German Jordanian University

School of Applied Medical Sciences

Chemical and Pharmaceutical Engineering Department

Separation Processes Lab (PCE562)

Experiment (C1+C2): Batch Distillation

Section Number: 4
Group member, ID#:

Farah Sa’adeh 20219301006

Mira Alabbassi 20219301010

Yara Roussan 20219301019

Zeena Laswi 20219301007

Instructors:
Eng. Ranya Khader
Eng. Ayar Abudaeij

Date of preforming experiment: 24/7/2024

Date of report submission: 27/7/2024
1- Results and Discussion:
1.1 Tables
Table 1: Displays the measured values of the Index of Refraction for a high mole fraction of
ethanol in water at various concentrations of the water-ethanol mixture.

Mole 0% 25% 50% 75% 100%

Fraction
Index of 1.3324 1.3390 1.3639 1.3639 1.3602
refraction

Table 2: Displays the measured values of the Index of Refraction for a low mole fraction of
ethanol in water at various concentrations of the water-ethanol mixture.
Mole 0% 5% 10% 20% 25%
Fraction
Index of 1.3324 1.3390 1.3455 1.3523 1.3542
refraction

Table 3: Illustrates the following: The number of theoretical stages (N), The efficiency η (%) at
heating rate 10 and reflux ratio 5:2, The xLKD, The reboiler's refractive index for five different
trials, The average value of the reboiler's refractive index, TI1 (°C), TI4 (°C), αd, αb, and αAB,
and the total number of trials.
1 1.3611
2 1.3597
Refractive Index of distillate 3 1.3601
4 1.3602
5 1.3602
Average value of refractive 1.3626
index of Distillate
XLKD 0.622
1 1.3336
2 1.3321
Refractive Index of reboiler 3 1.3317
4 1.3314
5 1.3317
Average value of refractive 1.3321
index of reboiler
XLKB 0.244
TI1 (°C) 91.5
TI4 (°C) 88.9
αd 1.488
αb 11.21
αAB =√(αdαb) 13.67

2
 N 0.60
η (%) 8.57%

Table 4: Displays the temperatures T1–T6°C that were recorded using six thermocouples at five-
minute intervals for thirty minutes at a heating rate of 10 and a five-to-two reflux ratio at various
locations within the distillation tower.V

Time (min) T1 (°C) T2 (°C) T3 (°C) T4 (°C) T5 (°C) T6 (°C) Volume

0 84.7 82.4 82.2 81.4 27.0 30.5 0
5 86.6 83.9 82.9 81.8 27.3 31.2 250
10 87.1 84.1 83.2 82.2 27.5 31.0 300
15 87.9 85.0 84.4 83.9 27.5 31.5 375
20 88.5 85.8 85.0 85.1 27.6 31.5 480
25 88.9 86.7 85.9 86.2 27.8 31.9 575
30 89.1 87.1 86.6 86.3 27.9 32.0 630
35 90.3 88.3 87.0 86.5 28.2 32.0 750
40 91.5 89 88.9 88.9 28.5 32.0 850

Table 5: Batch 2

Time (min) T1 (°C) T2 (°C) T3 (°C) T4 (°C) T5 (°C) T6 (°C) Volume

0 84.7 82.4 82.2 81.4 27.0 30.5 0
15 89.1 86.5 86 84.9 24.7 32.6 475

1.2 Figures

Low
1.36
1.355
f(x) = 0.000860930232558143 x + 1.3343488372093
Index of Refraction

1.35 R² = 0.958753089670616
1.345
1.34
1.335
1.33
1.325
1.32
0 5 10 15 20 25 30

Mole Fraction (%)

Figure 1: Shows calibration curve for the values mole fraction of ethanol for low
concentrations of ethanol in water vs. index of refractive

3
 High
1.37
f(x) = 0.0002612 x + 1.34156
Index of Refraction 1.36 R² = 0.634831945784354
1.35

1.34

1.33

1.32

1.31
0 20 40 60 80 100 120

Mole Fraction (%)

Figure 2: Displays a calibration curve for the values mole fraction of ethanol for High concentrations of
ethanol in water vs. index of refractive

Temperature (°C) vs. Time (min)

94
92
Temperature (°C)

90
88
86
84
82
80
78
76
0 5 10 15 20 25 30 35 40 45

Time (min)

T1 (°C) T2 (°C) T3 (°C) T4 (°C)

Figure 3: Displays the temperature change for T1-T4 °C vs Time in mins during the distillation
process.

