KWAME NKRUMAH UNIVERSITY OF SCIENCE AND TECHNOLOGY

COLLEGE OF ENGINEERING

DEPARTMENT OF CHEMICAL ENGINEERING

TITLE: COMPUTER CONTROLLED DISTILLATION COLUMN

GROUP 2B

NAME INDEX NUMBER SIGNATURE

KYERMANTENG LINDA ADWOA 3650418

ATSIA

AMUZU DELADEM KWASI 3645318

OWUSU RICHARD ANSAH 3645718

DICKSON PRECIOUS

BEDIAKO-POKU MARY 3647018

KYEI MAAME AKOSUA ODEI 3654218

OTEN JOSEPH 3651818

BENTIL ASIEDU KWAME 3647318

NUHU-ABDUL MAJID 3650918

 CONTENTS
LIST OF FIGURES...........................................................................................................2

LIST OF TABLES............................................................................................................2

CHAPTER 1......................................................................................................................3

1.0 INTRODUCTION...................................................................................................3

1.1 AIMS AND OBJECTIVES.....................................................................................6

1.2 RAOULT’S LAW....................................................................................................7

1.3 AZEOTROPIC MIXTURES...................................................................................8

1.4 MCCABE-THIELE METHOD USING WATER AND ETHANOL.....................9

CHAPTER 2....................................................................................................................10

2.0 CHEMICALS AND APPARATUS......................................................................10

2.1 PROCEDURE........................................................................................................11

CHAPTER 3....................................................................................................................12

3.0 RESULT AND DISCUSSION..............................................................................12

3.1 RESULTS OF EXPERIMENT..............................................................................12

3.2 CALCULATION OF XB-VALUES BY INTERPOLATION...............................15

3.3 DISCUSSION........................................................................................................18

CHAPTER 4....................................................................................................................19

4.0 CONCLUSION......................................................................................................19

4.1 SAFETY AND PRECAUTIONS..........................................................................19

4.2 SOURCES OF ERROR.........................................................................................20

CHAPTER 5....................................................................................................................21

5.0 POST LAB QUESTIONS.....................................................................................21

5.2 REFERENCES......................................................................................................25
 LIST OF FIGURES

Figure 1. 1: Computer Controlled Distillation Unit..........................................................6

Figure 1. 2: T-X-Y diagram of an ideal mixture...............................................................8
Figure 1. 3: T-X-Y diagram of an azeotropic mixture......................................................8
Figure 1. 4: McCabe Thiele Illustration............................................................................9

Figure 3. 1: Calibration curve..........................................................................................14

Figure 3. 2: Equilibrium curve........................................................................................14
Figure 3. 3: Determination of vapour mole fraction at minimum reflux ration..............16
Figure 3. 4: Determining the number of stages using Maccabee and Thiele Method.....17
Figure 3. 5: Schematic diagram of a batch reactor..........................................................24

LIST OF TABLES

Table 3. 1: Data for Calibration curve.............................................................................12

Table 3. 2: Result of distillation......................................................................................12

Table 3. 3: Equilibrium data for water-ethanol system...................................................13

Table 3. 4: Boiler and Distillate mole Fraction...............................................................15

Table 3. 5: Differences between Continuous distillation and Batch distillation.............23

 CHAPTER 1

1.0 INTRODUCTION
Distillation is a method of separating the components of a solution which depends upon

the distribution of the substances between a liquid and a gas phase, applied to cases

where all components are present in both phases (Treybal, 1980). Instead of introducing

a new substance into the mixture in order to provide the second phase, as is done in gas

absorption or desorption, the new phase is created from the original solution by

vaporization or condensation. During most of the century, distillation was by far the

most widely used method for separating liquid mixtures of chemical components.

(Taylor and Krishna, 1993). Despite the high energy requirements, distillation is

typically favoured over other separation processes since it needs less upfront investment

and produces high purity products. Despite the recent advent of various novel separation

technologies (e.g., membranes), distillation remains the most popular chemical

engineering unit activity.

In chemical factories known as distilleries, distillation is used to produce gasoline,

xylene, distilled water, alcohol, paraffin, kerosene, and a number of other liquids. It is

also used to cleanse and separate liquid mixes of one or more liquids. Distillation is

used to separate components from a liquid combination based on the variations in

boiling points of the constituent components. Furthermore, the boiling point of the

liquid will vary based on the amounts of the components present. As a result, distillation

operations are dependent on the vapour pressure properties of liquid mixtures. A

combination of liquids can be separated by heating it to drive components with differing

boiling points into the gas phase. The gas is then condensed and collected in liquid

form. The overhead distillate and a bottom product are among the products. Double

distillation is the technique of repeating the procedure on the collected liquid to increase

the purity of the result.

