Separation Operations, Reactions and Control Laboratory

Batch Distillation
Laboratory Guide

Ashley Michelle Santoro Duarte

Senior Chemical Engineering Student

Chemical and Environmental Engineering Department

National University of Colombia

Bogota, Colombia

2023

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Contents

1. Introduction ......................................................................................................................................................3
2. Methodology ....................................................................................................................................................3
3. Theoretical Framework ....................................................................................................................................4
3.1. Base concepts ...........................................................................................................................................4
3.2. Operation of a batch distillation unit .......................................................................................................5
3.2.1. Start-up of the column .....................................................................................................................5
Modes of operation ..................................................................................................................................7
3.2.2. .................................................................................................................................................................7
3.3. Energy requirements ..............................................................................................................................10
3.4. Simulation in Aspen Plus V10: Plots of variable profiles against time ...................................................11
4. Case Study ......................................................................................................................................................15
4.1. Problem statement .............................................................................................................................15
4.2. Objectives of the laboratory practice .................................................................................................15
4.3. Equipment Description .......................................................................................................................16
4.4. Preparation calculations .....................................................................................................................19
4.5. Materials and experimental procedure..............................................................................................23
4.6. Data acquisition ..................................................................................................................................26
4.7. Simulation in Aspen Plus V10.0 ..........................................................................................................28
5. References ......................................................................................................................................................36
Annexes ..................................................................................................................................................................38
A.1. Vapor-liquid equilibrium diagram ...............................................................................................................38
A.2. Simulation in Aspen Plus V10 ......................................................................................................................39

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 1. Introduction

As a senior Chemical Engineering student, I understand the importance of having access to

comprehensive laboratory guides that not only provide theoretical knowledge but also encourage the
acquisition of different practical skills. With that in mind, the Batch Distillation Laboratory Guide was
developed to equip undergraduate Chemical Engineering students with the necessary tools to operate
a batch distillation unit effectively. This unit operation is widely used at a low production scale for
separating two or more components in liquid phases through heating and vaporizing a mixture and
subsequently condensing and collecting the produced vapor. In this guide, students can find a proposed
methodology to address an experimental study of a batch distillation process. Such guide consists of six
main blocks, including an overview of the theoretical framework of batch distillation, a practical case
study, the description of the available equipment at the Chemical Engineering Laboratory at the
National University of Colombia in Bogota, detailed experimental procedures, data acquisition, and
further calculations.

By following this methodology, students can develop a deeper understanding of batch distillation
principles and practical skills that can be applied in the laboratory, which certainly will come handy in
future engineering projects. Last but not least, upon the completion of the laboratory practice proposed
in this guide, students will gain a sense of confidence in operating a pilot plant unit, which will
undoubtedly instill a sense of confidence in their knowledge and capabilities as future chemical
engineers.

2. Methodology

The guide proposes two steps to fulfill the objective of providing students with the theoretical and
practical knowledge to operate a batch distillation unit. Firstly, it is encouraged to review the theoretical
framework presented in the guide and then, it is suggested to proceed reading the case study, as
explained below.

1. Theoretical Framework (section 3): A theoretical framework on the principles of batch distillation
is provided. This includes a description of the base concepts (section 3.1.), startup of the column
(section 3.2.1.), ways of operating the column (section 3.2.2.), energy requirements for the
separation (section 3.3.) and the simulation of an example in Aspen Plus V10 (section 3.4.).
2. Case Study (Section 4): The laboratory guide proposes a case study involving the distillation of an
ethanol-water solution. This case study will be intended to be executed at the chemical engineering
laboratory facilities. The case study introduces a problem statement (section 4.1.), proposes a
series of objectives for the laboratory practice (section 4.2.), describes the batch distillation setup
available in the chemical engineering lab at the university (section 4.3.), presents the required pre-
laboratory calculations (section 4.4.), describes the materials and experimental procedure (section
4.5.), and finally provides a guide for the tables where data will be registered (section 4.6.).

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 3. Theoretical Framework

3.1. Base concepts

Distillation is a physical process used to separate liquid mixtures of two or more components by
exploiting differences of relative volatilities among them; by heating the liquid up to its bubble point,
the more volatile components evaporate and they are condensed separately to achieve a certain
degree of splitting. Since the maximum separation is determined by the vapor-liquid equilibrium, it is
necessary to carry out several separation stages under countercurrent contact between vapors and
liquids of different concentrations to enable a higher degree of purification. Exploiting the difference
of densities between the gas and the liquid phases (i.e. buoyancy forces), the countercurrent contact
stages can be arranged vertically within a tube called distillation column. The vapor-liquid contact could
also be promoted by centrifugal forces instead; thus, the separation could be arranged within a
centrifugal or rotary distillation drum. The last is less common because the high energy required to
operate the rotating device.

In the case of a distillation column, the contact stages are called trays. In such trays, a rising vapor
interacts with an accumulated amount of liquid that flows downwards. The vapor is produced from the
bottom stage of the column called reboiler, and it continues rising up through the different stages
interchanging energy and mass with the accumulated liquid, being enriched in the more volatile
components. Once this vapor reaches the top trays of the column, it is removed and condensed. One
fraction of this liquid is removed as product or distillate, and the remaining is sent back to the column
(i.e., reflux stream) to fill the trays and to promote the countercurrent contact. Finally, the liquid
reaches the bottom trays of the column being enriched in the less volatile components. There, a fraction
is removed as bottom’s product, and the remaining is boiled up to generate the operating vapor of the
column (Apostolou, n.d.; Doherty et al., 2019). This operation can be implemented in a batch or
continuous manner, and this mainly depends on the intended operating flowrates. Particularly, a batch
distillation unit is preferred over a continuous one when the mixture contains solids, tars, or resins that
could cause issues with a continuous unit. Furthermore, using a batch column can often be more
efficient in terms of purity than using several simple continuous distillation columns (Doherty et al.,
2019). Nonetheless, energy consumption is higher in such batch devices.

In the chemical industry, batch distillation is a commonly used method for purifying products after a
reaction process or to recover compounds from a separation train. The primary objective of industrial
batch distillation is to maximize production rate while maintaining purity and yield constraints and
under reduced energy consumption. Usually, one or more compounds are separated from a
multicomponent mixture, obtaining the intended product with the desired specifications either as a
distillate or as bottom stream (Doherty et al., 2019). In the case of a batch distillation, the operating
compositions and temperatures change with time. If the products are removed from the distillate, they
are removed as “cuts” at different times, and the composition of such cuts will depend on the operating

4
conditions (i.e., feed composition, pressure), the number of stages of the column, the reflux ratio, and
the heat duty.

