Momentum Transfer and Mechanical Operations Lab

Batch Distillation
30th September, 2024

Team: MTMO 2
Team Members: Aayush Bhakna (CH22B008), Deepanjhan Das (CH22B020), Atharva
Sunilkumar Ghodke (CH22B035), Anmol Upadhyay (CH22B053), Lakkireddy Vishnu
Vardhan Reddy (CH22B076)
Smail IDs: ch22b008@smail.iitm.ac.in, ch22b020@smail.iitm-.ac.in, ch22b035@smail-
.iitm.ac.in, ch22b053@smail.iitm.ac.in, ch22b076@smail.iitm.ac.in
Instructors: Dr. Abhijit Deshpande, Dr. Nitin Muralidharan, Dr. Sankha Karmakar,
Dr. Khushboo Suman
Department of Chemical Engineering, IIT Madras

1 Abstract with Graphics

Batch distillation (schematically shown in the following figures) is a common method used
in chemical engineering to separate liquid mixtures based on the differing volatilities of
their components. Unlike continuous distillation, batch distillation operates in discrete
cycles, with mixtures placed in a reboiler and heated until the most volatile components
vaporise. As the vapour rises through the distillation column, it is partially condensed
and collected as distillate.
In this batch distillation experiment, the objective was to validate Rayleigh’s Law and
determine the equilibrium line for a binary mixture of ethanol and water by analysing data
obtained during the distillation process. The experiment aimed to collect the distillate
and analyse its composition, comparing it with the residue left in the reboiler after a
significant portion of the mixture had been distilled.
The experiment involved charging a two-necked round bottom flask with a mixture of
200ml of water and 400ml of ethanol, gradually heating it, and collecting the distillate.
The temperature at which the first drop of distillate appeared was recorded as the dew
point, and the distillation continued until approximately three-fourths of the initial mix-
ture volume had been distilled. The refractive indices of the distillate and residue were

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measured to determine their ethanol concentrations. A calibration curve was created by

preparing mixtures of water and ethanol with varying volume fractions and measuring
their refractive indices. The experimental data was used to plot the equilibrium line and
verify Rayleigh’s equation, which describes the relationship between the amount of liquid
remaining in the reboiler and the composition of the distillate over time.
The results showed that the distillation process efficiently separated the components,
and the refractive index measurements accurately reflected the ethanol concentration
in the mixture. However, potential sources of error included parallax error in volume
measurements, leakage during sample collection, and thermo-couple calibration drift.

2 Aim & Objectives

• To obtain equilibrium data for ethanol-water from literature.

• To plot the volume calibration data and to use it for calculating volume fraction.
Rx
• To validate Rayleigh equation, ln( LL12 ) = x21 (y∗dx−x) .

3 Background and Motivation

Batch distillation (figure 2) is a crucial separation process widely used in industries such
as pharmaceuticals, petrochemicals, and fine chemicals, particularly for small-scale or

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flexible production. Unlike continuous distillation, batch distillation operates in discrete

cycles, making it ideal for processes where feed composition changes between batches or
where high-purity products are required. The process separates components of a liquid
mixture based on differences in their boiling points, with the more volatile components
vaporizing first and being collected as distillate, while the less volatile components remain
in the liquid phase.
The Rayleigh equation, which describes the relationship between the vapor and liquid
compositions in ideal binary mixtures, plays a vital role in understanding and controlling
the batch distillation process. It helps predict how the composition of the liquid and
vapor phases evolve during distillation, providing a theoretical basis for optimizing the
separation.

Figure 2: Overall Representation of the workflow of Batch Distillation

The motivation for studying batch distillation lies in its broad industrial applications
and its potential for improving product purity, reducing energy consumption, and mini-
mizing waste. As demand grows for more efficient and sustainable separation techniques,
understanding the fundamental principles of batch distillation becomes increasingly im-
portant. This experiment provides an opportunity to explore these principles in practice,
offering insights into the design, operation, and optimization of batch distillation systems
for real-world applications. By mastering this process, one can make informed decisions
about the best separation method for specific industrial needs, enhancing both economic
and environmental sustainability.

