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A Report on the Distillation Column Experiment

Abstract

An experiment of the batch distillation of an ethanol–water binary mixture was performed in a

laboratory. An evaporator, a long tube with eight stages, and a water-cooled condenser are the

apparatus used in the experiment. The findings revealed that the mass ethanol percentage in the

original mixture, top, and bottom products varied with time. At 13.5 wt % ethanol mass

fractions, it was found that heating the initial combination to 90.2 °C ensured that the mixture

fell in the vapor-liquid zone between the bubble and dew point temperatures, allowing

distillation separation to occur. As a result of the higher volatility of ethanol, the top product had

the largest ethanol mass fraction of 75 wt %. Still, the bottoms had the lowest because most

ethanol was evaporated, leaving roughly 90 wt %water. Additionally, an examination of the

column temperature measurements revealed no difference between the theoretical and

experimental values of ethanol mass fractions in the bottom product because both were 10 wt %.

Still, the top product theoretical value was observed to be 77 wt %, which differed slightly from

its experimental value of 75 wt %, resulting in a 2.66% percentage error.

 
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Introduction

A distillation column is a basic requirement in the distillation of liquid mixtures to

separate the mixture into its constituent parts, depending on differences in volatilities. Simple,

fractionating, and vacuum distillation columns are among the various types of distillation

columns, each designed to perform a specific type of separation. In a simple distillation column,

two liquids with different boiling points are separated by directly passing the vapors from the

reboiler to a condensing column which condenses the vapor components. As such, it is said to

only condense the liquid once, and the boiling temperatures of the two experimental liquids must

be far apart for it to be effective.

 On the other hand, Fractional distillation operates on the same concept; however, it tends

to combine numerous simple distillations into a single device. It involves boiling the mixture in a

fractionating column, a long tube that permits the liquid to evaporate and condense numerous

times to optimize the distillation process and achieve higher purity products than ordinary

distillation. The number of times the liquid is vaporized and condensed is what differentiates

between simple and fractional distillation. Similarly, vacuum distillation is used when the
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materials to be distilled have very high boiling points and atmospheric pressures; hence the

pressure is reduced below atmospheric.

Basic Operation of Distillation Column

Distillation columns are made up of many different parts, each utilized to transfer heat or

improve material transmission. The apparatus begins with heating a feed mixture to its boiling

point, with the more volatile or low-boiling components going to the upper part and the less

volatile or high-boiling components going to the lower part. A condenser then splits the vapor

stream, leaving the top into two completely or partially condensed streams. One stream is

recirculated as a reflux stream through the column, while the latter is drained as distillate. The

reflux drum's purpose is typically to hold the condensed vapor from the top of the column so that

the liquid can be recycled back to the column to increase the purity of the desired product.

 
Figure 1: Industrial Scale Distillation Column  

             

The less volatile component is then separated into two streams at the bottom section. One

stream is discharged as bottoms product, while the other is reboiled in a reboiler and returned to

the column to remove any remaining amounts of the more volatile component. This procedure is
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repeated until vapor-liquid equilibrium is reached. The combination is heated, and the liquid with

the lower boiling point is evaporated, condensed, and drips into the final vessel in a simple

distillation. 

Distillation columns are mainly used to separate fuels with differing boiling points in the

oil and petrochemical industries. The experiment is always undertaken in both batch and

continuous mode. The evaporator is charged in batch mode, and the distillation is continued until

no more distillate is produced. At this point, another batch is injected until the desired ethanol

purity is achieved. In continuous mode, the feed mixture is continually pumped while the

distillate and residue are continuously discharged. The distillation of a binary mixture of ethanol

and water was carried out in batch mode in this experiment, with the goals of determining the

ethanol mass fraction in the initial mixture and both the top and bottom products, depicting the

change in the ethanol mass fraction in the top product over time, and recording and analyzing the

temperature profile in the column.

A procedure called fractional distillation is used to separate an ethanol and water mixture.

The fact that the chemicals in the mixture have various boiling points is used in this procedure.

Because ethanol boils at 78.4°C and water at 100°C, when this mixture is heated, the ethanol

vaporizes faster and gets more concentrated in the vapor phase. In contrast, the majority of the

water remains in the liquid phase. The apparatus in this experiment uses the same fractional

distillation technique, with the ethanol/water mixture being poured into a round-bottom flask to

which the fractionating column is attached. There's also a condenser where the vaporized alcohol

(ethanol) is condensed and captured as distillate. At 78.2 °, however, this mixture of ethanol and

water tends to form an azeotrope, resulting in a persistent boiling mixture whose proportions

cannot be altered or changed by fractional distillation. When an azeotrope is cooked, the vapor
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has the same constituent proportions as the unboiled combination. As a result, during distillation,

this temperature should be avoided.

Conclusion and Recommendation

In summary, the experimental and theoretical ethanol mass fractions in the top and

bottom products were compared after determining the ethanol mass fraction in the initial mixture

and analyzing the temperature profile in the distillation column. When the temperature of the

evaporator was increased to 92.2 °C, the ethanol-water combination moved into the vapor-liquid

zone between the bubble and dew point temperatures, resulting in distillation separation at the

provided ethanol mass fraction of 15 wt %. It was also noticed that the top product had the

highest mass fraction of ethanol with a value of 75 wt %, while the bottom product had the

lowest value of 10 wt %. This is mainly because ethanol is the more volatile component, and

when heated, it vaporizes and reaches the top product to a greater extent than the less volatile

component. 

In addition, from the findings, there was a decreasing profile in the temperature column,

with the highest temperature of the column being at 92.2 °C, which kept on decreasing as it got

closer to the evaporator. From there, it can be concluded that, as the vapor travels up the column

through the stages, its pressure decreases along with its temperature due to heat loss as it gets

farther from the reboiler and closer to the condenser until it hits 81.7 °C, which is the lowest

temperature. Consequently, the findings revealed no difference between the theoretical and

experimental values of ethanol mass fractions in the bottom product. This was discovered after

drawing the number of theoretical stages of the column inside the constructed Txy. From this, we

found the theoretical top and bottom products ethanol mass fractions because both had a value of
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10 wt %. In comparison, the theoretical top product value was 77 wt %, which differed slightly

from its experimental value. Therefore, to avoid errors, it is important to properly heat the initial

combination to achieve the necessary separation distillation, follow adequate sample protocols

and avoid operating temperatures around the azeotrope temperature of 78.2 °C.