 60

Overall: Lb = 100 - 47.63 Va

Xwb is unchanged at 0.8939


Hence Lb = (60 147.63ywa)/(0.8939 ywa)

Va = 147.63- Lb

By trial, estimate ywa to be 0.028

Lb=64.52; Va = 83.11

ya = (40 0.1Lb)/Va = 0.404

From the equilibrium data for ya = 0.404, ywa = 0.028 (as estimated). Hence the upper end of the
operating line is at xa = 0.40, ya=0.404

The lower end is at xb = 0.10, yb = 0

Intermediate point. Set x=0.25

Estimate xT to be 0.01; xw = 1-.25- 0.01 = 0.74

Overall balance from feed end:

V = L + Va La = L + 83.11 100

=L 16.89 (A)

Estimate: y = 0.22, yw = 0.0089

From an acetone balance:

yV= (0.404 x 83.11) + 0.25L 40

y = (0.25L 6.42)/V (B)

Water balance:

ywV = 0.74L + (0.028 x 83.11) 60 (C)

From Eqs. (A) and (C):

L = 78.69, V=61.80

From Eq. (B), y = 0.214. From the equilibrium curve, yw = 0.0089, as estimated. The coordinates
of the intermediate point are x= 0.25, y= 0.214

The operating line is almost straight. From the diagram 2.8 stages are needed. Use 3 stages.
(c) The flow rates, in kg/h, are

Feed: 100 Extract: 83.11

Solvent: 47.63 Raffinate: 64.52

23.6 A mixture containing 40 weight percent acetone and 60 weight percent water is contacted
with an equal amount of MIK. (a) What fraction of the acetone can be extracted in a single-stage
process? (b) What fraction of the acetone could be extracted if the fresh solvent were divided
into two parts and two successive extractions used?

Solution:

(a) Adding an equal amount of MIK to the feed gives a mixture with 0.5 MIK, 0.2 acetone,
and 0.3 H2O. A tie line through this point on Fig. 23.8 shows the extract to be 0.725 MIK,
0.232 acetone, and 0.043 H2O. The raffinate composition is 0.023 MIK, 0.132 acetone,
and 0.845 H2O.

Per unit mass of feed, an acetone balance gives


0.4 = 0.23E + 0.132R
E+R= 1 + 1 = 2.0
0.4 = 0.232E + 0.132(2-E)
0.40.264
E=0.232=0.132= 1.36
1.32(0.232)
Fraction acetone extracted = = 0.789
0.4

(b) If onlye half the MIK is added in the first step, the mixture is 0.333 MIK, 0.267 acetone,
and 0.4 H2O. The phase compositions are

Extract Raffinate

MIK 0.615 0.035

Acetone 0.325 0.210

Water 0.060 0.755

By a material balance, E + R = 1.5

0.4 = 0.325E + 0.21(1.5-E)

0.4 0.315
= = 0.739, = 0.761
0.325 0.21

Acetone extracted = 0.739 (0.325) = 0.24

Adding 0.5 parts MIK 50 0.761 parts of raffinate gives a mixture with the following
compostions

0.5+0.76(0.35)
MIK = = 0.418
1.261
0.21(0.761)
Acetone = = 0.127
1.261
0.755(0.761)
H2O = = 0.455
1.261

This separates to give an extract with 0.20 acetone and a raffinate with 0.075 acetone. A
acetone balance give

0.16 = 0.20E + 0.075(1.261-E)


E = 0.523

Acetone extracted: 0.523 x 0.20 = 0.105


Total extracted: 0.24 + 0.105 = .345
Fraction acetone extracted: 0.345/ 0.4 = 0.863
Solved Problems
10.5. A pyridine-water solution, 50% pyridine, is to be continuously and counter-currently
extracted at the rate of 2.25kg/s (17800 lb/h) with chlorobenzene to reduce the pyridine
concentration to 2% in the final raffinate. Using the coordinate systems plotted in (b) and (c) of
prob. 10.1:
(a) Determine the minimum solvent rate required.
(b) If 2.3 kg/s (18250 lb/h) is used, what are the number of theoretical stages and the saturated
weights of extract and raffinate
Solution:

Pyridine Chlorobenzene Water Pyridine Chlorobenzene Water

0 99.95 0.05 0 0.08 99.92

11.05 88.28 0.67 5.02 0.16 94.82

18.95 79.90 1.15 11.05 0.24 88.71

24.10 74.28 1.62 18.90 0.38 80.72

28.60 69.15 2.25 25.50 0.58 73.92

31.55 65.58 2.87 36.1 1.85 62.05

35.05 61.0 3.95 44.95 4.18 50.87

40.60 53.0 6.40 53.20 8.90 37.90


49 37.8 13.2 49 37.8 13.2

Basis: 2.25 kg/s of pyridine-water solution feed

= 0.5
Weight fraction at final raffinate: = 0.02
Solvent flowrate: = 2.3 /
Refer to Fig. E.2.14 (a) and (b)
Plot x v/s y and x, y v/s weight fraction of chlorobenzene
Mark point F on y-axis at xf=0.50. Mark the point S at the B-apex as the solvent is pure. Make a
line using point F and S.
Now locate M on FS such that:

=

2.3
= = 1.022
2.25
= 1.022
We have: = + = 112 (, )

1.022 + 1 = 2.022 = 112


= 55.4
= 112 55.4 = 56.6
So locate M on FS such that line MF=56.6 units and line MS =55.5 units
OR: = + = 2.25 + 2.3 = 4.55/
+ =

2.25(0.5) + 2.3(0) = 4.55


= 0.247
Mark point M on FS at xm=0.247(read from x-axis)
Both the above mentioned procedures give the same location for point M on FS. Locate
Rn(raffinate from nth stage) on the bimodal solubility curve corresponding to 2% pyridine(i.e., at
xn=0.02) Join RnM and project it to meet the equilibrium curve at E1. Join FE1 and project these

lines to meet at g.
Read y1 corresponding to E1 and from the x vs. y plot, get the value of x1 (in equilibrium with y1)
Mark R1 on the bimodal solubility curve at location corresponding to x1 value. Join Re1E1 which
is a required tie line for first stage. From the x vs. y plot, get the value of x2 corresponding to y2.
Mark R2 on the bimodal curve at location corresponding to x2 value. Join R2E2, which is a tie line
for stage-2, join R2g. The line R2g meets the curve at E3. The working is continued in this way
till we cover Rn(i.e. xn=0.02) and then count the theoretical stages required.

In our case, the tie line R3E3 is such that R3 is exactly xn=0.02
From Fig. E 2.14(a), number of theoretical stages required = n = 3
10.8 Water-dioxane solutions form a minimum-boiling azeotrope at atmospheric pressure and
cannot be separated by ordinary distillation methods. Benzene forms no azeotrope with dioxane
and can be used as an extraction solvent. At 25C, the equilibrium distribution of dioxane
between water and benzene [J. Am. Chem. Soc., 66, 282 (1944)] is as follows:

Wt% dioxane in water 5.1 18.9 25.2

Wt% dioxane in benzene 5.2 22.5 32.0

At these concentrations, water and benzene are substantially insoluble, and 1000 kg of a 25%
dioxane-75% water solution is to be extracted with benzene to remove 95% of dioxane. The
benzene is dioxane-free.
(a) Calculate the solvent requirement for a single batch operation
(b) If the extraction were done with equal amounts of solvent in five crosscurrent stages, how
much fsolvent would be required?

Solution: (a) single-stage operation:


Basis: 1000kg of solution containing 25% dioxane.
A-water, B-benzene, C-dioxane

Dioxane in feed solution = 0.25 1000 = 250


Water in feed solution = 0.75 1000 = 750
Cs1 is the equilibrium value of picric acid concentration in extract, Cs1 and CA1 are the
equilibrium values of picric acid concentration as the effluent streams leaving theoretical stage
are in equilibrium. So read the value of CS1 from the plot corresponding to CA1=0.02mol/liter.
From the plot: CS1=0.0155 mol/l
Amount of solvent (benzene) used = B liters
Picric acid in extract =0.08 mol

Concentration of picric acid in extract = CS1=


Volume of solvent B: =
1

0.08
= 0.0155 = . solvent required per liter feed

Cross-current operation:
Number of stages=3, Feed solution = 1 liter
Concentration of picric acid in feed solution =Cf=0.1 mol/liter
80% of the picric acid is removed.
Picric acid in final raffinate=20% of its original value
= 0.2 0.1 = 0.02
0.02
Concentration of picric acid in final raffinate = = 0.02
1


3 = 0.02/3 = 0.0155 ( )

For stage 1:
1 0
= =
1
1 0
For stage 3: = 1

As the equal amount of solvent is used in each stage, the operating lines will have the same slope
(-A/B). We have to construct/draw three operating lines parallel to each other (as the slope is the
same) starting from point F(CF,CS0) and ending/covering exactly CA3, the final raffinate
concentration. The operating line for the first stage passes through the point F(CF,CS0) and the
operating line of the third stage passes through the point Q(CA3,CS3)

So locate point F(CF,CS0) i.e. F(0.1,0) that represents the feed solution and draw the
operating line through it which will cut equilibrium curve at P(CA1,CS1 and through CA1 on x-
axis, draw the operating line parallel to the first one and so on and construct exactly three stages.
For this, we have to adopt a trial and error procedure. Once we construct exactly three stages,
measure the slope of any one of these operating lines.