Although most people associate distillation with liquids, it may also be used to separate

gases by liquefying components using temperature and/or pressure variations. For

example, nitrogen, oxygen, and argon may all be distilled from air.

Steam distillation, simple distillation, fractional distillation, and vacuum distillation are

all forms of distillation. Heat-sensitive components are separated via steam distillation.

When steam is introduced to the mixture, some of it vaporizes. This vapor is condensed

into two liquid parts after cooling. The fractions are sometimes collected separately or

given distinct density values so that they can separate on their own. Steam distillation of

flowers, for example, produces volatile oil and a water-based distillate. When the

boiling points of two liquids are significantly different, simple distillation can be

employed to separate liquids from solids or nonvolatile mixers. A mixture is heated to

convert the most volatile component from a liquid to vapor in simple distillation. The

vapor rises to the top and condenses in a condenser. Typically, the condenser is cooled

(e.g., by circulating cold water around it) to promote vapor condensation and collection.

Vacuum distillation is employed to separate components that have high boiling points.

Lowering the pressure of the equipment also lowers boiling points. Otherwise, the

method is comparable to other types of distillation and it is especially useful when the

conventional boiling point exceeds the decomposition temperature of a compound.

When the boiling points of the components of a mixture are close to one other, as

indicated by Raoult's law, fractional distillation is used. A fractionating column is used

to separate the components via rectification, which is a sequence of distillations. A

mixture is heated so that vapor rises and enters the fractionating column in fractionation.

As the vapor cools, it condenses on the column's packing. This liquid vaporizes again as

a result of the rising vapor's temperature, pushing it up the column and finally giving a

higher purity sample of the mixture's more volatile component.

The Computer Controlled Continuous Distillation Unit, "UDCC", is used in this

experiment and it is basically composed of a boiler on which different types of columns

can be adapted (plate columns and Raschig rings column). An eight-plate column, a

reflux system, a tank for distillation, a vacuum pump and a feeding pump (for

continuous feeding) are included. The steam that goes to the head of the column is sent

to a total condenser. The cooling water flow that crosses the condenser is regulated and

indicated in a flow sensor. Distillation can be carried out at low pressures with the help

of an adjustable vacuum pump. The pressure loss in the column can be measured with a

pressure sensor. It allows continuous operation and batch operation. For proceeding to

continuous feeding, a pump that can inject the substance directly into the boiler or in

any of the plates is available. The temperatures of the system are measured by sensors

placed in strategic positions. This Computer Controlled Unit is supplied with the

EDIBON Computer Control System (SCADA), and includes: The unit itself, a control

interface box, a data acquisition board, a computer control, data acquisition and data

management software packages, for controlling the process and all parameters involved

in the process. The use of the computer-controlled distillation unit helps to analyze real-

time data for the distillation of alcohol and water in this lab work. A brix refractometer

is then used to measure the %brix of the distillate and reboiler at various time intervals

in order to determine their compositions.

Figure 1. 1: Computer Controlled Distillation Unit

1.1 AIMS AND OBJECTIVES

i) To offer a fundamental understanding of distillation so that students are

familiar with the UDDC unit's functioning and idea.

ii) To analyze the distillation operating line using the McCabe Thiele diagram.
1.2 RAOULT’S LAW
The value of the mole fraction of alcohol in water at a given temperature is obtained
using Raoult's Law, allowing the bottom curve of the phase diagram to be drawn. It is
mathematically defined as;
¿
¿ ¿ P−P B (T )
P= X A P (T )+(1− X A )P (T )=¿ X A = ¿
A B ¿
P A (T )−P B (T )

The relationship between the mole fractions of the elements in the liquid and vapor
phases must be employed to depict the upper curve of the diagram.

PA P¿A P−P¿B (T ) P¿A (T )

y A = =X A = .
P P P¿A ( T )−P¿B (T ) P

Where X A = mole fractions of component A,

X B = mole fractions of component B at the temperature of the system.

P = the total pressure of the ideal mixture

¿
P A = the partial pressure of component A

¿
PB = the partial pressure of component B
1.3 AZEOTROPIC MIXTURES
A minimal boiling azeotrope is formed at a certain composition by a solution that

deviates from Raoult's law in a positive way. An ethanol–water combination, for

instance. After distillation, azeotropic mixtures have the same chemical ingredient ratio;

at a given pressure, boiling creates a vapor with the same chemical constituent ratio as

the liquid. An ideal mixture follows Raoult’s law. The point at which the vapor and the

liquid compositions are the same is called an azeotropic point. At the Azeotropic point,

the mixture cannot be separated into its component.