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4 Materials and Methods

4.1 Apparatus & Materials Required
• Materials: Water (with ethanol as a mixture and also used as cooling Water Inlet
and Outlet), Ethanol.

• Apparatus: Still (Distillation Flask), Electric Heater, Condenser, Thermometer,

Condenser Receiver, Rubber Tubing, Funnel, tand with Clamps.

4.2 Experimental Setup Description

The experimental setup is shown in the figure 3.

Figure 3: Experimental Set-up of the Batch Distillation Experiment

• Distillation Flask Setup: The still flask containing the liquid mixture to be
distilled is placed on the electric heater.

• Thermometer Placement: The thermometer is placed at the neck of the still

flask to measure the vapor temperature.

• Condenser Attachment: The condenser is connected to the vapor outlet of the

still flask. Coolant water flows through the condenser’s jacket from the inlet to the
outlet.

• Distillate Collection: The condensed vapor (now liquid) flows into the condenser
receiver flask.

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• Heating: The electric heater (shown in figure 4) is turned on to gradually heat the
liquid mixture in the still flask until it starts boiling and producing vapor.

• Cooling Water Flow: Water is circulated through the condenser to cool and
condense the vapor into liquid distillate.

• Collection of Distillate: The distilled liquid is collected in the receiver flask, and
the process is monitored and controlled using the thermometer readings.

This setup ensures that the vapor is condensed back into a liquid efficiently and that
the distillation process is conducted safely.

Figure 4: Heater and Thermometer in the Experimental Set-up

4.3 Procedure
• Pour 300 mL of water and 300 mL of ethanol into a beaker and mix thoroughly
using a glass rod. Transfer the ethanol-water solution into a three-necked round
bottom flask. Ensure the condenser is set up with running water flowing through
it.

• Gradually increase the temperature of the heating mantle, monitoring the mixture’s
temperature using a thermo-couple.

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• As the temperature rises, the mixture will begin to vaporize. The first drop of
distillate will appear, with the temperature recorded at the dew point.

• Continue the distillation process, collecting the distillate in the receiving flask until
approximately three-quarters of the original solution volume has been distilled.

• Allow the distillate and the remaining residue to cool to room temperature. Once
cooled, measure the density and volume of each.

• Use a densitometer to accurately determine the density of the collected distillate.

• Prepare mixtures of water and ethanol with ethanol volume fractions of 0, 0.2, 0.4,
0.6, 0.8, and 1, each having a total volume of 10 mL.

• Measure the density of each prepared mixture to create a calibration curve, which
will be used to analyze the composition of both the distillate and the residue.

5 Observation Tables
The tabulations include the observed data of the experiments and are tabulated in the
following table 1;

Volume of Volume of Volume Fraction

Density of mixture (g/cm3 )
Ethanol (mL) Water (mL) of Ethanol
10 0 1.0 0.784
8 2 0.8 0.844
6 4 0.6 0.900
4 6 0.4 0.936
2 8 0.2 0.995
0 10 0.0 0.997

Table 1: Volume Calibration data for Ethanol-Water mixture

Rest of the important data observed from the onset experiment are in the Appendix
section uploaded as Lab Data.

6 Results & Conclusions

This section includes all the results and conclusions obtained using the Lab Data and
using some of the theoretical equations to meet all the aim and objectives of this report.

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6.1 Calculating Van-Laar paramters

To obtain the equilibrium curve of the Ethanol-Water solution, we fit the data obtained
from one paper into the Van-Laar equation to calculate the model parameters A12 and
A21 . Then we check the model accuracy by using it on the data of another paper.

