Heriot-Watt University

Stage 3
Chemical Engineering

Laboratory Report 1
Name Aytaj Abdin
Group Number CE-14.1
Experiment Title Continuous Rectification CE600
Date of Experiment 09.02.2018
Date of Submission 26.02.2018
Demonstrator Asrar Ahmad Sheikh
Table of Contents
1. Synopsis: ......................................................................................................................... 2
2. Introduction: .................................................................................................................... 2
3. Theory: ............................................................................................................................. 3
3.1. Continuous multi-stage distillation:.............................................................................. 3
3.2. Batch distillation: ........................................................................................................ 5
4. Experimental details: ....................................................................................................... 6
4.1. Equipment functions and components:......................................................................... 6
4.2. Procedure: .................................................................................................................. 7
4.2.1. Batch distillation: ................................................................................................ 7
4.2.2. Continuous distillation. ....................................................................................... 8
5. Results: ............................................................................................................................ 8
5.1. Run A: Batch distillation at 35% Reflux. ....................................................................... 8
5.2. Run C: Batch distillation at 65% Reflux. ..................................................................... 13
5.3. Run D: Continuous distillation at 35% Reflux. ............................................................ 19
6. Discussion: .................................................................................................................... 21
7. Conclusion: .................................................................................................................... 23
8. Appendix: ....................................................................................................................... 23
9. References:..................................................................................................................... 24

1
1. Synopsis:
The report will analyse the distillation column under the different operating conditions. The main
objectives of the experiment are to study the basic characteristics of column, to carry out the experiment
with batch and continuous distillation modes, to determine how the composition of MVC in distillate
changes with time and to define the number of equilibrium plates.
The experiment is carried out for ethanol/water mixture depending on the operating conditions. In the
report T-x-y and y-x diagrams are plotted to define the number of equilibrium stages and to analyse
different distillation modes. The operating line equations are found using the McCabe-Thiele Method on
the x-y equilibrium curve diagram. For continuous distillation with reflux 35% the operating line and q-
line equations are found as: The top operating line:𝑦 = 0.35𝑥 + 0.37; bottom operating line:𝑦 = 2.998 −
0.14; q-line: 𝑦 = 8.925𝑥 − 1.28, which is illustrated in Table 5.3.5 and Graph 5.3.2. Finally, the number
of theoretical plates is determined for all operations to be 6 for Run A, 4 for Run C and 3 (2 plates +
reboiler) for Run D. Moreover, it is also determined from the experiment that the composition of MVC
(ethanol) in liquid remaining in still 𝑥𝑠2 is 0.116 for Run A and 0.110 for Run C.

2. Introduction:
Distillation is the most common procedure for chemical separation that depends on differences in
volatility or boiling temperatures of components. The greater difference in volatility means that it will be
easy to separate the mixture. When feed material enters the column, the components are distributed in
different proportions between liquid and vapor. Then, liquid flows down the column and vapor moves up
the column counter-currently, contacting liquid at each plate. When a liquid phase and vapor phase are
brought into contact on theoretical plates in the distillation column, the less volatile component (LVC)
will consist of the liquid phase, while the more volatile component (MVC) is evaporated by latent heat of
LVC. Liquid reaching the stripping section of column is vaporized in a reboiler and sent back to the
column in order to supply the vapor flow, while the remainder of liquid is taken as a bottom product
(residue). At the top of column, the vapor is condensed into liquid phase in a condenser; some of liquid
enters back to the column as reflux and the other part is removed as overhead product (distillate).
Distillation is widely used operation for separation in many industries such as petroleum refining,
petrochemicals, natural gas processing, the production of alcoholic beverages and food processing.
There are several types of distillation depending on the procedure: [1]
In the simple distillation, liquids are separated by evaporating in a distillation flask: Vapors formed rise
through the tube and are collected at different points and then immediately directed into a condenser.
As liquid is heated, vapor formed will be richer in more volatile component which boils at lower
temperature. The simple distillation is used for liquid mixture with the boiling temperature which differs
by 70℃. In this process the material is separated from non-volatile components or solid contaminants
(less than 10% contamination).
[1]
Azeotropic distillation is used for constant boiling point mixture if the bubble point of a mixture is either
greater or smaller than the bubble points of individual components. There are there methods to
accomplish the separation: 1) adding another compound to change the activity coefficients (for example:
addition of benzene to the mixture of ethanol and water); 2) altering the pressure between two columns;
3) combining different separation principles such as adsorption (distillation and molecular sieves) and
pervaporation (distillation and membranes), which is called hybrid processes.
[1]
Vacuum distillation is a special technique used to separate compounds at a pressure below the vapor
pressure. The separation of temperature sensitive materials is conducted under the vacuum in order to
2
prevent the product from the damaging. Under the operating conditions, the boiling points of compounds
are decreased and the amount of heat required to boil the mixture is also reduced. Vacuum distillation
is applied in a refining process to separate heavier oils left from the atmospheric distillation column
without cracking or degrading.
The distillation process can be carried out in continuous and batch modes. A batch distillation consists
of a still (reboiler), a condenser, a rectifying column and one or more product tanks. The still is initially
charged with the feed mixture, which evaporates and vapor produced in the reboiler, which is richer in
MVC, is condensed at the top. Part of the liquid is returned to column as reflux, while the other is
collected in receiving tanks. The MVC concentration in the liquid remaining in the still decreases as the
distillate is removed. However, in the continuous distillation column operation, the feed is supplied to
the column at any in-between stage and the top and bottom products are produced under a steady-state
operation. The upper section of the feed point is called the rectifying section, as the MVC is enriched,
while the lower part is referred to as the stripping section, as the down-flowing liquid is stripped of a low-
boiling-temperature component by the rising vapor. [[2], 3]
The main advantages of batch distillation process are related to lower capital cost and its flexibility,
which allows to separate different mixtures with different compositions and specifications in one column
by switching the operating conditions. Moreover, the batch distillation is suitable for small production
rates and for reactions which have superior sensitivity such as in polymerization process. The
continuous distillation columns are designed to operate for longer hours and to produce a large amount
of products. [2]

