UNIVERSITY OF SABRATHA

FACULTY OF ENGINEERING DEPARTMENT OF CHEMICAL ENGINEERING

UNIT OPERATION 2 CHE 432

EXP3
determine the rate constant of saponification reaction by using CSTR

Prepared By

Students Name Sign

-1 ‫مرام الطاهر محمد أبوالقاسم‬

-2 ‫آالء محمد الهادي القمودي‬

Under the supervision of

Mr. Nader Kmal

Date of experimental 02/06/2022

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OBJECTIVES

To determine the rate constant of saponification reaction undertaken in a continuous

stirred tank reactor.

ABSTRACT

Experiment is conducted to carry out manual conversion determination on

experiment samples to verify the conductivity measurement values. A part from that,
the objectives to study saponification reaction between sodium hydroxide solution,
NaOH and ethyl acetate in CSTR, to calculate the reaction rate constant of the
experiment. In order to accomplish the objectives, the unit used to perform this
experiment is CSTR. In this experiment, sodium hydroxide solution and ethyl acetate
react in continuous stirred tank reactor. Both of reactants feed to the reactor at equal
molar flow rate for certain time., the conductivity is changing with time with changing
in the concentrations the conductivity becomes stable when the concentration is
stable,. The conversions is 82.3% at 4.6 min residence time, From the calculation the
rate constant, K =2.7619 L/mol.min

INTRODUCTION

In the industrial chemical processes, mostly a reactor is the key item of equipment in
which raw materials undergo a chemical change to form desired products. The
design and operation of chemical reactors are very crucial to whole success of the
industrial operation. There are many types of reactors depending on the nature of the
feed materials and products. Understanding non-steady behavior of process
equipment is necessary for the design and operation of automatic control system.
The rate of reaction is the most important thing will be consider in the reactor
because it showed effectiveness of the processing in the reactor. One particular type
of process equipment is continuous stirred tank reactor (CSTR).
In this experiment, the CSTR unit used for study on chemical reaction in liquid phase
which is under adiabatic and isothermal condition. The unit comes complete with
vessels for raw material and product, feed pumps and thermostat. The reactor is
modeled in order to perform the saponification reaction where the reaction is occurs
between the sodium hydroxide, NaOH and ethyl acetate, Et (Ac). The saponification
process between this compounds produced sodium acetate in a batch and the
continuous stirred tank reactor evaluate the rate data needed to design a production
scale reactor.

THEORY
A type of reactor used very commonly in industrial processing is a stirred tank
operated continuously. It is referred to as the continuous-stirred tank reactor (CSTR)
or back mix reactor. The CSTR is normally run at steady state and is usually
operated so as to be quite well mixed. As a result of the latter quality, the CSTR is
generally considered as it doesn’t have spatial variation in concentration,
temperature and reaction rate throughout the vessel. Since the temperature and
concentration are identical everywhere within the reaction vessel, they are the same
at the exit point as they are elsewhere in the tank.
The conductivity of the reacting solution in the reactor changes with the degree of
conversion and this provides a convenient method for monitoring the progress of the
reaction either manually or by computer. The reaction is the saponification of ethyl

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acetate by sodium hydroxide as it can be carried out under safe conditions of
temperature and pressure and is well documented.

The reaction chosen for the isothermal demonstration is the saponification of ethyl
acetate by sodium hydroxide.

The reaction:

NaOH + CH3COOC2H5 → CH3COONa+ C2H5OH

sodium hydroxide+¿ ethyl acetate → sodium acetate + ethanol

The steady state conditions will vary depending on concentration of reagents,

flowrate, volume of reactor and temperature of reaction.

The following information can be used to solve the problem.

