HUMG Advanced Program

ECH 155A
Chemical Engineering Laboratory
Distillation Experiment
Goals of the Experiment
Primary goal of this experiment is to (i) estimate the efficiency of a distillation column, (ii)
investigate whether the column is operating at steady state, constant molar overflow and (iii)
provide an estimate of the column energy balance and energy efficiency.
Theoretical Background
McCabe and Thiele [4] provide a graphical method of analysis for distillation columns (see
also the handout distill.pdf). Their analysis requires knowledge of the vapor-liquid equilibrium
curve. Some tabulated data can be found in the paper by Arce et al. [1]. That paper
also provides a thermodynamic model from which the equilibrium curve may be constructed (see
also the handout thermo.pdf, or the text by Smith and Van Ness [5]). In this lab, an 12 sieve plate
distillation column will be used to separate a water-ethanol mixture which is approximately 1525% ethanol by volume. The column will be run at reflux ratio.
Experimental Apparatus
The experiment will be run on the Didacta IC 18 DV continuous distillation column.
Thermocouple locations are numbered T1-T12. Valves are numbered EV1- EV5. The top
product is sampled using valve V1. The bottom product (waste) is sampled using V2. To measure
the percentage of ethanol in the product and waste streams and along the column we will use a
Refactometer.
Experimental Procedure
Fill the boiler with approximately 5 liters of 25 volume percent that ethanol solution. Close
all valves, except for V 5 which regulates cooling water. To ensure the cooling water
backpressure does not cause the tubing to come off, V 5 should be fully open before turning on
the cooling water at the wall. A low flow rate (~300cc/min) should be sufficient and should be
primarily set with the source water valve on the wall. Only small adjustments can be made with V
5 to ensure there is not a large back pressure. Consult with TA when adjusting the water flow
rate.
All data collected by the groups will be carefully recorded in an organized manner to enable easy
sharing of data among groups.
When considering optimal operating conditions, the desired product composition is 60 mole %
ethanol or as stated by the TA. The highest production rate of this composition under the most
energy efficient means is the desired operating condition.

Reflux ratio of :
1. Turn the reflux pump off to use a reflux ratio . Heat the column using 1.5kW power until
condensate if observed, then reduce power to 0.75kW. Allow column to reach steady state (~1530min once the volume in the reboiler is heated).
Observe behavior of the column and appearance of the liquid on the various trays by
moving insulation periodically. Record observations of column behavior on the trays.
Allow column to reach steady state.
Record column temperatures including the temperature at each plate, the boiler, and the
reflux stream as well as the cooling water. This can also be done via the computer if you
keep track of the time stamp.
Record water flow rate.
Sample top product (V 1). When measuring from V 3, 5-10 ml of sample must be
discarded because the tubing will contain fluid that is not well mixed. (Note: you must
keep some fluid in the line to ensure that vapor does not escape from the column as you
take your sample. Thus, valve V 3 can only be fully opened while there is fluid in the line
to prevent vapor from leaving the column. It would be very helpful to know the
production rate for your energy balance. Use your engineering skills to try to figure out a

means to determine this. CAREFULLY time how long it takes to collect a 1-5mL sample
of product. Repeat this measurement in a second collection tube.
Sample the boiler content (V 2).
Measure the concentration of the fluid collected from the top and bottom of the column.
The density meter needs at least a 3 ml sample at a temperature between 0-40C. Thus,
you may need to cool the sample before taking a measurement.
Measure the composition of the liquid phase at each tray as necessary for any additional
information you deem necessary.

2. Change the power to the reboiler, cooling water flow rate, etc. to operate the column more
efficiently. At steady state, repeat measurements listed above or as many as you deem necessary.
Data Analysis
Estimate the column efficiency.
Plot a temperature-composition ethanol-water phase diagram. For the studied reflux ratio, plot
measured plate temperatures. Infer from this plot the equilibrium compositions on each plate and
compare against the McCabe-Thiele analysis and sampled fluid concentrations.
Compute liquid and vapor enthalpies corresponding to measured plate temperatures and estimated
plate compositions. (A few measurements of plate liquid composition will be helpful for this
analysis. However, you only need a few plate measurements for this comparison.) Investigate the
validity of the McCabe-Thiele assumption that molar liquid and vapor fluxes are constant. (Excess
enthalpy data is given by Costigan et al. [2]).
Carry out an energy balance on the column using your engineering skills and estimate the energy
efficiency (heat loss) of the column under the various operating conditions. Relate this balance to
the constant molar overflow assumption. Suggest conditions for maximum energy efficiency to
obtain the maximum production rate of the desired ethanol product composition.
References
[1] A. Arce, J. Martinez-Ageitos, and A. Soto, VLE for water + ethanol + 1-octanol mixtures.
Experimental measurements and correlations, Fluid Phase Equilibria 122, 117, 129, 1996.
[2] M. J. Costigan, L. J. Hodges, K. N. Marsh, R. H. Stokes, and C. W. Tuxford, The isothermal
displacement calorimeter: design modifications for measuring exothermic enthalpies of mixing,
Aust. J. Chem., 33, 2103-2119, 1980.
[3] K. N. Marsh and A. E. Richards, Excess volumes for ethanol+water mixtures at 10-K intervals
from 278.15 to 338.15K, Aust. J. Chem., 33, 2121-2132, 1980.
[4] W. L. McCabe and E. W. Thiele, Graphical Design of Fractionating Columns, Ind. Eng.
Chem., 17(7), 605-611, 1925.
[5] J. M. Smith and H. C. Van Ness, Introduction to Chemical Engineering Thermodynamics, 3rd
ed., McGraw-Hill, New York, 1975.