College of Engineering

Chemical Engineering
Department
School Year 2023-2024

Experiment No. 4

Batch Distillation

ChE LAB 2 (51085)

10:00-13:00 Tuesday

Batario, Szalay Michael 202014442

Concepcion, Eliah Mae 202013770

Cortes, Patrick Alvin 202015161

Huerta, Jerico 201812058

Sapigao, Julia Marie 202011633

Group 7

Dr. Ariel Melendres

Instructor

Date Performed
February 27, 2024
 College of Engineering
Chemical Engineering
Department
School Year 2023-2024

Date Submitted
March 5, 2024

I. Introduction

Distillation, a prevalent method employed for the separation and purification of liquids, is
grounded in the differential boiling points of constituents within a liquid amalgam. The
downward movement within the column is attributed to less volatile components, whereas more
volatile counterparts ascend. The term "batch distillation" pertains to the application of
distillation in reduced volumes, typically executed in a batch still incorporating an affixed
column representative of multiple equilibrium phases. Following a concise initiation phase,
product extraction occurs from the column summit after the introduction of a feed into the still
and the activation of heat. This procedural iteration transpires until the distillation apparatus is
reengaged, marking the conclusion of each cycle. Batch distillation emerges as the method of
choice when modest product quantities are necessitated, as continuous distillation proves
economically unfeasible in such instances. The present experimentation adopts batch distillation
to scrutinize the ramifications of vapor velocity and, concomitantly, the boil-up rate on the
pressure differentials across the column.

II. Objectives
The objective of this experiment are listed below:
 To separate the total product from the mixture of water and ethanol using a batch
distillation
 To maintain the heating source at less volatile component temperature.
 To obtain the certain desired concentration of the ethanol from the mixture at time
intervals.
 College of Engineering
Chemical Engineering
Department
School Year 2023-2024

III. Materials and Equipment

Beakers Volumetric Flask Digital Thermometer

Heating Mantle Ethyl Alcohol (95%)

Distillation Set-up
 Distilling Flask
 College of Engineering
Chemical Engineering
Department
School Year 2023-2024

 Condenser
 Clamp Stand
IV. Theoretical Background
Unlike continuous distillation, which focuses on ongoing flow rates, batch distillation is
concerned with the total quantities of products obtained at the end of the process. This difference
is reflected in the mass balance equations used for each type (Wankat, 2016).
F=W final+ D total (Eq. 1)
In the context of batch distillation with a feed containing C components (C-1 being the
number of components excluding one), Equation (2) describes the mass balance for a specific
component, typically the more volatile component (MVC).
The mass balance for any volatile component can be shown as,
F X F =W final X final + Dtotal X D ,avg (Eq. 2)

This equation relates the initial feed characteristics, F moles with mole fraction X final of
the MVC, to the final state of the distillation. W final moles of the bottoms with a final mole
fraction of X final. Additionally, if the distillate is collected in separate fractions throughout the
process, the total distillate amount ( Dtotal ) needs to be further divided into individual distillate
fractions denoted by X.
In this scenario, the initial feed characteristics (F total moles and mole fraction X F of the
light component) are usually known. Moreover, we may have a target value for either the final
light component concentration in the bottoms ( X final) or the average light component
concentration in the entire distillate ( X D , avg). However, with these three unknowns ( Dtotal - total
distillate moles, W final - final moles in the bottoms, and X final or X D , avg), an additional equation is
required for a complete solution.
The Rayleigh equation completes the solution. Derived from a differential mass balance
focusing on the light component, the Rayleigh equation assumes negligible holdup (material
trapped) in the distillation column and accumulator. With this assumption, the equation relates a
small change in material removed from the system ( −dW ) at a specific light component
concentration ( X D) to the remaining material in the still pot and its light component
concentration.
−Out=accumulation∈reboiler (Eq. 3)
Or
 College of Engineering
Chemical Engineering
Department
School Year 2023-2024

−X D dW =−d ( W X W ) (Eq. 4)

By expanding Eq. 4, the following equation can be derived

−X D dW =−Wd X W −X W dW (Eq. 5)

By differentiating,

dW d XW
= (Eq. 6)
W X D− X W

By integrating,
W final X final
dW d XW
∫ W
=∫
X D−X W
(Eq. 7)
W= F X F

[ ]
XF
W final d XW
ln =− ∫ (Rayleigh Equation, Eq. 8)
F X
X D− X W
final

The negative sign in Equation (8) arises from a mathematical maneuver called switching
the limits of integration. This specific form of the Rayleigh equation is remarkably versatile. It
applies to various batch distillation scenarios, including simple and multistage setups, as well as
binary and multicomponent mixtures. However, to fully utilize this equation, we need to
establish a relationship between the light component concentration in the distillate ( X D) and the
light component concentration remaining in the still pot ( X W ).