A batch distillation column or batch rectifier consists of a pot or reboiler, a rectifying column, a
condenser, a device for accumulating and splitting off the condensed distillate for reflux, and one or
more product receivers (see Figure 1). The temperature of the distillate is controlled near the bubble
point, and the reflux is returned at or near the upper column temperature to improve column operation
(Doherty et al., 2019).

Figure 1. Schematic of a batch rectifier. Taken from Doherty et al., 2019.

3.2. Operation of a batch distillation unit

3.2.1. Start-up of the column

During operation, the start-up consists of charging and heating a batch of liquid in the pot and achieving
a steady state under a total reflux. Heating is carried out slowly to avoid boiling the liquid too rapidly,
which can reduce the contact time between the liquid and vapor phases and thus, decreasing the
efficiency of the separation. Also, the condenser could be overflowed with gas and liquid, generating
and overpressure in the top and pushing fluid through the vent connection. After certain time under
total reflux operation, it is possible to determine whether steady state has been achieved by monitoring
the temperature and composition of the distillate; once they stabilize, it can be assumed that the whole
column has reached steady state and the distillation can proceed. After this stabilization period, the
column is operated according to the operating policy that must have been previously stablished, namely
constant reflux ratio with varying overhead composition, or constant overhead composition with
varying reflux (Doherty et al., 2019).

During start-up under total reflux, the behavior of the column resembles that of a simple batch
distillation or Rayleigh distillation. In that case, the batch distillation is carried out as a simple distillation
without fractionation trays or packing, and without reflux. Thus, the Rayleigh equation can be used to
predict the behavior of the batch distillation column during start-up. This equation was introduced by
Rayleigh in 1902 and is based on a differential material balance with respect of the more volatile

5
component (Eqs. 1 and 2). Considering the control volume of the whole column in Figure 1, it is possible
to describe the overall mass balance as in Equation 1

𝑑𝐻
𝐷̇ = − (1)
𝑑𝑡

Then, the corresponding material balance of component i is presented in Equation 2.

𝑑(𝐻𝑥)
−𝑥𝐷 𝐷̇ = (2)
𝑑𝑡

In these equations , 𝐷̇ (mol/min) is the molar flowrate of distillate exiting the column at time t (min),
𝑥𝐷 is the mole fraction of the more volatile component in the distillate, 𝐻 (mol) is the number of moles
of liquid in the pot at time t, and 𝑥 is the mole fraction of the more volatile component in the liquid
within the pot at time t. Replacing the overall in the component balance, the substitution and expansion
of the derivative term give:

−𝑥𝐷 𝑑𝐻 = 𝐻 𝑑𝑥 + 𝑥 𝑑𝐻 (3)

Finally, it is possible to rearrange and integrate the above expression as

𝐻𝑖 𝑥 𝑑𝑥
ln = ∫𝑥 𝑖 (4)
𝐻𝑓 𝑓 𝑥𝐷 −𝑥

Here, the subindexes i and f, denote the initial and final conditions in the pot during the batch
distillation, respectively. It is important to point out that, differently from traditional Raleigh equation
for a single stage batch distillation without reflux, the removed distillate and the liquid in the reboiler
are not related through phase equilibrium. In this case, 𝑥𝐷 is the mole fraction of the more volatile
component on the distillate which depends on the reflux ratio and the number of stages. Then, the
𝑑𝑥
expression 𝑥 in Equation 4 can be integrated graphically or numerically using tabulated equilibrium
𝐷 −𝑥

data or an equilibrium curve (Reilly, 2010; Doherty et al., 2019), the operating line of the column and
the corresponding number of stages. Thereafter, using Equation 4, it would be possible to calculate the
total moles of liquid remaining in the still (𝐻𝑓 ) for a given target composition in the bottom’s product
(𝑥𝑓 ). Now, neglecting hold-up, the difference between the initial and final number of moles would

enable to determine the accumulated mass of distillate (𝐷 ) during the entire batch operation, and the
corresponding average composition (𝑥𝐷,𝑎𝑣𝑔 ) with Equations 5 and 6.

𝐷 = 𝐻𝑖 − 𝐻𝑓 (5)
𝐻𝑖 𝑥𝑖 −𝐻𝑓 𝑥𝑓
𝑥𝐷,𝑎𝑣𝑔 = (6)
𝐷

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The corresponding yield or recovery (𝑌) of the volatile component in the distillate can be obtained with
equation 7

𝐷𝑥𝐷,𝑎𝑣𝑔
𝑌 = 100 (7)
𝐻𝑖 𝑥𝑖

In section 4, it will be presented an example of the graphic integration for the ethanol-water batch
distillation under constant reflux in an existing column.

3.2.2. Modes of operation

Batch distillation columns can be operated in two different ways: constant reflux ratio with varying
overhead composition (see section 3.2.2.1), or constant overhead composition with varying reflux (see
section 3.2.2.2). The choice of operating method will largely depend on the desired purity of the
distillate, the heat sensitivity of the components of the mixture to be separated, and the available
equipment. Once the method of operation has been chosen, it is possible to estimate the time required
to carry out the desired separation (see Equations 8 and 9). Finally, it is possible to interconnect this
computed time with an energy balance, to determine the rate of heating and the vapor rate required
to complete the process (see Equations 10 and 11) (Wankat, 2017; Doherty et al., 2019; Diwekar, 2014).
Considering this, students can prepare and have an idea of the time required for the column to reach
steady state before conducting the laboratory practice, which can be beneficial for the execution of the
case study.

3.2.2.1. Constant reflux ratio, varying overhead composition

In this mode of operation, the reflux ratio is set at a predetermined value and maintained constant
throughout the run. Both the pot liquid composition and the distillate composition change over time:
the liquid inside the reboiler becomes poorer in the lighter component while the distillate becomes
richer in it (see Figure 2). In this case, distillation is continued until the average distillate composition
reaches the desired value (Doherty et al., 2014).

Figure 2. Variation in distillate and reboiler compositions with the amount of distilled in binary batch
distillation at a constant reflux ratio. Taken from Doherty et al., 2019.