3. Theory:
3.1. Continuous multi-stage distillation:
Material and heat balance equations are given for stage 𝑛 in distillation column as: [4]
𝑉𝑛−1 + 𝐿𝑛+1 = 𝑉𝑛 + 𝐿𝑛 (3.1)
𝑉 𝐿
𝑉𝑛−1 × 𝐻𝑛−1 + 𝐿𝑛+1 × 𝐻𝑛+1 = 𝑉𝑛 × 𝐻𝑛𝑉 + 𝐿𝑛 × 𝐻𝑛𝐿 + ℎ𝑒𝑎𝑡 𝑙𝑜𝑠𝑠𝑒𝑠 + ℎ𝑒𝑎𝑡 𝑜𝑓 𝑚𝑖𝑥𝑖𝑛𝑔 (3.2)
𝑉 𝐿
Where: 𝑉𝑛 and 𝐿𝑛 are molar vapor and liquid flows (𝑘𝑚𝑜𝑙/𝑠) across stage 𝑛; 𝐻 and 𝐻 are the specific
enthalpies of vapor and liquid phases (𝑘𝐽⁄𝑘𝑚𝑜𝑙 ), respectively.
3
Assuming that mixture components have equal molar latent heat of vaporization so that the energy
provided from the condensation of a kmol of vapor on a stage is sufficient to evaporate a kmol of liquid.
It is also assumed that heat of mixing or sensible heat effects and heat losses are negligible as the
column is well insulated. This condition is called constant molar overflow or equimolar overflow: The
molar flow rates of liquid and vapor do not change and remain constant in column. These assumptions
are substantially true in practice for near-ideal liquid mixtures: [4]
𝑉𝑛−1 = 𝑉𝑛 = 𝑉𝑛+1 𝑎𝑛𝑑 𝐿𝑛+1 = 𝐿𝑛 = 𝐿𝑛−1 (3.3)
Considering the top section of the column which includes stages 𝑛 and 𝑛 + 1, a condenser in Figure 3.1
gives the following equations: [4]
𝑉𝑛 = 𝐿𝑛+1 + 𝐷 (3.4)
For MVC: [4]
𝑉𝑛 × 𝑦𝑛 = 𝐿𝑛+1 × 𝑥𝑛+1 + 𝐷 × 𝑥𝑑 (3.5)
Where: 𝐷–distillate flow rate (𝑘𝑚𝑜𝑙/𝑠); 𝑦𝑛 –mole fraction of MVC in the vapor stream from stage 𝑛; 𝑥𝑛+1-
mole fraction of MVC in the liquid stream from stage 𝑛 + 1; 𝑥𝑑 –mole fraction of MVC in distillate. It is
assumed that 𝐿𝑛+1 is identical to 𝐿𝑛 in rate due to the constant molar overflow, therefore, equation (3.5)
can be expressed in an alternative form: [4]
𝐿𝑛 𝐷
𝑦𝑛 = × 𝑥𝑛+1 + × 𝑥𝑑 (3.6)
𝑉𝑛 𝑉𝑛
It is the top operating line equation for continuous multi-stage distillation which relates liquid and vapor
compositions between stages.

Material balance equations for the bottom of the column in Figure 3.2 can be written as: [4]
𝐿𝑚+1 = 𝑉𝑚 + 𝑊 (3.7)
For MVC: 𝐿𝑚+1 × 𝑥𝑚+1 = 𝑉𝑚 × 𝑦𝑚 + 𝑊 × 𝑥𝑤 (3.8)
Where: 𝑊-flow rate of bottom product (𝑘𝑚𝑜𝑙/𝑠); 𝑥𝑚+1 - mole fraction of MVC in liquid from stage 𝑚 + 1;
𝑦𝑚 -mole fraction of MVC in vapor from stage 𝑚; 𝑥𝑤 -mole fraction of MVC in bottom product.
As 𝐿𝑚+1 = 𝐿𝑚 , the rearrangement gives: [4]
𝐿𝑚 𝑊
𝑦𝑚 = × 𝑥𝑚+1 − × 𝑥𝑤 (3.9)
𝑉𝑚 𝑉𝑚
It is the bottom operating line equation. The reflux ratio is the amount of liquid (kmol) sent back to column
as reflux per kmol top product taken off: 𝑅 = 𝐿𝑛 ⁄𝐷

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The number of theoretical plates to achieve separation depends on reflux ratio, hence, the top operating
line equation can be expressed by reflux ratio. Substituting equation (3.4) into (3.6) gives: [4]
𝐿𝑛 𝐷
𝑦𝑛 = × 𝑥𝑛+1 + × 𝑥𝑑
𝐿𝑛 + 𝐷 𝐿𝑛 + 𝐷
𝐿 𝑛 ⁄𝐷 𝐷 ⁄𝐷
𝑦𝑛 = × 𝑥𝑛+1 + × 𝑥𝑑
𝐿𝑛 𝐷 𝐿𝑛 𝐷
+ +
𝐷 𝐷 𝐷 𝐷
𝑅 𝑥𝑑
𝑦𝑛 = × 𝑥𝑛+1 + (3.10)
𝑅+1 𝑅+1
McCabe-Thiele method provides a graphical technique to find the number of equilibrium stages for
analysis of separation systems and uses x-y diagram with operating lines. The procedure for the
construction of the diagram is as follows: [4], [5]
1. Vapor-liquid equilibrium curve is plotted by using the data available at column operating conditions.
2. The compositions of feed, top and bottom products (𝑥𝑓 , 𝑥𝑑 and 𝑥𝑤 , respectively) are marked on the
𝑥 = 𝑦 line by plotting vertical lines from each of these points.
3. The intersection point of two operating lines depends on condition of feed. The line which passes
through the intersection point is called q-line. The equation of the q-line is given as:
𝑞 𝑥𝑓
𝑦𝑞 = × 𝑥𝑞 − (3.11)
𝑞−1 𝑞−1
(𝑇7 − 𝑇1 ) 𝑐𝑝 + 𝜆
𝑞 =
𝜆
Where: 𝑥𝑞 𝑎𝑛𝑑 𝑦𝑞 -the co-ordinates of intersection point; q-heat required to vaporize 1 𝑘𝑚𝑜𝑙 feed to
saturated vapor divided by the molar latent heat of feed; 𝑇7 - temperature in the stripping section of
column (𝐾); 𝑇1 -temperature of feed (𝐾); 𝐶𝑝 -specific heat capacity of mixture (𝑘𝐽/𝑘𝑔 𝐾); 𝜆-latent heat
of mixture (𝑘𝐽/𝑘𝑔).
Slope of the q-line intersects the 𝑥 = 𝑦 line at feed composition 𝑥𝑓 .
4. The operating line for rectifying section is plotted from the point of 𝑥𝑑 on 𝑥 = 𝑦 line to y-intercept
𝑥𝑑
( ) where TOL cuts y-axis.
𝑅+1
5. The operating line for stripping section is plotted from 𝑥𝑤 on 𝑥 = 𝑦 line to the intersection point of
the top operating line and q-line.
6. Starting from 𝑥𝑑 on 𝑥 = 𝑦 line, a horizontal line is sketched to the equilibrium curve. Then, a vertical
line is drawn down from the point on the equilibrium line to one of operating lines. The process is
repeated until the required the composition of MVC in bottom product is reached.
7. The number of steps on the diagram is the number of theoretical plates.