After determining the amount of W final using the Rayleigh equation, we can determine the
total moles of distillate ( Dtotal) using the overall mass balance for the entire batch process.
Finally, by performing a mass balance specifically on the light component (MVC), we can
calculate the average concentration of the MVC in the entire collected distillate ( X D , avg).
D=F−W final (Eq. 9)
 College of Engineering
Chemical Engineering
Department
School Year 2023-2024

F X F −W final X final
X D , avg= (Eq. 10)
F−W final

Moreover, there are two operating modes under batch distillation, the constant reflux
mode and variable reflux mode (Kim & Diwekar, 2005). Pioneering the analysis of constant
reflux in binary batch distillation with no holdup, Smoker and Rose leveraged the Rayleigh
equation alongside the McCabe-Thiele graphical method. Their approach involved using the
McCabe-Thiele method to iteratively determine the relationship between the distillate
composition ( X D) and the still composition ( X W ). Subsequently, they employed graphical
integration by plotting 1/( X D - X W ) versus X W . The area under this curve, encompassing the
range from feed composition ( X F ) to still composition ( X W ) yields the value of the integral,

ln[ ]
W final
F
. This value, along with the provided equation, allows for the calculation of the average

composition in the collected distillate.

F X F −W X W
X D , avg= (Eq. 11)
F−W
Building upon Smoker and Rose's (1940) work on constant reflux, Bogart (1937)
introduced the concept of variable reflux for binary batch distillation. While the overall
calculation approach remains similar, the key difference lies in manipulating the reflux ratio
(amount of condensate returned to the column) instead of the distillate composition throughout
the process. Interestingly, the Rayleigh equation, still applicable here, simplifies due to the
constant distillate composition in binary systems. This simplification leads to a new form of the
equation, presented as follows:

B X D− X F
= (Eq. 12)
F X D− X W

Equations 11 and 12 can be manipulated further to obtain an expression for determining

batch time and the area under a specific curve. This additional equation might be useful for
specific calculations but isn't essential for understanding the core principles of variable reflux
distillation.

V. Procedure
1. Set-up the apparatus needed for the experiment inside a fume hood.
2. Prepare the reagents for the experiment, i.e., a technical grade ethanol (95% EtOH),
distilled water.
 College of Engineering
Chemical Engineering
Department
School Year 2023-2024

3. Incorporate the desired amount of distilled water in the ethanol to make the mixture
homogeneous. Set the temperature at the boiling point of the ethanol to maximize the
vaporization of the component.
4. Turn on the cooling water inside the fume hood to speed up the condensation process
of the ethanol vapors.
5. Record and measure every batch of the distillate every 5 minutes. Tally the overall
record after the desired time span of operation.
6. After the experiment, turn off the cooling water and the heating mantle. Clean the
used apparatus and compute for the remaining distillate in the residue.
 College of Engineering
Chemical Engineering
Department
School Year 2023-2024

VI. Results and Discussion

Distilled Water: 250 mL
Ethanol (Technical Grade, 95% EtOH): 100 mL
Computing for the concentration of ethanol after dilution,
( 0.95 ) (100 mL )
xF=
100 mL+250 mL
x F =0.2714

Computing for the residue,

F=D+W
W =F−D
F x F =Dx D +W x W

F x F −D x D
xW=
W

Material Balance per time

Ethanol
Time Distillate Distillate Residue Feed
Concentration
5 8.2 8.2 341.8 350 0.2539
10 9.9 18.1 331.9 350 0.2317
15 9.7 27.8 322.2 350 0.2086
20 9.5 37.3 312.7 350 0.1845
25 8.9 46.2 303.8 350 0.1606
30 9 55.2 294.8 350 0.1350
35 9.2 64.4 285.6 350 0.1071
40 9 73.4 276.6 350 0.0781
45 9.4 82.8 267.2 350 0.0457
50 8.6 91.4 258.6 350 0.0139
91.4
Overall Material Balance:
F=D+W
W =F−D
 College of Engineering
Chemical Engineering
Department
School Year 2023-2024