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To determine the time required to carry out the desired separation, Block (1961) developed an equation
based on the work of Smoker and Rose (1940) assuming a constant rate of vaporization and negligible
hold up in the column:

𝐻𝑖 (𝑒 𝜉 −1)
𝑡 = (𝑅 + 1) (8)
𝑉𝑒 𝜉
Where:
𝑡= time (h)
𝑅= reflux ratio
𝐻𝑖 = initial amount of liquid charged to the pot (moles)
𝑉= vaporization rate (mol/h)

Additionally, the symbol 𝜉 in Equation 8 represents the integral on the right side of Equation 4 (Smoker
and Rose, 1940):

𝐻 𝑥 𝑑𝑥𝑝
𝜉 = ln 𝐻 𝑖 = ∫𝑥 𝑝𝑖 𝑥 −𝑥 (9)
𝑓 𝑝𝑓 𝐷 𝑝

Similar to equation 6, it is possible to determine the average or accumulated distillate composition,

𝑥𝐷,𝑎𝑣𝑔 , by means of an overall material balance on the light component in the bottoms:

𝐻𝑖 𝑥𝑝𝑖 −𝐻𝑓 𝑥𝑝𝑓

𝑥𝐷,𝑎𝑣𝑔 = (10)
𝐻𝑖 −𝐻𝑓

Where:
𝐻= liquid in the pot (moles)
𝑥𝑝 = mole fraction of the more volatile component from the liquid in the pot
*Note: the subindexes i and f, denote the initial and final conditions, respectively.

To determine the time necessary to achieve the desired distillate composition, an iterative calculation
is required, as depicted in Figure 3. The process commences by drawing several operating lines with a
slope equivalent to L/V on the vapor-liquid equilibrium diagram at the established working pressure.
The point of interest is the composition at the 45° intersection, and after locating it, a specific number
of stages must be traversed to obtain the pot composition. By employing these composition pairs, the
integral on the right-hand side of Eq. 4 can be calculated, and subsequently 𝐻𝑓 can be determined.
Using Eq. 10 and the iterative procedure, 𝑥𝐷,𝑎𝑣𝑔 can be obtained. Once all the terms in Eq. 8 are known,
the time required for separation can be computed.

8
 Figure 3. Procedure to determine distillation time (𝑡) during an operation with constant reflux

3.2.2.2. Constant overhead composition, varying reflux

In this case the goal is to maintain a constant overhead composition. For binary mixtures, the amount
of reflux returned to the column must be constantly increased throughout the run to achieve such
condition. As time proceeds, the pot is gradually depleted of the lighter component, so the increase in
reflux is typically gradual at first and more rapid near the end of a cut. Finally, a point is reached at
which there is little of the lighter component remaining in the pot, and the reflux ratio has attained a
very high value. The receivers are then changed, the reflux is reduced, and an intermediate cut is taken
as before. This technique can also be extended to multicomponent mixtures (Doherty et al., 2014). To
determine the time required to carry out the desired separation, Bogart (1937) developed an equation
assuming that the column holdup is negligible and a constant vaporization rate:

𝐻𝑖 (𝑥𝐷 −𝑥𝑝𝑖 ) 𝑥𝑝𝑖 𝑑𝑥𝑝

𝑡= ∫𝑥 (11)
𝑉 𝑝𝑓 (1−𝐿/𝑉)(𝑥𝐷 −𝑥𝑝 )2

Where:
𝐻= liquid in the pot (moles)
𝑥𝑝 = mole fraction of the more volatile component from the liquid in the pot
𝑥𝐷 = mole fraction of the more volatile component in the distillate (see Figure 1)
𝑡= time (h)
𝑅= reflux ratio
𝑉= vaporization rate (mol/h)
𝐿 = liquid flow rate (mol/h)
*Note: the subindexes i and f, denote the initial and final conditions, respectively.

In this case, operating lines with varying slopes (i.e., L/V) are drawn from the known distillate
composition and the given number of stages is stepped off to find the corresponding bottoms
composition (Doherty et al., 2019) (see Figure 4). On the other hand, the quantity of distillate can be
found by material balance, and is given by:

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 𝐻𝑖 (𝑥𝑝𝑖 −𝑥𝑝𝑓 )
𝐻𝑖 − 𝐻𝑓 = (12)
𝑥𝐷 −𝑥𝑝𝑓

Figure 4. Procedure to determine distillation time (𝜃) and quantity of distillate (𝐻𝑖 − 𝐻𝑓 ) for an
operation with variable reflux

3.3. Energy requirements

It is possible to determine the theoretical amount of heating energy required to achieve the desired
separation by means of an energy balance between the heating vapor and the mixture to be distilled
(see Equations 13 to 16):

𝑄𝑚𝑖𝑥 = 𝑄𝐻𝑉 (13)

Where:
𝑄𝑚𝑖𝑥 = Energy received by the mixture (J)
𝑄𝐻𝑉 = Energy provided by the heating vapor (J)

Assuming ideal behavior of the mixture, the energy required to reach the bubble temperature plus the
energy required to vaporize the liquid is given by:

𝑄𝑚𝑖𝑥 = ∑𝑛𝑖=1 𝑚𝑖 (𝑐𝑝,𝑖 ∆𝑇 𝑖 + ∆𝐻𝑣𝑎𝑝,𝑖 ) (14)

Where:
𝑚𝑖 = mass of the component i in the mixture charged to the pot (kg)
𝐶𝑝,𝑖 = heat capacity of the component i in the mixture (J/kg K)
∆𝑇𝑖 = difference of the initial and bubble temperatures of the mixture (K)

For a subcooled charge of a binary mixture (n=2) that is heated up to the bubble point, it is possible to
rewrite equation 14 as follows:

𝑄𝑚𝑖𝑥 = (𝑚𝐶𝑝 ∆𝑇 + 𝑚∆𝐻𝑣𝑎𝑝 )𝐿𝐶 + (𝑚𝐶𝑝 ∆𝑇 + 𝑚∆𝐻𝑣𝑎𝑝 )𝐻𝐶 (15)

𝑄𝑚𝑖𝑥 = [𝑚𝐶𝑝 (𝑇𝐵𝑃 − 𝑇𝑖𝑛𝑖𝑡𝑖𝑎𝑙 ) + 𝑚∆𝐻𝑣𝑎𝑝 ]𝐿𝐶 + [𝑚𝐶𝑝 (𝑇𝐵𝑃 − 𝑇𝑖𝑛𝑖𝑡𝑖𝑎𝑙 ) + 𝑚∆𝐻𝑣𝑎𝑝 ]𝐻𝐶 (16)

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Where:
𝑚 = mass (kg)
𝐶𝑝 =heat capacity (J/kg K)
𝑇𝑖𝑛𝑖𝑡𝑖𝑎𝑙 = Initial temperature of the mixture charged to the pot
𝑇𝐵𝑃 = boiling point of the given component at the operating pressure (K)
∆𝐻𝑣𝑎𝑝 = heat of vaporization of the given component at the operating pressure (J/kg)
*Note: LC, lighter component; HC, heavier component.

