DISTILLATION

EUGENE L. CANENCIA

Department of Chemical Engineering, College of Engineering and Architecture, Cebu Institute

of Technology- University, N. Bacalso Ave., Cebu City, 6000 Philippines

To determine the reflux ratio required to recover ethanol of desired purity from an ethanol-
water mixture is the aim of conducting the experiment. The setup was done using a distillation
process through a distillation column with steam as the heating medium. The data required were
the time elapsed where the product receiver was half-filled with the recycle valve being fully
closed and the time elapsed where the product receiver was half-filled with the recycle valve three-
fourths closed. Calculations resulted in a reflux ratio of 0.554 with retrieved distillate being 60%
pure ethanol.
1. Introduction

There are different separation processes involved in the chemical and other physical
processing industries and the food and biological processing industries. This includes
evaporation, drying, distillation, absorption, membrane separation, liquid-liquid extraction,
adsorption, ion-exchange and etc. These processes are involved depending on factors such
as purity of substance to separate, cost-efficiency, type of mixture to process and even
sensitivity of the substances involved. For distillation, the unit operation involved for the
experiment, is used to purify or separate alcohol in the beverage industry and hydrocarbons
in the petroleum industry.

Distillation is the operation whereby components of a liquid mixture are separated

by boiling because of their differences in vapor pressure. The more volatile component
separates first from the mixture and is condensed to obtain a more concentrated liquid of
such component. A typical distillation column has a vertical shell where the separation of
liquid components is carried out, trays and packings which enhances the separation, a
reboiler, a condenser, a reflux drum that holds the liquid reflux that would be returned to
the column, and stream lines both for inlet and outlet flows. The column is classified
depending on the continuity of operation, nature of feed to process, number of product
streams, type of column internals and type of distillation carried out (e.g. Steam distillation,
Vacuum distillation, Simple distillation, etc.).

Since distillation process is done for component enrichment purposes, reflux ratio
is introduced to achieve a specific level of enrichment. Reflux is the liquid condensed from
the rising vapor which returns to the column and the reflux ratio is the ratio between the
amount of the condensed vapor component that returns back to the column and the
component that is collected in the receiver which is also known as the distillate. In this
experiment, the objective is to determine the reflux ratio needed to achieve a desired
concentration of an ethanol-water mixture using the steam distillation column located in
the laboratory.
2. Materials and Methods

2.1 Apparatus

The following apparatus are needed for the experiment:

Steam distillation glass column with condenser and reflux flow control

Pycnometer

Mixing pail

Graduated cylinder

2.2 Materials

The following materials are needed for the experiment:

Ethanol

Water

2.3 Methods

2.3.1 Preparation of the Ethanol – Water Mixture and the Distillation Setup

With the mixing pail in hand, ethanol and water was mixed thoroughly to
achieve an approximately 30% concentration. The mixture was covered to prevent mass
atmospheric vaporization since the mixture is very volatile by nature. The mixture was set
aside and the boiler was turned on to generate the steam required for the process. The
mixture was introduced to the feed spherical vessel. Steam set at 20 psig was introduced to
the column ensuring that the vent lines are open and the overhead condenser was turned
on.

2.3.2 Doing the Experiment to obtain the Reflux ratio

The product off-take valve was closed to set the reflux divider at a total
reflux. After the column has settled down to a uniform total reflux operation, the valve
between the upper product receiver and lower product receiver was closed. The recycle
valve was closed so that the condensate will start to fill the upper product receiver. The
 time to accurately half-fill the upper product receiver was recorded. The time recorded is
the time t1 needed to solve the reflux ratio. After the first part was done, the liquid that
filled up the upper receiver was introduced back to the still via the recycle line. The column
was allowed to settle for 15 minutes and after that, the recycle valve was adjusted to 3/4
open ensuring that there is positive reflux ratio. The time that was needed to half-fill the
upper receiver was recorded as time t2. With the data table being complete for t1 and t2, the
reflux ratio for the setup was calculated and the density of the distillate from the product
receiver was determined using a pycnometer. The density that was determined was used to
find out the concentration of ethanol in the distillate.

3. Results

3.1. Tabulation of Results

Steam Pressure Trial t1 t2 R Density of Distillate

20 psig 1 27.317 minutes 42.45 minutes 0.554 0.903 g/ml

4. Discussion

The experiment was done at a 20 psig pressure for 1 trial only due to time constraint
in the operation of the column. Time in the second part of the experiment tends to be longer
than time t1 because there is already a portion of the condensate recycling back to the still.
Considering the time values obtained from the first and second part of the experiment,
calculations showed that the reflux ratio of the experiment is 0.554 which means that for
every 554 parts of reflux going back to the column there are 1000 parts collected as
distillate. In theory, higher reflux ratios results to a higher purity of the distillate because
more vapor-liquid contact can occur in the column, however, it would mean a slower
collection rate for the distillate. This is also one of the reason why the second part of the
experiment was longer in time record and had a positive value in the reflux ratio which
resulted to a purer distillate. The purity of the distillate was approximately 60%, determined
using density – concentration chart for ethanol-water system at 20°C, using the recorded
 density from a pycnometer test with a value of 0.903 g/ml. This is a purer product compared
to the 30% ethanol concentration fed in the spherical vessel at the start of the experiment.
Data analysis for reflux ratio in any distillation processes is beneficial because it would
determine the number of stages that can be employed to achieve a desired product purity
and determine the effect of achieving such level of purity to the condenser and reboiler
duties.

5. Conclusion

Distillation is a type of separation process utilized to achieve a high purity product.

Involving reflux ratios in any distillation setup will help achieve the desired product purity
while considering the capability of the setup or the equipment. Higher reflux ratios results
to a purer product but longer time of collection with increase in condenser and reboiler
duty at a disadvantage. For an ethanol-water mixture, approximately 60% concentration of
ethanol can be achieved from the distillation process when considering 0.554 value for the
reflux ratio.

6. Recommendation

For the experiment, it would be a recommendation to introduce variations in reflux

ratios so that there will be comparison on how changing the reflux ratio can affect the
resulting product purity and also to prove that the underlying theory for such relation is
true. It would be also helpful to vary the pressure operation and the type of mixture
introduced for the distillation setup so that it can be observed how these parameters could
affect in relation to reflux ratio.
APPENDIX

Appendix A. Calculation for the Reflux Ratio for the Setup

𝟏 𝟏
𝒕𝟏 − 𝒕𝟐
𝑹=
𝟏
𝒕𝟏

𝟏 𝟏
−
𝑹= 𝟐𝟕. 𝟑𝟏𝟕 𝒎𝒊𝒏 𝟒𝟐. 𝟒𝟓 𝒎𝒊𝒏 = 𝟎. 𝟓𝟓𝟒
𝟏
𝟐𝟕. 𝟑𝟏𝟕 𝒎𝒊𝒏

Appendix B. Image of the Steam Distillation Setup

Appendix C. Image of the Ethanol-Water Concentration-Density Table at 20°C
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