DE GRUYTER International Journal of Chemical Reactor Engineering.

2017; 20160174

Mohammed K. Al Mesfer1

Experimental Study of Batch Reactor

Performance for Ethyl Acetate Saponification
1
Department of Chemical Engineering, College of Engineering, King Khalid University, Abha 61411, KSA, E-mail: almes-
fer@kku.edu.sa

Abstract:
The objective of the current research work is to investigate the performance of batch reactor for saponification
of ethyl acetate with sodium hydroxide. Temperature, volume of reaction mixture, rate of agitation, and initial
concentration of reactants are the operating conditions considered for analysis. The NaOH concentration de-
creases from 1.13 × 10−2  mol/L to 0.57 × 10−2  mol/L when reaction temperature increases from 293 K to 313 K
after the completion of the reaction. The conversion of NaOH increases with increased reaction temperature
under the studied range of reaction temperatures until the stable condition is achieved. Reactant concentration
declines with increased volume of reaction mixture from 1.2 L to 1.8 L. Sodium acetate concentration and reac-
tion conversion decrease with increased volume of reaction mixture within the studied range. Concentration of
sodium acetate decreases with increased rate of agitation. The conversion of sodium hydroxide declines with
increased agitation rate from 70 rpm to 150 rpm. Higher initial reactant concentration leads to decreased reac-
tion conversion. The results obtained may be used to optimize the production of ethanol and sodium acetate
using saponification reaction.
Keywords: batch reactor, saponification, conversion, performance
DOI: 10.1515/ijcre-2016-0174

1 Introduction
Batch reactors are tanks used extensively at all levels of the chemical industry. These tanks are often equipped
with an agitator and heat transfer coil. Batch reactors are primarily used for relatively slow reactions that require
significant time for reaction completion.
Batch reactors are used for small-scale operations, for testing new chemical processes that have not been
fully developed, for the manufacture of high-priced products, and for processes that are difficult to convert
to continuous operations (Fogler 2006). High conversion can be achieved in a batch reactor by leaving the re-
actant in the reactor for a longer period of time. The batch reactor is usually operated isothermally and at a
constant volume because it is easy to interpret the results of such runs and because little auxiliary equipment
or instrumentation is needed (Levenspiel 1999).
The reaction that takes place in alkaline conditions is called saponification (Bursali, Ertunc, and Akay 2006).
The hydrolysis of ethyl acetate with sodium hydroxide to produce ethanol and sodium acetate is known as
a saponification reaction. The end products of saponification reaction (i. e., sodium acetate and ethanol) are
used in various fields – for instance, the petroleum, textile, cosmetics, and paint industries. Saponification
is used in the textile industry to remove insoluble calcium salts; in the paint industry, it is used to intensify
colors. It is also used in the food industry as a tampon and protector. Saponification plays a very significant
role as tampon in haemodialysis. In the leather industry, it is used in the neutralization of mineral acids. The
hydrolysis of ethyl acetate is characterized by a model of second-order reaction (Kapoor 2004). Ethyl acetate
saponification reaction has been studied by other researchers using a variety of techniques (Daniels et al., 1941;
Schneider and Stoessel 2005). A very mild and fast saponification method has been established, which utilizes
dichloromethane/methanol (9:1) as a solvent with low NaOH concentration at room temperature (Theodorou
et al. 2007).
The conductometric technique, which depends on the conductivity measurement to determine the compo-
sition, was reported by Walker (1906). The saponification of ethyl acetate by sodium hydroxide was studied in
a batch-type reactor by continuously measuring the electric conductivity of reaction solution (Tsujikawa and
Inoue 1966). An initial rate constant at 25°C was determined as 0.112 L/mol.sec, and the activation energy was
11.56 Kcal/mol. A study on saponification of ethyl acetate using conductivity-monitoring instrument has also
been conducted (Kuheli et al. 2011). The results agreed with some of the literature data. Mukhtar et al. (2015)
Mohammed K. Al Mesfer is the corresponding author.
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have conducted a study of estimating the parameters of the Arrhenius equation for the same saponification re-
action in a batch reactor. The effect of reaction temperatures (range: 25–50°C) on conversion has been analyzed,
and an activation energy equal to 43.094 KJ/mol was calculated.
Experimental investigation of the ethyl acetate hydrolysis by sodium hydroxide was carried out in a contin-
uous stirred tank reactor by Danish, Al Mesfer, and Rashid (2015). They found that conversion decreases with
increased reactant flow due to reduced residence time. Batch and semi-batch reactors were used to carry out the
comparative study of acid-base ethyl acetate hydrolysis and an oxidation–reduction reaction (Garu, Nougues,
and Puigjaner 2002), and it was concluded that reactors can be operated in both modes.
In 2014, Wijayarathne et al. conducted a modeling and simulation study of ethyl acetate saponification by
sodium hydroxide using Aspen Plus. It was concluded that simulated results were in close agreement with ex-
perimental results and the rate of reaction increased with higher temperature. A relative study using statistical
designs to increase the reaction conversion in a batch and plug flow reactors has also been completed (Ahmad
et al. 2013).
The NaOH fractional conversion of 0.96 was tabulated at an initial concentrations of NaOH (0.01 mol/L)
and CH3 COOC2 H5 (0.07 mol/L) in plug flow and batch reactors. Ullah, Ahmad, and Younas (2015) studied
optimization of saponification reaction in a continuous stirred tank reactor (CSTR) using two-level factorial
design and surface methodology to maximize the reaction conversion. The conversion of 96.71 % was reported
under optimum values of NaOH and CH3 COOC2 H5 equal to 0.01 mol/L and 0.1 mol/L, respectively. It was
concluded that the initial concentrations of reactants (sodium hydroxide and ethyl acetate) are the significant
factors, whereas temperature, agitation rate, and feed ratio were considered as insubstantial factors, validating
the work reported previously by Bursali, Ertunc, and Akay (2006).
A potential study devoted to process intensification using the fixed-point method of design has been re-
ported (Li et al. 2016), with goals of reducing the production of undesired byproducts, improving the reaction
conversion and yield, and enhancing the energy efficiency. The objective of the current work is to study the
performance of batch reactor for hydrolysis of ethyl acetate by sodium hydroxide. The operating conditions
considered for analyzing the performance of batch reactor were temperature, reactants concentration, agitation
rate, and volume of reaction mixture. To our knowledge, the influence of reaction mixture volume on reaction
conversion has not been explored comparing with other operating variables.