3.2. Batch distillation:

The batch distillation column can be operating under different conditions: constant product composition
by varying reflux ratio or constant reflux by varying the product composition. Distillate composition is
kept constant at the variable reflux mode of operation and the amount of reflux sent back to the column
is increased. The concentration of light component in the still is gradually depleted with time and finally,
the reflux ratio reaches very high value. The material balance at constant product composition is given
as: [4]
𝑆1 = 𝑆2 + 𝐷 (3.12)
𝑆1 × 𝑥𝑠1 = 𝑆2 × 𝑥𝑠2 + 𝐷 × 𝑥𝑑 (3.13)

5
Where: 𝑆1 -total amount of liquid initially fed to still (𝑘𝑚𝑜𝑙); 𝑆2 -quantity of liquid remaining in still (𝑘𝑚𝑜𝑙);
𝐷-quantity of distillate (𝑘𝑚𝑜𝑙); 𝑥𝑠1 -mole fraction of MVC in liquid initially charged to still; 𝑥𝑠2 -mole fraction
of MVC in liquid remaining in still; 𝑥𝑑 -mole fraction of MVC in distillate.
After rearranging and substituting, the amount of distillate can be calculated: [4]
𝑆1 × 𝑥𝑠1 = (𝑆1 − 𝐷) × 𝑥𝑠2 + 𝐷 × 𝑥𝑑
𝑆1 × 𝑥𝑠1 = 𝑆1 × 𝑥𝑠2 − 𝐷 × 𝑥𝑠2 + 𝐷 × 𝑥𝑑 = 𝑆1 × 𝑥𝑠2 + 𝐷 × (𝑥𝑑 − 𝑥𝑠2 )
𝑥𝑠1 − 𝑥𝑠2
𝐷 = 𝑆1 × ( ) (3.14)
𝑥𝑑 − 𝑥𝑠2
For constant reflux mode of operation, the concentration of MVC in still falls with time as distillate
composition changes. Distillation process is continued until the desired value of average composition in
distillate is reached. The differential material balance can be written as: [4]
𝑥𝑑 𝜕𝐷 = −𝜕(𝑆𝑥𝑠 ) (3.15)
𝜕𝐷 = −𝜕𝑆 (3.16)
Where: 𝑆-amount of liquid remaining in still (𝑘𝑚𝑜𝑙); 𝐷-quantity of distillate (𝑘𝑚𝑜𝑙); 𝑥𝑠 -mole fraction of
MVC in liquid remaining in still; 𝑥𝑑 -mole fraction of MVC in distillate.
Substituting gives: [4]
−𝑥𝑑 𝜕𝑆 = −𝑆𝜕𝑥𝑠 − 𝑥𝑠 𝜕𝑆
𝑆𝜕𝑥𝑠 = 𝜕𝑆(𝑥𝑑 − 𝑥𝑠 )
𝑆2 𝑥𝑠2
1 1
∫ 𝜕𝑆 = ∫ 𝜕𝑥
𝑆 (𝑥𝑑 − 𝑥𝑠 ) 𝑠
𝑆1 𝑥𝑠1
𝑥𝑠1
𝑆1 1
ln ( ) = ∫ 𝜕𝑥 (3.17)
𝑆2 (𝑥𝑑 − 𝑥𝑠 ) 𝑠
𝑥𝑠2
The right-hand side of equation (3.17) can be calculated by plotting 1⁄(𝑥𝑑 − 𝑥𝑠 ) against 𝑥𝑠 as the area
under the curve gives the value of integral.

4. Experimental details:
4.1. Equipment functions and components:
The Continuous rectification CE 600 unit is designed to separate liquid mixtures (ethanol/water) by
means of rectification. Rectification is a multi-stage distillation where the rising vapor mixture and
returning condensate flow counter to one another. The main part of system consists of electric heater,
feed tanks, phase separation tank, condenser and product tanks. The heater is operated as an
evaporator and used to heat the liquid mixture, which is delivered by the feed pump. The vapor produced
is richer in the component with the lower boiling temperature (ethanol) and moves up along the column.
The vapor at the top is condensed using the water-cooled condenser and phase separation tank. Then,
distillate is discharged to the top product tank by a tap. Part of the condensate from the downstream of
phase separation tank is fed to the column as a reflux by using the switching valves. The cooling water
for the condenser should be provided from an external source. The flow of cooling water is measured
from the flowmeter and adjusted using the hand valve. For the experiment a packed column and a sieve
tray column with eight plates are available. A heat exchanger is used to preheat the feed by the draining
bottom product for the continuous mode operation. A glass filter pump can be used to produce a vacuum
for vacuum rectification. The data is taken by sensors and all control functions can be processed on a
PC.