4
 Temperature (°C) vs. Time (min)
94
92
Temperature (°C) 90
88
86
84
82
80
78
76
0 5 10 15 20 25 30 35 40 45

Time (min)

T1 (°C) T4 (°C)

Figure 4: Displays the temperature change for T5 & T6°C vs Time in mins during the
distillation process

1.3 Sample of calculations

The experiment was operated with:
1. isobaric pressure 0.96 ATM
2. 100 L/h flow rate of cooling water
3. Heating rate of 10
4. Reflux ratio of 5:2

Table 3 Calculations :

 Average Refractive Index of distillate:

Σ refractive index of distillate

n
1.3611+1.3602+1.3602+1.3601+1.3597
¿
5
=1.36026

 Mole fraction of the light key component in liquid state in distillate XLKd
We need to use from Figure 1 high concentration of ethanol in water from the calibration

𝑦 = 𝑎𝑥 + 𝑏
curve

𝑦 = 0.0003𝑥 + 1.3416
Where 𝑦 is the average refractive index for distillate product
y =1.36026

5
 𝑥 = XLKd
1.36026=0.0003𝑥 + 1.3416
62.2
=¿
100

𝑥= 0.622

 Average refractive index of the reboiler:

Σ refractive index of distillate

n
1.3336+1.3317+1.3317+ 1.3314+1.3321
¿
5
¿ 1.3321

6
  Mole fraction of the light key component in liquid state in reboiler XLKb
We need to use from Figure 1 Low concentration of ethanol in water from the calibration

𝑦 = 𝑎𝑥 + 𝑏
curve

𝑦 = 0.0009𝑥 + 1.3343
Where 𝑦 is the average refractive index for distillate product
y =1.3321

𝑥 = XLKb
1.3321=0.0009x+1.3343
2.444
=
100
XLKb = 0.002444

 Geometric Average Relative Volatility (αAB)

For distillate:

XLKd= 0.622

XHKd= 1- XLKd

XHKd= 1- 0.622
XHKd= 0.378 mol/mol

 To Calculate YLKd
YLKd is the mole fraction of light key component in vapor state at equilibrium in the
distillate
We use Appendix A

XLKd YLKd
0.65250 0.72555
0.70000 0.74950

y 2− y 1
y= y 1+ ∙(x−x 1 )
x 2−x 1

0.74950−0.72555
y=0.72555+ ∙(0.622−0.65250)
0.70000−0.65250

7
 YLKd= 0.710 mol/mol
 To Calculate YHKd
YHKd which is the mole fraction of heavy key component in vapor state at equilibrium in the
distillate

YHKd= 1- YLKd

YHKd= 1- 0.710

YHKd= 0.2898 mol/mol

 αd,
Which is the relative volatility of the distillate product:

Y LKd / X LKd
αd =
Y HKd / X HKd

0.710/0.622
αd =
0.2898/0.378

𝛼𝑑 = 1.488

 Bottom:

XLKb= 0.02444 mol/mol

 XHKb

XHKd is the Mole fraction of heavy key component in liquid state in the
distillate

XHKb= 1- XLKb
XHKb= 1- 0.0244
XHKb= 0.9756 mol/mol

 To calculate YLKb we need to use Appendix A

YLKb is the Mole fraction of heavy key component in liquid state in the bottom product
XLKb YLKb
0.03150 0.25050
0.06000 0.37650

y 2− y 1
y= y 1+ ∙(x−x 1 )
x 2−x 1
8
 0.37650−0.25050
y=0.25050+ ∙ ( 0.0244−0.03150 )
0.06000−0.03150
𝑦LKb= 0.2191

9
 To calculate YHKb:
Where YHKb is the Mole fraction of heavy key component in vapor state at equilibrium in
the bottom product.
YHKb=1-YLKb
YHKb=1-0.2191
YHKb=0.7809 mol/mol

 To calculate αB
Which is the relative volatility of the bottom product:

Y LKb / X LKb
αb=
Y HKb / X HKb

0.2191/0.0244
αb=
0.7809 /0.9756

𝛼𝑏 = 11.21

 To Calculate αAB,
Which indicates the geometric relative volatility at the temperature of distillate and bottom
product.

