DISTILLATION SEPARATION OF ETHYL ACETATE AND WATER

Beltrán María, Cortés Paula, Garzón María, Vargas Nayarith

Group 1

1. INTRODUCTION

In this work we evaluate the ability to solve a problem of separation of two components to be able
to reuse some this could be solved by means of an extractive or azeotropic separation process
depending on the case. Our specific group was asked to separate ethyl acetate from water since it
is the most volatile component and was requested with a 99% piglet. Next we will talk about the
compounds that are going to be used in the process in order to contextualize more to what is going
to be done and the importance of the separation of the ethyl acetate in the mixture with water, as it
is a mixture with water, only an introduction to ethyl acetate will be made.

2. RESULTS

After analyzing all possible cases the separation could be resolved in different ways such as
azeotropic distillation since as shown in Figure N.1, an azeotrope is presented in a composition of
0.672, however there is another process which corresponds to the flash distillation where it was
carried to the azeotropic point, there is a curve of misibility and two phases are formed, after that it
is taken to an evaporator at the boiling point of ethyl acetate and then that vapor current is sensed
and sent to a binary distillation column to finally obtain a purity of 99% ethyl acetate. This method
facilitates the process since both water and ethyl acetate have boiling points far away according to
the atmospheric pressure that is handled in Bogota.

The process that is carried out involves in principle a Flash distillation, this distillation is generally
used for the separation of components by phase change, taking advantage of the chemical
balance of the basic operations of chemical engineering. In this case we have a mixture of ethyl
acetate and water at a composition of 15 percent by weight to weight of ethyl acetate, which
corresponds to a molar fraction in the feed of 0.035 of ethyl acetate; the first consideration is the
selection of the method for the simulations are developed in ASPEN PLUS V9, since we have a
pressure below 10 bar, likewise the method used was UNIQUAC.

Taking into account the main purpose of flash distillation, to achieve maximum recovery of ethyl
acetate, the purity with which the ethyl acetate will be recovered must also be analyzed and this
depends directly on the temperature and pressure conditions inside the drum. The purity in a
mixture is defined by the molar fraction obtained, either vapour or liquid, and relates the amount of
mol of the desired compound (Ethyl Acetate). (4) Regardless of the temperature and pressure
conditions under which it will operate. At first, the thermodynamics of the mixture were analyzed in
order to obtain the maximum possible composition and to observe if there were any azeotrophs.
The Txy diagram for this mix is shown below:

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 T-xy diagram for ETHYL-01/WATER
105,0

x 1,1 atm
102,5 y 1,1 atm

100,0

97,5

95,0

92,5
Temperature, C

90,0

87,5

85,0

82,5

80,0

77,5

75,0

72,5
0,00 0,05 0,10 0,15 0,20 0,25 0,30 0,35 0,40 0,45 0,50 0,55 0,60 0,65 0,70 0,75 0,80 0,85 0,90 0,95 1,00
Liquid/vapor mole fr action, ETHYL-01

Figure 1: Temperature diagram with respect to the mole fraction of ethyl acetate and water at a pressure of 1.1
atmospheres

From this graph we can analyze that the mixture has an azeotropic point located at a molar fraction
of 0.672, which indicates that this is the maximum composition that can be obtained in the first
distillation, it can also be observed that to reach this azeotrope the mixture must be fed to the
distillation drum at a temperature of 73,5 °C, according to the boiling point of the Ethyl Acetate
corresponding to 70,06 °C, making the temperature correction with respect to the pressure which
is 1,1 atmospheres, for this reason the mixture would enter a state of Liquid-Vapour equilibrium. To
reach this temperature it is necessary that the feed is heated by a boiler before entering the drum.

To establish the temperatures in the equipment, the temperatures of the compounds were
calculated at the atmospheric pressure of Bogotá 0.7368 atm. This is because the liquids undergo
a change in boiling temperature due to variations in sea level altitude. The higher a site is above
sea level, the lower the boiling temperature [1]. The calculations that defined the temperature of
each compound are as follows:

Pressure in Bogotá: 560 Torr (0,7368 atm)

WATER (100°C – 1 atm)

ETHYL ACETATE (77 °C – 1 atm)

[2]

As the difference in boiling points is high at about 20°C, a flash distillation was performed to
separate the ethyl acetate from the water.
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The recovery of hydrogen is one of the most important points for this design, as it is the objective
of the first Flash distillation to be carried out, this is done with the aim of recovering the greatest
amount of ethyl acetate from the initial mixture. The % of recovery can be analyzed from the
simulations, this percentage is calculated from the initial feed and composition of the target
compound (Ethyl Acetate) as well as those obtained for each current. The initial feed of the mixture
is 2,037 kmol/hour and a mole fraction of 0,035 for ethyl acetate, when the simulation is carried
out, steam and liquid molars are fractionated with their respective flow rates in kmol/hour and
according to these results it is analysed whether the separated quantity corresponds to the largest
possible quantity introduced into the distiller, taking into account the law of conservation of mass
and azeotrope of this binary mixture.

Considering the costs, in principle the design was focused on the integration of a solvent into the
Ethyl Acetate/Water mixture, however due to the difference in boiling temperature in the binary
mixture, it was enough to start with a Flash Distillation, However, the money that would be used for
the purchase of solvents that would be introduced to the mixture is now used for the design of the
equipment and the pre-treatment of the mixture because it cannot be handled at atmospheric
pressures but it is necessary to raise this value to a Pressure of 1.1 atmospheres that were initially
taken into account to add to the mixture were: Dimethyl sulfoxide, glycerin, 1-naphthol, among
others. These were selected according to their properties, for example they should have low
volatility, a higher boiling point than water and ethyl acetate and should not be able to form an
azeotrope the other two components of the mixture.

Once the distillate vapor is obtained in the first distillation, a condenser is introduced, this is done in
order to return the mixture that came out of the distillation stream to miscible liquids, as the
objective of this design is to reach a purity of 99. the reason why the condensing function is
condensed, the function of this condenser is the phase change, for this reason the nature remains
of 0,672 after leaving the condenser and for the conservation of mass it has a molar flow of 0, 0724
Kmol / hour. Once this mixture of miscible liquids is obtained, it goes through a decanting process
due to the fact that in this mixture there are still minimal quantities of water, after it is decanted,
ethyl acetate is obtained. However, even after decantation, a binary distillation is carried out to
further purify the ethyl acetate and obtain it in a vapour state, for this reason this distillation column
only has a condenser in the enrichment part and has no reboiler on the stripping side

3. CONCLUSIONS
4. REFERENCES

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