From the graph:


slope of operating line FP

0.0255 0
= = 0.773
0.1 0.067

= 0.773


= ; = 1
0.773
1
= = 1.3
0.773
Benzene required per stage= 1.3L
Total benzene requirement: = 3 1.3 = .
Principles of Transport Processes and Separation
Processes John Geankoplis
Sample Problems
12.1-1 Adsorption Isotherm for Phenol in Wastewater

Batch tests were performed in the laboratory using solutions of phenol in water and particles of
granular activated carbon (R5). The equilibrium data at room temperature are shown in Table
12.1-1. Determine the isotherm that fits the data.

TABLE 12.1-1 Equilibrium Data for Example 12.1-1 (R5)

c, (kg phenol / m3 solution) q, (kg phenol / kg carbon)

0.322 0.150

0.117 0.122

0.039 0.094

0.0061 0.059

0.0011 0.045

Solution:

Plotting the data as 1/q versus 1/c, the results are not a straight line and do not follow the
Langmuir Equation (12.1-3).
qo c
q=
K+c
A plot of log q versus log c in Fig. 12.1-2 gives a straight line

and, hence, follow the Freundlich isotherm Eq. (12.1-2).


q=Kc n

The slope n is 0.229 and the constant K is 0.199, to give

q=0.199c 0.229

12.2-1 Batch Adsorption on Activated Carbon (Geankoplis Example)

A wastewater solution having a volume of 1.0 m3 contains 0.21 kg phenol/m3 of solution (0.21
g/L). A total of 1.40 kg of fresh granular activated carbon is added to the solution, which is then
mixed thoroughly to reach equilibrium. Using the isotherm from Example 12.1-1, what are the
final equilibrium values, and what percent of phenol of phenol is extracted?

Solution:

cF = 0.21 kg phenol/m3
S = 1.0 m3
M = 1.40 kg carbon
qF = is assumed zero

0(1.40) + 0.21(1.0) = q(1.40) + c(1.0)


At the intersection, q = 0.106 kg phenol / kg carbon and c = 0.062 kg phenol / m3. The
percent of phenol extracted is
0.2100.062
% extracted = (100) = (100) = 70.5
0.210

12.3-1 Scale-up of Laboratory Absorption Column (Geankoplis Example)

A waste stream of alcohol vapor in air from a process was absorbed by activated carbon particles
in a packed bed having a diameter of 4cm and length of 14cm containing 79.2 g of carbon. The
inlet gas stream having a concentration co of 600 ppm and a density of .00115 g/cm3 entered the
bed at a flow rate of 754 cm3 per s. Data in Table 12.3-1 give the concentrations of the
breakthrough curve. The break-point concentration is set at c/co = .01. Do as follows.

(a.) Determine the break-point time, the fraction of total capacity used up to the break point, and
the length of the unused bed. Also determine the saturation loading capacity of the carbon.

Table 12.3-1. Breakthrough Concentration for Example 12.3-1

Time, h c/co
0 0
3 0
3.5 0.002
4 0.030
4.5 0.155
5 0.396
5.5 0.658
6 0.903
6.2 0.933
6.5 0.975
6.8 0.993
(b.) If the break-point time required for a new column is 6.00 h, what is the new total length of
the column required?

Solution (a):

c/co = 0.01
tb = 3.65 h
td = 6.95 h approximately
A1 = 3.65 h graphically integrating
A2 = 1.51 h graphically integrating

The time equivalent to total or stoichiometric capacity of the bed is




= (1 ) = 1 + A2 = 3.65 + 1.51 = .
0
The time equivalent to the usable capacity of the bed up to the break-point time is,
= 3.65

= (1 ) = 1 = .
0
Hence, the fraction of total capacity used up to the break point is tu /tt = 3.65/5.16 =
0.707. The length of the used bed is HB = (tu /tt)HT = 0.707(14) = 9.9 cm.

= (1 ) = (1 0.707)(14) = .

Solution (b):

For a new tb of 6.0 h, the new HB is obtained simply from the ratio of the break-point
times multiplied by the old HB.
6.0
HB = 3.65(9.9) = 16.3 cm

= HB + = 16.3 + 4.1 = 20.4 cm

We determine the saturation capacity of the carbon.