𝛼𝑏𝑑 = √𝛼𝑏 ⋅ 𝛼𝑑
𝛼𝑏𝑑 = √1. 488 ⋅ 11.21
𝛼𝑏𝑑 = 13.67

 To Calculate N
N indicates the theoretical number of trays we use Fenske’s equation:

N +1=
ln
( x d 1−x b
∙
1−x d x b )
ln α AB

Xd=XLKd and Xb=XLKb

we substitute these values in the equation

0.622 1−0.0244
ln ⁡( ∙ )
1−0.622 0.0244
N +1=
ln ⁡(13.67)

𝑁 + 1 = 1.60
𝑁 = 0.600

 To Calculate (η) which is the efficiency:

10
 N
ղ= ∙100 %
NR

N : is the theoretical number of plate

NR is the actual number of plates which is 7.
0.6
ղ= ∙ 100 %
7

𝜂 = 8.57%

11
2- Discussion:
A common technique for separating mixtures according to variations in boiling points or relative
volatilities is distillation. This procedure is vital in many sectors where component separation
and purification are critical, such as alcohol manufacturing, petrochemicals, and medicines. This
separation is made possible by the distillation machine, also known as a distillation column or
unit, which uses controlled heating, vaporization, condensation, and phase separation.

Continuous distillation and batch distillation are very distinct from one another. Continuous
distillation involves continually adding feed to one of the trays and continuously withdrawing the
distillate without pausing or interfering with the operation. For steady and large-scale production,
this approach works well. In contrast, the feed mixture is added at the start of the operation in
batch distillation. When the distillation is finished, the apparatus is turned off and the whole
distillate is removed. After that, the feed is refilled, and the procedure is restarted. Products that
need a high level of purity, those with limited manufacturing capacity, and seasonal goods are
usually the best candidates for batch distillation. Because the two components of the binary
mixture in this experiment had sufficiently different volatility (or boiling points) from one
another, distillation was determined to be the most effective separation technique. Since ethanol
vaporizes more easily than water at 100°C due to its lower boiling point of 78.37°C, it is the
lightest component in the distillation process.