2 Materials and method

2.1 Chemicals

AR-grade sodium hydroxide (NaOH) and ethyl acetate (CH3 COOC2 H5 ) were used to conduct the experiments.
The stock solutions of desired concentration of sodium hydroxide and ethyl acetate were prepared using high-
purity distilled water.

2.2 Experimental setup

A batch reactor (see schematic diagram in Figure 1) obtained from Armfield (U.K.) with a maximum reactor vol-
ume of 2 L was used to conduct the experimental work. The reactor is specially designed to allow detailed study
of the process and reactor is in the form of an insulated flask. A coil inside the reactor is used for controlling
the temperature of the reaction, and the contents of the reactor are stirred by a propeller agitator.

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Figure 1: Experimental setup diagram

2.3 Experimental procedure

The required concentrations of prepared solutions of sodium hydroxide and ethyl acetate were used, and data
were collected at a pressure of 1 atmosphere. The reactor was filled with required volumes of reagents (i. e.,
NaOH and CH3 COOC2 H5 ). Agitator speed (70–150 rpm) was adjusted using the speed selector switch. Both
NaOH and CH3 COONA contribute conductance to the reaction, whereas ethyl acetate and ethanol do not. The
conductivity of sodium hydroxide solution at a fixed concentration and temperature is not the same as that of
sodium acetate at the same molarity and temperature.
During a chemical reaction, the conductivity of reaction solution changes as more of the reactants are con-
verted. The change in conductivity is used to observe the hydrolysis of ethyl acetate; based on this principle,
relationships among the conductivity, conversion, and concentrations (Bursali, Ertunc, and Akay 2006) were
used to calculate the desired reaction kinetics. Previous studies (Garu, Nougues, and Puigjaner 2002; Mata-
Segreda 2002; Ortiz, Romero, and Irabien 1989; Tsujikawa and Inoue 1966) on saponification of ethyl acetate
have specifically focused on kinetics and reaction mechanics.

