A Study on the Overall Column Efficiency under Different

Operation Conditions of the Distillation Device in UCSB

Chemical Engineering Lab
Jun Lu
August 30, 2018

Abstract
The overall distillation column efficiency in UCSB chemical engineering lab was measured
experimentally at different reflux ratios and reboiler powers. At total reflux, the column
efficiency (46.8 ± 2.1 %) was affected by the reboiler powers (120 ± 2W to 143 ± 2W) by less
than 8 %. At a constant reflux ratio (R=5), overall column efficiency was 57.0 ± 0.3 %.It was
observed that a smaller reflux ratio and a higher reboiler power input increased the overall
column efficiency.

1 Introduction
Separation processes are crucial in chemical engineering. Typical Chemical plants spend 40 % to 70
% of capital cost in separations [1]. Batch distillation, as a major branch of liquid separation, is used
for small-scale operations, up-stream operations, and test runs for new products. By understanding
how the batch distillation column behaves under different conditions, we can maximize the running
efficiency and minimize the capital cost. In this lab, vapor-liquid equilibrium (VLE) principles,
McCabe-Thiele analysis, and Rayleigh method were used to analyze the batch distillation of a
Methanol-Isopropanol mixture.

2 Objectives
The objectives of this study was to (1) measure the overall efficiencies of a batch column in
total reflux using McCabe-Thiele analysis under different power inputs, (2) measure the overall
efficiency of the column under a fixed reflux ratio (R=5), and (3) apply observations for optimizing
the column operating conditions to maximize the overall distillation efficiency.

3 Theoretical Backgrounds
3.1 VLE and Raoult’s Law
Distillation separates liquids based on their different volatilities. When a mixture reaches its boiling
point, it starts evaporating. The more volatile component dominates the vapor phase and the less
volatile component dominates the liquid phase. For a binary mixture at VLE, the degree of freedom
(DOF) is two, meaning that two intensive variables (e.g., temperature, pressure, or composition)
can be specified. Unspecified variables can be calculated by modified Raoult’s Law [Eqn (1)]:

yi P = xi Pi γi (1)
where yi = vapor mole fraction of species i, xi = liquid mole fraction of species i,γi = activity
coefficient of species i, P = the total pressure of the system, and Pi = partial pressure of species i.

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3.2 McCabe-Thiele Analysis
McCabe-Thiele analysis can theoretically predict the compositions of distillate and bottoms based
on assumptions of CMO and adiabatic operation. It provides the following operating line (OL):
R 1
y= x+ xD (2)
R+1 R+1
where y and x are vapor and liquid mole fractions of MVC, respectively, R is reflux ratio, and
xD is the mole fraction of MVC in the distillate. For a binary mixture, modified Raoult’s Law is
applied to both components. VLE curve is obtained by solving two equations simultaneously. It
is plotted as y vs. x with y=x line and the OL. The number of theoretical stages (N theoretical)
is found by stepping off between the VLE curve and the OL from xD to xw , where xw is the mole
fraction of MVC in the reboiler. The overall column and reboiler efficiency (η) is then determined:
N theoretical
η= (3)
N actual
where N actual is the number of actual stages, including the reboiler.

4 Apparatus and Experimental Procedure

As shown in Figure 1, A 10 tray Oldershaw batch distillation column was used to separate a
mixture of methanol and iso-propanol in this lab. The column is vacuum jacketed and silvered for
insulation. Above the column there was an overhead condenser. The reflux ratio was controlled
using a reflux splitter operated by a time activated reflux ratio solenoid valve. The power of this
distillation column comes from the reboiler below distillation column which is heated by a heating
jacket.

Figure 1: Schematic diagram of batch distillation system.

The experiment consists of two parts. For the first part, the batch reactor was run under total
reflux at 130 W. Once the reactor has reached steady state, bottom sample, distillate sample and
last tray sample were collected. Their compositions were then measured by the refractometer. For
the measurement of internal liquid flow rate, the stopcock below last tray was then closed and the
time to reach the 50ml mark was recorded. Internal vapor flow rate was measured by dividing the
mass of distillate by the time used for collection. Above procedure was then repeated at the power
rate of 140W and 120W. For the second part of the experiment, the batch reactor was operated at

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140 W with 850 ml feed at 20% methanol composition. Though adjusting the reflux ratio solenoid,
reflux ratio was set at 5. At steady state, 8 distillate samples with 10ml each were collected and
the collection time were recorded. Their compositions were then measured by the refractometer.

5 Results
Figure 2 shows McCabe-Thiele analysis used for attaining the theoretical number of stages required
for the batch distillation process at total reflux, and thereby the overall column efficiency. In the
case when the power input is 120 ± 2 W, the plot starts from xw = 0.180, the reboiler methanol
molar fraction. The steps go up between the VLE curve and the operating line, until it reaches xD
= 0.768, the methanol liquid molar fraction from the distillate. The fraction of the last stage takes
account for the column inefficiency. In this case the theoretical number of stages (N theoretical) is
4.079, while the actual number of stages (N actual) is 11 (10 trays and one reboiler). The overall
column efficiency (η=37.1 %) is then calculated using equation (3).

Figure 2: McCabe-Thiele analysis. The system is at total reflux and the reboiler power input
is 120±2 W. Steps are plotted between the operating line (y=x) and the VLE curve to find the
theoretical number of stages needed starting from xw = 0.180 and ending when xD = 0.768. It is
found that N theoretical = 4.079 and η = 37.1 %.

Table 1 and Table 2 show the overall column efficiencies at total reflux and R=5 separately.
These efficiencies were analyzed to find under what condition was the efficiency maximized.It
turned out that the overall column efficiency was maximized at a smaller reflux ratio (R=5 instead
of ∞ ) and higher reboiler power input.

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6 Conclusions and Recommendations
This study on the distillation column in UCSB chemical engineering lab has successfully determined
the efficiencies under different operating conditions. The overall column efficiency is maximized
at low reflux ratio and high reboiler power input. Therefore, to perform a distillation task, it is
recommended to use low reflux ratio and high reboiler power inputs to achieve high efficiency. For
future studies, it is recommended that the experiment be performed under a wider range of reflux
ratios to attain a quantitative tendency of efficiency change with respect to the reflux ratio at some
given reboiler power input.

7 References
[1] Wankat, P. “Chapter 9: Batch Distillation.” Separation Process Engineering: Includes Mass
Transfer Analysis. 3rd Ed. Upper Saddle River, NJ. Prentice Hall. 2012.
[2] Gordon, M. “Tray Efficiency and Product Recovery of a Batch Distillation Column.” Written
for ChE 180 Laboratory. Dept. of Chemical Engineering, University of California, Santa Barbara
April 2018.