The distillation column has several major components. To start with, the heating source for the
batch distillation process is the reboiler, which is connected to an electrical heating element to
provide the heat required to evaporate the ethanol and water binary combination. By circulating
the heated mixture and causing vaporization, it guarantees uniformity of the mixture with respect
to temperature and composition. The vaporization process is successfully started by the
circulation and bubbling, which maintain a constant and uniform temperature throughout the
reboiler. Effective vaporization of the mixture is ensured by the reboilers consistent heating and
mixing, which is essential for the first component separation. The reboiler also serves as an
equilibrium stage, which improves the process's overall separation efficiency. Another major
component is a total condenser, the shell and tube heat exchanger serves as the condenser,
enabling the vapor phase to condense completely. In this experiment, the cooling agent is water.
A flow indicator (rotameter) is used to measure and control the cooling water flow rate. In the
condenser, the vapor at the top of the distillation column condenses back into liquid form. To get
a high-purity distillate, the condenser's cooling and condensing efficiency is essential.
Maintaining the overall efficiency of the distillation process and preventing any loss of distillate
are made possible by properly controlling the condenser's temperature to guarantee that the vapor
is thoroughly condensed. Also, the components are separated in the vertical borosilicate glass
distillation column, which has seven sieve plates. Mass transfer and component separation are
made easier when vapor rising from the reboiler comes into touch with liquid falling from the
reflux on the trays. A surface for vapor-liquid interaction is provided by each tray, which
improves the separation process. The liquid phase is helped to migrate between trays by the
overflow column on each tray, which keeps the liquid volume constant. The number of plates in
the distillation column has a big impact on its effectiveness; more plates offer a bigger surface
area for contact, which improves separation and boosts efficiency. The effectiveness of
separation improves with the number of equilibrium phases, which are represented by each tray.
The entire distillation process, including the reflux valve, electrical heating element, and process
switches, is managed by the control panel. It also has a knob to alter the solenoid valve's opening
and shutting timings, which govern the reflux ratio, and the heating rate. Optimization of the
separation process is made possible by the exact control of the reflux ratio and heating rate.
Furthermore, the distillation's overall efficiency and operational flexibility are enhanced by the
control panel's ability to make real-time modifications. The reflux ratio is managed via electrical
control of the solenoid valve. When the reflux ratio is 5:2, for instance, the valve opens for 5
seconds to collect condensate and closes for 2 seconds to force the condensate to be recycled
back into the column. The purity and yield of the distillate are impacted by changes in the reflux
ratio, which also affects the contact between vapor and liquid. To maintain the appropriate
separation efficiency and guarantee the best possible performance of the distillation process,
precise management of the reflux ratio is crucial. In order to guarantee that the distillate is
sufficiently cold before collection, the concentric tube heat exchanger uses cooling water from
the condenser to cool the distillate product. When the distillate is properly cooled, further
vaporization is prevented, guaranteeing the end product's great purity and quality. Furthermore,
useful heat exchange keeps the system's overall thermal balance, which enhances the efficacy
and efficiency of the distillation process. The high-purity distillate generated during the
distillation process is stored in the distillate collecting tank, which also gathers the top product
that is rich in the light key component (ethanol). The distillate is collected without loss,
maintaining purity and optimizing the production of the light essential component thanks to the
collecting tank's design and capacity. The number of plates is one factor that affects efficiency:
the more plates, the better the phase contact and separation efficiency. Another important factor
is the reflux ratio; greater ratios increase purity but lower production rates, necessitating the ideal
balance between yield and efficiency. Furthermore, the heating rate affects both production rates
and efficiency; greater rates may result in lower efficiency because of shorter contact times
between stages, but they also increase production. The high-purity distillate generated during the
distillation process is stored in the distillate collecting tank, which also gathers the top product
that is rich in the light key component (ethanol). The distillate is collected without loss,
maintaining purity and optimizing the production of the light essential component due to the
collecting tank's design and capacity.

The volatility differential between ethanol and water is what drives the distillation process. Since
ethanol has a lower boiling point (78.37°C) than water (100°C), it vaporizes more easily,
therefore it is expected to produce an initial distillate that is high in ethanol. Early in the
distillation process, ethanol will evaporate and separate from the water more readily than water
since it has a lower boiling point. Because of this, the distillate will have a high concentration of
ethanol, and the reboiler composition will start with the original mixture and progressively grow
richer in water as ethanol is eliminated. The reboilers ethanol content drops during the
distillation process, producing a distillate with a gradually reduced ethanol level. This keeps
happening until the reboiler is primarily made of water, which represents the ethanol's gradual
depletion.

The differences between Batch 1 and Batch 2 as we increased the heating rate could be compared
through the observations. In Batch 2 the process of heating, thus bubbling occurred at a much
faster rate than Batch1, the bubbling in the reboiler in Batch 1 was not continuous it increased at
times and stopped at others. On the other hand, in Batch 2, the bubbling into the reboiler from
the heating element was continuous within the first 5 minutes of the operation. In the distillation
column, in Batch 1 there was more internal bubbling than external bubbling. In batch 2 there was
mostly external bubbling. This is a bad indication. Within the first 7 minutes all external sieve
trays had vigorous bubbling. Despite Batch 2 resulting in more product, it is the least efficient
operation. This is due to the fact that at higher heating rate, vigorous external bubbling results in
lower residence time, thus less contact between components and less mass transfer, this may lead
to unpurified product.