F A (Sodium hydroxide flow rate in the feed)
F B (Ethyl acetate flow rate in the feed)
a μ (sodium hydroxide concentration in the feed bottle)
a 0 (sodium hydroxide concentration in mixed feed)
b μ (Ethyl acetate concentration in the feed bottle)
b 0 (Ethyl acetate concentration in mixed feed)

FA FB
a 0= ×a μ , b0= × bμ
F A+ FB F A+ FB

Λ a 0=0.195(1+0.0184 (T −294)) a0

Λ a ∞=0.195(1+ 0.0184(T −294)) a∞

a ∞=0 if a0 <b0

a ∞=a 0−b 0 if a0 ≥b 0

Λ c∞ =0.07(1+0.0284 (T −294)) c ∞

c ∞ =a0 , b0 ≥ a0

c ∞ =b0 , b0 <a 0

Λ ∞= Λ a ∞ + Λ c ∞

a t = ( a∞ – a 0 )
( Λ 0− Λ t
Λ0 − Λ∞ )+ a0

at
X A =1−
a0

To calculate the specific rate constant, k:

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 K=
( V Reactor )
F A + F B a0−at
×
at
2

The reactor’s residence time ( τ )is defined as the reactor volume divided by the total
feed flow rate.
V Reactor
τ=
F A+ FB

the equipment and the equipment Description:

1. sensor for conductivity and temperature.

2. overflow.
3. stirrer.
4. stirred tank.
5. chambered bottom as heat exchanger.
6. water supply.
7. reactants A/B supply.
8. intermediate delivery.
9. product drain.
10. water drain.

• The Armfield CEP-MKII Stirred Tank Reactors in Series Unit is designed to follow
the dynamics of the perfectly mixed multistage process. Dynamic behavior can
be studied as can multistage chemical reaction. Bench mounted and self-
contained, the unit requires only to be connected to a single-phase electrical
supply for operation.
• There are three reactor vessels connected in series, each containing a propeller
agitator driven by a variable speed electric motor.
• Two reagent vessels and two variable speed feed pumps feed reagents into the
first reactor in line
• Each reactor and the exit port of the dead time coil are fitted with conductivity
probes for monitoring the process.
• Conductivity is displayed on a digital meter on the console through a selector
switch and all four probes can be connected to the optional Armfield data logging
accessory.

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 Figure1- The Armfield CEP-MKII Stirred Tank Reactors

Experimental procedure

1. Solution Preparation

Dilution of Sodium hydroxide :

 Take 6 g of sodium hydroxide (Mw = 40 g/mol) to prepare 2L of sodium hydroxide

0.075M.
m 6
C= = =0.075 mol/ L
Mw ×V 40 × 2
Dilution of ethyl acetate :
 prepare 0.075mol/L of ethyl acetate in 2L. of ethyl acetate ( ρ = 0.89 g/cm3 , Mw =
88.11 g/mol) :

m=Mw × V ×C
m=88.11 × 0.075× 2=13.2 g

m m
ρ= →V =
V ρ

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 13.2
V= =14.83 cm3
0.89

2. Carefully add ethyl acetate solution to the feed tank and add Sodium hydroxide to
the other feed tank.
3. Connect the both feed tanks to the reactor.
4. Set the pump speed controls to 1.11 cm 3/s flowrate of sodium hydroxide.
5. Set the pump speed controls to 1.315 cm 3/s flowrate of ethyl acetate.
6. Switch on the main switch and start the stopwatch.
7. Record the conductivity for every minute, for about 20min until the conductivity
becomes stable.

Raw data

Table1 – raw data

t (min) Λ (mSiemens /cm)
0 0.55
1 1.89
2 2.56
3 2.66
4 2.64
5 2.58
6 2.51
7 2.46
8 2.45
9 2.42
10 2.42
11 2.42
12 2.42
13 2.42
14 2.42
15 2.42
16 2.42
17 2.42
18 2.42
19 2.42
20 2.42

:Calculations

FA
a 0= ×a μ
F A+ FB

a μ=bμ =0 .075 mol/ L

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 3 3
s/ F A=1.11 cm /s , F B =1.315 cm