6
Figure 4.1.1: The unit components: 1-Feed pump; 2-Feed tank; 3-Control cabinet; 4-Top product tank; 5-Glass
filter pump; 6-Pressure gauge; 7-Switching valve; 8-Phase separation tank; 9-Product condenser; 10-Switching
valve; 11-Differential pressure sensor; 12-Solvent tank; 13-Column; 14-Flowmeter for cooling water; 15-
Evaporator; 16-Bottom heat exchanger; 17-Bottom product tank.

4.2. Procedure:
4.2.1. Batch distillation:
In order to conduct the batch distillation, the following steps should be done:
1. 7 L of liquid mixture in two feed tanks is carried using the pump and opening valves V1 and V2 at
the bottom of the tank;
2. Samples are taken from tanks via a pipette into a 50 mL density bottle;
3. The pump is turned off and valves (V1 and V2) are closed when the level in the reboiler is 7L;
4. The reflux and heater power are set to 100%;
5. Wait until the column begins to heat and the liquid mixture reaches to boiling point;
6. It should be considered that higher temperature can cause a decrease in the product purity and
uncontrollable operation, therefore, the temperature of the top stage should not be more than 82°C
and the differences between the temperatures of stages should be little like 1-2°C;

7
7. The heater power is lowered to required value (45%);
8. It must be ensured that volumetric flow rate of cooling is at approximately 150 to 180LPM;
9. After reaching steady state condition in the column, the reflux is turned into the needed value and
samples are obtained from the condenser;
10. The reflux inlet to the column should be 22-25°C. When the temperature in reflux increases higher
than 35°C, the reflux, cooling water flow rate, feed pump power and reboiler power are set to 100%,
200LPM, 90% and 10%, respectively. Pressure gauge should show 1 atm. The emergency
shutdown button is used in the case of overpressure;
11. The weights of samples, the temperatures and volume of condensate in the product tank are
recorded;
12. When the temperature in the condenser is close to 100°C, the experiment is stopped by setting the
power 0% and reflux to 100%.

4.2.2. Continuous distillation.

The experiment is performed as:
1. Steps from 1 to 7 in batch distillation operation are repeated;
2. It is ensured that valve V9 is close, then valve V8 on the reboiler is opened.
3. After reaching 5L in the reboiler, the reflux and pump speed are set to the needed values;
4. Valve V9 is gradually opened to withdraw the product from reboiler as the level in the reboiler
increases;
5. The samples are taken from the condenser and feedline of bottom product tank. The temperatures
and liquid level in all tanks are also recorded;
6. When low level alarm turn off the heater, valve V9 should be closed in order to increase the level in
the reboiler. The heater should be shut on after the level reaches the desired value.

5. Results:
5.1. Run A: Batch distillation at 35% Reflux.
Table 5.1.1: Experimental data of samples.
Time Sample number Empty (g) Full (g) 𝑻𝟏 (℃)
14:06 S1 34.33 81.84 20.00
14:21 S2 34.37 81.56 20.00
14:22 S3 34.33 81.86 20.00
Time Sample number Empty (g) Full (g) 𝑻𝟏𝟑 (℃)
16:05 S4 34.33 76.35 21.10
16:15 S5 34.33 75.83 21.80
16:20 S6 34.36 75.48 22.30
16:25 S7 34.34 75.17 22.40
16:30 S8 34.33 74.98 22.30
16:40 S9 34.28 75.07 22.60
16:45 S10 34.36 75.28 22.40
16:50 S11 34.33 75.33 22.30
16:55 S12 34.30 75.39 22.20
17:00 S13 34.31 75.45 22.20
17:05 S14 34.28 75.47 22.00
8
 17:17 S15 34.37 75.52 21.80
17:43 S17 34.27 75.52 21.30
17:57 S18 34.34 75.52 21.10

Table 5.1.2: The density, mass and mole fractions of MVC.

Table 5.1.3: Experimental data for the temperatures at given time.

T1 T2 T3 T4 T5 T6 T7 T8 T9 T10 T11 T12 T13
Time
(℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃)
16:05 16.1 13.8 87.6 80.1 79.1 79 79 78.8 78.6 78.3 78.1 78 21.1
16:15 16.2 13.7 86.9 80.2 79 78.8 78.8 78.6 78.7 78.2 78.1 78 21.8
16:20 16.1 13.7 86.8 82.2 80.3 79.7 79.2 78.9 78.7 78.4 78.3 78.2 22.3
16:25 16.1 13.6 86.9 83.9 82 80.6 79.8 79.2 79.3 78.7 78.4 78.4 22.4
16:30 16.3 13.7 87.6 85.3 83.8 82 80.2 79.8 79.7 79.1 78.5 78.4 22.3
16:40 16.3 13.8 88.2 85.8 84.4 82.5 80.6 80.1 79.9 79.6 79.4 79.4 22.6
16:45 16.1 13.8 88.2 86.1 84.4 82.5 80.8 80.1 80.1 79.7 79.5 79.4 22.4
16:50 16.2 13.8 88.6 86.4 84.6 82.5 80.9 80.1 80.1 79.8 79.5 79.5 22.3
16:55 16.2 14.1 88.9 86.9 84.9 82.8 80.7 80.2 80.1 79.8 79.6 79.5 22.2
17:00 16.4 14.3 89.4 87.2 85 82.8 80.6 80.3 80.1 79.8 79.5 79.6 22.2
17:05 16.5 14.4 89.3 87.2 84.9 82.6 80.6 80.3 80.1 79.8 79.7 79.6 22
17:17 16.6 14.7 90.5 88.4 85.6 82.5 80.4 80.2 80.1 79.9 79.7 79.6 21.8
17:25 16.6 14.2 91.1 89.1 86.1 82.7 80.5 80.2 80.1 79.8 79.6 79.6 21.9
17:43 16.5 13.9 92.5 89.9 84.6 82.3 80.2 80 80 79.7 79.5 79.4 21.3
17:57 16.3 13.8 93.5 91.5 85.8 82.6 80.3 80.1 80 79.5 79.1 79 21.1

9
Table 5.1.4: The data for Sample numbers 13 and 14 for T-x-y diagram.
S13 S14
T (℃) x y T (°C) x y
89.40 0.068 0.375 89.30 0.070 0.380
87.20 0.091 0.428 87.20 0.091 0.428
85.00 0.132 0.480 84.90 0.138 0.483
82.80 0.233 0.542 82.60 0.243 0.548
80.60 0.406 0.617 80.60 0.405 0.615
80.30 0.442 0.630 80.30 0.442 0.630
80.10 0.470 0.640 80.10 0.470 0.640
79.80 0.510 0.660 79.80 0.510 0.660
79.50 0.547 0.672 79.70 0.520 0.660

100
T x y Diagram for Ethanol-Water
99
98 Dew Point Line
97
96 Bubble Point Line
95
94 S13
93
92 S13
91
90 S14
T (°C)

89
88 S14
87
86
85
84
83
82
81
80
79
78
77
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Mole fraction of Ethanol (x or y)
Graph 5.1.1: T-x-y diagram for Ethanol-Water.