Air flow rate = (754 cm3/s)(3600 s)(0.0015 g/cm3) = 3122 g air/h
600
Total alcohol adsorbed = ( ) (312 )(5.16 )
106
= 9.67 g alcohol

Saturation capacity = 9.67 g alcohol/79.2 g carbon


= 0.1220 g alcohol/ g carbon

The fraction of the new bed used up to the break point is now 16.3/20.4 = 0.799

12.5-1 Material Balance for Equilibrium Layers (Geankoplis Example)


An original mixture weighing 100 kg and containing 30 kg of isopropyl ether (C), 10 kg of acetic
acid (A), and 60 kg water, (B) is equilibrated and the equilibrium phases separated. What are the
compositions of the two equilibrium phases?

Solution: The composition of the original mixture is xC = 0.30, xA = 0.10, and xB = 0.60.

The composition of the extract (ether) layer is yA = 0.04, yC = 0.94, and yB = 0.02 mass
fraction. The raffinate (water) layer composition is xC = 0.02, xA = 0.12, and xB = 0.86.
12.5-2. Amounts of Phases in Solvent Extraction (Geankoplis Example)

From the compositions obtained in Example 12.5-1, determine the amounts of V and L. The
original mixture contained 100 kg and xAM = 0.10

Solution:

V + L = M = 100
V(0.04) + L(0.12) = 100(0.10)

L = 75.0
V = 25.0

12.7-1
Material Balance for Countercurrent Stage Process. Pure solvent isopropyl either at the
reate of Vn+1= 600kg/h is being used to extract an aqueous solution of Lo=200kg/h containing 30
wt% acetic acid (A) by countercurrent multistage extraction. The desired acetic acid
concentration in the aqueous phase is 4%. Calculate the compositions and amounts of the ether
extract V1 and the aqueous raffinate LN. Use equilibrium data from Appendix A.3.
Solution: The given values are Vn+1= 600, yAN+1=0, yAN+1=1.0, Lo=200, xAO=0.30, xBO=0.70,
xCO=0.04.
In figure 12.7-3, Vn+1 and Lo are plotted. Also, since LN is on the phase boundary, it can be
plotted at xAN=0.04. For the mixture point M, substituting into Eqs. (12.7-3) and (12.7-4),
+ +1 +1 200(0)+600(1.0)
= = = 0.75
+ +1 200+600

+ +1 +1 200(0.30)+600(0)
= = = 0.075
+ +1 200+600

Using these coordinates, the point M is plotted in Fig 12.7-3. We locate V1 by drawing a line
from LN through M land extending it until it intersects the phase boundary. This gives yA1=0.08
and yC1=0.90. For LN a value of xCN=0.017 is obtained. By substituting into Eqs. (12.7-1) and
(12.7-2) and solving, LN=136kg/h and V1=664kg/h.

12.7-2
Number of Stages in Countercurrent Extraction. 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.
Solution:
The known values are VN+1=450, yAN+1=0, yCN+1=1.0, LO=150, xAO=0.30, xBO=0.70,
xCO=0, and xAN=0.10.
The points VN+1, LO, and LN are plotted in Fig. 12.7-5. For the mixture point M,
substituting into Eqs. (12.7-3) and (12.7-4), xCM=0.75 and xAM=0.075. the point M is plotted and
V1 is located at the intersection of line LN M with the phase boundary to give yA1=0.072 and
yC1=0.895. This construction is not shown.
The lines LO V1 and LN VN+1 are drawn and the intersection is the operating point as
shown. Alternatively, the coordinates of can be calculated from Eq. (12.7-10) to locate point .
Starting at LO we draw line LO, which locates V1. Then a tie line through V1 locates L1 in
equilibrium with V1. (The tie-line data are obtained from an enlarged plot such as the bottom of
Fig. 12.5-3.) Line L1 is next drawn locating V2. A tie line through V2 gives L2. A line L2 gives
V3. A final tie line gives L3, which has gone beyond the desired LN. Hence, about 2.5 theoretical
stages are needed.

12.7-3
Extraction of Nicotine with Immiscible Liquids. 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.