Figure 1. 2: T-X-Y diagram of an ideal mixture

Figure 1. 3: T-X-Y diagram of an azeotropic mixture

1.4 MCCABE-THIELE METHOD USING WATER AND ETHANOL
The heat (energy) required to vaporize or condense a mole of ethanol is approximately

equal to the heat (energy) required to vaporize or condense a mole of water, and is

approximately equal to the heat (energy) required to vaporize or condense any mixture

of the two, according to an analysis of the ethanol-water distillation system. Because of

this link, the tower may be explored using visual techniques that employ straight lines.

The 45° line depicts the probable areas where the vapor concentration equals the liquid

concentration; it represents instances where distillation is not feasible. Distillation to

such vapor-liquid mix would need an endlessly tall distillation tower if the equilibrium

curve passes the 45°line. In addition, if the equilibrium curve crosses the 45° line, the

combination has generated an azeotrope. Simple rectification would not be able to distill

past that stage, based on this.

Figure 1. 4: McCabe Thiele Illustration

 CHAPTER 2

2.0 CHEMICALS AND APPARATUS

 Ethyl Alcohol

 Water

 Computer Control Distillation Unit with SCADA and PID control (UDCC)

 Test tubes

 Beaker

 Volumetric flask

 Alcohol meter

 Measuring cylinder

 Funnel

 Stop watch
2.1 PROCEDURE
The alcohol meter's calibration curve was created by measuring the percent V of water,

pure ethanol, and a few combinations of water and ethanol whose compositions were

known.

The percent volume was then shown as a function of the mole fraction of ethanol (x).

To make the operation easier, the test solution was poured into the boiler through the

proper intake using a funnel. The refrigeration system was turned on. The SCADA

program's data file was stored.

The heating mantle was turned on, and the set-point was set to a temperature that was

greater than the boiling temperature of the most volatile component and lower than the

boiling temperature of the least volatile component.The reflux valve was turned to the

100% reflux setting.

The distillate flow was stabilized, the solenoid valve AVS-1 was close, volume of

distillate was measured. The distillate tank (using V-2 &3 valve) was drained, at the

same time a sample in the boiler was taken into another beaker (using V-1 valve).

The time that indicates the table of values from the SCADA program was written down,

to be able to find the temperature (and pressure) when the sample was taken. The

sample was allowed to cool down quickly and the vessel that contain them was kept

closed. Every 10 minutes, steps 7 and 8 were repeated, and the time provided by the

software was typed down once again. The samples were labeled, and the time and

location of their collection were specified. The alcohol meter was used to evaluate the

samples. Using tables, the relevant values of the mole fraction of each ingredient in the

mixture were calculated using percent volume and the density value. The mole fractions

of the distillate and residue were determined by these studies.

 CHAPTER 3

3.0 RESULT AND DISCUSSION

3.1 RESULTS OF EXPERIMENT
Table 3. 1: Data for Calibration curve

XA VA VB Brix (%)

0.0 0.00 10.00 0.3

0.2 4.38 5.62 14.3

0.4 6.75 3.25 18.2

0.6 8.24 1.76 19.3

0.8 9.26 0.74 19.3

1.0 10.00 0.00 18.6

A and B represent Ethanol and Water respectively. Also, V A and VB represent the

volume of ethanol and water as well. XA represent the mole fraction of ethanol.

Table 3. 2: Result of distillation

Sample Time, Boiler % Brix of Distillate % Brix of

min sample, ml reboiler Sample, ml Distillate sample

sample

1 5 16 15.5 92 19.1

2 10 7.3 15.1 48 19.2

3 15 12.2 13.9 38 19.2

4 20 11.8 13.0 40 18.7

5 25 16.8 12.8 6.1 19.4

Table 3. 3: Equilibrium data for water-ethanol system

X Y

0.0190 0.1700

0.0721 0.3891

0.0966 0.4375

0.1238 0.4704

0.1661 0.5089

0.2337 0.5445

0.2608 0.5580

0.3273 0.5826

0.3965 0.6122

0.5079 0.6564

0.5198 0.6599

0.5732 0.6841

0.6763 0.7385

0.7472 0.7815

0.8943 0.8943
 CALIBRATION CURVE
25

20

15
Brix(%)

10

0
0 0.2 0.4 0.6 0.8 1 1.2

Mole Fraction of Alcohol, Xa

Figure 3. 1: Calibration curve

EQUILIBRIUM CURVE
1
0.9
0.8
Vapour Mole Fraction, Y

0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Liquid Mole Fraction, X

Figure 3. 2: Equilibrium curve

 Table 3. 4: Boiler and Distillate mole Fraction

Reboiler % brix xB Distillate % xD

brix

15.5 0.270 19.1 0.850

15.1 0.242 19.2 0.830

13.9 0.197 19.2 0.830

13.0 0.184 18.7 0.900

12.8 0.182 19.4 0.725

3.2 CALCULATION OF XB-VALUES BY INTERPOLATION

1. (0.2,14.3); (x,15.6); (0.4,18.2)