This energy would be the required to vaporize all the liquid in the pot. However, as the column operates
under a certain reflux, part of the distilled liquid is recycled to the column and more energy is required
during operation. This energy could be estimated with equation 17, where V is the time-dependent
vapor flow rate from the reboiler.

𝑡
𝑄 = ∫0 𝑉∆𝐻𝑣𝑎𝑝 𝑑𝑡 (17)

3.4. Simulation in Aspen Plus V10: Plots of variable profiles against time

Instead of using a graphic method with the above-mentioned assumptions, the behavior of the batch
distillation column along time can be precited by mean of a rigorous simulation. In this case, it is possible
to solve the MESH equations (Mass balance, phase Equilibrium, Summation of compositions and Energy
balance) in a dynamic mode using a commercial software such as Aspen Plus. Despite it has been
designed mostly for continuous processes, Aspen Plus has also incorporated in their simulation
environment different modules for batch processes where the block BatchSep can be found. In order
to explain how to use the batchSep module, the step-by-step procedure for a specific simulation is here
presented. For verification, the module will be used to solve example 13.9 from Seader, Henley, and
Roper’s textbook, Separation Process Principles, 3rd Edition. The problem statement and the profiles
obtained with the simulator will be described in this section. The step-by-step procedure is presented
in Annex 2 (see section A.2. at the end of the document).

The problem states that it is needed to distill 100 lbmol of 25 mol% benzene, 50 mol%
monochlorobenzene (MCB), and 25 mol% ortho-dichlorobenzene (DCB) in a batch rectifier. The rectifier
consists of a reboiler, 10 equilibrium stages in the column, a reflux drum, and a distillate product
accumulator. The condenser-reflux drum holdup is 0.20 ft3 and each stage in the column has a liquid
holdup of 0.02 ft3. Pressures are 17.5 psia in the reboiler and 14.7 psia in the reflux drum, with a linear
profile in the column from 15.6 psia at the top to 17 psia at the bottom. Following initialization at total
reflux, the batch is distilled with a vapor boil-up rate of 200 lbmol/h and a reflux ratio of 3. Thus, the
distillate rate is 50 lbmol/h. It is requested to determine the amounts and compositions of the
accumulated distillate at the point when the mole fraction of benzene in the instantaneous distillate
drops below 0.1. Additionally, it is desired to visually inspect the profiles of variables against time.

11
Once the simulation has been completed, it is possible to generate different plots that evidence the
change in several variables with time, namely: pot temperature, pot pressure, pot composition, receiver
composition, pot holdup, receiver holdup, and pot duty. Additionally, it is possible to generate a
temperature profile, pressure profile and composition profile. Some of these graphics are presented
below, so the behavior of different variables during the operation of the column can be observed, both
at total reflux (first half hour of operation) and at the operation reflux (see Figures 5 -11). For instance,
in Figure 5 it is presented the pot temperature variations with time during the operation of the batch
column. During the startup, the pot temperature will initially rise due to the heating of the reboiler.
Once the batch is fully heated and reaches total reflux, the pot temperature will stabilize at the bubble
point of the mixture. During normal operation, the pot temperature will gradually increase as the
mixture is distilled and the composition of the remaining liquid changes. The pot temperature will reach
its maximum value at the end of the batch distillation when there is very little liquid left in the column.

155
150
Pot temperature (°C)

145
140
135
130
125
120
115
110
0 0.2 0.4 0.6 0.8 1 1.2

Time (hr)
Figure 5. Pot temperature variations against time during the operation of the batch column

Figure 6 shows that during the startup, the mole fraction of all three components in the pot remain
constant due to the total reflux condition. However, as the batch distillation progresses, the more
volatile components, which are benzene and MCB, preferentially evaporate and their mole fraction in
the pot decreases. Meanwhile, the less volatile component, DCB, remain in the pot, leading to an
increase in its mole fraction.

0.6
Mole fraction (liquid phase)

0.5

0.4

0.3
Benzene
0.2 MCB
DCB
0.1

0
0 0.2 0.4 0.6 0.8 1 1.2
Time (hr)

Figure 6. Pot mole fraction of benzene, monochlorobenzene (MCB), ortho-dichlorobenzene (DCB)

against time during the operation of the batch column

12
Figure 7 presents the concentration of each component in the distillate over time during the batch
distillation. Benzene is the most volatile component and its mole fraction in the distillate increases
rapidly until it reaches a maximum. MCB and DCB have lower volatilities and their mole fractions in the
distillate remain close to zero throughout most of the operation. Near the end of the distillation, the
mole fraction of MCB starts to increase, while the concentration of benzene begins to decrease. This is
attributed to the fact that most of the initial benzene has already been distilled off the system.

1
Mole fraction (liquid phase)

0.9
0.8
0.7
0.6 Benzene
0.5 MCB
DCB
0.4
0.3
0.2
0.1
0
0 0.2 0.4 0.6 0.8 1 1.2
Time (hr)
Figure 7. Variation of the composition in the distillate receiver (mole fraction) against time during the
operation of the batch column. (MCB) monochlorobenzene; (DCB) ortho-dichlorobenzene

Figure 8 shows the variation of the total moles of liquid in the pot over time during the batch distillation.
At the beginning of the distillation, the total moles of liquid in the pot are at their maximum value. As
the distillation proceeds, the total moles of liquid in the pot decrease due to the separation of the more
volatile components. The rate of decrease slows down as the distillation progresses, and eventually
reaches a minimum value at the end of the operation. The final total moles of liquid in the pot depend
on the degree of separation achieved during the distillation and the amount of each component that
remains in the pot at the end of the operation.

50
Pot liquid moles (kmol)

45

40

35

30

25
0 0.2 0.4 0.6 0.8 1 1.2
Time (hr)

Figure 8. Pot content (by mole) against time during the operation of the batch column

13
Figure 9 presents the variation of the pot heat duty during the operation of the batch column. As
observed, there is a quick decrease during the startup, reaching a minimum and then remaining
constant. After reaching a desired temperature, the heat duty remains constant at this lower heat input.
During the normal operation phase, there is a small increase in the heat duty, which could be attributed
to the decrease in reflux, leading to an increase in concentration of heavy compounds in the pot and of
the corresponding operating temperature. Besides the heat of vaporization of the bottom’s liquid
changes, becoming closer to that of the heavy components. This increase is followed by a decrease as
the more volatile component is removed from the system.

270

260
Pot duty (kcal/s)

250

240

230

220

210
0 0.2 0.4 0.6 0.8 1 1.2
Time (hr)

Figure 9. Pot duty (heat input to the reboiler) variation against time during the operation of the batch
column

In Figure 10, the operating temperature profile along the column stages is presented. As expected, the
temperature at the bottom of the column is the highest and gradually decreases towards the top.
During the operation, the temperature profile changes, with the greatest changes happening in the pot.
This is due to the changes in the composition of the mixture being separated and the changes in the
heat input.