Solution:
The given values are LO =100 kg/h, xO =0.010, VN+1 =200 kg/h, yN+1 =0.0005, xN =0.0010. The
inert streams are
L = L(1 x) = LO (1 - xO) = 100(1 0.010) = 99.0 kg water/hr
V = V(1 y) = VN+1 (1 yN+1) = 200(1 0.0005) = 199.9 kg kerosene/hr

Making an overall balance on A using Eq (12.7-12) and solving, y1 =0.00497. These end points
on the operating line are plotted in Fig. 12.7-6. Since the solutions are quite dilute, the line is
straight. The equilibrium line is also shown. The number of stages are stepped off, giving N=3.8
theoretical stages.

Solved Problems
12.5-2 (Geankoplis, 4th Ed) A single-stage extraction is performed in which 400 kg of a solution
containing 35 wt % acetic acid in water is contacted with 400 kg of pure isopropyl ether.
Calculate the amounts and compositions of the extract and raffinate layers. What percent of the
acetic acid is removed?

Given:
V1 V2 = 400 kg isopropyl ether

L0= 400 kg acetic acid solution L1


xA0= 0.35
xB0= 0.65

OMB:
L0 + V2 = V1 + L1
V1 + L1 = 400 + 400
V1 + L1 = 800 = M

Acetic Acid Balance:


L0xA0 + V2yA2 = MxAM
(400)(0.35) + (400)(0) = 800xAM
xAM = 0.175

Isopropyl Ether Balance:


L0yC0 + V2yC2 = MyCM
(400)(0) + (400)(1) = 800yCM
yCM= 0.50

Plot point M on graph. Tie line through M gives L1 and V1.

L1 (Raffinate Layer):
xA1= 0.255
xB1= 0.03
xC1= 0.715

V1 (Extract Layer):
yA1= 0.11
yB1= 0.86
yC1= 0.03

Calculate L1 and V1:

L1xA1 + V1yA1 = MxAM


L1(0.255) + V1(0.11) = (800)(0.175)

V1 + L1 = 800

Solving simultaneously,

V1= 358 kg
L1= 442 kg

Amount of acetic acid in feed = 400(0.35) = 140 kg


Amount of acetic acid in extract = 442(0.11) = 48.62 kg
48.62
% = 100 = 34.7%
140

Graph for problem 12.5-2:


12.5-4 (Geankoplis, 4th Ed) A mixture weighing 1000 kg contains 23.5 wt % acetone and 76.5 wt
% water and is to be extracted by 500 kg methyl-isobutyl ketone in a single stage extraction.
Determine the amounts and composition of the extract and raffinate phases.

Given:
V1 V2 = 500 kg methyl-isobutyl ketone

L0= 1000 kg acetone solution L1


xA0= 0.235
xB0= 0.765

OMB:
L0 + V2 = V1 + L1
Let: V1 + L1 = M
1000 + 500 = M
M = 1500 kg

Acetone Balance:
L0xA0 + V2yA2 = MxAM
1000(0.235) + 500(0) = 1500xAM
xAM = 0.1567

Methyl-isobutyl Ketone Balance:


L0yC0 + V2yC2 = MyCM
1000(0) + 500(1) = 1500yCM
yCM = 0.333

Plot points M, L0, and V2 on graph, tie line through M gives L1 and V1 compositions.

L1 (Raffinate Layer):
xA1= 0.120
xC1= 0.022

V1 (Extract Layer):
yA1= 0.205
yC1= 0.748
Calculate L1 and V1:

L1xA1 + V1yA1 = MxAM


L1(0.120) + (1500- L1) (0.205) = (1500)(0.1567)

V1= 852 kg
L1= 648 kg

12.7-2 (Geankoplis, 4th Ed) An aqueous feed of 200 kg/h containing 25 wt % acetic acid is being
extracted by pure isopropyl ether at the rate of 600 kg/h in a countercurrent multistage system.
The exit acid concentration in the aqueous phase is to contain 3.0 wt % acetic acid. Calculate the
compositions and amounts of the exit extract and raffinate streams.

Given:
VN+1 = 600 kg/h isopropyl ether

L0= 200 kg/h acetic acid solution xAN= 0.03


xA0= 0.25
xB0= 0.75

0 0 + +1 +1 (200)(0) + (600)(1.0)
= = = 0.75
0 + +1 200 + 600
0 0 + +1 +1 (200)(0.25) + (600)(0)
= = = 0.0625
0 + +1 200 + 600

Plot points M, L0, and VN+1 on graph; LN on phase B.


Locate V1 by drawing line MLN to intersect extract phase boundary at V1.