3 Results and discussion

3.1 Temperature

Data were collected at a total reaction mixture volume of 1.4 L and an agitation rate of 130 rpm. The reactor
was filled with 0.7 L NaOH and 0.7 L CH3 COOC2 H5 , summing up a total volume of 1.4 L. Initial concentration
of 0.05 M of both the reactants was used. Data were recorded using conductivity meter at 4-minute intervals
for reaction mixture temperatures of 293 K, 298 K, 303 K, 308 K, and 313 K until the reaction is complete. The
range of reaction temperatures reported in the literature (Ahmad et al. 2013; Bursali, Ertunc, and Akay 2006;
Garu, Nougues, and Puigjaner 2002; Mukhtar et al. 2015; Tsujikawa and Inoue 1966; Ullah, Ahmad, and Younas
2015; Wijayarathne and Wasalathilake 2014) was used to select the desired range for studying the effect of
reaction temperatures, thus easing the comparison of the current findings with literature data. The dependence
of reactant concentration of sodium hydroxide on reaction time at different temperatures is shown in Figure 2.

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Figure 2: Dependence of NaOH concentrations on reaction time at different reaction temperatures

The concentration of NaOH decreased with increased time of reaction under all conditions of reaction tem-
peratures as reaction proceeded towards completion. Hydrolysis reaction approached completion at a batch
time of 2880 sec (reaction temperature,T = 293 K), whereas completion time was reduced to 2160 sec at a re-
action temperature of 313 K. At a lower reaction temperature, the concentration of NaOH remained higher,
highlighting the large amount of unconverted reactant after the completion of the reaction. The progress of the
hydrolysis reaction was monitored by measuring the conductivity of the reaction mixture at regular intervals.
The NaOH concentration of 1.13 × 10−2  mol/L was reached at a reaction temperature of 293 K as compared with
a concentration of 0.56 × 10−2  mol/L at a reaction temperature of 313 K after achieving the stable condition.
The dependence of product concentration (sodium acetate) on time is shown in Figure 3. The similar con-
centration profiles (Figure 2 and Figure 3) of reactant (NaOH) and product (CH3 COONa) with reaction time
for the batch reactor have been reported in the literature (Garu, Nougues, and Puigjaner 2002). Data were ob-
tained under the constant reaction conditions of reaction mixture volume, agitation rate, and initial reactant
concentrations. The concentration of CH3 COONa increased with higher reaction temperature, and the maxi-
mum concentration was recorded at a reaction temperature of 313 K. Sodium acetate concentration of 4.44 ×
10−2  mol/L was obtained at a reaction temperature of 313 K compared with a concentration of 3.87 × 10−2  mol/L
at a reaction temperature of 293 K. Also, CH3 COONA concentration increased from 4.08 × 10−2  mol/L to 4.24 ×
10−2  mol/L when the temperature of the reaction mixture increased from 303 K to 308 K. Batch time required
for completion of reaction decreased with increased temperature of the reaction mixture within studied range
of temperatures.

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Figure 3: Dependence of sodium acetate concentrations on reaction time at different reaction temperatures

The dependence of reaction conversion on reaction time for different reaction temperatures is shown in
Figure 4.The NaOH conversion increases with increased reaction time until the stable condition is achieved.
The maximum reaction conversion of 88.79 % was achieved at a reaction temperature of 313 K as compared
with a lower conversion of 77.44 % at a reaction temperature of 293 K, whereas Wijayarathne and Wasalathi-
lake (2014) reported maximum conversion of 80 % and 76 % at temperatures of 313 K and 308 K, respectively.
The increase of NaOH conversion with increased temperature agrees with previous findings (Danish, Al Mes-
fer, and Rashid 2015; Ullah, Ahmad, and Younas 2015; Wijayarathne and Wasalathilake 2014). Using design of
experiments, Bursali, Ertunc, and Akay (2006) and Ullah, Ahmad, and Younas (2015) suggested that the effect
of temperature on reaction conversion is inconsequential. Also, batch time required for the reaction completion
decreases with increased reaction temperature, as evident from the curves. The reaction conversion is higher at
maximum temperature (313 K) as reaction progresses until attaining the stable condition. The reaction conver-
sion is 85.91 % corresponding to a reaction temperature of 308 K, whereas it reduced to 82.99 % corresponding
to a reaction temperature of 303 K at the same batch time of 1920 sec.