155

150
Temperature (°C)

145

140

135

130

125

120
1 2 3 4 5 6 7 8 9 10 11
Stage number

Figure 10. Temperature profile across the column.

14
Figure 11 presents the composition profiles along the column at the beginning of the operation. As
benzene is the most volatile component, it is mostly removed from the pot and accumulates within the
top stages of the column. At the same time, being the intermediate component, MCB is present in
most stages of the fractionation column, but it diminishes near the top of the column. In contrast, as
DBC is the least volatile component, it is absent from most of the stages of the column. However, it
begins to appear towards the 7th plate and continues to increase towards the bottom of the column.

1
0.9
Mole fraction (liquid phase)

0.8
0.7
0.6 Benzene

0.5 MCB

0.4 DCB

0.3
0.2
0.1
0
1 2 3 4 5 6 7 8 9 10 11
Stage number

Figure 11. Mole fractions (liquid) profile across the column. (MCB) monochlorobenzene. (DCB) ortho-
dichlorobenzene

4. Case Study

In this section, a case study will be presented and it intends to elaborate on a real-life engineering
problem. The case study will be described in detail, including the problem statement, objectives,
equipment description, pre-laboratory calculations, materials and experimental procedure, and data
acquisition tables.

4.1. Problem statement

It is desired to distill 48 L of an ethanol-water solution with an initial concentration of 30% v/v ethanol
to obtain a distillate with a higher average concentration of ethanol. The system operates at 74.5 kPa
(average atmospheric pressure in Bogotá) and the initial load to the still pot is made at room
temperature (average temperature in Bogotá: 20 °C). The batch-operated column is equipped with 20
trays, a reboiler and a total condenser. For further information regarding the available equipment at
the pilot plant, see Section 4.3.

4.2. Objectives of the laboratory practice

The general objective of this laboratory session is to distill a solution that contains 30% v/v ethanol and
70% v/v water to obtain a distillate with a higher concentration of ethanol. It is known that the available

15
equipment can distill ethanol-water solutions reaching a distillate composition up to 96% v/v.
Nevertheless, the student must determine the distillate composition they desire to obtain considering
the time limitation (2-3 hours reducing setting up and shut down) in this laboratory practice.

The specific objectives are as follows:

− To determine the distillate composition to be achieved and the operating conditions required to
accomplish the desired separation (see Section 4.4.).
− To start-up and operate a batch column and generate relevant plots to determine when conditions
have stabilized. It is suggested to generate temperature vs time diagrams for the vapor at the top
of the column and the liquid in the reboiler.
− To generate a composition (% alcohol by mole) vs time diagram to monitor the separation and
assess the product purity.
− To determine the overall column mass efficiency by comparing the theoretical number of stages
required for the achieved separation to the actual number of stages present in the equipment.
− To determine the energetic efficiency of the distillation process by comparing the theoretical
amount of heat required for the separation to the actual amount of heat used in the experiments.
− To simulate the process in Aspen Plus V10.0 and compare the profiles (temperature, composition,
etc.) obtained by the software with those obtained from the pilot scale experiment.

4.3. Equipment Description

The batch distillation unit utilized in the pilot plant comprises three primary pieces of equipment,
namely, a reboiler, a rectification column, and a condenser (see Figure 12). Based on a previous guide
(Antolines, et al., 2003), a brief description of these components, as well as the relevant valves,
pressure, and temperature indicators, is provided below.

16
 Figure 12. Diagram of the batch distillation unit at the pilot plant in the Chemical Engineering
Laboratory.

4.3.1. Reboiler
The reboiler is a cylindrical copper tank of 0.6 m in diameter and 0.65 m in height, with a maximum
capacity of 120 L. It is recommended to feed loads above 40 L to submerge the heating coil. The tank
has a hemispherical bottom, and it is equipped with an external sight glass tube that serves as a level
indicator. The tank is thermally insulated using glass wool and tarpaulin to prevent heat loss. To initiate
the distillation process, the problem mixture is introduced in the reboiler through a screwed cap, and
heat duty is provided using a steam stream that flows through a coil located inside the tank at the
bottom part. The steam enters the tank through a thermally insulated pipe, which is equipped with a
manually controlled globe valve, a pressure gauge, and a safety valve. The condensate is removed via a
pipeline with a steam trap, and it can be collected to track the mass flowrate of the heating fluid and
the heat duty in the reboiler. Also a manometer is located in the upper part of the reboiler, which
indicates the internal pressure in the tank during operation. In the lower part of the reboiler there is a
drainage valve that is used to evacuate the contents of the tank at the end of the experiment.

17
 4.3.2. Rectification column
The plate column utilized in this study has a diameter of 26 cm and a height of 4.66 m with an elevation
of 1.80 m above ground level. It is comprised of four sections, with three sections measuring 0.30 m in
height and the fourth section measuring 1.20 m in height. The column contains a total of 20 plates, with
each section containing five plates that are spaced 15.40 cm apart. Each plate features a valve for
sample collection. On the other hand, the top plate features an outlet for the vapors generated within
the column and an inlet for the liquid which is used as reflux. At a distance of 0.45 m from the base of
the tower, a level indicator tube and a thermometer (ranging from 0 °C to 50 °C) are installed. Another
thermometer (ranging from 0 °C to 300 °C) is located at the top of the column. The plates themselves
have a diameter of 20 cm and are fitted with three bubbling caps. The height of the weir is 4.96 cm, the
diameter of the downpipe is 2.95 cm, and the maximum liquid level in each plate is 2.47 cm.

4.3.3. Condenser
The condenser is located at the top of the distillation column and comprises a vertical copper shell and
tube heat exchanger. It uses a 1-1 countercurrent flow configuration, with the cooling water flowing
through the shell and the vapor from the column passing through the tubes in the opposite direction.
The condenser has a single pass in both the shell and the tubes. The water inlet valve is located at the
bottom of the condenser.

4.3.4. Steam Trap

The steam trap is located in the line that exits from the bottom of the boiler and it is an inverted cup
trap that directs the passage of condensed steam to a pipe. The pipe terminates in a collection vessel
that is placed on a scale to determine the steam consumption throughout the practice.

4.3.5. Dial Pressure Gauge

The unit is equipped with two Dial Pressure Gauges, each capable of measuring pressure within the
range of 0 to 10 psig. The first gauge registers the pressure of the steam at the boiler inlet, while the
second gauge registers the pressure inside the boiler.