Ln (Raffinate Layer):
xAN= 0.030
xCN= 0.017

V1 (Extract Layer):
yA1= 0.070
yC1= 0.905

Calculate L1 and V1:

OMB:
L0 + VN+1 = V1 + LN
Let: V1 + LN = M
200 + 600 = M
M = 800 kg

Isopropyl Ether Balance:


L0xC0 + VN+1yCN+1 = MxCM
LNxCN + V1yC1 = MxCM
LN(0.017) + (800- LN)(0.905) = (800)(0.75)

V1= 660.4 kg/h


LN= 139.6 kg/h

12.7-4 (Geankoplis, 4th Ed) An aqueous feed solution of 1000 kg/h of acetic acid-water solution
contains 30.0 wt % acetic acid and is to be extracted in a countercurrent multistage process with
pure isopropyl ether to reduce the acid concentration to 2.0 wt % acid in the final raffinate. (a)
Calculate the minimum solvent flow rate that can be used. (b) If 2500 kg/h of ether solvent is
used, determine the number of theoretical stages required.

Given:
VN+1 = Pure isopropyl ether

L0= 1000 kg/h acetic acid solution xAN= 0.02


xA0= 0.30
xB0= 0.70

a. Minimum solvent
Tie line through L0 gives V1min. Line LNVN+1 and L0V1min (tie line) gives pt. min. Draw line
LNV1min and L0VN+1 and intersection gives Mmin.
From graph:
xA= 0. 114

0 0 + +1 +1 (1000)(0.25) + +1 (0)
= 0.114 = =
0 + +1 1000 + +1

VN+1 = VN+1min = 1630 kg/h

b. Number of Stages

VN+1 = 2500 kg/h isopropyl ether

L0= 1000 kg/h acetic acid solution xAN= 0.02


xA0= 0.30
xB0= 0.70

0 0 + +1 +1 (1000)(0) + (2500)(1.0)
= = = 0.714
0 + +1 1000 + 2500
0 0 + +1 +1 (1000)(0.30) + (2500)(0)
= = = 0.0857
0 + +1 1000 + 2500

This point checks graphical determination of M on lines LNV1 and L0VN+1. Draw line LNVN+1
and L0V1 to obtain operating point graphically.

Algebraic calculation of operating point:


xAN = 0.02
xCN = 0.015
yA1 = 0.010 (off graph)
xC1 = 0.863

OMB:
L0 + VN+1 = V1 + LN
Let: V1 + LN = M
1000 + 2500 = M
M = 3500 kg
+ 1 1 ( )(0.02) + (3500 )(0.010)
= 0.0857 = =
+ 1 3500

V1= 2874 kg/h


LN= 626 kg/h

0 0 + 1 1 (1000)(0) + (2874)(0.863)
= = = +1.32
0 + 1 1000 + 2874
0 0 + 1 1 (1000)(0.30) + (2874)(0.10)
= = = 0.0067
0 + 1 1000 + 2874

This checks the graphical op. point. Use op. point to determine the number of stages.
Plot stages up to V4. Then, plot expanded scale as shown. The operating points on expanded
scales as L1, V2, L2V3, etc. determined by lines from L to operating point.

Nmin = 7.5 stages


Graph for problem 12.7-4:
Unit Operations of Chemical Engineering
McCabe, Smith, Harriott
Sample Problems
Example 23.2

Penicillin F is recovered from a dilute aqueous fermentation broth by extraction with amyl
acetate using 6 volumes of solvent per 100 volumes of the aqueous phase. At pH = 3.2 the
distribution coefficient KD is 80. (a) What fraction of the penicillin would be recovered in a
single ideal stage? (b) What would be the recovery with two-stage extraction using fresh solvent
in both stages?(c) How many ideal stages would be needed to give the same recovery as in part
(b) if a counterflow cascade were used with V/L = 0.06?

Solution:

(a) By a material balance, since y0 = 0,

L(x0 x1) = Vy1

y1 = KD x1
VKD
x1 ( + 1) = x0
L

The extraction factor is


VKD 6 x 80
E= = = 4.8
L 100

x1 1 1
Thus = = 5.8 = 0.172
x0 1+E

Recovery is 1 - 0.172 = 0.828, or 82.8%

(b) With the same value of E,

x2 1
=
x1 1+E
x2 1
= = 0.0297
x0 (1 + E)2

Recovery is 1 0.0297 = 0.9703 or 97.0%

(c) With KD and V/L constant, the number of ideal stages can be calculated from the stripping
form of Kremser equation using E in place of its equivalent, the stripping factor S.
ln[(xa xa )/(xb xb )
N = ln E

Let xa = x0 = 100 Then xb = 3.0 and ya = 97(100)/6 = 1617

ya 1.617
xa = = = 20.2
KD 80

xb = 0
10020.2
ln[ ]
3
N = = 2.09
ln 4.8

Example 23.3

A countercurrent extraction plant is used to extract acetone (A) from its mixture with water by
means of methyl isobutyl ketone (MIK) at a temperature 25C. The feed consists of 40 percent
acetone and 60 percent water. Pure solvent equal in mass to the feed is used as the extracting
liquid. How many ideal stages are required to extract 99 percent of the acetone fed? What is the
extract composition after removal of the solvent?