Figure 4: Dependence of NaOH conversions on reaction time at different reaction temperatures

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3.2 Volume of reaction mixture

Investigations were carried out at a constant temperature of 303 K with an agitation rate of 130 rpm. The batch
reactor was charged with the same initial concentrations of both the reactants (NaOH and CH3 COOC2 H5 ) equal
to 0.05 mol/L. Experiments were conducted at total reaction mixture volumes of 1.2 L, 1.4 L, 1.6 L, and 1.8 L for
analyzing the reactor performance. The selected various volumes of reaction mixture ranging from 1.2 to 1.8 L
(Max.V: 2 L) are in concurrence with previously reported work at nearly the same volume, as available in the
literature (Ahmad et al. 2013; Bursali, Ertunc, and Akay 2006; Tsujikawa and Inoue 1966).
The dependence of reactant concentration (CNa ) on reaction time is shown in Figure 5. The concentration
of NaOH suddenly drops to lower values; after that sudden drop, the change is gradual with reaction time
under different volumes of reaction mixture. NaOH concentration of 1.477 × 10−2  mol/L was calculated at a
total reaction mixture volume of 1.2 L compared with a higher concentration of 2.555 × 10−2  mol/L at a reaction
mixture volume of 1.8 L at stable condition. Further, the reaction time required for completion of the reaction
decreases with increased volume of reaction mixture.

Figure 5: Dependence of NaOH concentrations on reaction time at different volumes of reaction mixture

The dependence of product concentration (sodium acetate) on reaction time for various volumes of reaction
mixture is shown in Figure 6. A significant amount of product (sodium acetate) was formed (3.52 × 10−2  mol/L)
at a reaction mixture volume of 1.2 L as compared with a lower value of 2.45 × 10−2  mol/Lat a reactor volume
of 1.8 L. The CH3 COONA concentration is always higher in case of reaction mixture volume of 1.2 L at any
reaction time until the completion of reaction. The reaction time required for the reaction completion decreases
with increased total reactor volume. A batch reaction time of 1200 sec is needed at a reaction mixture volume
of 1.8 L, compared with 2160 sec batch time at a reactor volume of 1.2 L for the completion of the hydrolysis
reaction.

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Figure 6: Dependence of CH3 COONa concentrations on reaction time at different volumes of reaction mixture

The variation of NaOH conversion with reaction time is shown in Figure 7. Reaction conversion increases
with increased reaction time until stable condition is achieved. It is also concluded that the time required to
achieve stable condition decreases with increased reaction mixture volume. Decreased batch reaction time with
increased volume of reaction mixture will lead to the increased production capacity of a plant at industrial scale.
Until now, to our knowledge, no investigation has been carried out to study the effect of reaction mixture volume
on reaction kinetics. The reaction conversion of 70.45 % was obtained at a total volume of 1.2 L as compared
with a conversion of 48.99 % at a reactor volume of 1.8 L. The reaction conversions obtained at reaction mixtures
volumes of 1.6 L and 1.8 L are nearly the same. The reaction conversions of 60.22 % and 62.39 % were reached
corresponding to working volumes of 1.4 L and 1.6 L, respectively. It is clear that a higher volume of reaction
mixture leads to decreased reaction conversion results in the presence of more unconverted reactant in the
product stream.

Figure 7: Dependence of NaOH conversions on reaction time at different volumes

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3.3 Agitation rate

Experiments were conducted at a temperature of 303 K to investigate the effect of agitation on reactor perfor-
mance. The reactor was charged with a 700 mL NaOH solution and 700 mL CH3 COOC2 H5 (total volume of
reaction mixture: 1.4 L). Concentrations of both the reactants were equal to 0.05 mol/L. The dependence of re-
actant concentration (CNa ) on reaction time is presented in Figure 8. The study has been conducted at three
different agitation rates of 70 rpm, 110 rpm, and 150 rpm; other similar studies (Bursali, Ertunc, and Akay 2006;
Ullah, Ahmad, and Younas 2015) reported hydrolysis of CH3 COOC2 H5 at around the same agitation rates.

