Mass Transfer and Reaction Engineering Lab

CL 352

Batch Reactor

Instructor Name: Prof. Abinaya Sampath

Name: Abhinav Anand

Roll No.: 21110006
CL-352
Date: 27-01-2024

Purpose and Objective: We need to experimentally determine the rate constant of a reversible
reaction of Sodium Hydroxide and Ethyl acetate which is also known as saponification reaction. We
will also make a calibration curve of the NaOH concentration vs Conductivity to use later in the
calculation.

Theory: A batch reactor is a closed vessel that does not have input and output flow during the
reaction. This means that all the reactants are added to the vessel at the beginning of the reaction,
and the vessel is then sealed shut. The reaction proceeds inside the vessel, and the products are
removed only after the reaction is complete. It can be used in industries like pharmaceuticals or
chemicals. It is mainly used for expensive chemicals or experiments that are done at small scale. It
can also be used where the continuous reactor is difficult to control.
 Schematic of Batch Reactor

There are some advantages and disadvantages of a batch reactor:

● It is relatively easy to control or manipulate the reaction condition in a batch reactor.
● It is often used for hazardous reactions, as the reaction can be easily contained.
● However, it is less productive than continuous reactors, as the reactor must be emptied and
cleaned after each batch.

Derivation:

Mole Balance:

𝑉 𝑑𝑁𝐴
𝐹𝐴0 − 𝐹𝐴 + ∫ 𝑟𝐴𝑑𝑉 = 𝑑𝑡
0

Assumption:
1. There is no inflow or outflow in the Batch reactor:

𝐹𝐴0 = 𝐹𝐴 = 0

𝑑𝑁𝐴 𝑉

𝑑𝑡
= ∫ 𝑟𝐴𝑑𝑉
0
2. The reaction is well mixed:

𝑉
∫ 𝑟𝐴𝑑𝑉 = 𝑟𝐴𝑉
0

𝑑𝑁𝐴
𝑑𝑡
= 𝑟𝐴𝑉

Conversion of a batch reactor can be derived as:

𝑁𝐴0 − 𝑁𝐴
𝑋 = 𝑁𝐴0

𝑁𝐴 = 𝑁𝐴0𝑋
𝑑𝑁𝐴 = − 𝑁𝐴0 𝑑𝑋
𝑑𝑋 −𝑟𝐴𝑉
𝑑𝑡
= 𝑁𝐴0

𝑋
𝑑𝑋
𝑡 = ∫ 𝑟𝐴𝑉
0

Apparatus required: Magnetic stirrer, conductivity meter, glass beakers, measuring cylinders,
pipettes, and stopwatch.

Chemicals required: Sodium Hydroxide, Ethyl Acetate, and Distilled Water.

Procedure:
1. Calculate the weight of Sodium hydroxide to make a 0.05N solution in distilled water.
2. Take 10 ml of the solution in another beaker and measure its conductivity using a conductivity
meter.
3. Dilute the solution by half and measure the conductivity. Repeat this process till we get at least
four different conductivity to make a graph for the calibration curve.
4. Now, find out the volume of ethyl acetate to make an equimolar mixture of sodium hydroxide
and ethyl acetate. Add that NaOH to the ethyl acetate volume, start the stirrer, and switch on
the conductivity meter to measure the conductivity during the reaction
 5. Start the stopwatch while adding the ethyl acetate because the reaction has started here.
6. Now, take the conductivity meter reading after time intervals of 1 minute, 2 minutes, 3 minutes,
5 minutes, and so on until the change in the conductivity meter reading is negligible.
7. Using the calibration curve of NaOH concentration vs Conductivity, find the concentration of
unreacted NaOH in the reaction taken during the experiment.

Observation Table:

Concentration of NaOH, Conductivity meter reading,

gmol/L mS/cm
0.05 12.17
0.025 6.351
0.0125 3.338
0.00625 1.754

Calibration Curve:
Calculation:
For 2nd order reversible reaction:
−𝑑𝐶𝐴 𝐶𝐶𝐶𝐷
− 𝑟𝐴 = 𝑑𝑡
= 𝑘[𝐶𝐵 − 𝐾𝐶
]

3885.44

Where: 𝐾𝐶 = 10 298
at 298K.

