Engineering 435 Lab Report

Distillation Column

Team Members

Brian Vandagriff
Marc Moss
James Linder
Corita Suber

November 30, 1998

Introduction

The function of distillation is to separate, by vaporization, a liquid mixture of

miscible and volatile substances into individual components or, in some cases, into
groups of components. The separation of a mixture of alcohol and water into its
components; of liquid air into nitrogen, oxygen, argon; and of crude petroleum into
gasoline, kerosene, fuel oil, and lubricating stock are examples of distillation. Suppose
there are two components, A and B. Both of these components are found in both phases.
There are four variables: pressure, temperature, and concentrations of component A in the
liquid and vapor phases (the concentrations of component B are unity less those
concentrations of A). If the pressure is fixed, only one variable, e.g., liquid-phase
concentration, can be changed independently and temperature and vapor-phase
concentration follow. In practice, distillation may be carried out either of two principal
methods. The first method is based on the production of a vapor by boiling the liquid
mixture to be separated and condensing the vapors without allowing any liquid to return
to the still. There is then no reflux, which is called batch distillation. The second method
is based on the return of part of the condensate to the still under such conditions that this
returning liquid is brought into intimate contact with the vapors on their way to the
condenser. Either of these methods may be conducted as a continuous steady-state
distillation process, including single-stage partial vaporization without reflux (flash
distillation) and continuous distillation with reflux (rectification), for systems containing
only two components.

Background

The distillation column experiment is a purification experiment to separate a

binary mixture of methanol and water. After becoming familiar with the column and its
setup, several experiments were conducted to observe the operation and performance of
the column. The holding reservoir, which contained the methanol-water mixture, was
analyzed to determine the composition of the liquid. We performed a boiling point test
on the mixture to determine the unknown composition of the liquid. The data obtained
from the boiling point test allowed us to determine the composition using an x, y, T data
plot for methanol-water. Two experiments were performed during the four-week period.
A batch distillation was performed first. The distillation column was monitored until the
reboiler started to boil. The time was recorded and the volume change was monitored in
the reboiler. The second experiment involved a continuous distillation experiment. The
column was allowed to reach steady state. Once steady state was obtained the time was
recorded and the compositions of each tray were determined during a specific time
interval. The collection of this data would allow us to determine the tray efficiency and
plot the separation line on the equilibrium diagram. The diagram of our system is given
on the following page as Figure 1.
Figure 1. Distillation Column
Procedure

Batch Distillation:
1. Determine the composition of the liquid that is in the holding reservoir containing the
mixture by using the boiling point test and an x, y, T plot for methanol-water.

2. Use the LabView program to initiate startup of the heating process to the reboiler.

3. Allow distillation column to reach steady-state.

4. Do composition analysis on the distillate (boiling point test).

5. Record time and volume readings in the rebolier from the time the reboiler begins to
boil.

Continuous Distillation:
1. Repeat steps 1-3 from above procedure.

2. Record the temperatures of each tray while at steady-state.

3. Perform calculations with the data obtained to determine tray efficiency.

Results

The batch distillation data results are given in Table 1 below.

Table 1. Batch Distillation Data

E 435 Distillation Column Analysis
Actual Theoretical
o
Time (min) Volume (L) Temperature ( C) Time (min) Volume (L) Temperature (o C)
0 15 77.509 0 15 77.874
1 14.994 77.648 1.772 14.74 78.064
2 14.988 77.57 3.511 14.486 78.256
3 14.983 77.646 5.216 14.237 78.451
4 14.976 77.635 6.889 13.993 78.65
5 14.968 77.649 8.531 13.754 78.852
6 14.961 77.649 10.142 13.52 79.057
7 14.953 77.649 11.724 13.291 79.265
8 14.946 77.65 13.278 13.066 79.477
9 14.939 77.691 14.804 12.845 79.693
10 14.932 77.794 15 12.817 79.722
11 14.925 77.651
12 14.918 77.75
13 14.91 77.794
14 14.903 77.791
15 14.896 77.792
The continuous distillation data is given in Table 2, which is provided below.

Table 2. Continuous Distillation Data

Tray Temperature (oC) Xm Efficiency (%)
7 64.83 0.992 125
8 65.8 0.932 54.5
9 66.18 0.89 42.9
10 68.59 0.75 110
11 69.53 0.69 34
12 74.63 0.42 89.3
Reboiler 79.45 0.265 41.2

Discussion of Results

The data provided in Table 1 for the batch distillation experiment illustrates that
we may have a problem with the column or the batch distillation spreadsheet. The
spreadsheet shows that the volume in the reboiler should be changing at a much higher
rate than the column actually performed. Since the spreadsheet had been successfully
used on previous occasions, it is likely that the error is in the column. Attached on the
following pages are the results of the batch distillation experiment (spreadsheet solution
and graphical solutions).
The data provided in Table 2 for the continuous distillation experiment illustrates
that trays 1 through 6 had temperature readings slightly below the boiling point of
methanol. This is likely due to the RTD's not being calibrated correctly. This sheds some
doubt on the accuracy of the results for the remaining trays, which are given in Table 2
provided above. The liquid compositions shown in Table 2 were obtained by using a
methanol-water x, y, T diagram. The useable data was plotted on a x, y diagram to
determine the individual tray efficiencies. The plot illustrating the individual tray
efficiencies is attached on the following page.

Conclusions/Recommendations

During experimentation of the distillation column the group noticed distillate

being formed even during total reflux. This could indicate a problem with the reflux
valve. This could also explain the problem with the reboiler volume during batch
distillation experiments. The behavior of the reflux valve should be monitored to
determine whether it is functioning correctly.
Being able to perform experiments on the distillation column was very useful task
as it provides practical experience in using the theoretical knowledge acquired in the Unit
Operations class throughout the semester.
 Table of Contents

I. Introduction

II. Background

III. Results

IV. Discussion of Results

V. Conclusions/Recommendations

VI. Appendix
APPENDIX