4.3.6. Dial Thermometer and thermocouples

There is one dial thermometer situated at the bottom of the reboiler, connected to the line that leads
the condensed steam. Along the column there are thermocouples that allow to register the
temperature in each plate and these values can be observed in a display unit.

4.3.7. Valves
The batch distillation unit features a total of 38 valves, including 18 operating valves for the
processing steams and 20 valves destined to samples withdrawal from the plates. The valves serve
several functions, such as:
− Water inlet for boiler flushing
− Boiler drainage

18
 − Outlet for the boiler residue
− Column drain
− Boiler drain
− Passage of steam from the column to the condenser
− Inlet of steam to the condenser from the reboiler
− Exit of distillate from the condenser
− Reflux to the column
− Feed to the column
− Passage of liquid from the column to the reboiler
− Inlet of steam to the reboiler
− Exit of steam from the reboiler
− Boiler load level
− Tower load level
− Controlling the water inlet to the condenser

4.4. Preparation calculations

Before conducting the laboratory experiment, certain decisions and calculations should be performed
to determine the required operating conditions of the batch distillation column. In order to facilitate
the task of choosing the purity of the solution obtained as distillate, an example of calculations will be
presented, selecting a distillate purity of 96% v/v. Initially, it is necessary to establish the mode of
operation of the column according to the specific requirements of the process, the minimum and the
operating reflux ratio, the operating procedure for the case of varying reflux, and the time required for
the separation. In this example, it is intended to obtain a product with an average concentration of 96%
v/v ethanol, and the column will be operated with a constant reflux, which implies a varying distillate
composition. Using a constant reflux ratio enables to maintain a relatively stable distillate composition
over time, which is important in ensuring that the desired purity of 96% v/v ethanol is achieved.
Additionally, a constant reflux ratio is relatively easy to control and monitor, making it a suitable choice
for students who may not have extensive experience with distillation or that do not want to deal with
the variation of the reflux along the distillation time.

19
 Figure 13. Vapor-liquid equilibrium curve for the ethanol-water system at 74.5 kPa. Retrieved from
Aspen Plus V10.0.

Now, considering the selected reflux policy, it is necessary to determine which reflux ratio will be used
during operation. For this purpose, firstly the minimum reflux ratio is computed and then, the actual
reflux ratio is determined as a multiple of this value. It is possible to compute the minimum internal
reflux ratio using the equilibrium curve for the ethanol-water system at 74.5 hPa (see Figure 13) by
determining the slope of the tangent line to the inflection point of the equilibrium curve (see Equations
18 and 19). In the other cases where the equilibrium curve does not have an inflection point, the
minimum reflux ratio corresponds to the slope of the operating line that is formed by connecting the
charge composition to the product composition (Doherty et al., 2019).

𝐿 𝑦𝐷 −𝑦𝑃
(𝑉) = (18)
𝑚𝑖𝑛 𝑥𝐷 −𝑥𝑃

Where:
𝐿 = liquid flow rate (mol/h) (see Figure 1)
𝑉 = vapor rate (mol/h) (see Figure 1)
𝑦𝐷 = 𝑥𝐷 = desired distillate composition
𝑦𝑃 = composition of the vapor at point P (see Figure 4)
𝑥𝑃 = composition of the liquid at point P (see Figure 4)

(𝐿 ⁄𝑉 )𝑚𝑖𝑛
𝑅𝑚𝑖𝑛 = (19)
1−(𝐿 ⁄𝑉 )𝑚𝑖𝑛

20
Where:
𝑅𝑚𝑖𝑛 = minimum reflux ratio

By locating in the equilibrium diagram (Figure 13) the points corresponding to the desired distillate
composition (converted to molar fraction) and the point of inflection, “P” (𝑦𝐷 = 𝑥𝐷 = 0.857; 𝑥𝑃 =
0.800; 𝑦𝑃 = 0.821). Substituting these values in Equation 17:

𝐿 0.857 − 0.821
( ) = = 0.631
𝑉 𝑚𝑖𝑛 0.857 − 0.800

Thus, equation 18 yields:

0.631
𝑅𝑚𝑖𝑛 = = 1.710
1 − 0.631

In general, operating reflux can be 1.1 to 10 times the minimum reflux (Doherty et al., 2019). However,
in this case the operating reflux ratio was defined as 1.5 times the minimum:

𝑅 = 1.5𝑅𝑚𝑖𝑛 = 2.565

At this point, it is possible to determine the amount of moles of product obtained as distillate, the
composition of the pot residue, and time required for the distillation process. For this purpose, the
equations presented in section 3.2.2.1 are used. The initial charge of a 48 L ethanol-water solution that
contains 30% v/v ethanol corresponds to a charge of 2110 mol (𝐻𝑖 ) with 12 mol% ethanol (𝑥𝑝𝑖 ),
respectively. Moreover, the product specification of 96% v/v ethanol equals 85 mol% ethanol (𝑥𝐷,𝑎𝑣𝑔 ).
The vaporization rate (𝑉) can be determined using equation 20, by estimating an ethanol recovery of
95% and restricting the operation window to only 2 hours out of a total of 4 hours that students possess
to carry out the practice (see equation 21). Finally, as calculated above, the reflux ratio R=2.565,
corresponding to a L/V=0.719. The column section has 20 theoretical plates, and the pot provides an
additional one (i.e., 21 stages in total).

𝑉 = 𝐷(𝑅 + 1) (20)
Where:
𝑉 = vapor rate (mol/h)
𝐷 = distillate rate (mol/h)
𝑅 = operation reflux ratio

𝐸𝑡ℎ𝑎𝑛𝑜𝑙 𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑒𝑑 𝑖𝑛 𝑡ℎ𝑒 𝑑𝑖𝑠𝑡𝑖𝑙𝑙𝑎𝑡𝑒 (𝑚𝑜𝑙)

𝐷= (21)
𝑀𝑎𝑥𝑖𝑚𝑢𝑚 𝑜𝑝𝑒𝑟𝑎𝑡𝑖𝑜𝑛 𝑡𝑖𝑚𝑒 (ℎ)

In this case, equations 19 and 20 yield:

0.95 ∗ 2110 𝑚𝑜𝑙 ∗ 0.12 𝑚𝑜𝑙
𝑉= (2.565 + 1) = 428.76
2ℎ ℎ

21
Considering the above, the procedure begins with drawing several parallel operating lines at a slope
equivalent to L/V=0.719 in the vapor-liquid equilibrium diagram at 74.5 kPa (see Figure 14a). Then, as
the operating line crosses the diagonal when having a total condenser, it is required to locate the
changing composition of the distillate at the 45° line. Once this point is located, it is necessary to step
down the 21 stages of the laboratory Column (including the reboiler) to find the corresponding initial
value of the pot composition (see Figure 14b). Then, having the distillate and the corresponding pot
composition from the initial pot concentration to a given final one, it is possible to construct a plot of
1
vs. 𝑥𝑝 . This can be used for a graphical integration of the right-hand side of Eq. 4. Once
𝑥𝐷 −𝑥𝑝

integrated, 𝐻𝑓 is determined and finally, 𝑥𝐷,𝑎𝑣𝑔 is obtained from Eq. 6 and the iterative procedure
begins (see H).

a)

22
 b)
Figure 14. Graphical method for constant reflux operation. a) Drawing of parallel lines with a slope
equal to L/V. b) Process of stepping off the total number of stages. Pressure: 74.5 kPa. Retrieved from
Aspen Plus V10.0.