Solution:
Use the data in Fig 23.7 to prepare a plot of the equilibrium relationship yA versus xA, which is
the upper operating line in Fig 23.10. The terminal points for the operating line are determined
by material balances with allowances for the amounts of water in the extract phase and MIK in
the raffinate phase.

Basis: F = 100 mass units per hour

Let n = mass flow rate of H2O in extract

M = mass flow rate of MIK in raffinate

For 99% recovery of A, the extract has 0.99 x 40 = 39.64, and the raffinate has 0.44. The total
flows are

At the top, La = F = 100 = 40A +60 H2O

Va = 39.6A + nH2 O + (100 m)MIK = 139.6 + n m

At the bottom, Vb =100MIK

Lb = 0.4A + (60 n)H2 O + mMIK = 60.4 + m n

Since n and m are small and tend to cancel in the summation for Va and La, the total extract flow
Va is about 140, which would make yA,a 39.6/140 = 0.283. The value of XA,b is about 0.4/60 =
0.006. These estimates are adjusted after calculating values of n and m.
From Fig 23.7 for yA = 0.283, yH2O = 0.049
0.049
n= (39.6 +100 m)
10.049

0.049
If m is very small n (0.951) (139.6) = 7.2

From Fig 23.7 for xA = 0.007, xMIK = 0.02,

0.02
m= (0.4 + 60 n)
1 0.02
0.02
(0.4 + 52.8) = 1.1
0.98
Revised n = (0.049/0.951)( 139.6 1.1) = 7.1

Va = 139.6 + 7.1 1.1 = 145.6

39.6
yA,a = = 0.272
145.6
Lb = 60.4 + 1.1 7.1 = 54.4

0.4
xA,,b = = 0.0074
54.4
Plot points (0.0074, 0) and (0.4, 0.272) to establish the ends of the operating line.

For an intermediate point on the operating line, pick yA = 0.12 and calculate V and L. From Fig.
23.7, yH2O = 0.03, and yMIK = 0.85, Since the raffinate phase has only 2 to 3 percent of MIK,
assume that the amount of MIK in the extract is 100, the same as the solvent feed:

100
100
0.85 = 117.6

By an overall balance from the solvent inlet (bottom) to the intermediate point,

+ = +

54.4 + 117.6 100 = 72.0

A balance on A over the same secion gives xA:

+ = +

0.4 + 117.6(0.12) 0
14.5
= 0.201
72
This value is probably accurate enough, but corrected values of V, L and xA can be determined.
For xA = 0.201, 0.03(Fig 23.7). A balance on MIK from the solvent inlet to the
intermediate point gives + MIK = Lb xMIK,b + VyMIK

VyMIK = 100 + 72(0.03) 1.1

101.1
Revised V = = 118.9
0.85
Revised L = 54.4 + 118.9 100 = 73.3
0.4+ 118.9(0.12)
Revised xA = = 0.200
73.3

Plot xA = 0.20, yA = 0. 12, which gives a slightly curved operating line. From Fig 23.10, N =
3.4 stages

Solved Problems
23.7

An antibiotic that has been extracted from a fermentation broth using amyl acetate at low pH is
to be extracted back into clean water at pH = 6, where Kp = 0.15. If the water flow rate is set at
0.45 times the solvent rate, how many ideal stages would be needed for 98 percent recovery of
the antibiotic in a countercurrent cascade?
Solution:

KD = 0.15 = ye / xe
xa = 0

Lx = Vy
L = 0.45V
Ya = 0.02yb

Neglect changes in L and V


Operating line slope = 0.45 = L/V
ya* = 0

For extraction,
KDV
E=
L
[(Eq. 23.5)], but this is for transfer into the organic phase. Here solute is extracted from the
organic phase into the water, so KD = 1 / KD = 1 / 0.15 = xe / ye and appropriate factor is

LK'D 0.45
= = 3.0
V 0.15

This factor corresponds to absorption factor A in absorption.

