CL-352

MASS TRANSFER
AND
ENGINEERING LAB

Lab Report

Experiment No.: 11

BATCH REACTOR

Name: Jayanti Jangir

Roll No.: 21110086

12/02/2024
 BATCH REACTOR

Aim:

To main objective of this experiment is to determine the rate constant of a reversible second
order saponification reaction at room temperature using Batch Reactor

Reaction:

In the experiment, the reaction of interest is the saponification of ethyl acetate (CH₃COOC₂H₅)
with sodium hydroxide (NaOH) to form sodium acetate (CH₃COONa) and ethanol (C₂H₅OH).
This reaction is a reversible second-order reaction, meaning that it involves two reactants and
the rate of reaction is proportional to the product of their concentrations. The reaction can be
represented by the following chemical equation:

CH₃COOC₂H₅ (aq) + NaOH (aq) ⇌ CH₃COONa (aq) + C₂H₅OH (aq)

The rate constant of this reaction is determined by monitoring the conductivity of the reaction
mixture over time, as the conductivity is directly related to the concentration of unreacted
NaOH in the solution. The reaction is carried out in a batch reactor, which allows for the
control of reaction conditions and the measurement of reaction kinetics.

Apparatus required:

The materials used in the experiment include:

1. Chemicals:

- Ethyl acetate (CH₃COOC₂H₅)

- Sodium hydroxide (NaOH)

- Distilled water

2. Apparatus:

- Magnetic stirrer: To ensure uniform mixing of the reactants.

- Conductivity meter: To measure the conductivity of the reaction mixture.

- Glass beakers: For preparing solutions and carrying out the reaction.

- Measuring cylinders: To accurately measure the volumes of reactants and solutions.

- Pipettes: For transferring precise volumes of solutions.

- Stopwatch
Procedure:

The detailed procedure for the experiment is as follows:

● Prepare a 0.05 N NaOH solution by dissolving the appropriate amount of NaOH pellets
in distilled water. Ensure complete dissolution.

● Calibrate the conductivity meter using standard solutions of NaOH. Measure the
conductivity of NaOH solutions of known concentrations and plot a calibration curve of
conductivity versus concentration.

● Set up the batch reactor with a magnetic stirrer and a conductivity meter. Ensure that the
temperature of the reaction mixture is maintained at room temperature.

● Measure the required volumes of ethyl acetate and NaOH solution. Mix them in the
batch reactor, ensuring that the total volume and concentration are consistent with the
reaction stoichiometry.

● Start the magnetic stirrer and begin monitoring the conductivity of the reaction mixture.
Record the conductivity at regular time intervals to track the progress of the reaction.

● Use the calibration curve to convert the conductivity measurements into concentrations
of unreacted NaOH. Plot the concentration of NaOH versus time to analyze the reaction
kinetics.

● Use the data obtained to calculate the rate constant of the saponification reaction. Apply
the appropriate rate laws and mathematical models to determine the rate constant from
the concentration-time profile.

● After the experiment, properly dispose of the reaction mixture and clean all the
equipment used. Follow all safety protocols for handling chemicals and operating the
batch reactor.

Theory:

The theory and introduction of the experiment revolve around the concept of a batch reactor
and the kinetics of a reversible second-order saponification reaction.

Batch Reactor:A batch reactor is a closed system where a reaction occurs without any input or
output of materials during the reaction period. It is commonly used in laboratory settings for
studying reaction kinetics, as it allows for precise control over reaction conditions such as
temperature, concentration, and mixing. In this experiment, the batch reactor is used to
conduct the saponification reaction and monitor its progress through conductivity
measurements.
 Saponification Reaction:Saponification is a chemical reaction between an ester and a base,
resulting in the formation of a carboxylate salt and an alcohol. In this case, ethyl acetate (an
ester) reacts with sodium hydroxide (a base) to produce sodium acetate (a carboxylate salt)
and ethanol (an alcohol). The reaction can be represented as:

CH₃COOC₂H₅ + NaOH → CH₃COONa + C₂H₅OH

This reaction is reversible and second-order, meaning that the rate of reaction depends on the
concentrations of both reactants. The rate constant of the reaction provides valuable
information about the reaction kinetics and is the primary focus of this experiment.

Reaction Kinetics:The study of reaction kinetics involves understanding the factors that
influence the speed of chemical reactions. In the context of this experiment, the kinetics of the
saponification reaction are explored by monitoring the change in conductivity of the reaction
mixture over time. Conductivity is directly related to the concentration of ions in the solution,
and in this case, it provides a measure of the concentration of unreacted sodium hydroxide. By
analyzing the change in conductivity, the rate of the reaction can be determined, and from this,
the rate constant can be calculated.

Understanding the kinetics of chemical reactions is crucial in various fields, including

chemical engineering, pharmaceuticals, and environmental science. The rate constant obtained
from this experiment can be used to predict the behavior of the saponification reaction under
different conditions, which is valuable for industrial processes involving ester hydrolysis.

This experiment aims to determine the rate constant of a reversible second-order

saponification reaction using a batch reactor. The study of reaction kinetics in this context
provides insights into the factors that govern the speed of chemical reactions and their
practical applications in various industries.

Safety and Precautions

● Handle Chemicals Carefully: Sodium hydroxide (NaOH) is a strong base that can cause
burns. Handle it with caution, and avoid direct contact with skin or eyes.

