An-Najah National University

Faculty of Engineering and Information Technology

Chemical Engineering department

Unit Operation Laboratory II (10626468)

Continous and Batch Distillation

(Experiment no. 2, performed on 2. May.2024)

Group Members:

Deema Tammam

Ruaa Al-Qasarwa

Sarah Rabaya

Sarah Salameh

Submitted to:

Dr. Abdulrahem Abusafa

Eng. Maha Fuqha

May 27, 2024

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2
Abstract
Separation is a method used to convert a mixture of chemical substances into
distinct product mixtures, removing unwanted materials and obtaining useful
components. This process exploits differences in chemical properties or physical
properties, such as size, shape, mass, density, or chemical affinity.

The distillation column is considered the most important separation method in

chemical engineering. It is a tube that provides surfaces on which condensation and
evaporation processes can occur before the gas enters the condenser to concentrate the
more volatile liquid in the first parts and the less volatile components in the later
parts.

In this experiment two types of distillation were tried: continuous distillation and
batch distillation.

The batch distillation experience, the experiment was done by using simple
Batch Distillation to distil ethanol from a binary mixture of ethanol and water. The
process involved setting up the system, preparing the mixture, heating it to 70°C,
collecting the distilled samples, and measuring their density.

A continuous distillation experiment was done to study the Steady-state

distillation of a binary mixture under continuous operation, the experiment was done
by placing an equal mixture of ethanol and water in the device and then monitoring
the temperatures at each point to study changes in proportions via a Txy diagram.

The experiment demonstrated the efficient separation of a binary mixture

using both batch and continuous distillation techniques. Batch distillation effectively
concentrated ethanol, while continuous distillation maintained a steady state, resulting
in consistent output quality.

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Table of Contents
Abstract.......................................................................................................... i
Introduction.................................................................................................... 1
Apparatus....................................................................................................... 4
Continues Distillation Column..........................................................................4
Batch distillation........................................................................................... 6
Procedure....................................................................................................... 7
Continues Distillation..................................................................................... 7
Simple Batch Distillation................................................................................. 7
Sample of calculation and Results.........................................................................8
Continuous distillation.................................................................................... 8
Simple Batch distillation................................................................................ 10
Discussion.................................................................................................... 12
Conclusion.................................................................................................... 13
References.................................................................................................... 14

Figures

Figure 1:Binary Distillation................................................................................. 1

Figure 2:Single Phase Flash Distillation..................................................................2
Figure 3:Cross Flow Trays with Downcomers..............................................3
Figure 4:Countercurrent Flow without Downcomers....................................3
Figure 5:Sieve Tray........................................................................................... 3
Figure 6: Distillation column Components...............................................................5
Figure 7:Continuous Distillation Column Sheet.........................................................5
Figure 8: Simple Batch Distillation........................................................................6
Figure 9: Txy Diagram for methanol -Water.............................................................8
Figure 10:X vs. 1/(Y-X)................................................................................... 11

Tables

Table 1:Continues distillation Results.....................................................................9

Table 2: Result for theoretical calculation..............................................................11

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Introduction
Distillation columns are essential in industries like beverage manufacturing,
chemical processing, and petroleum refining for separating mixtures into their
constituent parts. They involve engineering, chemistry, and thermodynamics to
maximize parameters like separation purity, energy consumption, and efficiency. The
primary goal is to remove unwanted materials and obtain useful components.[1]

One of the first essential procedures in the petroleum refining industry is crude
oil distillation, which involves gradually separating out several oil products with
varying distillation ranges (carbon and hydrogen compounds). [2]

The design of a binary distillation column faces constraints due to

nonlinearity, multivariable interactions, and disturbances. To address these
constraints, a modern control method is needed to track set point changes and reduce
or eliminate disturbances, ensuring the desired product composition output is
achieved.

Figure 1:Binary Distillation.

Multicomponent distillation involves multiple components, with the design
principle being like binary systems. Each part has a mass balance and enthalpy or heat
balances. In binary systems, one column is needed, while multicomponent distillation
requires two or more columns. Enthalpy or heat balances are similar.