W =350−91.4
W =258.6

Ethanol Balance:
x F =95 %

x D =100 %

F x F =Dx D +W x W

350 ×0.95−91.4 × 1
xW=
258.6
x W =0.0139
Ethanol Concentration, in residue xW

Ethanol Concentration in Residue, W vs. Time

0.30

0.25

0.20

0.15

0.10

0.05

0.00
0 10 20 30 40 50 60

Time (minutes)
 College of Engineering
Chemical Engineering
Department
School Year 2023-2024

VII. Conclusion and Recommendations

The experiment was performed to determine the time it may be required to
recover and separate ethanol from a homogeneous mixture of water-ethanol. An average
of 9.14 mL is being recovered per batch every 5 minutes. The separation achieved during
distillation indicates how well the process concentrates the desired components. The
observed distillate volume reflects distillation efficiency and the degree of separation
between the components based on their boiling points. From the findings, the amount of
ethanol recovered was 91.4 mL in a span of 50 minutes. Aligned with this data, the
percent recovery is determined to be 96.21% which is generally a good amount of
recovery since the experiment was only performed for 50 minutes.
Analyzing distillation data, such as temperature profiles and composition changes,
is critical for understanding the separation mechanism. The reflux ratio, heating rate, and
distillation column selection can all be optimized to improve the overall performance of
the batch distillation process.

Recommendations
1. In performing the experiment, it was assumed that the distillate ethanol concentration
is pure but there is a possibility it may be not even though the experiment was
performed at 87.5°C. It is better to run the distillate in a refractometer to determine
the exact concentration of the distillate.
2. The experiment should be run in a controlled environment to minimize the external
factors in a laboratory scale, but in an industry scale, it is better to perform it at
ambient temperatures to assume the percentage factor of external factors.
 College of Engineering
Chemical Engineering
Department
School Year 2023-2024

VIII. Appendices
Appendix A. Experimental Data
Distilled Water: 250 mL
Ethanol (Technical Grade, 95% EtOH): 100 mL
Computing for the concentration of ethanol after dilution,
( 0.95 ) (100 mL )
xF=
100 mL+250 mL
x F =0.2714
At a time interval of 5 minutes,

Time Interval Distillate Residue

(mins) (mL) (mL)
5 8.2 341.8
10 9.9 331.9
15 9.7 322.2
20 9.5 312.7
25 8.9 303.8
30 9.0 294.8
35 9.2 285.6
40 9.0 276.6
45 9.4 267.2
50 8.6 258.6

Obtaining the respective ethanol concentration per unit of time:

Time Interval Ethanol Concentration

(mins) (%vol EtOH)
5 0.2539
10 0.2317
15 0.2086
20 0.1845
25 0.1606
30 0.1350
35 0.1071
40 0.0781
45 0.0457
 College of Engineering
Chemical Engineering
Department
School Year 2023-2024

50 0.0139
Appendix B. Sample Calculation
Overall Material Balance:
F=D+W
350 mL=91.4 mL+W
W =258.6 mL
Water Balance:
( 0.7286 ) F=( 0 ) D+ ( 1−xW ) W

( 0.7286 )( 350 mL )=( 1−xW ) (258.6 mL )

x W =0.0139

Ethanol Balance:
( 0.2714 ) (350 mL )=( 1 ) ( 91.4 mL ) + x W ( 258.6 mL )
x W =0.0139

Therefore, the same since the two equations may be used

 College of Engineering
Chemical Engineering
Department
School Year 2023-2024

Reference
Bogart, M.J.P. (1937). The design of equipment for fractional Batch distillation. Trans. Am. Inst.
Chern. Eng., 33, 139.
Kim, K. and Diwekar, U. (2005). Batch Distillation. DOI: 10.1201/9781420028164.ch5
McCabe, W.L., Smith, J.C. and Harriott, P. (1993) Unit Operations of Chemical Engineering.
McGraw-Hill, New York.
Smoker, E.H. & Rose, A. (1940). Graphic determination of batch distillation curves for binary
mixtures. Trans. AIChE, 36, 285.
Wankat, P. (2016). Separation Process Engineering: Includes Mass Transfer Analysis, 4th
Edition. Pearson.