● Avoid Spills: Work carefully to prevent spills. If a spill occurs, clean it up immediately
using appropriate spill containment materials.

● Dispose of Waste Properly: Dispose of chemical waste according to your institution's

safety guidelines and environmental regulations.

● Emergency Procedures: Be familiar with emergency procedures, including the location

of eyewash stations, safety showers, and fire extinguishers.

Industrial Applications:
The saponification reaction, specifically the reaction between ethyl acetate and sodium
hydroxide, has several industrial applications:

● Soap Manufacturing: Saponification is the traditional method for making soap from
animal fats or vegetable oils and a strong base like NaOH.

● Biodiesel Production: The reaction is used in the production of biodiesel by converting

fats and oils into fatty acid methyl esters (biodiesel) and glycerol.

● Pharmaceuticals: Saponification is used in the synthesis of various pharmaceuticals,

including ester-based drugs, by hydrolyzing ester compounds.

● Food Industry:It is used in the food industry for modifying fats and oils to improve
their properties for use in food products.

● Cosmetics: Saponification is employed in the production of cosmetic products, such as

creams and lotions, by using fats and oils to create emulsifying agents.

Observation Table:

For Calibration curve: (At room temperature)

Vol of NaOH Concentration of NaOH , gmol / L Conductivity meter reading mS/cm

10 ml 0.05 8.29
10 ml 0.025 3.94
10 ml 0.0125 1.926
10 ml 0.00625 0.867

Calculation Table:

Time Conductivity meter Concentration of Conversion of

(min) reading mS/cm NaOH, gmol/L NaOH (Xa) dxA/dt CA0[(1-x)^2]
0 4.857 0.02985294118 0 0 0.05
2 4.374 0.02701176471 0.09517241379 0.0007931034483 0.04093564804
4 3.987 0.02473529412 0.1714285714 0.0006354679803 0.03432653061
6 3.731 0.02322941176 0.2218719212 0.0004203612479 0.03027416535
8 3.525 0.02201764706 0.2624630542 0.0003382594417 0.02719803732
13 3.183 0.02000588235 0.3298522167 0.0002246305419 0.02245490257
18 2.969 0.01874705882 0.3720197044 0.0001405582923 0.01971796258
0.0000958949096
23 2.823 0.01788823529 0.4007881773 9 0.01795274042
28 2.722 0.01729411765 0.4206896552 0.0000663382594 0.01678002378
 4
0.0000538587848
33 2.64 0.01681176471 0.4368472906 9 0.0158570487
38 2.58 0.01645882353 0.4486699507 0.000039408867 0.01519824116
0.0000321839080
43 2.531 0.01617058824 0.4583251232 5 0.01467058361
0.0000269293924
48 2.49 0.01592941176 0.4664039409 5 0.01423623772
53 2.44 0.01563529412 0.4762561576 0.0000328407225 0.01371538062
0.0000177339901
58 2.413 0.01547647059 0.4815763547 5 0.0134381538
63 2.391 0.01534705882 0.48591133 0.0000144499179 0.01321435803
68 2.361 0.01517058824 0.4918226601 0.0000197044335 0.01291221044
0.0000085385878
73 2.348 0.01509411765 0.4943842365 49 0.01278236502
0.0000091954022
78 2.334 0.01501176471 0.4971428571 99 0.01264326531
83 2.332 0.015 0.4975369458 0.0000013136289 0.01262345604
88 2.33 0.01498823529 0.4979310345 0.0000013136289 0.01260366231

Rate equation for a second-order reversible reaction:

The rate of the reaction is determined by the difference between the rate of the forward
reaction and the rate of the reverse reaction. In the context of the saponification experiment,
the reactants are ethyl acetate and sodium hydroxide, and the products are sodium acetate and
ethanol.
For a second-order reversible reaction, the rate equation can be expressed as:

Where 𝑘𝑐 = 10^(3885.44/T)
At room temperature, the value of Kc is very small; hence, we can assume the reaction to be
irreversible.

For CA0 = CB0

Design equation in terms of conversion:
Graph:

Fig. Conductivity vs. concentration of NaOH

Fig. dxA/dt vs. CA0[(1-x)^2]

Result:
The rate constant for the saponification of ethyl acetate with NaOH at a temperature of 28ºC
is, k = 8099133138187 (L/g.mol s).

Conclusion:
1. The experiment aimed to determine the rate constant of a reversible second-order
saponification reaction using a batch reactor.

2. Sodium hydroxide and ethyl acetate were used as the reactants for the saponification
reaction.
3. The conductivity of the reaction mixture was monitored over time to track the progress of
the reaction.

4. A calibration curve of conductivity versus NaOH concentration was used to convert

conductivity measurements into concentrations of unreacted NaOH.

5. The rate of the reaction was determined by analyzing the change in conductivity of the
reaction mixture.

6. The rate constant was calculated using the rate of reaction and the concentrations of the
reactants.

7. The experiment demonstrated the usefulness of a batch reactor in studying the kinetics of a
reversible second-order reaction.

8. The results showed that the rate constant is a crucial parameter in understanding the
behavior of the saponification reaction.

9. The experiment highlighted the importance of accurate measurement and calibration in

determining reaction kinetics.

10. The findings contribute to a better understanding of the kinetics of saponification

reactions and the use of batch reactors in chemical experimentation.

Reference
1. lab manual
2. link