Flash distillation occurs in a single stage, a liquid mixture is partially

vaporized. The vapor is allowed to come to equilibrium with the liquid, and the vapor
and liquid phases are then separated, this can be done in batch or continuous [3]

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 Figure 2:Single Phase Flash Distillation.
An atmospheric pressure high-Boiling liquids cannot be purified by
distillation, since the components of the liquid may decompose at the hot
temperatures needed. The high-Boiling substances are essentially insoluble in water,
so a separation at lower temperatures can be obtained by simple steam distillation.

An anomalous but not uncommon behaviour in some binary systems is the

occurrence of an azeotrope. An azeotrope is shown by the presence of a maximum or
minimum in the bubble and dew lines.

The azeotropic point is the maximum or minimum on a phase diagram, where

the bubble and dew lines meet, and the vapor and liquid compositions are identical. A
liquid solution with the same azeotropic composition boils as a pure part, maintaining
constant temperature throughout boiling, and a vapor with the same concentration
condenses as a pure component. [4]

Reactive distillation is a combination of separation and reaction in a single

vessel. The concept of combining these two important functions for enhancement of
overall performance. [5]

Atmospheric distillation is the first and most fundamental step in the refining process.
The primary purpose of the atmospheric distillation tower is to separate crude oil into
its components (or distillation cuts, distillation fractions) for further processing by
other processing units. [6]

A vacuum distillation is used when the boiling point of the compound is too high to
distill the compound without substantial decomposition. The setup is like a micro-
scale or semi-macroscale distillation.

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Distillation can be conducted in a tray or a packed column. The major considerations
involved in the choice of the column type are operating pressure and design
reliability.

Tray columns are more efficient when pressure increases as they can tolerate pressure
drop, distillation trays are classified as crossflow trays with downcomers and counter
current flow without downcomers as shown in the following figures.

Figure
cross 3:Cross
flow traysFlow
withTrays with
downcomers Figure 4:Countercurrent Flow without
Downcomers. Downcomers.

There are
three common types of trays, sieve tray, bubble cap tray, and valve tray.

Sieve trays offer high capacity and efficiency, low pressure drop, ease of cleaning,
low capital cost and are satisfactory for most applications, but smaller turndown ratio.

Figure 5:Sieve Tray.

Valve trays should be considered if the specified turn-down ratio cannot be met with
sieve plates. [7]

Batch distillation Type of distillation where the entire batch of liquid feed is placed
into the still at the start of the process and then heated. The vapor is collected and
condensed to a distillate some of which is as reflux. The composition of the remaining
liquid and the distillate are functions of time.[8]

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Apparatus
Continues Distillation Column
As figure 8 shows the components of continues distillation column are a 50
mm diameter sieve plate column with two glass sections (3) and (4), each containing
four sieve plates, arranged vertically for counter-current vapor/liquid flow. Alongside
this are components such as a Reboiler (13), two 5-litre feed tanks (5), (6), a
Peristaltic-type feed pump (7), a Condenser (8), Bottom (9) and Top (10) product
tanks, a Decanter (11), a Reflux valve (12), an Azeotropic dosing vessel (24), and a
Vacuum pump (20).

The Reboiler (13), made of 316 stainless steels, features a flameproof immersion-type
heating element for both batch and continuous distillation. In continuous operation,
bottom product flows from the reboiler through a bottom product cooler (15) to the
bottom product tank (9), with an option to preheat the column feed using heat
transferred from the reboiler. During batch operation, the reboiler is filled with an
initial charge of a binary mixture, with valve (V1) closed.

A level sensor (17) within the reboiler prevents overheating due to low operating
levels, while a sight glass (18) allows observation of the liquid level.

The feed mixture from either tank is pumped by pump (7) to the column's base,
centre, or top at connections (A), (B), or (C).