Also, The ethanol-water mixture's composition affects the index of refraction. The distillate's
index of refraction drops as its ethanol concentration drops. On the other hand, the reboiler
mixture's index of refraction rises as it gets more concentrated in water. The reboilers index of
refraction will progressively increase as the concentration of water increases as a result of
ethanol evaporation. The index of refraction changes as a result of the distillate and reboilers
compositions changing due to the increasing elimination of ethanol from the combination, which
leaves a higher percentage of water behind. Moreover, It is expected that the temperature would
rise and then stabilize at various points along the distillation column. The temperature in the
reboiler will rise gradually as the concentration of the higher boiling component—water—
increases after first rising swiftly to the mixture's boiling point. This happens as a result of the
remaining mixture in the reboilers increasing water content, which raises the mixture's boiling
point as the ethanol is distilled off. As the distillation process progresses, the temperatures in the
column eventually approach a steady state, reflecting the dynamic equilibrium between the liquid
and vapor phases. When the combination gets closer to boiling, the temperature in the reboiler
first rises quickly. The residual combination gets richer in water as the ethanol is distilled out,
causing the temperature rise to slow and then steadily climb. The dynamics of heat transmission
and phase changes are reflected in the temperatures at various locations in the distillation
column. The trays at the top that are closest to the condenser are cooler than the trays at the
bottom that are closer to the reboiler. As the system achieves equilibrium, these temperatures
gradually stabilize.

Furthermore, it is anticipated that a greater reflux ratio will improve the efficiency of the
separation process by increasing contact between the liquid and vapor phases and producing a
purer distillate. But doing so also means that less distillate is gathered in each amount of time.
Lower production rates but higher distillate quality are the results of higher reflux ratios.
Additionally, raising the heating rate accelerates the rate of vaporization, which boosts distillate
output. Rapid vaporization shortens the time that the vapor and liquid phases in the column have
in touch with one another, which lowers separation efficiency. Nevertheless, this can also result
in less effective separation. While increasing production, higher heating rates will reduce
separation efficiency. Striking a balance between the two variables is necessary for optimal
distillation since higher reflux ratios increase separation but reduce output volume by increasing
contact between the liquid and vapor phases. However, faster vaporization and higher output
might come at the expense of reduced purity and efficiency of the separation process since a
higher heating rate shortens the time that phases are in contact with one another.

Discussing the 5 tables present in given report, both tables 1 and 2 require to
.calculations
Tables 1 and two represent the refractive index of solutions containing high
concentrations of ethanol in water and low concentrations of ethanol in water
respectively. The results were obtained using a refractometer, in which light is passed
through the material being tested and is then refracted at a certain angle. Table 3
illustrates the refractive indices of the distillate (product) and the reboiler and shows
the averages 1.3626 and 1.3321respectively. Studying these averages, it could be
deduced that the refractive index of the distillate falls into the ranges of high mole
factions of ethanol in water, and the opposite is true for the reboiler. Additionally,
:Table 3 provides the number of stages N which is calculated from the Fenske equation

N +1=
ln
( x d 1−x b
∙
1−x d x b )
ln α AB

Variables such as the 𝑥𝐿𝐾𝑏: 𝑚𝑜𝑙𝑒 𝑓𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑓 𝑡ℎ𝑒 𝑙𝑖𝑔ℎ𝑡 𝑘𝑒𝑦 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 𝑖𝑛
𝑙𝑖𝑞𝑢𝑖𝑑 𝑠𝑡𝑎𝑡𝑒 𝑖𝑛 𝑡ℎ𝑒 𝑟𝑒𝑏𝑜𝑖𝑙𝑒𝑟. 𝑦𝐿𝐾𝑏: 𝑚𝑜𝑙𝑒 𝑓𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑓 𝑡ℎ𝑒 𝑙𝑖𝑔ℎ𝑡 𝑘𝑒𝑦
𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 𝑖𝑛 𝑣𝑎𝑝𝑜𝑢𝑟 𝑠𝑡𝑎𝑡𝑒 𝑎𝑡 𝑒𝑞𝑢𝑖𝑙𝑖𝑏𝑟𝑖𝑢𝑚 𝑖𝑛 𝑡ℎ𝑒 𝑟𝑒𝑏𝑜𝑖𝑙𝑒𝑟 (𝐹𝑟𝑜𝑚
𝐴𝑝𝑝𝑒𝑛𝑑𝑖𝑥 𝐴 𝑎𝑡 𝑥𝐿𝐾𝑏)