Table 5.1.5: The top operating line equations for Sample numbers 13 and 14.
S13 S14
𝑦 = 0.35𝑥 + 0.4368 𝑦 = 0.35𝑥 + 0.429
x y x y
0.000 0.437 0.000 0.429
0.100 0.472 0.100 0.464
0.200 0.507 0.200 0.499
0.300 0.542 0.300 0.534
0.400 0.577 0.400 0.569

10
 0.500 0.612 0.500 0.604
0.600 0.647 0.600 0.639
0.650 0.664 0.650 0.657
0.672 0.672 0.660 0.660

y-x Diagram for Ethanol-Water

1
Mole Fraction of Ethanol in Vapor Phase y

0.9

0.8

0.7

0.6

0.5
Equilibrium line
0.4
x=y line
0.3 S13
TOL (S13)
0.2
S14
0.1 TOL (S14)

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Mole Fraction of Ethanol in Liquid Phase x
Graph 5.1.2: y-x diagram with operating lines for Sample numbers 13 and 14.

11
Graph 5.1.3: y-x diagram showing the number of stages for Sample number 13 (S13).

Graph 5.1.4: y-x diagram showing the number of stages for Sample number 14 (S14).

12
 Mole fraction of Ethanol in Distillate, xd
0.74
Dependence of xd on time

0.73

0.72

0.71

0.7
Theoretical
0.69
Experimantal
0.68

0.67

0.66

0.65
16:59 17:00 17:00 17:01 17:02 17:03 17:03 17:04 17:05
Time
Graph 5.1.5: Dependence of theoretical and experimental values of 𝑥𝑑 on time.

5.2. Run C: Batch distillation at 65% Reflux.

Table 5.2.1: Experimental data for samples.

Table 5.2.2: The density, mass and mole fractions of MVC.

13
Table 5.2.3: Experimental data for temperatures at given time.
𝑇1 𝑇2 𝑇3 𝑇4 𝑇5 𝑇6 𝑇7 𝑇8 𝑇9 𝑇10 𝑇11 𝑇12 𝑇13
Time
(℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃)
14:15 16.9 14.6 87.1 85.7 84.8 84.4 83.6 82.1 80.3 79.8 79.6 79.5 23.5
14:20 17.1 14.7 87.6 86.3 85.3 84.9 83.9 82.1 80.3 79.9 79.8 79.6 25.1
14:30 17.0 14.4 88.8 87.4 86.5 86.0 84.6 82.3 80.5 80.0 79.9 79.7 25.5
14:40 16.9 14.2 90.0 88.7 87.7 87.1 85.2 82.5 80.6 80.0 79.9 79.6 25.6
14:50 16.8 14.2 91.6 89.9 89.4 88.7 86.1 82.5 80.5 79.9 79.8 79.6 25.8
15:00 16.8 14.1 93.4 91.5 90.9 90.2 87.4 82.7 80.6 79.8 79.7 79.5 25.4
15:10 16.8 14.1 94.9 93.2 92.7 92.3 89.7 83.4 80.3 79.7 79.5 79.3 26.1
15:20 16.7 14.0 96.4 94.9 94.5 94.2 93.1 86.0 81.0 79.7 79.6 79.4 26.4
15:30 16.7 14.1 97.4 96.3 95.9 95.7 94.5 86.7 81.3 79.6 79.4 79.2 26.4
15:48 16.7 14.0 99.0 98.3 97.8 97.8 97.9 96.4 86.2 79.7 79.3 79.1 26.0
15:57 16.7 14.1 99.5 98.8 98.4 98.4 98.7 98.6 98.4 97.9 90.4 90.1 25.7
16:03 16.7 14.0 99.7 99.1 98.7 98.7 99.0 98.9 98.7 98.1 92.8 92.9 24.2
16:06 16.7 14.1 99.8 99.2 98.7 98.9 99.1 99.0 99.0 98.7 98.6 98.3 24.2
16:10 16.7 14.1 99.9 99.4 98.9 99.0 99.3 99.2 99.0 98.6 98.3 97.9 24.0
16:12 16.8 14.1 100.0 99.4 99.0 99.0 99.3 99.2 99.1 98.8 98.7 98.6 24.1

14
Table 5.2.4: The data of T-x-y diagram for Sample number 6, 8, 10 and 12 (S6, S8, S10 and S12).
S6 S8 S10 S12
T (°C) x y T (°C) x y T (°C) x y T (°C) x y
90.00 0.065 0.355 93.40 0.037 0.240 96.37 0.015 0.136 99.00 0.005 0.036
88.70 0.077 0.394 91.50 0.050 0.305 94.91 0.024 0.190 98.30 0.007 0.062
87.70 0.084 0.417 90.90 0.056 0.323 94.45 0.027 0.204 97.80 0.010 0.082
87.10 0.092 0.430 90.20 0.060 0.350 94.24 0.030 0.214 97.80 0.010 0.082
85.20 0.127 0.473 87.40 0.090 0.422 93.06 0.039 0.251 97.90 0.011 0.078
82.50 0.250 0.550 82.70 0.235 0.542 85.97 0.110 0.454 96.40 0.016 0.132
80.60 0.404 0.617 80.60 0.404 0.617 80.97 0.371 0.601 86.20 0.108 0.450
80.00 0.483 0.648 79.80 0.507 0.658 79.73 0.520 0.660 79.70 0.515 0.660
79.90 0.500 0.650 79.70 0.515 0.660 79.55 0.533 0.666 79.30 0.570 0.688