So, the Van-Laar equation can be written as :

 −2
A12 x1
ln(γ1 ) = A12 1 + (1)
A21 x2
 −2
A21 x2
ln(γ2 ) = A21 1 + (2)
A12 x1

We used optimization functions in MATLAB to calculate the parameters by minimizing

the following equations :
 
y1 P
F1 (A12 , A21 ) = norm γ1 − (3)
x1 P1sat
 
y2 P
F2 (A12 , A21 ) = norm γ2 − (4)
x2 P2sat

Here, we x1 and y1 are the mole fractions of Ethanol in Liquid and Vapor phase respec-
tively. The T-x-y values were taken from the paper (Hadrich, 2009).
The values of P sat were calculated using the Antoine equation :
B
log10 P sat = A − (5)
T +C
The values of A, B and C were taken as :

Compound A B C
Ethanol 4.92531 1432.526 -61.819
Water 4.6543 1435.264 -64.848

Table 2: Antoine Equation parameter values

After running the MATLAB scripts, we obtain the following values :

A12 = 1.730296 (6)

A21 = 0.9939354 (7)

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Figure 5: T-x-y plot of Ethanol-Water Solution

Figure 6: x-y plot of Ethanol-Water Solution

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6.2 Checking Model Accuracy

Now, we check the accuracy of our fitted Van-Laar parameters by testing them on the
VLE data obtained from another paper (Cornell, 1933). We obtain the following results :
X
SSres ≡ (yi − ŷi )2 = 0.004348 (8)
R2 = 0.997784 (9)
We observe that the R value is larger than 0.995, meaning that our model is very accurate
2

and can be used in further calculations.

Figure 7: Plot of Experimental Data from Cornell, 1933 and Fitted Van-Laar Model

6.3 Density Calibration

We plot the density of Ethanol-Water solution at different mole fractions obtained from
experiment, and obtained from literature data.
As observed in this graph, there is one outlier (x = 0.2, ρ = 0.995) in the experimental
values. After removing it, we get the following fitted equation of Mixture Density (ρmix )
in terms of Ethanol mole fraction (x):
ρmix = 0.1343x2 − 0.3454x + 0.9939 (10)
R2 = 0.999878 (11)

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Figure 8: Plot of Density values (one outlier)

Figure 9: Plot of Density values (zero outliers)

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6.4 Initial and Final Values

The following are the values of variables corresponding to Still Volume in the flask at the
start of the experiment :

Compound Mass (g) Volume (mL) Density (g/mL) Moles (mol) Mole Fraction
Ethanol 156.56 200 0.7828 3.3985 0.1334
Water 397.55 400 0.9939 22.0679 0.8666
Total 554.11 583.16 0.9502 25.4664 -

Table 3: Initial Values of Still Volume

The following are the values of variables corresponding to Residual Volume in the flask
at the end of the experiment :

Compound Mass (g) Volume (mL) Density (g/mL) Moles (mol) Mole Fraction
Ethanol 15.68 20.03 0.7828 0.3404 0.0180
Water 333.96 336.02 0.9939 18.5381 0.9820
Total 349.64 354 0.9877 18.8785 -

Table 4: Final Values of Residual Volume

Finally, the given below values are of variables corresponding to the Distillate condensed
into another beaker :

Compound Mass (g) Volume (mL) Density (g/mL) Moles (mol) Mole Fraction
Ethanol 117.03 149.50 0.7828 2.5404 0.3988
Water 69.00 69.42 0.9939 3.8300 0.6012
Total 186.03 212 0.8775 6.3704 -

Table 5: Final Values of Distillate

6.5 Checking Mass Conservation

Initial : Mi = 554.11 grams (12)
F inal : Mf = 349.64 + 186.03 = 535.67 grams (13)
Mf − Mi
Error : · 100% = 3.33% (14)
Mi

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6.6 Checking Rayleigh’s equation

 
Ni
LHS : ln = 0.2993 (15)
Nf
Z xi
1
RHS : dx = 0.4082 (16)
xf y∗ −x
Ninitial
T heoretical N̂f = = 16.9308 (17)
exp(RHS)
Nf − N̂f
Error : · 100% = 11.50% (18)
N̂f

6.7 Remarks
• It is seen that the batch distillation on Ethanol-Water solution gives good results
due to the large difference between their boiling points; Tethanol = 78o C and Twater =
100o C.

• It is observed that the temperature at which saturated vapor starts to condense

(Dew Point) is at about 87o C.

• The temperature at which liquid starts to vaporize in the flask (Bubble Point) is
about 79o C.

• Considering that the error calculated while checking Rayleigh equation is quite low,
we can conclude that the equation does hold true for batch distillation.