𝑥𝐻𝐾𝑏: 𝑚𝑜𝑙𝑒 𝑓𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑓 𝑡ℎ𝑒 ℎ𝑒𝑎𝑣𝑦 𝑘𝑒𝑦 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 𝑖𝑛 𝑙𝑖𝑞𝑢𝑖𝑑 𝑠𝑡𝑎𝑡𝑒 𝑖𝑛

𝑡ℎ𝑒 𝑟𝑒𝑏𝑜𝑖𝑙𝑒𝑟
= 1 − 𝑥𝐿𝐾𝑏. 𝑦𝐻𝐾𝑏: 𝑚𝑜𝑙𝑒 𝑓𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑓 𝑡ℎ𝑒 ℎ𝑒𝑎𝑣𝑦 𝑘𝑒𝑦 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 𝑖𝑛
𝑣𝑎𝑝𝑜𝑢𝑟 𝑠𝑡𝑎𝑡𝑒 𝑎𝑡 𝑒𝑞𝑢𝑖𝑙𝑖𝑏𝑟𝑖𝑢𝑚 𝑖𝑛 𝑡ℎ𝑒 𝑟𝑒𝑏𝑜𝑖𝑙𝑒𝑟 = 1 − 𝑦𝐿𝐾𝑏

Where calculated using the straight-line equation of obtained from Figures 1 and 2, and the y
components were calculated using interpolation.

αAB = √(αdαb) = The geometric average relative volatility at the temperature of distillate and of

bottom product. Relative Volatility of the Bottom product: 𝛼𝑏 =

yLKb /xLKb
and of the
yHKb /xHKb

distillate 𝛼𝑑 =
yLKd/ xLKd
yHKd . xHKd

N
Lastly the efficiency was calculated by η = . 100
NR

All the above was calculated at operating conditions of isobaric pressure 0.96 ATM, flow rate of
cooling water at 150l/h, a heating rate of 10 and at reflux ratio of 5:2 .

Tables 4 and 5 present data at different thermocouples throughout the operation at time intervals
of 5 minutes.

Referring to the Figures above, Figures 1 and 2 display the calibration curves of the values mole
fraction of ethanol for low and high concentrations of ethanol in water vs. index of refraction.
The positive slope in figure one indicates that as the mole fraction of light key component in the
distillate increases so does the refractive index. The positive slope of figure 2 indicates that as
the mole fraction of heavy key component in the bottom product increases so does the refractive
index.

Figure 3 illustrates the temperature gradients in Thermocouples 1-4, which as time increases so
does the temperature. The highest temperature is at T1 which is at the reboiler, then the
temperature ranges from one thermocouple to the other decrease as we move up the column to
the reflux shell and tube heat exchanger. Figure 4 studies the difference in temperature between
T5 and T6 which are at the inlet and outlet of the condenser throughout the operation. T6 is
greater than T5 indicating the heat transfer process as we go from heating to cooling.
After conducting the pilot experiment, a thorough comparison between the experimental and
expected results showcased that the experiment complied with all expected results. It was
previously stated that as the concentration of ethanol in the binary mixture increases, the
refractive index is expected to increase, this expectation proved to be true as seen in table 1 and
along with it in figure 2. The index of refraction values increased from 1.3324 to 1.3602 as the
composition of ethanol increased from 0% to 100%, and along with that a linear increase was
displayed in figure 2. Additionally, it is seen that even at low concentrations of ethanol, the
refractive index increases with increasing composition, seen in table 2. The experimental results
were also consistent with those expected for the distillate and reboiler compositions, as the
distillate contained a likely 75% ethanol and the reboiler composition is a likely 0% ethanol
meaning pure water seen in table 2.