Table 5.2.5: The top operating line equations for Sample numbers 6, 8, 10 and 12 (S6, S8, S10 and S12).
S6 S8 S10 S12
𝒚 = 𝟎. 𝟔𝟓𝒙 + 𝟎. 𝟐𝟐𝟕𝟓 𝒚 = 𝟎. 𝟔𝟓𝒙 + 𝟎. 𝟐𝟑𝟏 𝒚 = 𝟎. 𝟔𝟓𝒙 + 𝟎. 𝟐𝟑𝟑𝟏 𝒚 = 𝟎. 𝟔𝟓𝒙 + 𝟎. 𝟐𝟒𝟎𝟖
y x y x y x y x
0.228 0.000 0.231 0.000 0.233 0.000 0.241 0.000
0.293 0.100 0.296 0.100 0.298 0.100 0.306 0.100
0.358 0.200 0.361 0.200 0.363 0.200 0.371 0.200
0.423 0.300 0.426 0.300 0.428 0.300 0.436 0.300
0.488 0.400 0.491 0.400 0.493 0.400 0.501 0.400
0.553 0.500 0.556 0.500 0.558 0.500 0.566 0.500
0.618 0.600 0.621 0.600 0.623 0.600 0.631 0.600
0.650 0.650 0.660 0.660 0.656 0.656 0.663 0.650

T x y Diagram for Ethanol-Water

100
99 Bubble Point Line
98 Dew Point Line
97 S6
96 S6
95 S8
94 S8
93 S12
92 S12
91 S10
90 S10
T (˚C)

89
88
87
86
85
84
83
82
81
80
79
78
77
0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0.4 0.45 0.5 0.55 0.6 0.65 0.7 0.75 0.8 0.85 0.9 0.95 1
Mole Fraction of Ethanol (x or y)
Graph 5.2.1: T-x-y diagram for Ethanol-Water.

15
 y-x Diagram for Ethanol-Water
1

0.9
Mole Fraction of Ethanol in Vapor Phase y

0.8

0.7

0.6
Equilibrium line
0.5 x=y line
S6
0.4 S8
S12
0.3 S10
TOL (S6)
0.2 TOL (S8)
TOL (S12)
0.1 TOL (S10)

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Mole Fraction of Ethanol in Liquid Phase x
Graph 5.2.2: y-x diagram with operating lines of Sample numbers 6, 8, 10 and 12 (S6, S8, S10 and S12).

Graph 5.2.3: y-x diagram showing the number of stages for Sample number 6 (S6).

16
Graph 5.2.4: y-x diagram showing the number of stages for Sample number 12 (S12).

Graph 5.2.5: y-x diagram showing the number of stages for Sample number 8 (S8).

17
Graph 5.2.6: y-x diagram showing the number of stages for Sample number S10 (S10).

Dependence of xd on time
0.695
Mole fraction of Ethanol in Distillate, Xd

0.690

0.685

0.680

0.675

0.670
Theoretical
0.665
Experimental
0.660

0.655

0.650

0.645
14:24 14:38 14:52 15:07 15:21 15:36 15:50 16:04
Time
Graph 5.2.7: Dependence of theoretical and experimental values of 𝑥𝑑 on time.
18
5.3. Run D: Continuous distillation at 35% Reflux.
Table 5.3.1: Experimental data for samples.

Time Sample number Empty Full 𝑻𝟏 (℃)

13:59 S1 34.30 81.44 20.00
13:59 S2 34.30 82.04 20.00
Time Sample number Empty Full 𝑻𝟏𝟑 (℃)
15:13 S3 34.30 82.00 21.18
15:16 S4 34.30 82.36 21.33
15:17 S5 34.30 80.06 25.33
15:22 S6 34.30 79.03 50.21
15:23 S7 34.30 82.25 47.28
15:33 S8 34.30 79.33 33.75
15:37 S9 34.30 82.39 64.48
15:40 S10 34.30 82.40 48.28
15:40 S11 34.30 79.45 48.28

Table 5.3.2: The density, weight, mass and mole fractions of MVC.
Sample Density
Sample Ethanol mass Ethanol mole
weight (𝒌𝒈⁄𝒎𝟑 )
number fraction (%) fraction
(g)
S1 47.14 942.80 36.50 0.18
S2 47.74 954.80 29.40 0.14
S4 48.06 961.20 18.90 0.08
S5 45.76 915.20 50.00 0.28
S6 44.73 894.60 59.90 0.37
S8 45.03 959.00 57.15 0.34

Table 5.3.3: The temperatures of samples at given time.

𝑇1 𝑇2 𝑇3 𝑇4 𝑇5 𝑇6 𝑇7 𝑇8 𝑇9 𝑇10 𝑇11 𝑇12 𝑇13

Time
(℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃) (℃)
15:13 20.2 17.6 87.5 82.6 81.6 81.5 81.4 81.2 80.8 80.3 79.6 79.0 21.2
15:16 20.2 17.7 88.5 83.7 82.8 82.7 82.6 82.4 82.2 81.6 81.4 81.2 21.3
15:17 20.2 18.4 89.0 84.1 83.2 83.1 82.9 82.7 82.5 81.9 81.7 81.4 25.3
15:22 20.4 18.9 89.2 84.4 83.4 83.3 83.2 83.0 82.9 82.3 82.2 81.9 50.2
15:23 20.4 19.0 88.2 82.9 81.1 79.0 75.1 81.9 81.6 81.1 80.8 80.3 47.3
15:33 20.4 18.2 87.9 84.1 83.1 83.0 82.9 82.7 82.6 82.1 81.8 79.7 33.8
15:37 20.5 18.7 88.8 84.8 83.6 83.5 83.2 83.3 83.2 82.8 82.7 82.5 64.5
15:40 20.6 19.0 89.0 84.5 83.4 83.3 83.3 83.2 83.1 82.6 82.4 82.2 48.3
15:40 20.6 19.0 89.0 84.5 83.4 83.3 83.3 83.2 83.1 82.6 82.4 82.2 48.3

19
Table 5.3.4: The data for T-x-y diagram.
T (°C) x y
88.9 0.070 0.390
84.0 0.170 0.510
83.1 0.212 0.535
83.0 0.220 0.539
82.9 0.226 0.540
82.7 0.236 0.545
82.5 0.248 0.550
82.0 0.281 0.565
81.8 0.300 0.570

T x y Diagram for Ethanol-Water

100
99
98 Bubble Point Line
97
96
95 Dew Point Line
94
93
92
91
90
T (˚C)

89
88
87
86
85
84
83
82
81
80
79
78
77
0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0.4 0.45 0.5 0.55 0.6 0.65 0.7 0.75 0.8 0.85 0.9 0.95 1
Mole Fraction of Ethanol (x or y)

Graph 5.3.1: T-x-y diagram for Ethanol-Water.