7 Error Analysis
Least Count of (large) measuring cylinder ≡ ∆VL = 2 mL
Least Count of (small) measuring cylinder ≡ ∆VS = 0.1 mL
Least Count of Stopwatch ≡ ∆t = 0.01 sec
Least Count of Densitometer ≡ ∆ρ = 0.0001 g/mL
Error in Temperature ≡ ∆T = 1 K
Error in Generated Heat ≡ ∆VM = 1 Watt

7.1 Sources of Error

• Leakage of saturated vapor through gaps or holes.

• Reading density at a higher temperature than the temperature at which density

calibration was performed.

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• Presence of Outliers in data collected from experiment.

• Human error (spilling the solution over the table, misreading the value shown in
densitometer, ignoring effects of parallax, etc.)

8 Precautions
• Verify that all components of the distillation apparatus, including the three-necked
flask, condenser, and receiving flask, are properly assembled and tightly sealed to
prevent leaks or loss of vapor.

• Ensure the thermocouple is correctly positioned to accurately measure the temper-

ature of the vapor phase, as this is critical for validating Rayleigh’s equation.

• Maintain a consistent flow of cooling water through the condenser to efficiently

condense the vapor, preventing the loss of ethanol vapor into the surroundings.

• Conduct the experiment in a well-ventilated area or under a fume hood to avoid the
buildup of ethanol vapor, which is flammable and can be hazardous when inhaled
in high concentrations.

• Regularly check for pressure buildup in the system, especially in the round-bottom
flask and condenser, to ensure safe operation during the distillation process.

• Do not fill the distillation flask above two-thirds of its capacity to prevent splashing
of the liquid into the condenser or uneven boiling.

• Ensure that all measuring instruments, such as thermocouples and density meters,
are properly calibrated before starting the experiment for precise measurements.

9 Thought Question / Open-Ended

Q. Can you distill crude oil into petroleum products using batch distillation? If yes, how?
If no, then what are the limitations? How will the Rayleigh Equation change in case of
multi-component distillation?
A. (Note. Two papers were taken as a reference before answering the open-ended ques-
tion and they are mentioned in the answer as per their usage arrives and also referred in
Reference section)
Batch distillation can technically be used to separate crude oil into different petroleum
fractions, but it is not the preferred method for crude oil processing in industrial settings.
Instead, continuous distillation is used in refineries for this purpose. Below are the reasons
why batch distillation is not ideal for distilling crude oil and what limitations arise:

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1. Limitations of Batch Distillation for Crude Oil Processing:

• Crude oil contains a very wide range of hydrocarbons with varying boiling points,
from gases to heavy residues. This makes it impractical to separate all components
efficiently in a batch distillation setup, which works better for simpler mixtures.
• Crude oil components require precise temperature control across a broad range of
boiling points. Heating crude oil in a batch distillation would demand frequent
adjustments in temperature, making the process inefficient.
• In batch distillation, the oil is heated and kept at high temperatures for extended
periods. This prolonged heating can cause thermal cracking or decomposition of
heavier components, leading to undesirable products.
• Large-scale processing of crude oil requires continuous operation to handle the high
volume of crude. Batch distillation is typically done in smaller quantities, making
it impractical for industrial-scale separation.

2. Continuous Fractional Distillation is Used:

• They operate without interruption, allowing for the processing of large quantities
of crude oil.
• They enable the separation of various fractions (e.g., gasoline, kerosene, diesel) based
on their boiling points through multiple stages of condensation and vaporization
within the column.
• The heat used in continuous distillation is better managed and recycled within the
system, reducing overall energy consumption and continuous fractional distillation
produces petroleum products of consistent quality because of the better control over
the separation process.
“Simulation and Optimization of Crude Oil Distillation Unit” (Nasiri et al., 2008) ex-
plain how continuous fractionating columns are optimized for energy efficiency and yield,
showing the advantages over batch distillation.

