DEPARMENT OF CHEMICAL ENGINEERING

UNIVERSITY OF CALIFORNIA, SANTA BARBARA

ChE 180B Experiment
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Tray Efficiency and Product Recovery of a

Batch Distillation Column
Revised: January, 2010 (Dale Seborg)

Objectives
1. To measure the overall column efficiency and the reboiler efficiency of a batch
distillation column at total reflux.
2. To use this data to calculate the theoretically expected composition of a given
distillate volume at a given reflux ratio.
3. To carry out a second experiment to test theory with experiment.
4. To develop mass and methanol balances and to analyze the errors of closure using
error analyses.
Equipment and Materials
A batch distillation column (or still) will be used to separate a binary feed mixture of
methanol and 2-propanol (isopropanol). The apparatus is a 10 tray Oldershaw batch
distillation column that is shown in Fig. 1. Each sieve tray is 1 in. in diameter and has a
single downcomer. The column is vacuum jacketed and silvered for insulation but the
trays are still visible through one part of the jacket. The reflux ratio is controlled using a
reflux splitter operated by a time activated solenoid valve which either directs all
overhead liquid to the product line or back into the column. The compositions of liquid
samples can be measured using a bench refractometer. The calibration curve for the
refractometer and detailed diagrams of the column are available in the lab.

Pre-lab Preparation
This experiment requires two full laboratory sessions of distillation column operation. It
also involves considerable pre-lab preparation, as indicated below. This preparation will
take several hours; it is essential that you do it prior to the first lab session. During
your pre-lab interview (5 to10 min), you will show your calculations and graphs, discuss
the main aspects of the experimental procedure, and identify the main safety issuesboth
of a general nature and specific to your experiment. Your state of preparedness and your

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answers to questions will count towards your final grade. You will not be allowed to
operate the column if you are not sufficiently prepared.
In particular, your pre-lab activities should include:
1. Review the theory of batch distillation (see References).
2. Go to the lab and become familiar with the equipment.
3. Calculate and plot the vapor-liquid equilibrium curve for the methanol/2-propanol
system at 1 atm., and the saturation temperature versus composition curve using
the data given below. Use a computer to produce both plots.
4. Determine how you will use the equilibrium curve and the McCabe-Thiele
method to calculate the overall column efficiency at total reflux. Obtain any
physical property information that you will need for these calculations.
5. Make a list of the procedures you intend to follow and a table to record data you
will acquire during the various stages of your experiments. These activities will
include taking of samples at various locations (check where), recording of internal
temperatures at various locations (check where), heater settings, the time at which
these recordings were done, and anything else that may be relevant. Use ink,
never pencils, when recording experimental data.
6. Prepare to be a "good observer," noting the unexpected, and anticipating possible
danger spots in the equipment that will require keeping an eye on. Do not plan to
rely on your partner.
Determination of the Vapor-Liquid Equilibrium Curve
The equilibrium data for the methanol/2-propanol system at 1 atmosphere can be
determined using the Wilson and Antoine equations. If methanol (B.P. 64.7C) is
component 1 and 2-propanol (B.P. 82.4C) is component 2, the activity coefficients of
the components are given by the approximate equations:
Methanol:

ln 1 = - ln ( R1 ) + x2 ( G12 / R1 - G21 / R2 )

(1)

2-propanol:

ln 2 = - ln ( R2 ) - x1 ( G12 / R1 - G21 / R2 )

(2)

where xi = mole fraction of component i in liquid phase, R1 = x1+ x2G12, R2 = x2+ x1G21,
G12 = 1.689, and G21 = 0.5445.
The vapor composition is determined from Eq. (3)

yi P = xi Pi* i

(3)
*

where yi = mole fraction in vapor, P = total pressure, Pi = vapor pressure of pure i. Pure
component vapor pressures as a function of temperature are given by the Antoine
equations:

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methanol (20 to 140C):

log10 ( P1* ) = 7.87863 - 1473.11/ ( T + 230.0 )

(4)

2-propanol (0 to 113C):

log10 ( P2* ) = 6.66040 - 813.055/ ( T + 132.93)

(5)

where P* = vapor pressure (in mm Hg), T = temperature (in C).

Suggested Experimental Procedure
First session: At the beginning of the first session, prepare a mixture 1400100 ml of
123 mole% methanol - 883 mole% 2-propanol. Use any solution remaining from
previous groups. Run the column at total reflux, placing four or five fresh boiling chips
in the reboiler (or still pot) and starting with a heater control setting of no greater than 40.
After steady state has been attained, collect all data necessary to characterize the column
operation and the overall column and reboiler efficiencies. Repeat for no less than three
different internal liquid flow rates. Determine the liquid flow rate where flooding of the
column first occurs.
Between sessions: Use the McCabe-Thiele method and the overall efficiency to
calculate the cumulative distillate composition as a function of the volume of distillate
product recovered (See Ref. 1). Assume an initial charge in the range of 100050 ml and
172 mole% methanol 832 mole% 2-propanol and select a constant reflux ratio
between 5 and 7. Make accurate and careful plots using computer software. Bring all
calculations and plots to the lab for the second session. You will not be allowed to
proceed with the second lab session until these theoretical calculations are
completed.
Second session: Carefully prepare and charge the still pot with the solution of the same
volume and composition as assumed in the distillate recovery calculation. Establish the
desired column characteristics and internal flow rates, as assumed in the calculation.
After steady state during total reflux has been attained, set the reflux timer and vapor
dividing device to the selected value of the reflux ratio. Ensure that the device is yielding
the desired reflux ratio; do not simply trust the timer. Collect the volume of distillate
instructed by the TA, generally 4 x 25 ml samples (approx.100 ml total), and measure the
cumulative composition. Measure the volume and composition of all "waste" solutions
accumulated during the session and of the solution in the reboiler after it cools to room
temperature.
Suggested Presentation of Results and Discussion

Present your most important figures (illustrations, graphs) and tables, (if necessary),
at appropriate places in the main text, not at the end. In particular, include a
schematic diagram of the apparatus, the figures which provided the overall and still
efficiencies at the different liquid flow rates, and the graphs from which you
determined the optimal reflux ratio. Also include a table of mass and methanol

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balance errors of closure and the related error analyses. Other figures and tables can
be placed in the appendices.

Critically comment on any differences between the calculated and experimental

values. Refer to your error analysis and the inherent errors associated with the
calculations in your discussion of results. Discuss in detail what the results mean in
relation to the operation of this distillation column. Do not present results without
also providing an interpretation of them.

Place the error analysis and data reduction calculations in an appendix. Quantify the
magnitudes of all sources of errors associated with the experiment.

References

1. Wankat, P.C., Separation Process Engineering, 2nd ed., Prentice-Hall, Upper

Saddle River, NJ. (2007).
2. Seader, J.D. and E.J. Henley, Separation Process Principles, 2nd ed., Wiley, NY
(2005).
3. Oldershaw, D. F., "Perforated Plate Columns for Analytical Batch Distillation,"
Ind. Eng. Chem., Anal. Ed., 13, 265 (1941).
4. Collins, F. C., and V. Lantz, "Evaluation of Laboratory Distillation Apparatus,"
Ind. Eng. Chem., Anal. Ed., 18, 673 (1946).

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Figure 1. Schematic diagram of the batch distillation apparatus.

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Figure 2. Calibration data for the bench refractometer.

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