The glass column, split into two sections, houses eight sieve plates (four in each
section), each plate supported by a central rod, featuring a weir and downcomer to
create a liquid seal between stages. Vapours from the column's top pass through a
water-cooled coil-in-shell condenser (8), equipped with a pressure relief valve
(PRV1) for system protection. Condensate typically collects in a glass decanter (11),
bypassed during regular distillation experiments by opening valve (V10). When open,
condensate flows through the decanter to the solenoid-operated reflux ratio control
valve (12), directing it either back to the column's top or to the top product collecting
vessel (10) based on reflux timers.

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Temperature monitoring relies on fourteen thermocouple sensors (T1 to T14), while a
U-tube manometer (P1) indicates the total pressure drop across the column through
appropriate tapings fitted with isolating valves (V6) and (V7) as shown in figure 7.[9]

Figure 6: Distillation column Components.

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 Figure 7:Continuous Distillation Column Sheet.

Batch distillation
Simple batch distillation is consisting of: heat source to provide the energy
needed for vaporization in the distillation pot, round bottom flask contain the mixture
want to be distilled it, thermometer is essential for monitoring the temperature of the
system to provides information about the boiling points of the components being
distilled, Condenser is responsible for cooling the vapours and turning them back into
liquid form, cool water circulates around the condenser to facilitate condensation,
beaker to collect distillate sample.

The following figure shows what was described previously.

Figure 8: Simple Batch Distillation.

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Procedure
Continues Distillation
1- The feed solution was prepared by Eng.Maha 7 L methanol and 3 L water with
concentration equal 50% in boiler.
2- At total reflux, to reach steady state the power of boiler was set at 0.54 Kw.
3- The temperature from one to nine were taken (look at figure 7).
4- The distilled solution was collected in cylinder to measure the flow rate.
5- Measure ∆P from top and bottom of the system.
6- The previous steps were repeated by changing the reflux.

Simple Batch Distillation

In this experiment simple Batch Distillation was used to distil ethanol from an
ordinary binary mixture composed of two components ethanol and water as the
following steps:

1. The system was set up.

2. The mixture of 100 ml of ethanol and 100 ml of water was prepared in round
bottom flask.
3. The mixture was heated to 70 0C by the mantel heater.
4. Distilled samples were collected per time.
5. The volume was measured for the sample taken.
6. The density meter was used to measure density for each sample.

7
Sample of calculation and Results
Continuous distillation
From the following Txy Diagram at 1atm, the composition of methanol and water in
liquid or vapor phase were calculated.

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 Figure 9: Txy Diagram for methanol -Water.
X water=1−x ethanol

Y water =1−Y ethanol

The number of temperatures is related to a position in Figure 7.

To correct the error in calculating the temperatures in the sensors, 15 degrees Celsius
was added to all the observed temperatures, considering the heat lost in calculating all
the temperatures as a constant.

Table 1:Continues distillation Results.

Number Temperature Improved XM XW YM YW

(C) Temperature From From
diagram diagram
T1 62.7 75.7 0.394 0.606 0.735 0.265

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 T2 62.1 75.1 0.391 0.609 0.749 0.251
T3 62 75 0.41 0.59 0.751 0.249
T4 62 75 0.41 0.59 0.751 0.249
T5 62.5 75.5 0.4 0.6 0.742 0.258
T6 62.67 75.67 0.401 0.599 0.741 0.259
T7 63.7 76.7 0.35 0.65 0.708 0.292
T8 65.3 78.3 0.3 0.7 0.672 0.328
T9 62.7 75.7 0.39 0.61 0.735 0.265
T10 61.7 74.7 0.459 0.541 0.789 0.211
T11 22.2 35.2 1 0 1 0
T12 23.7 36.7 1 0 1 0
T13 25.1 38.1 1 0 1 0
T14 24 37 1 0 1 0

Heat duty= 0.54 KW

Pressure drop= 63

Condenser flow rate =0.63 m/s

To calculate the Condenser flow rate:

Q=mC P ∆ T

Q=0.1791× 4.18 × ( 78.3−75.7 )

Q=6.65 m/ s

The results showed that the mixture enters the distillation and is equal, and with
increasing steps, the proportions are affected by increasing the composition of water
and decreasing the composition of methanol until all the methanol reaches the top at
the condenser and all the water reaches the bottom at the reboiler in the ideal case.