We can ignore Kc as its value at room temperature is negligible.

So, − 𝑟𝐴 = 𝑘[𝐶𝐴𝐶𝐵]

For equimolar reaction, 𝐶𝐴0 = 𝐶𝐵0

𝑑𝑋𝐴 ∆𝑋𝐴 2
𝑑𝑡
≈ ∆𝑡
= 𝑘𝐶𝐴0[(1 − 𝑋𝐴) ]

We will use the above calibration curve to find the concentration of NaOH.
Concentration of NaOH = (Conductivity - 0.341)/237 (from the graph equation)
∆𝑋𝐴
To find ∆𝑡
, we will use: ΔXA/Δt = (XA2 - XA1)/(t2 - t1)

Calculation Table:
Conductivity Concentration of Conversion of
Time, min meter reading, mS/cm NaOH, gmol/L NaOH ΔXA/Δt
0 5.852 0.02325316456 0.5349367089
1 5.367 0.02120675105 0.5758649789 0.000682137834
2 5.032 0.01979324895 0.6041350211 0.0004711673699
3 4.76 0.01864556962 0.6270886076 0.000382559775
4 4.54 0.01771729958 0.6456540084 0.0003094233474
6 4.192 0.01624894515 0.675021097 0.0002447257384
8 3.93 0.01514345992 0.6971308017 0.0001842475387
10 3.732 0.01430801688 0.7138396624 0.0001392405063
12 3.571 0.01362869198 0.7274261603 0.0001132208158
15 3.386 0.01284810127 0.7430379747 0.00008673230192
20 3.164 0.01191139241 0.7617721519 0.00006244725738
25 3.012 0.01127004219 0.7745991561 0.00004275668073
30 2.895 0.01077637131 0.7844725738 0.00003291139241
35 2.81 0.01041772152 0.7916455696 0.00002390998594
40 2.736 0.01010548523 0.7978902954 0.00002081575246
45 2.669 0.00982278481 0.8035443038 0.0000188466948
Graph:
∆𝑋𝐴 2
Title: ∆𝑡
vs 𝐶𝐴0[(1 − 𝑋𝐴) ]

Result:
From the graph, the rate constant for the saponification reaction is 0.0852 (L/g.mol s).

Discussion & Conclusion:

1. The experiment investigated the rate constant of reversible saponification reaction at 298K. We first
created the calibration curve of NaOH concentration vs conductivity using a conductivity meter.
2. From the calibration curve, we can see that the conductivity value of NaOH is linearly proportional to
the concentration of NaOH.
3. The result shows that the concentration of NaOH in the batch reactor decreased from 0.02325316456
gmol/L to 0.00982278481 gmol/L over the course of the reaction.
4. The conversion of NaOH is about 80% after 45 minutes, and stable conditions are achieved.
5. The rate constant of this reaction is 0.0852 L/g.mol s.
∆𝑋𝐴 2
6. The plot of ∆𝑡
vs. 𝐶𝐴0[(1 − 𝑋𝐴) ] to find the rate constant is not linear. It might be due to a
number of factors, such as human error or unstable room temperature.

Industrial Applications:
1. Saponification reaction has many applications in the industrial and academic fields. Some
industries that rely on these calculations/experiments are
a. Soap manufacturing: To produce different types of soap like laundry soap, cleaning
soap, or lubricating soap.
 b. Detergent Manufacturing: To provide different types of detergent such as laundry,
dishwashing, or industrial detergent.
c. Fire extinguisher manufacturing: To produce fire extinguishers.
d. Chemical Manufacturing: To produce fatty acid, glycerol, and sodium acetate.
e. Organic Chemistry: Used to study the kinetics and find the concentration of many
organic compounds like amides and esters.

References:
1. Lab Manual
2. https://www.chemistrylearner.com/saponification.html
3. https://www.researchgate.net/figure/Batch-stirred-experimental-apparatus-1-Magnetic-stirrer-2
-100mL-pyrex-reactor-and_fig1_330264193