Figure 8: Dependence of NaOH concentrations on reaction time at different rates of agitation

The concentration of NaOH suddenly drops at a reaction time of about 240 sec minutes for all agitation
rates. The NaOH concentration of 1.82 × 10−4  mol/L was reached at an agitation rate of 70 rpm, whereas a
concentration of 1.79 × 10−2  mol/L under stable conditions was noticed at a stirrer speed of 150 rpm, signifying
the importance of agitation. It can be concluded from the findings that the amount of reactant converted to
product decreases with increased rate of agitation. On the other hand, the reaction time required to achieve a
stable condition decreases with increased agitation rate.
The variation of sodium acetate concentration with reaction time is shown in Figure 9. Product formation
declines with increased agitation rate. A concentration of sodium acetate 4.98 × 10−2  mol/L was calculated at
an agitation rate of 70 rpm as compared with 3.20 × 10−2  mol/L at an agitation rate of 150 rpm. The product
concentration of 3.82 × 10−2  mol/L was obtained at an agitation rate of 110 rpm. The reaction time required
to achieve stable condition decreases with an increased rate of agitation, as evident from the curves. A batch
reaction time of 2640 sec required at an agitation rate of 70 rpm, whereas it reduced to 1920 sec at an agitation
rate of 150 rpm for reaction completion.

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Figure 9: Dependence of CH3 COONa concentrations on reaction time at different rates of agitation

The dependence of NaOH conversion on reaction time is shown in Figure 10. It is evident that reaction
conversion increases with increased reaction time at different agitation rates until stable condition is achieved.
A low agitation rate of 70 rpm contributes towards higher conversion. Maximal conversion of 99.64 % was
achieved at an agitation rate of 70 rpm as compared with a lower conversion at agitation rates higher than 70
rpm. Reaction conversions of 76.25 % and 60.19 % were achieved at an agitation rates of 110 rpm and 150 rpm,
respectively, after attaining a stable condition in the system. It was suggested that reaction conversion decreases
from 99.64 % to 60.64 % with an agitation rate increase from 70 rpm to 150 rpm, signifying the importance of
low agitation; whereas Ullah, Ahmad, and Younas (2015) reported that fractional conversion increases with
increased agitation rate from 140 to 230 rpm. Using experimental design, Bursali, Ertunc, and Akay (2006)
found that agitation rate has no effect on reaction conversion and considered agitation rate as an extraneous
factor, along with reaction temperature. The batch reaction time required to achieve stable condition decreases
with increased rate of agitation. The batch time required for reaction completion decreases from 2400 to1680 sec
with a corresponding increase of agitation rate from 70 rpm to 150 rpm at end of reaction.

Figure 10: Dependence of NaOH conversions on reaction time at different rates of agitation

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3.4 Initial reactant concentrations

Data were collected at a constant temperature of 303 K and at total reaction mixture volume of 1.4 L. Agitator
rate was adjusted to 130 rpm to analyze the effect of different initial concentrations on reactor performance.
Equal initial reactant concentrations of both sodium hydroxide and ethyl acetate were used in each case. Ini-
tial reactants concentrations of 0.025 mol/L, 0.0375 mol/L, 0.05 mol/L, and 0.075 mol/L were used for analysis,
whereas similar concentrations of reactant were used to study saponification reaction as reported in the litera-
ture (Ahmad et al. 2013; Bursali, Ertunc, and Akay 2006; Mukhtar et al. 2015; Ullah, Ahmad, and Younas 2015;
Wijayarathne and Wasalathilake 2014).
The dependence of reactant concentration (sodium hydroxide) on reaction time at different initial concen-
trations of the reactant is shown in Figure 11.The reaction time required for achieving stable condition decreases
with increased initial concentrations of both reactants. NaOH concentration reduced to 5.62 × 10−2  mol/L in
cases in which initial concentrations of both reactants were kept equal to 0.025 mol/L, whereas concentration
decreased to 4.34 × 10−2  mol/L from initial reactants concentration of 0.075 mol/L.