Lxb = V(0.98)yb

1
= (0.98) = 2.18
0.45

yb* = 0.15xb = 0.15(2.18)yb

Solving for N.
yb 0.327yb
ln[ 0.02yb ]
N= = 3.20 stages
3.0

23.8

Oil was extracted from small particles of rapeseed, averaging 0.58mm in size, by contact with
hexane. The particles originally contained 43.82 percent oil and 6.43 percent moisture. After
drying, the oil content of the dried meal was reported for different extraction times. The results
are given in the table below. Determine the effective diffusion coefficient for oil in the hexane-
soaked particles using the equation for transient diffusion in spheres. Assume that a large excess
of hexane was used and that the external mass transfer resistance was negligible.

Time, min 75 90 105 120

Oil in dry meal, 11.5 7.97 4.35 3.88


kg/100 kg inert
material

Answer:

Assume the packing 40% voids.


Dp = 0.015 m
av = 6(1-) / Dp = (6 x 0.6) / 0.015 = 240 m2/m3
c = 62.15 x 16.018 = 995 kg/m3
c = 0.801 cP = 8.01 x 10-4 Pa.s
= 36.1 x 10-3 = 0.0361 N/m
d = 53.64 x 16.018 = 859.2 kg/m3
= 136.3 kg/ m3

Assume R =2, = 1.0 (continuous wetting). For spheres, use C1 = 0.208. Then

2 av 0.5
Vs,c (1+R0.5 ) ( ) =27.35Vs,c
g
0.15

136.3 0.41 1 136.32 x 9.805 1 0.3 8.01 x 10-4


=1.0 x 0.208 x 1.041.54 ( ) [ ( ) 3] x [ ]
859.2 240 8.01 x 10-4 136.3 x 0.0361 0.5
( 240 )
= 0.0615

Vs,c =0.0615/27.35= 0.00225 m/s

23.9 (From Unit Operation of Chemical Engineering by McCabe and Smith)

A spray-tower extractor operates at 30C with hydrocarbon drops dispersed in water. The density
of the hydrocarbon phase is 53 lb/ft3. If the average drop size is 2.0 mm, calculate the terminal
velocity of the drops. If the slip velocity is assumed to be independent of the holdup and if the
dispersed-phase volumetric flow rate is taken to be twice that of the continuous phase, at what
flow rate of the dispersed phase would the fraction holdup be 0.30 (close to flooding)? For
different ratios of flow rates, is either the sum of the flow rates or the sum of their square roots
nearly a constant at a given holdup? (Note the correlation in Figure below)
Fig. 23.7 Flooding velocities in packed extraction towers

Solution:

Dp = 0.2 cm, p = 53 / 62.4 = 0.849 g / cm3


For water at 30C, = 0.996 g / cm3, = 0.801 cP
To get t, try Stokes Law
980(0.2)2 (0.996-0.849)
t = =39.97 cm/s
18(0.0081)

0.2(39.97)(0.996)
Rep = =994
0.0081

This is well beyond the range of Stokes Law, so t must be calculated using Eq. (7.37) and Fig.
7.6. Guess Rep = 100, which gives CD = 1.0
4()
Eq. (7.37) = 3

4(980)(0.147)(0.2) 1/2
= ( ) = 6.21 /
3(1.0)(0.996)

0.2(6.21)(0.996)
= = 154, = 0.9
0.00801

Guess CD = 0.85
t = 6.74 cm / s
Re = 167, CD = 0.85 (OK)

cm 3600
t =6.74 x =796 ft/h
s 30.5
Let h = volume fraction holdup of drops
Vd , Vc = actual velocities of drops or continuous phase (both positive)
Then t = Vd + Vc = 796 ft/h

Given:
First Part
Vs,d = 2Vs,c h = 0.30

Vd = Vs,d / h Vc = Vs,c / (1-h)

Vs,d Vs,d
+ =796
0.3 2(0.7)

Vs,d(3.33+0.714) = 796

Vs,d = 197 ft / h

Vs,d + Vs,c = 197 + 0.5(197) = 296

Vs,d + Vs,c =14.0+9.9=23.9


Second Part
For Vs,d = Vs,c and h = 0.30
796
Vs,d = =167=Vs,c
3.33+1.43

Vs,d + Vs,c =334

and Vs,d +Vs,c =25.8

For Vs,d = 0.5Vs,c and h = 0.30


796
Vs,d = =129
3.33+2.86

Vs,c =258

Vs,d + Vs,c = 387


31% higher than for Vs,d = 2Vs,c

but Vs,d +Vs,c =11.4+16.1=27.5


15% higher than for Vs,d = 2Vs,c
The sum of the square roots is more nearly constant than the sum of the velocities.

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