Batch Distillation with Rectification

Excel-based Solution

B. Batch Distillation at Constant Distillate Composition

The schematic diagram of batch distillation with rectification is given in figure 1.

Condenser

Distillate

Reflux
Liquid

Still

Figure 1: Schematic Diagram of Batch Distillation with Rectification

Recall that the first droplet of the distillate contains the riches composition of the more volatile component.
However, as time progresses, the distillate composition approaches the initial still composition (if the reflux
is kept constant). Thus, to produce a constant distillate composition, the reflux ratio of the column is varied
continuously. This can be achieved by controlling the valve of the reflux liquid.

Analysis of the distillation process is simpler in terms of material balance than that of the batch distillation at
constant reflux. However, prediction of the operating time of the distilling process is quite complex and
requires several steps. The material and component balances as well as operating time equation are as
follows.

OMB: Hi = Hf + D equation 1

Component Balance: Hi xpi = Hf xpf + D xd equation 2

Operating time (Based on Perry’s Handbook 8th Edition, Section 13, equation 13-139, page 13-113):
 Hi (xd -xpi ) xpi dxp
Equation 3: θ= ∫
V L 2
xpf (1 - ) (xd - xp )
V

Note that L/V = R/(R+1). Thus,

Hi (xd -xpi ) xpi dxp

Equation 4: θ= ∫
V R 2
xpf (1 - ) (xd - xp )
R+1

This can be rewritten as,

Hi (xd -xpi )(Area)

Equation 5: θ=
V
xpi dxp
Equation 6: Area = ∫
R 2
xpf (1 - ) (xd - xp )
R+1

1
Equation 7: F(x) =
R 2
(1 - ) (xd - xp )
R+1

where:

Hi = initial amount of the still, mol

Hf = final amount of the still, mol
xd = distillate composition
xpi = initial still composition
xpf = final still composition
R = reflux ratio
V = vapor flow rate/boil up rate, mol/time

Sample Problem:

Five hundred moles of methanol-water mixture is distilled to produce a constant distillate composition of 60
mol% methanol at 1 atm absolute. If the initial and final still composition is 20 mol% and 5 mol% methanol,
respectively,

1. Determine the amount left in the still

2. Calculate the amount of distillate produced
3. Approximate the operating time of the distilling column. The distilling column has four trays and
operates with a boil-up rate of 2.63 moles per minute.

Given:

Hi = 500 moles
xpi = 0.2
xd = 0.6
xpf = 0.05
V = 2.63 moles/min
N = 5 equilibrium stages (4 trays + 1 reboiler)

Solution:

OMB: Hi = D + Hf equation Ex. 1

D + Hf = 500 equation Ex. 2

Component Balance (Methanol Balance):

Hi xpi = Hf xpf + D xd equation Ex. 3

0.05Hf + 0.6D = (500*0.2) equation Ex. 4

Solving equations Ex. 2 and Ex. 4,

Answer 1. Hf = 363.6364 moles

Answer 2. D = 136.3636 moles

Steps for question 3:

1. Draw the equilibrium curve and 45-degree line. The equilibrium data was adapted from Perry’s
Chemical Engineering Handbook 7th Edition, Section 13, page 13-13, Table 13-1,
1
0.9
y, mol fraction of vapor

0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0 0.2 0.4 0.6 0.8 1
x, mol fraction of liquid

Equilibrium Data 45-Degree Line

 Figure 2: Equilibrium curve of Methanol with 45-degree Line

2. Assume a Reflux ratio (say R = 1.6), then determine the operating line
R xd
Equation Ex. 5 y= ( )x +
R+1 R+1
Equation Ex. 6 y = 0.615x + 0.231
3. Plot the operating line in figure 2.

1
0.9
y, mol fraction of vapor

0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0 0.2 0.4 0.6 0.8 1
x, mol fraction of liquid

Equilibrium Data 45-Degree Line Operating Line

Figure 3: Equilibrium curve of Methanol with 45-degree Line and Operating line
 4. Step-off the given number of stages (in this case 5 equilibrium stages) starting at (x d, xd).
1
0.9
0.8

x, mol fraction of liquid

0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0 0.2 0.4 0.6 0.8 1
x, mol fraction of liquid

Equilibrium Data 45-Degree Line Operating Line Step Line:

Figure 4: Complete Plot at R = 1.6

5. Record the last value of x (x-coordinate of the last stage). This will be the xp1 at the assumed R1.
6. Repeat procedure 2 to 5 until sufficient data is obtained. Note, the x-values of the data must
contain both values of xpi and xpf.
7. Compute for the values of F(x) (Equation 7) corresponding to the value of R and xp. The data
obtained is shown table 1.
8. Plot F(x) vs. xp. Determine the equation that best fit F(x) as a function of xp. The equation
generated by Microsoft Excel is presented in figure 5. Note: Predicted values using the equation
provided by Excel is more accurate than that of Matlab.
9. Solving for the Area (Equation 6), Area = 0.9619.
10. Computing for the operating time (Equation 5),  = 73.1474 minutes.
 R x_p F(x)
0 0.21881 6.882054
0.1 0.180851 6.261181
0.2 0.152968 6.004876
0.3 0.132461 5.947139
0.4 0.116915 5.999025
0.5 0.104744 6.115504
0.6 0.094951 6.272668
0.7 0.08689 6.456951
0.8 0.080131 6.660165
0.9 0.074377 6.877102
1 0.069416 7.104293
1.1 0.06509 7.339351
1.2 0.061284 7.580575
1.3 0.057907 7.826718
1.4 0.054889 8.076852
1.5 0.052177 8.330268
1.6 0.049724 8.586414

Table 1: Summary of data

9
8.5
y = -161410x5 + 121454x4 - 36286x3 + 5540.9x2 - 439.76x + 20.507
8
R² = 0.9999
7.5
F(x)

7
6.5
6
5.5
5
0 0.05 0.1 0.15 0.2 0.25
x_p

Figure 5: Plot of Area as a function of still composition (xp)