18.2−14.3 18.2−15.6
= x = 0.270
0.4−0.2 0.4−x

2. (0.2, 14.3); (x, 12.8); (0.09, 5)

14.3−12.8 0.2−x
=
14.3−5 0.2−0.09

x=0.182

3. (0.6, 19.3); (x, 18.7); (0.4, 18.2)

19.3−18.7 0.6−x
=
19.3−18.2 0.6−0.4

x=0.491

The results for the interpolation are shown in table 4.

The operating line of rectification is given by the equation below:

R 1
y= x+ x ………………………….. (1)
R+1 R+1 D

At the y-intercept of a line, x=0. Hence, equation (1) can be written as:

R 1
y= (0)+ x
R+1 R+ 1 D

1
y= x ……………………………........... (2)
R+1 D

1
y∗¿ x …………………………….... (3)
Rmin +1 D

Minimum reflux ratio can be found by making Rmin the subject of equation (3).

Assumptions: Feed condition is saturated liquid feed, R=1.5 R min, Let composition of

ethanol in feed be E f =0.5

E f =0.5 , x B =0.262, x D =0.850

EQUILIBRIUM CURVE
1

0.9
Vapour mole fraction, y

0.8

0.7

0.6

0.5

0.4

0.3

0.2

0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Liquid mole fraction, x

Figure 3. 3: Determination of vapour mole fraction at minimum reflux ration

From the graph, at the minimum reflux ratio, y∗¿ 0.35
1
y∗¿ xD
Rmin +1

1
0.35= 0.85
R min +1

Rmin =1.4286

R=1.5 R min=1.5 ( 1.4286 )=2.1429

Now the actual operating line of rectification can be found by using the equation below.

R 1
y= x+ x
R+1 R+1 D

At the y intercept, x=0. The above equation is further reduced to the equation below.

1
y= x
R+1 D

1
y= 0.85=0.2545
2.1429+1
Figure 3. 4: Determining the number of stages using Maccabee and Thiele Method

3.3 DISCUSSION
Distillation preferentially separates a more volatile component from a less volatile one

in a feed solution by partial vaporization of the feed followed by condensation. The

vapour produced is richer in the more volatile component. In order to have a larger

degree of separation, multistage contact between the vapour and the liquid phases is

arranged in the distillation column. Some part of the condensate is withdrawn as the top

product and the rest is fed back into the column as reflux which flows down the trays.

The more the number of trays and higher reflux ratio, the better the degree of

separation.

Observations from the calibration curve, shows the mole fraction of ethanol increased

with increasing %Brix to a peak value of 19.3. Ethanol is known to evaporate first from

the mixture and condenses as distillate because of its lower boiling point. As a result,

the mole fraction and volumes of ethanol in the reboiler and distillate showed that

ethanol is highly concentrated in the distillate compared to the reboiler.

The minimum reflux ratio corresponds to the minimum vapour flow in the tower and

hence the minimum reboiler and condenser sizes. From the results obtained, the

minimum reflux ratios decreased substantially as the mole fraction of ethanol in the

distillate (XD) decreased.

From the McCabe and Thiele graphical method, 15 number of stages were obtained. A

high number of stages signifies that there is a higher degree of separation of ethanol

from the mixture. Therefore, the degree of separation of ethanol from the mixture was

same in all the stages.

 CHAPTER 4

4.0 CONCLUSION
The graph of T as a function of vapour and liquid composition shows that water-ethanol

mixture is not an ideal binary mixture and therefore does not obey Raoult’s law; it

exhibits an azeotropic behavior. The number of trays in a distillation column affects the

quality of products at the top and bottoms product of the distillation column and

likewise the number of stages which stands at 15.

4.1 SAFETY AND PRECAUTIONS

 In order to avoid contamination, the measuring cylinders and the distillation

flask were rinsed well with the appropriate reagent before use.

 Careful transfer of test solution into the boiler to prevent spillage and damage to

distillation unit.

 Pre-rinsing of alcohol meter with sample solution before actual measurements to

help accuracy.

Vigorous swirling of test solution to ensure homogeneity.

 Bottom liquids were allowed to cool before the percentage volumes were

measured.