Simple Batch distillation

By taking the first test sample with volume=10.5 ml, Density=0.857 g/cm3

at Temp=26 ℃

10
 g
ρWater at 25 ℃=0.997857 3
cm

g
ρethanol at 25℃=0.79 3
cm

V total=10.5+ 8.5+8+30.5+23.5+ 20.5+10.5+15=127 ml

Volume fraction(V A )=V A × V total

¿ 10.5 ×127=0.0827

mass fraction ( X A ) =ρ ×V A =0.857 ×0.0827

¿ 0.070854

mA 0.070854
y avg = = =0.00071
X A +mWater
0.070854+ (
100
0.997 g /ml )
m1=( V Water × ρWater ) + ( V ethanol × ρ ethanol )

¿ ( 100 ×0.997 )+ ( 100+0.79 ) =178.7 g

m2=Sample Volume ( ml ) × ρ
( c gm )=10.5 ×0.857=8.999
3

y avg =( m1−m2 )=(m1 × X 1)−(m2 × X 2 )

30 × X 2=1.407(experemantal)… .

Theoretical sample:

Since that m1=178.7g, m2=8.9985g (for the first sample)

ln (m1 /m2 )=ln ⁡¿

Take X1=0.7472, Y=0.7815 (from the equilibrium data for ethanol-water)

x1
ln ( )
m1
=∫
dX
m2 x 2 y −x
=−ln | y−x 1|+ln ⁡∨ y−x 2∨¿ ¿

−ln|Y −X 1|=¿=− ( ln ( 0.7815−0.7472 ) )=3.373

2.9887=3.373+ln (0.7815− X 2)

By solving the equation for X2

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X 2 =0.10034 (theoretical)
Table 2: Result for theoretical calculation.

xEtoh yEtoh 1/y-x

0 0 #DIV/0!
0.019 0.17 6.622516556
0.0721 0.3891 3.154574132
0.099 0.4375 2.954209749
0.1238 0.4704 2.885170225
0.1661 0.5089 2.917152859
0.2337 0.5445 3.217503218
0.2608 0.558 3.36473755
0.3273 0.5826 3.916960439
0.3965 0.6122 4.636068614
0.5198 0.6599 7.137758744
0.5732 0.6841 9.017132552
0.6763 0.7385 16.07717042
0.7472 0.7815 29.15451895
0.8943 0.8943 #DIV/0!
1 1 #DIV/0!

x Vs. 1/(y-x)
30
25
20
1/(y-x)

15
10
5
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
x

Figure 10:X vs. 1/(Y-X)

The first distillate collected should be more concentrated than the second distillate
sample and the remaining samples will have a higher ethanol concentration than the
initial sample.

But here there are some errors in the results, mostly from mathematical operations, as
the values of X must range between 0 and 1.

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Discussion
Distillation is the technique of separating components in a mixture via
continuous heating and cooling. There are two major forms of distillations: batch
distillation and continuous distillation. The difference between batch and continuous
distillation is that the batch distillation is done in batch-wise whereas continuous
distillation is done as a continuous process.

Batch Distillation is good to produce high purity products, is capable of

separating multiple components, Ideal for small volume separation, good flexibility as
units can be modified to operate based on the different chemical compositions of each
batch, but the batch processes require more energy to operate than a continuous
process, higher risk of contamination between different batches if processing units are
not cleaned out ,not as good as continuous distillation for very high volume processes.
[10]

There are two main categories for condenser, differentiated by the extent of
condensation. In a total condenser, all the vapor leaving the top of the column is
condensed. Consequently, the composition of the vapor leaving the top tray y1 is the
same as that of the liquid distillate product and reflux, XD.

