Distillation is one the most common unit operations used in the industries.

It is a process wherein
the desired component is separated from the initial mixture by selective condensation or
evaporation. This separation process could be in partial or complete depending on the type of
distillation use [1].
Flash distillation, also known as equilibrium distillation, happens when a definite fraction of the
liquid feed is vaporized and is in equilibrium with the residual liquid. The process also involves
reducing the pressure suddenly to lower the boiling point of the component (hence, it is called
flash distillation). While in batch or differential distillation, the total vapor formed is not in
equilibrium with the residual liquid, therefore removing the bottoms product [2].
Batch distillation will be the focus of this experiment, wherein vapor from the reboiler rises up the
trays in the column and is finally liquefied in the condenser. This condensed liquid could be either
drawn off or reintroduced, also known as reflux, into the top of the column. Reflux are mostly
done to increase the efficiency of the column [2].
Efficiencies of the column can be calculated using several approaches namely graphical methods
like Mc-Cabe thiele, shortcut methods like Fenske-Underwood-Gilligand, and rigorous plate-plate
calculations using computer softwares [3].
The most conventional and accurate way to get the theoretical concentration is by using the Mc-
Cabe Thiele method. This method is mostly used in binary distillation with constant molar
overflow, which in this case, an ethanol-water mixture [4].
For ideal mixtures in thermodynamic vapour-liquid-equilibrium, it follows Equation 1 [5].
1
= Equation 1


Where: = . For real mixtures, = (y= activity coefficient)

For binary mixtures, the most common method to find the concentration of a certain component is
by the Rayleigh Equation [5].

ln ( ) = Equation 2

Where B = bottoms product

xB = mole fraction of the bottoms product
xD = mole fraction of the distillate product
F = Feed
For this experiment, it will focus on getting the most convenient and economical combination of
temperature and reflux ratio under constant time which will give the highest efficiency of the
distillate. The optimization process will be done once all other groups are finish doing the
experiment. The experiment will also focus on getting the final conversion and the efficiency of
the distillate by finding the theoretical distillate concentration at a certain temperature using the
McCabe-Thiele method.
METHODOLOGY
A 5L ethanol-water mixture was prepared by mixing 20% ethanol by weight and80% water by
weight. The specific gravity of the mixture () was then computed using a pycnometer. The ethanol-
water mixture was poured into the evaporator. The distillate drain valve in the reflux divider was
made close to avoid spillage. The reflux ratio was then set to 0 and the condenser was connected
to the faucet. Flow rate was then set to 150L/hr. The students measured the specific gravity of the
distillate every 3 minutes at 80oC (See Table 1.1 for the data). After collecting the data, the master
switch and water supply was turned off. Lastly, the system was cooled down before draining the
evaporator.
DATA AND RESULTS
At reflux=0 and T=80oC, the students obtained the weight of the pycnometer with the distillate at
3 minutes interval until it reaches the 30-minute mark. (See Table 1.1)
Table 1.1 At T=80oC, Reflux ratio=0
Time (min) Mass of the Distillate + pycnometer (g) *Density of the Distillate (g/mL)

3 42.6344

6 42.5886

12 42.4146

15 42.6215

18 42.7543

21 42.9019

24 42.8186

27 43.0841

30 42.7035

*See Appendix A for the sample calculation on how to get the density of the distillate.
CONCLUSION AND RECOMMENDATION
Some factors that may had affect the distillate concentration is that while getting the distillate every
3-minute intervals, the students did not cool down the mixture to the indicated temperature written
in the pycnometer. With this, the weight of the distillate was not constant throughout the process.
Also, it should be noted that if distillate production is too slow to generate, it is because of the air
pressure inside. Make sure to open the pressure valve that will release the trapped air and that will
release the distillate.
ANSWERS TO QUESTIONS
The use of reflux is widely used in industries that uses distillation columns as their main separation
process like in petroleum refineries and natural gas processing plants. The more reflux is done by
the system, the better is the column's separation (difference in boiling points) [6]. Therefore, reflux
is the term used to express the amount of top product, which is put back into the tower. Having a
100% reflux means that all distillate will be return to the column and no distillate will be collected.
It will be an endless cycle or loop.
One reason that the students had encountered during the experiment is when the temperature could
not increase even though it was set to 80oC (highest temperature was 30oC). This was due to the
fact that air bubbles are trapped inside the tubes, hindering the heat to go up the column. To fix
this, the valve connecting to the distillate tank should be opened minimally to let the pressure
inside the tubes be released therefore removing the air bubbles.
The temperature of the column will vary depending on what will be the desired distillate. For an
ethanol-water mixture, the ideal temperature should be higher than the boiling of ethanol which is
78oC but lower than the boiling point of water which is 100oC. If the columns temperature is
higher than 100oC, the distillate will now contain small amount of water for it already boiled too.
While the higher the reflux ratio, the more vapor-liquid contact will be. Therefore, a higher reflux
ratio means higher purity of the distillate but also means that the collection rate(volume) for the
distillate will be slower [6]. In the case of this experiment, if the time is limited, a high reflux ratio
is not recommended if a company wants a higher volume and a negligible purity concentration.
The common difference between batch distillation and continuous or flash distillation is that in
flash distillation the feed is continuously entering the column, while in batch distillation the feed
is charged into the evaporator at the beginning of the operation. The evaporator in batch distillation
gets empty over time, therefore giving the process an unsteady-state nature [7].