Furthermore, it was expected that the temperature profile over various places in the column will
increase initially then stabilize. This statement was also supported by the experimental results as
the temperature at T1, seen in table 4, increases drastically by almost 2 ℃ in the first 5 minutes
of the experiment, and then the temperature profile stabilized to an increase in temperature by
around 0.2℃ towards the end of the experiment at minute 40. It was also predicted that the
temperature readings at the lower trays near the reboiler will have higher values than those at the
top close to the condenser. This expectation was consistent with the reality as the temperature
near the reboiler at T1 was equal to 84.7 ℃ and that at T5 was equal to 27 ℃ . Finally, the effect
of changing the heating levels from 7 to 10 was expected to decrease efficiency as it decreases
the contact time between the vapor and liquid because of the high vaporization rate. This theory
was supported by the experimental observations in batch 2, seen in table 5, as the rate of
vaporization increased rapidly, thus causing higher levels of external bubbling which is not
favorable for efficiency.

A variety of errors in the experiment may contribute to any accuracy in the results which may
include; a systematic error in the ethanol and water distillation pilot experiment could lead to
inaccurate thermocouple and flow meter calibrations, which could result in constant variations in
the temperatures and flow rates recorded. Systematic variations in the real heating power
produced in relation to the specified value can also result from inaccurate calibration of the
heating element. Furthermore, if the composition of the ethanol-water mixture is not
homogeneous, contaminants or irregularities may induce systematic inaccuracies. On the other
hand, random errors could result from variations in the surrounding temperature and pressure,
which have an impact on the distillation process but are unpredictable and inconsistent.
Furthermore, if the composition of the ethanol-water mixture is not homogeneous, contaminants
or irregularities may induce systematic inaccuracies. However, this error is prevented by thermo-
cycler in the reboiler apparatus, which induces mixing by design. On the other hand, random
errors could result from variations in the surrounding temperature and pressure, which have an
impact on the distillation process but are unpredictable and inconsistent. Furthermore, random
variability in the data gathered may be introduced by operator handling and measuring
methodologies. The precision and dependability of the experimental results are impacted by
these flaws collectively, therefore careful control and several trials are required to decrease their
effects.

3- Conclusion and Recommendations:

The experiment involving batch distillation proved to be effective, with mostly consistent results.
The predicted and actual findings, including the differences in the indices of refraction,
temperature profiles, and the impact of the reflux ratio and heating rate on separation efficiency,
were mainly in line with each other. The experiment's overall efficiency was 8.57%, and the R2
value showed a significant connection between the theoretical and experimental results.
Operating parameters comprised a heating rate of 10, a reflux ratio of 5:2, an isobaric pressure of
0.96 ATM, and a cooling water flow rate of 150 l/h. Under these circumstances, the distillate had
a high ethanol concentration at first, but as ethanol was gradually distilled out, the concentration
of ethanol reduced with time. On the other hand, when the ethanol was withdrawn, the
composition of the reboiler gradually got richer in water, starting with the original combination.

In conclusion, the index of refraction of the distillate declined as the concentration of ethanol
decreased, but the index of refraction of the reboiler grew as the concentration of water
increased. Temperature profiles in the reboiler revealed a sharp spike at first, which was
followed by a progressive increase as the water content increased. With lower trays being hotter
than top trays, the temperature gradient in the column represented the dynamics of heat transport.
While greater heating rates boosted output but decreased separation efficiency, larger reflux
ratios produced distillates with higher purity but at lower production rates. Maintaining operating
efficiency, attaining a high purity distillate, and optimizing the distillation process all depended
on striking a balance between these parameters.

From the discussion above, several recommendations can be made in order to improve the
process design and operating conditions of a batch distillation. Advanced controls can be used to
enhance a batch distillation process, increasing its efficiency and reducing energy consumption.
Furthermore, Process efficiency can be increased by using automated systems, which will help
closely monitor temperature and pressure. In addition, reusing heat through helps reduce energy
expenses. The efficiency of a distillation column can also be improved by adding or removing
trays or packing, changing the feed location, adjusting the reflux ratio. Also, reduce emissions
and waste to make the process more environmentally friendly, efficient, and safe.

4- Bibliography

Separation Processes Lab Manual, 2022

Data Sheet