Changes in the Rayleigh Equation in case of multi-component distillation:

The derivation of Rayleigh Equation says that the equations are valid for multi-
component mixtures (discussed in section 9.7 Multicomponent Simple Batch Dis-
tillation in the book “Separation Process Engineering: Includes Mass Transfer Analysis,
4th Edition"). However, since the general equilibrium expression
yi = f (x1 , x2 , ..., xC , T, p) (19)

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depends on the concentration of all components. And for batch distillation the equilibrium
expression,
xj αj−ref
yj = PC (20)
i=1 (xi αi−ref )
The Rayleigh equation for the component A becomes,
Z x0 Z x0
L1 dx dx
ln( ) = − =− xA αA−ref (21)
L2 xf inal yA − xA xf inal PC − xA
i=1 (xi αi−ref )

10 Acknowledgements
We as a group contributed our respective parts into completing the above report on Batch
Distillation.

In terms of specifications, Atharva Sunilkumar Ghodke contributed in “Procedure"

& “Precaution" parts. Anomol Upadhyay delivered the content for “Aim (Objective)";
“Background & Motivation" along with Lakkireddy Vishnu Vardhan Reddy helping in
“Abstract” part of the report and rest of all the parts including calculations are collabo-
ratively done & organized by Deepanjhan Das (general editor) & Aayush Bhakna (proof
reader).
Regarding AI transcript for the open-ended thought question asked, we didn’t use
ChatGpt for our thought question. It was more confusing and so we, after discussing
the scenario and after reading some related papers, we wrote as per our understanding.
Therefore no such transcript is provided in the Appendix section.

And at last but not the least, we specially thank the respective TA for this experiment
for her kind help and to let us have a thorough understanding of the whole process and
the concept. We thank all the course instructors for their effective control and high
co-operation as per the need.

References
• Notes from the course CH5140 : Process Modelling Simulation and Analysis by Prof
Renganathan

• Notes from the course CH3030 : Applied Mass Transfer by Prof Ethayaraja

• Cornell, 1933 | Liquid-Vapor Equilibria in systems Ethanol-Water, Methanol-Water

and Acetic Acid-Water | University of Minnesota
https://drive.google.com/file/d/1lf5WHVy38lLte2laCpVks43LZcnWicT5/view?usp=
share_link

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• Hadrich, 2009 | Identification of the Best Model and Parameters for T-X-Y equilib-
rium data of Ethanol-Water Mixture | Imam Muhammad bin Saud Islamic Univer-
sity
https://drive.google.com/file/d/1wr89ulSt0FU0xOwHhRJIU0PxRilWxd9A/view?usp=
share_link

• Properties of Water (Antoine parameters, density, molecular weight, etc)

https://webbook.nist.gov/cgi/cbook.cgi?ID=C7732185&Mask=4&Type=ANTOINE&
Plot=on

• Properties of Ethanol (Antoine parameters, density, molecular weight, etc)

https://webbook.nist.gov/cgi/cbook.cgi?ID=C64175&Mask=4#

• Density of Ethanol-Water Solution at different weight% at 30o C

https://www.engineeringtoolbox.com/ethanol-water-mixture-density-d_2162.html

• “Simulation and Optimization of Crude Oil Distillation Unit” (Nasiri et al., 2008)
https://dergipark.org.tr/en/download/article-file/721742

• “Separation Process Engineering: Includes Mass Transfer Analysis, 4th Edition"

https://www.informit.com/articles/article.aspx?p=2738308&seqNum=8#:~:text=The%
20profiles%20of%20xi,numerically%20integrate%20the%20Rayleigh%20equation.&text=
where%20%CE%94xA%2Ck%20%3D%20x,%E2%80%93%20xA%5D)k%5D.

Appendix
Lab Data: All the experimental observations of the main experiment that was performed
and tabulated during the laboratory session are included in order in the following (in fig-
ures 10, 11, 12 & 13).

Reference to all the contents: The official GitHub repository which contains all
the related data and coded scripts for calculations is also provided below: https://github.
com/deep183Das/CH3510_MTMO_Lab_Group_2/tree/main/Experiment_7. One can
easily refer to all the related lab resources from this GitHub repository from where screen-
shots of few instances are shown in the above figures, in in this report.

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Figure 10: Group Members

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Figure 11: Volume Calibration Data

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Figure 12: Batch Distillation Data - 1

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Figure 13: Batch Distillation Data - 2

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