In a partial condenser, the vapor is only partially liquefied. The liquid produced is
returned to the column as liquid, and a vapor product stream is removed. The
compositions of these three streams (V1, D, and R) are different. Normally, D
(composition YD) is in equilibrium with R (composition X D). A partial condenser
functions as an equilibrium separation stage, so columns with a partial condenser
effectively have an extra ideal stage.[11][12]

The difference between boiler and reboiler, A boiler is a device that converts a liquid
into vapor, typically found in a steam power plant. It consists of a furnace for burning
fuel, heat transfer surfaces, and a space for steam formation and collection. Some
boilers use fossil fuels or waste fuels, while others use a nuclear reactor for pressure-
driven steam generation. [13]

A reboiler is a heat exchanger used to generate vapor for distillation columns,

partially vaporizing liquid from the bottom tray using a shell-and-tube type. Heating

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mediums include condensing steam or commercial heat-transfer fluids. Boiling occurs
in tubes or the shell, depending on the reboiler type.[14]

Thermal and hydraulic analyses of reboilers are more complex than single-phase
exchangers, as they are mostly partial reboilers, vaporizing only part of the liquid in
the column base. Reboilers can be thermosiphon, forced circulation, or stab-in types,
depending on their use. They draw liquid through heat exchangers, pumps, or column
sides. In complex columns, side stream reboilers can be used, which draw liquid off a
tray, heat it, and return it to the same or similar tray.

The pressure effect, Inverse relationship between pressure and relative volatility when
pressure decreases, relative volatility increases, A directly proportional relationship
between pressure and reflux ratio, A directly proportional relationship between
pressure and the number of theoretical stages, When pressure decreases, reboiler and
condenser temperatures decrease directly proportional to the relationship between
pressure, dew, and bubble temperature, Decreasing pressure led to a decrease in
efficiency.

Conclusion
Both batch and continuous distillation methods effectively separated. Batch
distillation is suitable for smaller-scale operations with the ability to control
distillation parameters manually. Continuous distillation, on the other hand, is ideal
for large-scale operations due to its ability to maintain a steady state and produce
consistent results. The experiment demonstrated the principles of distillation and its
practical applications.

References
[1] Yan, C., et al., Application of retrofitted design and optimization framework based
on the exergy analysis to a crude oil distillation plant. Applied Thermal Engineering,
2019. 154: p. 637-649.

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[2] Wahyudi, R.B.S., Ngatelan, and Budi Setiyono., Design of Adaptive Internal
Control Model on Binary Distillation Column. 2019

[3] Geankoplis, C.J., A. Hersel, and D.H. Lepek, Transport Processes and Separation
Process Principles. 2018: Pearson Education.
[4] Matsoukas, T., Fundamentals of Chemical Engineering Thermodynamics. 2012:
Pearson Education.
[5] Sundmacher, K. and A. Kienle, Reactive Distillation: Status and Future
Directions. 2006: Wiley.
[6] McKinsey&Company. Vaccum distillation. 2014 Nov 16 2023]; Available from:
https://www.mckinseyenergyinsights.com/resources/refinery-reference-desk/
vacuum-distillation/.
[7] Sinnott, R.K., J.M. Coulson, and J.F. Richardson, Chemical Engineering Design.
2005: Elsevier Butterworth-Heinemann

[8] Guest EXP 2 batch distillation, pdfcoffee.com. Available at:

https://pdfcoffee.com/exp-2-batch-distillation-pdf-free.html (Accessed: 22 May
2024).

[9] AbuSafa, A., et al., Unit Operations 2 Lab Manual. An-Najah National University.

[10] Kiss, A.A., Advanced Distillation Technologies: Design, Control and

Applications. 2013: Wiley.

[11] McCabe, W.L., J.C. Smith, and P. Harriott, Unit Operations of Chemical
Engineering. 1993: McGraw-Hill.
[12] Foust, A.S., Principles of Unit Operations. 1980: Wiley.

[13] BRITANNICA, BOILER | Types, Applications, and Maintenance. 31 August

2021, BRITANNICA.
[14] Serth, R.W., Process Heat Transfer: Principles and Applications. 2007: Elsevier
Academic Press

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