 Accurate time keeping to provide true reflection on molar flow rate.

4.2 SOURCES OF ERROR
 Loss of volatile component (ethanol) during the process.

 Over-heating of solenoid valve disrupted smooth flow of experiment.

 Properties of distilled water were assumed for tap water.

 The ebullition points of Ethanol and distilled water may vary from the standard

ranges in literature, as they may contain impurities

 CHAPTER 5

5.0 POST LAB QUESTIONS

1. CONTINOUS VERSUS BATCH DISTILLATION

In continuous distillation, the mixture is fed continuously into the column and separated

fractions are removed continuously as an output stream. In Continuous Distillation,

gravity acts on the liquid to run down the column whilst the vapour runs up the column.

The operation consists of a column containing the equivalent of N theoretical stages

arranged in a two-section cascade; a total condenser in which the overhead vapour

leaving the top stage is totally condensed to give a liquid distillate product and liquid

reflux that is returned to the top stage; a partial reboiler in which liquid from the bottom

stage is partially vaporized to give a liquid bottoms product and vapour boil-up that is

returned to the bottom stage; and an intermediate feed stage.

The feed, which contains a more volatile component-the light key, LK and a less

volatile component-the heavy key, HK-enters the column at a feed stage, f. At the feed-

stage pressure, the feed may be liquid, vapour, or a mixture of liquid and vapour, with

its overall mole fraction composition with respect to the light component. Vapour rising

in the section above the feed (called the enriching or rectifying section) is washed with

liquid to remove or absorb the heavy key. In the section below the feed (stripping or

exhausting section), the liquid is stripped of the light key by the rising vapour. Inside

the tower, the liquids and vapours are always at their bubble points and dew points,

respectively, so that the highest temperatures are at the bottom, the lowest at the top.
In Batch Distillation, the mixture is added to the distillation unit at the start of the

process and distillates are taken sequentially in time during the process and the bottoms

fraction is removed at the end. A bottom receiver Reboiler which is charged with the

feed to be processed and which provides the heat transfer surface. A rectifying column

(either a tray or packed column) superimposed on the reboiler, coupled with either a

total condenser or a partial condenser system. A series of product accumulator tanks

connected to the product streams to collect the main and or the intermediate distillate

fractions. Operation of such a column involves carrying out the fractionation until a

desired amount has been distilled off. The overhead composition varies during the

operation and usually a number of cuts are made. Some of the cuts are desired products

(main-cuts) while others are intermediate fractions (off-cuts) that can be recycled to

subsequent batches to obtain further separation. A residual bottom fraction may or may

not be recovered as product

Table 3. 5: Differences between Continuous distillation and Batch distillation

Continuous Distillation Batch Distillation

Each of the fraction streams is taken Only one exit point for distillate is

simultaneously throughout operation and needed and for different chemicals, the

hence needs separate exit for each distillate can be just switched to a

fraction which are located at different different fraction collecting container

heights

Optimal reflux ratio is easily obtained by Difficult to establish optimal reflux ratio

continuous distillation of a particular since pot composition continuously

mixture change

Can only process one mixture at a time. Gives production flexibility where

different chemicals can be processed in

the same equipment.

Process parameters are kept constant Making significant changes in process

throughout the process hence little parameters causes operating instabilities

instabilities in operating conditions are

experienced

Separated fractions are removed Some of the cuts are desired products

continuously as an output stream and no (main-cuts) while others are intermediate

cuts are required fractions (off-cuts) making it difficult to

establish when to switch from one switch

to the other.
Schematic Diagram for Batch Rectifier

Figure 3. 5: Schematic diagram of a batch reactor

5.2 REFERENCES
1. Treybal, R. E. (1980). Mass transfer operations. New York, 466.
2. Taylor, R., & Krishna, R. (1993). Multicomponent mass transfer (Vol. 2). John
Wiley & Sons.
3. J.M Coulson and J.F Richardson, 1992, Chemical Engineering Series volume 2,
McGraw-Hill Book Company, Inc. pages 498-504.
4. Davis, J. T., “Chemical Engineering: How Did It Begin and Develop?” in W. F

Furter (Ed), History of Chemical Engineering, Washington, D.C., American

Chemical Society, Adv. Chem Ser, 190, 15-43(1980)

5. Edibon. (2014). Computer Controlled Biogas Process Unit , with SCADA and PID

Control (Vol. EDO1).

6. Katzen, R., Madson, P. W., & Moon, G. D. (1999). Ethanol distillation : the

fundamentals. In The Alcohol Textbook: A reference for the beverage, fuel and

industrial alcohol industries (1st ed., pp. 269–288). Ohio: KATZEN International Inc.

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