In this case, using the vapor-liquid equilibrium data for the ethanol-water system at 74.5 kPa and
integrating between 𝑥𝑝𝑖 = 0,12 and various lower limits, it is found that 𝑥𝐷,𝑎𝑣𝑔 = 0.85 when 𝑥𝑝𝑓 =
0.017. Then, the value of the integral presented in Eq. 5 is found to be 0.157 and 𝐻𝑓 = 1803 mol.
Finally, the product collected is given by 𝐻𝑖 − 𝐻𝑓 = 2110 − 1803 = 307 mol and the time required to
achieve the desired separation is given by:

2110 𝑚𝑜𝑙 (𝑒 0.157 − 1)

𝑡 = (2.6 + 1) = 2.6 ℎ
𝑚𝑜𝑙 0.157
428.8 ∗𝑒
ℎ

While this is a way to calculate the required time, another approach that could be used is to specify the
intended distillation time considering the available time for the experimental session.

4.5. Materials and experimental procedure

The materials and experimental procedure for batch distillation at the pilot plant is provided in this
section. It includes a start-up and stabilization procedure at total reflux, as well as a procedure for
establishing operating conditions and the end of operation. Two flowcharts are included to visually

23
illustrate these procedures (see Figures 15 and 16). The guidelines presented here are intended to help
ensure reliable and reproducible results for distillation experiments.

4.5.1. Materials

− 6 buckets of 10 liters each

− 3 1-liter graduated cylinders
− 1 stopwatch/timer
− 2 alcoholometers
− Funnel
− 16'' adjustable wrench
− 2 harnesses
− Water and ethanol solution of known composition

4.5.2. Experimental procedure

Block diagrams describing the experimental procedure to start, operate and shut down the batch distillation
column are presented in Figures 15 and 16.

24
Figure 15. Start-up and stabilization procedure for batch distillation at the pilot plant (total reflux).

25
 Figure 16. Procedure for stablishing operating conditions and end of operation

4.6. Data acquisition

It is recommended to plot at least 3 diagrams with the experimental data: a temperature vs time
diagram for vapor at the top of the column, a temperature vs time diagram for liquid in the reboiler,
and a composition of bottom and distillate (%mol alcohol) vs time diagram. With these plots it is
possible to determine when conditions have stabilized, and they allow to further analyze the
experimental data. Additionally, students must determine the energy required to achieve the desired
separation. An outline of the data acquisition procedure, as well as guideline data recording tables, are
presented below.

− Temperature vs Time diagram for Vapor at the Top of the Column and Temperature vs Time diagram
for Liquid in the Reboiler: The temperatures can be measured using the available thermometers
both in the still pot and at the top of the column. It is needed to record the temperature readings
at regular intervals of time and use them to generate the plots.
− Composition (%mol Alcohol) vs Time diagram: The composition of the distillate can be determined
using an alcoholometer or a calibrated refractometer. To generate the composition vs time plot,
students should record bottoms and distillate concentration readings at regular intervals of time
during the distillation process.
− Mass of distillate collected during the distillation operation: students will need to periodically
register the weight indicated in the scale that is below the distillate collection tank.

26
− Heating energy used to achieve the desired separation: students can determine the amount of
energy employed during the process considering the mass of condensed steam. Then, they can
compare it to the theoretical value obtained with an energy balance in the reboiler (see Section
3.3.). Additionally, students need to consider that the heat to the reboiler is maximized during the
initial heating of the mixture (Doherty et al., 2019) to reduce heating times, this is reflected in an
increase in the heating vapor pressure. After start-up, the heat duty to the reboiler is stablished at
a lower value according to safety specifications for the equipment. Given these considerations, the
calculations that students compute must reflect the change in pressure of the heating steam.
− Determination of reflux flow rate: in the laboratory, students will need to experimentally determine
the reflux flow rate. The reflux flow rate (Total reflux) can be determined by measuring the time it
takes to fill a container which dimensions are known, usually a probe, while the distillate flow rate
can be determined by measuring the volume of distillate collected in a given time. The tables
provided below provides students with the measurements they will need to take to accomplish this
purpose.

Table 1. Temperature vs time profiles for vapor at the top of the column and liquid in the reboiler.
Time Temperature (°C)
Measurement a
(min) 1 2b 3c 4d
1
2
3
4
5
6
7
8
9
10
a: reboiler.
b: top of the column.
c: water inlet to the condenser.
d: water outlet from the condenser.

Table 2. Composition vs time profile of bottoms and distillate (% alcohol by mole) during distillation
process.
Measurement Time (min)a Ethanol composition (%v/v) Ethanol composition (%mol)
1
2
3
4
5
6
7
8
9
10
11
12
Average

27
 Table 3. Mass of distillate collected during distillation operation

Measurement Time (min) Weight (kg)

0 (initial weight of the container) 0
1
2
3
4
5
6
7
8
9
10

Table 4. Measurements for Heating Energy Calculation during the start-up.

Measurement Value
Pressure of heating vapor (psig)
Weight of empty pot (kg)
Weight of pot with condensed heating vapor (kg)

Table 5. Measurements for Heating Energy Calculation during operation.

Measurement Value
Pressure of heating vapor (psig)
Weight of pot at the end of operation (kg)

Table 6. Experimental determination of reflux flow rate at total reflux.

Measurement Value
Initial height of liquid in the probe (cm)
Final height of liquid in the probe (cm)
Time (seconds)
Internal diameter of the probe (cm)

Table 7. Experimental determination of distillate flow rate during operation.