1.11
a 0= ×0 .075=0.003433 mol / L
1.11+1.315

FB
b 0= ×b μ
F A+ FB

1.315
b 0= ×0 .075=0.0407 mol/ L
1.11+1.315

Λ a ∞=0.195(1+ 0.0184(T −294)) a∞

a ∞=0 , a 0< b0

Λ a ∞=0.195 ( 1+0.0184 ( 300 .15−294 ) ) ×0

Λ a ∞=0

Λ c∞ =0.07(1+0.0284 (T −294)) c ∞

c ∞ =a0 , b0 ≥ a0

c ∞ =a0 =0. 03433mol / L

Λ c∞ =0.07(1+0.0284 (300 .15−294 ))×0. 03433

Λ c∞ =0 .0002823 Siemens /cm

Λ c∞ =2.823 mSiemens/cm

Λ ∞= Λ a ∞ + Λ c ∞

Λ ∞=0+2.823=2.823 mSiemens/cm

a t = ( a∞ – a 0 ) ( Λ 0− Λ t
Λ0 − Λ∞ )+ a0

a ∞=0 , Λ0 =0 , a0 =0. 03433mol / L ,

Λ ∞=2.823 mSiemens/cm , Λ0=0.55 mSiemens /cm

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 K=
( V Reactor )
F A + F B a0−at
×
at
2

V Reactor =670 mL

Note :there lost volume but can be ignored

V Reactor
τ=
F A+ FB

670
τ=
1.11+1.315

τ =276.29 s=4.605 min

The conversion is;

at
X A =1−
a0

0.006084
X A =1−
0.03433

X A =0.823

Table 2 shows the results

Table 2- the results

t (min) Λt (mSietmens /cm) at K (L/mol.min)
0 0.55 0.03433 0
1 1.89 0.0141 0.3683
2 2.56 0.00397 6.972
3 2.66 0.002450 19.072
4 2.64 0.00276 15.000
5 2.58 0.003667 8.2533
6 2.51 0.004725 4.7995
7 2.46 0.00548 3.4771
8 2.45 0.00563 3.2772
9 2.42 0.006084 2.7619
10 2.42 0.006084 2.7619
11 2.42 0.006084 2.7619
12 2.42 0.006084 2.7619
13 2.42 0.006084 2.7619
14 2.42 0.006084 2.7619
15 2.42 0.006084 2.7619
16 2.42 0.006084 2.7619
17 2.42 0.006084 2.7619
18 2.42 0.006084 2.7619
19 2.42 0.006084 2.7619
20 2.42 0.006084 2.7619

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Results and Discussion:

1. The conductivity of the reaction mixture changes with conversion and therefore
the extent of the reaction can be monitored by recording the conductivity with
respect to time., but when the concentration is stable the conductivity becomes
stable too, The steady state conditions will depend on concentration of reagents,
flow rate, volume of reactor and temperature of reaction.

2. The conversion is taken at the stable conductivity Λt =2.42 mSietmens /cm.

X A =0.823

3. for NaOH in a reactor operating at steady state the volume may be assumed
constant. The steady state concentration of NaOH in reactor (CA) may be used to
calculate the specific rate constant (k):

so the reaction rate is:

K =2.7619 L/mol.min

Conclusions and Recommendations:

CONCLUSION :
As for the conclusion, the purpose of this experiment to determine the reaction rate
constant of sodium hydroxide solution, NaOH. CSTR is used in order to achieve the
objective of this experiment. By completing this experiment, the reaction rate is
collected.

Recommendations:

1. Measure the exact volume of water and weigh the chemicals.

2. Always use clean water and good quality chemicals and standard solution for
titration.
3. Use electronic balance for weighing of chemicals. Don't mix the droppers of
different chemicals.
4. Keep close all the drain valves and vent valve should open while tilling the
reactant in feed tanks.
5. Flow should not be disturbed during the experiments.
6. Handle the chemicals carefully.
7. It is recommended that this experiment should be repeated at various other
temperatures to investigate the relationship between the specific rate constant (k)
and the temperature of reaction.

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8. 2. It is further recommended that the experiment be repeated using dissimilar
flow rates for the caustic soda and ethyl acetate solutions to investigate the effect
that this will have upon the saponification process.

References:
1. https://armfield.co.uk/product/cem-mkii-continuous-stirred-tank-reactor-cstr/
2. continuous stirred tank reactor, mekelle university-mekelle institute of technology,
department of biological and chemical engineering.
3. Continuous Stirred Tank Reactor, University of Jordan Faculty of Engineering
and Technology Department of Chemical Engineering Chemical Engineering
4. Dr. Dayang Nurul Fairuz Bt Abang Zaidel, Saponification of Ethyl Acetate And
sodium hydroxide in cstr, chemical reaction engineering laboratory, university of
Malaysia'

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