Figure 11: Dependence of NaOH concentrations on reaction time at various initial concentrations

Figure 12 shows the variation of product concentration (sodium acetate) with time for different initial con-
centrations. The reaction time required for achieving stable condition decreases with increased initial concen-
tration of both reactants. Stable condition of the reactive system is achieved very quickly at higher initial re-
actant concentration as evident from the curves. Stable condition is achieved after a batch time of 960 sec at
an initial reactant (sodium hydroxide and ethyl acetate) concentration of 0.075 mol/L compared with a batch
time of 2640 sec at a lower initial reactant concentration of 0.025 mol/L. A CH3 COONa concentration of 1.94 ×
10−2  mol/L with initial concentration of 0.025 mol/L and CH3 COONa concentration of 3.16 × 10−2  mol/L with
initial concentration of 0.075 mol/L were obtained after the reaction was complete.

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Figure 12: Dependence of product concentrations on reaction time at various initial concentrations

Dependence of NaOH conversion on reaction time is shown in Figure 13. The time of reaction required
for the achieving the maximum conversion decreases with increased initial reactant concentrations from
0.025 mol/L to 0.075 mol/L. The maximum conversion of 77.54 % was obtained for reaction with an initial lower
concentration of 0.025 mol/L of both reactants. The sodium hydroxide conversion increases with decreased ini-
tial concentration of both reactants (0.075 mol/L to 0.025 mol/L). Bursali, Ertunc, and Akay (2006) reported a
maximum concentration of 98 % at optimum initial concentration of sodium hydroxide (0.01 mol/L) and ethyl
acetate (0.1 mol/L), whereas a conversion of 96 % at initial optimum concentration of NaOH (0.01 mol/L) and
ethyl acetate (0.07 mol/L) was reported by Ahmad et al. (2013).The conversion of 42.15 % has been calculated for
the reaction with an initial concentration of 0.075 mol/L. The reaction conversions of 53.05 % and 49.99 % were
obtained corresponding to the initial reactant concentrations of 0.0375 mol/L and 0.05 mol/L. It is concluded
that higher initial reactant concentration leads to decreased reaction conversion.

Figure 13: Dependence of NaOH conversions on reaction time at various initial concentrations

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4 Conclusions
The concentration of NaOH decreases with increased time of reaction until the completion of the reaction at
different reaction temperatures. Increased reaction temperatures from 293 K to 313 K lead to decreased NaOH
concentration from 1.13 × 10−2  mol/L to 0.57 × 10−2  mol/L respecively. The reaction conversion of NaOH
increases with increased reaction temperature within the studied range (293–313 K) until stable condition is
achieved. Reactant concentration declines with increased volume of reaction mixture from 1.2 to 1.8 L as saponi-
fication proceeds to completion. The reaction time required for achieving stable condition decreases with an
increased volume of reaction mixture. Product concentration (sodium acetate) decreases with increased volume
of reaction mixture within the studied range.
Reaction conversion decreases with increased volume of reaction mixture, and maximum reaction conver-
sion of 70.46 % is obtained at reaction mixture volume of 1.2 L compared with a conversion of 48.99 % at mixture
volume of 1.8 L. The reaction time required for achieving stable condition decreases with increased reaction
mixture volume, and this finding may lead to increased production capacity at the industrial level. Reactant
concentration decreases with reaction time as the rate of agitation increases from 70 rpm to 150 rpm. Con-
centration of sodium acetate decreases with an increased rate of agitation. Fractional reaction conversion of
sodium hydroxide declines with increased agitation rate. Maximum conversion was obtained at a slow agita-
tion rate of 70 rpm. The time of reaction required for achieving stable condition decreases with increased initial
concentrations of both reactants. Higher initial reactant concentrations lead to decreased fractional reaction con-
version. Maximum sodium hydroxide conversion of 77.54 % was noted with an initial reactant concentration
of 0.025mol/L, whereas it declined to 31.61 % with an increased initial concentration of 0.075 mol/L.

Acknowledgement

The author is thankful to the laboratory staff members of the Chemical Engineering Department of King Khalid
University for their valuable Support.

Notations
T Temperature of reaction mixture, K
t Time of reaction, sec.
S Agitation rate, rpm
X Reaction conversion
V Volume of reaction mixture, liter, L
C Concentration, mol/L

Subscripts

Na Sodium hydroxide
ac Sodium acetate
o Initial

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