Measurement Dynamic state Steady state
Collected volume (L)
Time (seconds)

4.7. Simulation in Aspen Plus V10.0

In this section, we dive into the simulation of the case study using Aspen Plus. Building upon the
previous example presented in section 3.4., it is possible to keep exploring batch distillation principles.
Through Aspen Plus, it is possible to model the intricate interactions among multiple components and
analyze system behavior under different conditions. The images below provide a step-by-step
walkthrough of the simulation setup (see figures 17-25), and visual representation of the results (see
figures 26-31) for student’s reference.

28
Figure 17. Flowsheet for the case study batch distillation.

Figure 18. Setup of the block “STILL” (configuration tab).

29
Figure 19. Setup of the block “STILL” (streams tab).

30
 Figure 20. Setup of the block “STILL” (pressures & holdups tab).

Figure 21. Configuration of the heat transfer specifications of the block “STILL”.

31
Figure 22. Specification of the initial conditions for the block “STILL”.

Figure 23. Selection of efficiency method and type.

32
 Figure 24. Setup of step named STARTUP.

Figure 25. Setup of step named PRODUCT.

Once the simulation is run, the following plots can be obtained. It can be observed that the mole
fraction of the more volatile compound (ethanol) increases in the distillate as the distillation progresses,
reaching a maximum and then it slowly starts to decrease.

0.9
Mole fraction (liquid phase)

0.8

0.7

0.6

0.5
Ethanol
0.4
Water
0.3

0.2

0.1

0
0 0.5 1 1.5 2 2.5
Time (hr)

Figure 26. Distillate receiver mole fraction (ethanol and water) against time during the operation of
the batch column.

33
 108

Temperature (°C) 104

100

96

92
0 0.5 1 1.5 2 2.5
Time (hr)

Figure 27. Pot temperature against time during the operation of the batch column.

0.9
Mole fraction (liquid phase)

0.8

0.7

0.6

0.5
Ethanol
0.4
Water
0.3

0.2

0.1

0
0 0.5 1 1.5 2 2.5
Time (hr)

Figure 28. Pot mole fractions (ethanol and water) against time during the operation of the batch
column.

34
 1230

1220

Duty (cal/sec) 1210

1200

1190

1180

1170

1160

1150
0 0.5 1 1.5 2 2.5
Time (hr)

Figure 29. Pot duty against time during the operation of the batch column.

110

106

102

98
Temperature (°C)

94

90

86

82

78

74

70
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21
Stage

Figure 30. Temperature profile across the batch column.

35
 1
0.9

Mole fraction (liquid phase)

0.8
0.7
0.6
0.5
Ethanol
0.4
Water
0.3
0.2
0.1
0
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21
Stage

Figure 31. Composition profile (ethanol and water) across the batch column.

It is to be noted that this simulation can be complemented by students by computing the stage
efficiency, including it in the simulation and comparing the experimental profiles with the ones
generated by the software program. This efficiency can be determined by plotting the equilibrium curve
using the mole fractions registered when operating the tower at total reflux, finding out the theoretical
number of stages required to achieve the desired separation, and dividing it by the actual number of
stages present in the rectification tower:

𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑠𝑡𝑎𝑔𝑒𝑠

𝐸0 = (22)
𝐴𝑐𝑡𝑢𝑎𝑙 𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑠𝑡𝑎𝑔𝑒𝑠

5. References

Antolines, A., Guancha, M., Romero, D., Muñoz, A., Gonzalez, A., Arias, A. M., . . . Luengas, A. T.
(2003). Guía Destilación Intermitente. Bogota: Universidad Nacional de Colombia.
Apostolou, K. (n.d.). Experiment 9: Distillation – Finite Reflux. Retrieved February 19, 2023, from
PROCTECH 2EC3 Lab Manual:
https://ecampusontario.pressbooks.pub/proctech2ec3labmanual/chapter/experiment-9/
Block, B. (1961). Batch distillation of binary mixtures provides versatile process operations. 68(87).
Bogart, M. J. (1937). The design of equipment for fractional batch distillation. Trans. Am. Inst. Chem.
Eng., 33(139).
Diwekar, U. (2014). Batch Processes: Modeling and Design. Boca Raton, FL: Taylor & Francis Group.
Doherty, M. F., Fidkowski, Z. T., Malone, M. F., & Taylor, R. (2019). Section 13: Distillation. In D. Green,
& M. Southard, Perry's Chemical Engineers' Handbook, 9th Edition (pp. 13-92 to 13-99).
McGraw Hill.
Reilly, M. A. (2010). Batch Distillation Manual. In ChE 473A. Chemical Engineering Unit Operations
Laboratory Manual (pp. 1-29). Washington University in St. Louis.

36
Seader, J. D., Henley, E. J., & Roper, D. K. (2010). Separation Process Principles. John Wiley
Incorporated.
Smoker, E. H., & Rose, A. (1940). Graphic Determination of Batch Distillation Curves for Binary
Mixtures. Trans. Am. Inst. Chem. Engrs, 36(285).
Wankat, P. C. (2017). Separation Process Engineering: Includes Mass Transfer Analysis, 4th Edition.
Prentice Hall.

37
 Annexes

A.1. Vapor-liquid equilibrium diagram

0.95

0.9

0.85

0.8

0.75
y, vapor mole fraction (ethanol)

0.7

0.65

0.6

0.55

0.5

0.45

0.4

0.35

0.3

0.25

0.2

0.15

0.1

0.05

0
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

x, liquid mole fraction (ethanol)

Figure A.1.1. Vapor-liquid equilibrium curve for the ethanol-water system at 74.5 kPa.
Note. Retrieved from Aspen Plus V10.0.

38
 A.2. Simulation in Aspen Plus V10

Figure A.2.1. Selection of components in the initial mixture.

Figure A.2.2. Selection of thermodynamic method for calculations.

39
Figure A.2.3. Selection of equipment and addition of streams for the batch distillation.

Figure A.2.4. Setup of the block “BatchSep” (configuration tab).

40
 Figure A.2.5. Setup of the block “BatchSep” (streams tab).

Figure A.2.6. Setup of the block “BatchSep” (Pressure & holdups tab).

41
Figure A.2.7. Configuration of the heat transfer specifications of the block “BatchSep”.

Figure A.2.8. Definition of the initial conditions for the block “BatchSep”.

42
Figure A.2.9. Definition of the operating steps for the block “BatchSep”. Note. Step STARTUP stands for the
operation at total reflux, whereas PRODUCT stands for operation at the reflux previously defined in the
example.

Figure A.2.10. Setup of step STARTUP.

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 Figure A.2.11. Setup of step PRODUCT.

Figure A.2.12. Run of the simulation with available results. Note. At the upper right-side corner, it is possible to
find the icons that generate diverse plots (see Section 3.4.).

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