Table 5.3.5: The operating line equations to find the number of stages.
TOL BOL q-line
𝒚 = 𝟎. 𝟑𝟓𝒙 + 𝟎. 𝟑𝟕𝟎𝟓 𝒚 = 𝟐. 𝟗𝟗𝟖𝟐 − 𝟎. 𝟏𝟑𝟗𝟗 𝒚 = 𝟖. 𝟗𝟐𝟓𝒙 − 𝟏. 𝟐𝟖𝟐𝟏
𝑥𝑛 𝑦𝑛 𝑥𝑚 𝑦𝑚 𝑥𝑞 𝑦𝑞
0.000 0.371 0.070 0.070 0.162 0.162
0.100 0.406 0.100 0.160 0.170 0.235
0.200 0.441 0.160 0.340 0.180 0.324
0.300 0.476 0.180 0.400 0.190 0.414
0.400 0.511 0.210 0.490 0.210 0.592

20
 0.500 0.546 0.220 0.520 0.220 0.681
0.570 0.570 0.230 0.550 0.230 0.771
0.240 0.580 0.240 0.860
0.280 0.700 0.250 0.949
0.270 1.128
0.280 1.217

y-x diagram for Ethanol-water

1

0.9
Mole Fraction of Ethanol in Vapor Phase y

0.8

0.7

0.6 Equilibrium line

x=y line
0.5
Sample
0.4 Top operating line

q line
0.3
Bottom operating line
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
Mole Fraction of Ethanol in Liquid Phase x

Graph 5.3.2: y-x diagram showing the number of stages with operating lines.

6. Discussion:
The experiment was designed to investigate the distillation processes in continuous and batch modes
with different reflux ratios, to determine the number of theoretical plates by plotting T-x-y and y-x
diagrams and to compare the theoretical and experimental values of mole fractions of MVC in
distillate(𝑥𝑑 ). The experiment consists of two parts: Firstly, the column was operated under batch mode
with two different reflux settings (Run A and Run C). Then, the continuous distillation was carried out at
a set feed rate and reflux value (Run D).
All experiments were performed using the ethanol/water mixture in which ethanol is more volatile and
has a higher vapour pressure and lower boiling temperature. In order to compare the operation of the
column, some samples, which were taken at regular time intervals from the key points of the column,

21
were chosen to make all calculations: S13 and S14 for Run A; S6, S8, S10 and S12 for Run C; S4 and
S6 for Run D. For batch distillation with reflux 35 % (Run A) the mass of the empty bottle and mass of
liquid inside the bottle for different samples is given in Table 5.1.1. It can be seen from the table that
samples were taken from the feed at the temperature of 20℃ (T1) and the top product in the condenser
(T13). Then, the weight of samples was calculated and converted into density in order to find the mass
and mole fractions of MVC (ethanol) in the sample. It should be noted that the relationship between the
concentration and density of ethanol/water mixture is not linear due to the hydrogen bonding structure.
The molecules in the mixture dissolve in each other, form additional binding forces and take up smaller
space. As a result, the volume of mixture is less than the sum of the input substance volumes. In order
to find the concentration of the mixture, table values are used and given in Lab manual [6]. As can be
seen from table [6], the values of concentration are given as a function of both the density and
temperature. The concentration was found from table [6] using interpolation with the measured density
for fixed temperature. Table 5.1.2 shows that the increase in mass and density of samples causes the
decrease the mass and mole fractions of MVC (ethanol).
The temperatures in the plates of the column are indicated in Table 5.1.3 where T3 and T11 are
temperatures at the bottom and top of the column, respectively. According to data, it can be noted that
the temperature decreases from the bottom to the top. Graph 5.1.1 shows the T-x-y diagram for mixture.
In Graph the lower line is the bubble point line while the upper one indicated the data of dew point. In
the graph the bubble and dew point compositions of MVC in S13 and S14 are illustrated by using the
data in Table 5.1.4. For example, it can be seen that the mole fractions of MVC in liquid and vapour for
sample S13 at 85℃ are 0.132 and 0.48, respectively
Graph 5.1.2 is the y-x diagram for ethanol/water mixture with the top operating lines (TOLs) of Samples
S13 and S14. In order to plot TOLs the equation (3.10) was used in which the mole fraction of MVC in
distillate (𝑥𝑑 ) is 0.672 for S13 and 0.66 for S14 with a reflux ratio of 0.538 kmol/kmol. It is indicated that
the equation of TOL for S13 is 𝑦 = 0.35𝑥 + 0.437, while the TOL for S14 is 𝑦 = 0.35𝑥 + 0.429. The 6
theoretical plates were found for each sample using the McCabe-Thiele method, which is represented
in Graphs 5.1.3 and 5.1.4.
Graph 5.1.5 shows the dependence of theoretical and experimental values of 𝑥𝑑 on time. It can be seen
that the mole fraction of ethanol in the top product decreases over time. The reason is that the newly
formed distillate contains greater proportion of ethanol than in the bottom product of evaporator. As a
result, the product of reboiler losses ethanol during the experiment, which causes the reduced
concentration in the distillate.
For batch distillation with reflux 65% (Run C) all tables and graphs are plotted as the previous one.
Finally, the TOL equations for the selected samples (S6, S8, S10 and S12) are found to be 𝑦 = 0.65𝑥 +
0.228, 𝑦 = 0.65𝑥 + 0.231, 𝑦 = 0.65𝑥 + 0.233 and 𝑦 = 0.65𝑥 + 0.24, respectively. The 4 theoretical plates
are determined for each sample. Graph 5.2.7 is plotted to compare experimental and theoretical 𝑥𝑑 on
time for Run C. From the graph, it is observed that both 𝑥𝑑 values increases up to 15:00, and then, the
fluctuation happens due to some deviations in the experiment. After analysing the two types of distillation
process with different reflux, it can be noted that the number of equilibrium stages decreases with
increasing reflux ratio for batch distillation.
For continuous mode of operation with reflux 35% (Run D) the top and bottom operating lines and q-
line are plotted in Graph 5.3.2. The TOL is drawn using the equation (3.10) where 𝑥𝑑 and reflux ratio
are 0.57 and 0.538, respectively. The value of q was calculated by the equation (3.11) in which the latent
heat of specific heat capacity of the mixture are equal to 3.62 𝑘𝐽/𝑘𝑔 and 1794 𝑘𝐽/𝑘𝑔 𝐾, respectively.
After finding the q value (𝑞 = 1.13), the q line is plotted by using the data in Table 5.3.5, in which the
co-ordinates 𝑥𝑞 and 𝑦𝑞 were given. It is also observed that the bottom operating line is sketched from
22
𝑥𝑤 = 0.07 to the intersection point of TOL and q-line. The equations are indicated in Table 5.3.5.
Additionally, Graph 5.3.2 also represents that 2 number of equilibrium stages (2 plates + reboiler) are
obtained for continuous distillation.
The mole fraction of MVC in liquid remaining in still 𝑥𝑠2 for batch distillation are found using the equation
(3.13) to be 0.116 for reflux 35 % and 0.11 for reflux 65%. It is obtained that the increasing reflux ratio
does not influence significantly the value of 𝑥𝑠2 .
Table 6.1 shows the variance between theoretical and experimental values of 𝑥𝑑 for different batch
modes. It is clear from the table that the variance is less for Run C. It can be concluded that the
theoretical and experimental values of 𝑥𝑑 are similar for high reflux ratio (reflux 65%).
Table 6.1: The variance between theoretical and experimental 𝑥𝑑 values for different reflux.
Batch distillation with reflux 35% (Run A) Batch distillation with reflux 65% (Run C)
Theoretical Experimental Variance Theoretical Experimental Variance
Time Time
𝑥𝑑 𝑥𝑑 (%) 𝑥𝑑 𝑥𝑑 %
17:00 0.672 0.73 8.63 14:40 0.650 0.664 2.154
17:05 0.660 0.72 9.09 15:00 0.66 0.689 4.394
15:20 0.666 0.683 2.553
15:48 0.688 0.692 0.581

