E4 - Batch Distillation for Ethanol and Water System

1. Objectives
The objective of this experiment is to compare the performance of the batch distillation of
ethanol and water. Comparison was done on the distillate composition obtained
experimentally and by calculation using Rayleigh Equation.
2. Introduction
It is generally used only for small scale processes, especially in pharmaceuticals and specialty
products. When small amounts of material of varying product compositions are required,
batch distillation is highly preferred. The charge i.e. feed is loaded into the still and after a
short startup period, the product can be withdrawn from the top of the column. The flexibility
of this type of distillation gives an advantage as compare to continuous distillation. In the
batch system, the column can handle different mixtures by changing its operating parameters.
Advantages of batch distillation are as:
Separation of small quantities of mixtures, i.e. capacity too small to justify continuous
separation
Flexibility to handle different feed stocks to produce different products
More than one product may be obtained light components are removed first.
Different purities of the same component can also be obtained.
Upstream is batch operated and composition of feed varies with time
Fouling is a serious concern

3. Equipment Description
This experiment consists of 2 parts. The first part is to obtain data points for plotting the
calibration curve using refractometer. The second part is to carry out batch distillation
process using packed column (refer to Figure 1).

Figure 1: Packed Column Distillation Equipment

4. Experimental Procedures
4.1 Part 1 Calibration Curve Determination
1. Prepare six samples solution with different composition of ethanol-water varies from the
range of 0% to 60% volume fraction of ethanol.
2. Obtain the value of refractive index for the six samples using refractometer.
3. Plot the calibration curve (refractive index versus volume fraction of ethanol).
4. Note that if the refractive reading is out of the range, dilute the sample with equal amount
(volume) of water until the index measurement falls within the range.
4.2 Part 2 Batch Distillation Process
1. Prepare 2.5 L of initial ethanol-water solution. This is done by mixing 300 ml of ethanol
and the rest is water to make up a solution of 2.5 L.
2. Obtain the refractive index of the initial mixture by using refractometer. Use the
calibration curve (from Part 1) to determine the vol% of ethanol in the initial solution.
3. Empty and clean the boiling flask (still) with distilled water first before filling the flask
with the initial ethanol-water solution.
4. Add few pieces of anti-bumping agents into the solution to avoid the bumping effect
during the distillation process. The agents work by providing nucleation sites so the
solution boils smoothly without becoming superheated.
5. Connect the mouth of the flask to the bottom end of the packed bed column.
6. Turn on the water supply for the condenser and cooler.
7. Set the reflux ratio as suggested by the lab assistant and then press the close button.
8. Switch on the the reboiler and set the heat controller to the maximum value (marked as
10).
9. Reduce the heat controller to 50% once the solution begins to boil.

10. Record the temperature of the solution once the reading on the thermocouple becomes
stable.
11. Press the normal button on the reflux ratio controller. Carry on the distillation process
until 100 ml of distillate is obtained.
12. Switch off the reboiler and press the close button on the reflux ratio controller.
13. Measure the refractive index of the distillate and also the solution remaining in the still.
Use the calibration curve (Part 1) to determine the volume composition of the distillate
and the remaining solution in the still. (Make sure the solution sample is cooled down to
room temperature before the refractive index is measured).
14. Repeat the whole process of Part 2 using different reflux ratio. Use the remaining solution
in the still as the initial feed.

5. Data Analysis and graphs:

1.

Prove that:
% mol of ethanol in the mixture =

100
m densityw 100

1 e
m
density
V

1
e e
w

State your main assumption.

Typical equilibrium data:
Table 1 shows the equilibrium data for ethanol-water system.
Temperature, T
(o F)
212.0
210.1
208.5
206.9
204.8
203.4
197.2
189.2
184.5
181.7
179.6
177.8
176.2
174.3
173.0
172.8
172.7
172.8
173.0

Mass fraction of ethanol

x (liquid)
0.00
0.01
0.02
0.03
0.04
0.05
0.10
0.20
0.30
0.40
0.50
0.60
0.70
0.80
0.90
0.94
0.96
0.98
1.00

y (gas)
0.00
0.103
0.192
0.263
0.325
0.377
0.527
0.656
0.713
0.746
0.771
0.794
0.822
0.858
0.912
0.942
0.959
0.978
1.000

2.
3.
4.
5.
6.
7.
8.
9.

10.
11.
11.
12.

Plot refractive index vs vol. fraction of ethanol. This will be your calibration curve.
Calculate S1, the initial amount in moles, of the mixture in the boiling flask (still).
Calculate the initial mole fraction of ethanol xS1, in the boiling flask (still).
Calculate the mole fraction of ethanol xd, the distillate collected.
Calculate the mole fraction of ethanol xS2, of the remaining mixture in the still.
Calculate the mole of distillate collected, D.
Calculate the amount of remaining mixture in the still, S2 (in moles).
Calculate the equivalent no. of theoretical stages assuming that:
HETP
=
0.1 m and
Height of packing
=
1 m.
Plot the equilibrium curve y-x diagram. Draw the ideal O/L line, y = x, i.e. 45o line.
At a specific reflux ratio, R, calculate the slope of operating line (O/L) and the yinterception of operating line.
Obtain the number of stages (Start constructing the number of stages from xd to xS2) for
the two value of R.
By applying, rearranging integrating Rayleigh equation, the final equation becomes:
xs1
S1
dx s
ln
S2
xs 2 x d x s

where, initial solution S1, distillate D, solution left in the still S2, are quantity in moles
and x the composition, in mole fraction of ethanol.
13. Again plot the equilibrium curve, the O/L of constant slope with
specific R. Choose several values of xd and using the theoretical number of stages
calculated from no. 9, determine values of xs.
14. Plot l/(xd xs) vs xs and then determine area under the curve which is equivalent to
xs1
dx
xs2 x d sx s . The area can be calculated using trapezoidal rule.
15.

From Rayleigh equation, the theoretical values of S2, D and xd can be obtained.
Compare these values with those obtained experimentally.

6. References:
1. Bennett, C. O., and J. E. Myers, Momentum, Heat and Mass Transfer, 3rd edition, McGrawHill, 1987.
2. Geankoplis, C. J., Transport Processes and Unit Operations, 2nd edition, Allyn and Bacon,
1983.
3. McCabe, W. L., and J. C. Smith, Unit Operation of Chemical Engineering, 2nd edition,
McGraw- Hill, 1967.

4. Perry, R. H., and D. Green, Perrys Chemical Engineers Handbook, 6th edition, McGraw-Hill,
1988.
5. Treybal, R. E., Mass Transfer Operations, 3rd edition, McGraw-Hill, 1980.

6. Coulson J.M., Richardson J. F. and Harker J.H., Chemical Engineering Volume 2: Particle
Technology and Separation Processes, 5th edition, Butterworth-Heinemann, 2002.
7. Seader J.D., and Henley E.J., Separation Processes Principles, 2nd edition, John Wiley &
Sons, Inc, 2006.