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CEBU INSTITUTE OF TECHNOLOGY – UNIVERSITY

COLLEGE OF ENGINEERING AND ARCHITECTURE DEPARTMENT OF CHEMICAL
ENGINEERING

Laboratory Experiment Report #7

Experiment #1 DISTILLATION

Author: Joshua L. Climaco

Date Started: September 26, 2019

Date Finished: September 26, 2019

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Abstract

The objective of the experiment is to determine reflux ratio required to recover ethanol of

desired specification for ethanol-water mixture. Distillation deals with a mixture, a solution

composed of two or more elements, that when boiled, will cause each element to vaporized at

different temperatures. Distillation is only effective if there is a significant difference between

the boiling of the two elements. Every element had a unique boiling point specific to the amount

of bonds and structure of that element. Fractional distillation is more effective form of

distillation because it more accurately separates the ethanol from the water in a specific volume

of ethanol-water solution.
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I. Objectives
The objective of the experiment is to determine reflux ratio required to recover ethanol
of desired specification for ethanol-water mixture. Distillation deals with a mixture, a solution
composed of two or more elements, that when boiled, will cause each element to vaporized at
different temperatures.

The purpose of a distillation column is to separate a compound containing two or more

MUTUALLY SOLUBLE solution by their variation of individual boiling points. For the example,
crude oil has many compounds in it, which you cannot separate by filtering or by other processes.
Hence you send the oil into the distillation column and out comes light gases like methane at the
top ( least boiling point / temperature) and tar in the bottom of the column ( highest boiling point)
and various compound like gasoline, diesel, kerosene etc in between.
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II. Equipment and Materials

2.1 Equipments and Materials

2.1. Materials and Apparatus:

• Glass distillation apparatus complete with condenser and reflux flow control
• Stem generation thermometer
• Westphal balance or refractometer
• Ethanol
• Water
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III. Relevant Theory and Background Information

Fractional distillation is the separation of a mixture into its component parts, or fractions.
Chemical compounds are separated by heating them to a temperature at which one or more fractions
of the mixture will vaporize. It uses distillation to fractionate. Generally the component parts have
boiling points that differ by less than 25 °C from each other under a pressure of one atmosphere. If
the difference in boiling points is greater than 25 °C, a simple distillation is typically used.

The reflux ratio is one of the main variables encountered in a large scale fractional
distillation. Reflux ratio can be defined as the weight of liquid retained as reflux divided by the
weight removed as overhead product. At total reflux, the separation desired is achieved with the
smallest packed height. In this experiment, the packed height is fixed and must be operated at a
reflux ratio below total reflux. An increase in the reflux ratio will improve the separation achieved
and consequently increases the proportion of ethanol in the overhead product.
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IV. Procedures
All the vent lines provided are opened. The overhead condenser cooling water
supply was turned on. The spherical vessel was charged up to the equator with 30% by
weight ethanol-water solution. The by-pass around the steam trap was opened and then
turned on the main stream carefully but positively. When the initial surge of condensate has
cleared, the steam trap by-pass valve was closed and then the steam pressure was set up to
a suitable figure between 20 and 50 psig. The reflux divider was set for total reflux by
closing the product off-take valve. When the liquid boiled in the still, the vapours were
passed up the column to the condenser. All the condensate passed back into the column.
The reboiler steam pressure was adjusted to a value which gives adequate loading on the
packed column. This was not less than 20 psig.

The unit time was given to settle down after each change in reboiler steam pressure.
This steam pressure was maintained for the duration of the experiment.
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V. Experimental Data Analysis and Discussion

Fig 5.1 Tabulated data and results

Steam
pressure Trial t1 t2 R
1 30.1667 33.6167 0.1143635
20
2 23.317 42.45 0.8205601
1 14.33 10.93 0.2372645
25
2 23.02 47.57 1.06646139

VI. Conclusion

Reflux Ratio is the ratio of the liquid that has returned to the distillation column to the
amount of liquid removed. The calculation of the Reflux Ratio includes the composition of vapor
pressure that is leaving the plate. There are two extreme considerations of Reflux Ratio: total reflux
and minimum reflux. Total reflux means that all the condensed water is returned without adding
any product or feed. It can be achieved in very fewer stages of separation. Minimum reflux, on the
other hand, a lot more stages are required than total reflux to achieve separation.
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VI.

Recommendations

The group would recommend to use the most functional equipment and unit

operations like the Distillation column. The outcome of the conclusion is highly

dependent on the data of the experiments. Patience and focus are highly needed

because the readings are not as consistent as the proponents would have wanted it

to be. The proponents should also already have familiarized the basic knowledge of

Distillation and its basic calculations and formulas before the experiment is

executed.

References

[1] Geankoplis, C.J. (2009) Principles of Transport Processes and Separation

Processes. 1st edition. Pearson Education South Asia PTE. LTD.

[2] http://www.separationprocesses.com/Distillation/DT_Chp04n.html
Retrieved on September 24, 2018

[4] Principles of Distillation [Online]: http://www.fao.org/3/t1838e/t1838e0u.htm.

Retrieved on Aug 29, 2019

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VII.

Appendices
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VIII.
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