7. Conclusion:
The experiment was conducted to make analysis of the distillation column in two modes: Continuous in
which the ethanol/water mixture is supplied and removed continually, and Batch where the composition
of distillate and product in the reboiler changes over time. Firstly, the mass and mole fractions of ethanol
were calculated using the density and temperatures of samples taken from the key point of the column
at regular time intervals. Additionally, T-x-y and y-x diagrams were plotted to find the number of trays
for each mode with different reflux. The operating lines were sketched using the McCabe-Thiele Method
to find the plates in rectifying and stripping sections of the column. Finally, theoretical and experimental
values for the composition of MVC (ethanol) in the top product were compared by plotting the graphs.

8. Appendix:
The sample calculation for Run A and sample number S13.
The volume of bottle: 𝑉 = 50 𝑚𝐿
The density of the sample is calculated as:
𝑚 (75.45 − 34.31) 𝑔
𝜌= = = 822.8 𝑘𝑔⁄𝑚3
𝑉 50 𝑚𝐿
The reflux ratio is defined:
𝑅% 35 %
𝑅= = = 0.5385
100 − 𝑅% 65 %
The mole fraction of MVC (ethanol) is calculated using the following equation:
𝑤1 87.40
𝑀1 46.068
𝑥1 = = = 0.73
𝑤1 100 − 𝑤1 87.40 100 − 87.40
𝑀1 + 𝑀2 46.068 + 18.015
Molecular weight of ethanol: 𝑀1 = 46.068 𝑘𝑔/𝑘𝑚𝑜𝑙
Molecular weight of water: 𝑀2 = 18.015 𝑘𝑔/𝑘𝑚𝑜𝑙

23
Mole fraction of ethanol in liquid initially charged to batch 𝑥𝑠1 is found as the average value of mole
fractions of ethanol in Samples S1, S2 and S3:
0.16 + 0.18 + 0.15
𝑥𝑠1 = = 0.162
3
Mole fraction of MVC in liquid remaining in batch 𝑥𝑠2 is calculated as:
𝑆1 × 𝑥1 − 𝐷 × 𝑥𝑑 294.45 × 0.162 − 21.51 × 0.75
𝑥𝑠2 = = = 0.116
𝑆1 − 𝐷 294.45 − 21.51

9. References:
1. Andrzej Gorak, Z. O. (Ed.). (n.d.). Distillation: Equipment and Processes . Retrieved from
https://www-sciencedirect-
com.ezproxy1.hw.ac.uk/science/article/pii/B9780123868787000012

2. Green, D. W., Perry, R. H., & Maloney, J. O. (n.d.). PERRY'S CHEMICAL ENGINEERS'S
HANDBOOK (7th ed.). McGraw-Hill. Retrieved from
https://accessengineeringlibrary.com/browse/perrys-chemical-engineers-handbook-
eighth-edition

3. Kiss, A. A. (n.d.). Advanced Distillation Technologies: Design, Control and Applications (1st
ed.). John Wiley & Sons. doi:10.1002/9781118543702

4. SEPARATION PROCESSES A. (n.d.).

5. SINNOTT, R. K. (n.d.). Coulson & Richardson’s Chemical Engineering (4th ed., Vol. vi).
Elsevier . Retrieved from http://www.zuj.edu.jo/download/coulson-richardson-s-
chemical-engineering-vol-6-pdf/

6. Experimental Instructions Manual, “Continuous Rectification GUNT. (n.d.).

24