CHE 322

COVENANT UNIVERSITY OTA

COLLEGE OF ENGINEERING
DEPARTMENT OF CHEMICAL ENGINEERING

EXPERIMENT 2

BATCH REACTOR

BY
IYOHA COLLINS JOSHUA
(16CF020531)

SUBMITTED TO
THE DEPARTMENT OF CHEMICAL ENGINEERING

IN PARTIAL FULFILMENT OF REQUIREMENTS

CHEMICAL ENGINEERING LABORATORY II
 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 decreases 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 reaction 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 reaction
conversion. The results obtained may be used to optimize the production of ethanol
and sodium acetate using saponification reaction.
 CHAPTER 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
reactant 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).
 CHAPTER 2: THEORY

There are four major types of reactors encountered by Chemical Engineers

among others': BATCH REACTOR, CSTR, PACKED OR FIXED BED REACTOR
and TUBULAR! PLUG-FLOW REACTORS. The concern of this experiment is the
BATCH REACTOR. It is a type of reaction which is widely used in
pharmaceutical industries as well as other sensitive industries. It is
technically most appropriate for slow reactions where high residence time is
usually required. Batch reactors are usually tanks provided with agitation
mechanism to ensure homogeneity of phases; uniform mixing and heat
transfer is ensured through coils or external jacket. The batch reactor study
under this experiment uses conductivity data instead of titration which is
inexact and error-prone, in determining the conversions.
The conductometric technique, which depends on the conductivity
measurement to determine the composition, 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) have
conducted a study of estimating the parameters of the Arrhenius equation for
the same saponification reaction 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 continuous 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 experimental
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 CH3COOC2H5 (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 CH3COOC2H5 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).
 CHAPTER 3: METHODOLGY

Materials Used:
Measuring Cylinder
Thermometer
Beaker
Batch Reactor
Stop Watch

AIM OF EXPERIMENT:
The first experiment involves the following:
1. Determination of reaction rate' constant under isothermal conditions of
30°C for given reactants.
2. Determination of reaction rate constant under isothermal conditions of
37°C for given reactants.
5. Determination of activation energy for the reaction studied in 1 and 2
above using Arrhenius equation.

The second experiment involves the following: 1.Determination of the effect of

change 111 concentration on the rate of reaction under specified modification
as stated below; a) Temperature: 30°C, NaOH: O.IM, CH3COOC2Hs: O.IM. b)
Temperature: 30°C NaOH: O.05M, CH3COOC2Hs: O.IM. c) Temperature: 30°C,
NaOH: O.1M, CH3COOC2Hs: O.02M. UNIT SETTING  The batch reactor should
be firmly positioned on the console. This must have been done for students) 
Hot water circulator and feed tanks are not required for batch reactor
experiment. DO NOT HANDLE.  Plug the temperature sensor and
conductivity sensor supplied with CEX into the appropriate sockets on the
side of the control console. Then, insert the sensors through the appropriate
glands in the lid of the reactor -check that the sensors are fully immersed, than
tighten the glands.  Connect to the appropriate electricity supply.  For a
temperature at below ambient temperature will require chiller unit To
connect the chiller unit, the following are the steps: -Through the reactor lid,
the feed and return loses' for the chiller are connected to the heating coil
within the reactor -The plug for the chiller solenoid valve connects to the
socket on the front of the control console Switch' on to' "CHILL"on the control
 console for experiment involving temperature below room temperature 
Ensure that the temperature and conductivity sensors are situated well below
the liquid surface inside the reactor.
 CHAPTER 4: RESULTS
0.1NaOH and 0.1CH3COOC2H5 at 30oC

Conductivity Concentration Ratio

Time (s) a1 (M) c1 (M) Xa Xc
(mS/cm) (a0-a1)/(a0. a1) (M-1)

0 9.98 0.10000 0.0000 0.00000 0.0000 0.0000

45 9.16 0.07248 3.7963 0.02752 0.2752 0.2752
90 8.72 0.05772 7.3256 0.04228 0.4228 0.4228
135 8.43 0.04799 10.8392 0.05201 0.5201 0.5201
180 8.19 0.03993 15.0420 0.06007 0.6007 0.6007
225 8.00 0.03356 19.8000 0.06644 0.6644 0.6644
270 7.85 0.02852 25.0588 0.07148 0.7148 0.7148
315 7.71 0.02383 31.9718 0.07617 0.7617 0.7617
360 7.61 0.02047 38.8525 0.07953 0.7953 0.7953
405 7.51 0.01711 48.4314 0.08289 0.8289 0.8289
450 7.43 0.01443 59.3023 0.08557 0.8557 0.8557
495 7.37 0.01242 70.5405 0.08758 0.8758 0.8758
540 7.31 0.01040 86.1290 0.08960 0.8960 0.8960
585 7.26 0.00872 104.6154 0.09128 0.9128 0.9128
630 7.22 0.00738 125.4545 0.09262 0.9262 0.9262
675 7.18 0.00604 155.5556 0.09396 0.9396 0.9396
720 7.15 0.00503 188.6667 0.09497 0.9497 0.9497
765 7.12 0.00403 238.3333 0.09597 0.9597 0.9597
810 7.10 0.00336 288.0000 0.09664 0.9664 0.9664
855 7.08 0.00268 362.5000 0.09732 0.9732 0.9732
900 7.05 0.00168 586.0000 0.09832 0.9832 0.9832
945 7.04 0.00134 735.0000 0.09866 0.9866 0.9866
990 7.02 0.00067 1480.0000 0.09933 0.9933 0.9933
1035 7.00 0.00000 - 0.10000 1.0000 1.0000
1080 7.00 0.00000 - 0.10000 1.0000 1.0000
1125 7.00 0.00000 - 0.10000 1.0000 1.0000
 Graph of NaOH Concentration (M) against Time (s)
at 30oC
0.12
NaOH COncentration (M)

0.1

0.08

0.06

0.04

0.02

0
0 200 400 600 800 1000 1200
Time (s)

Graph of Concentration Ratio (M-1) against Time

(s) at 30oC
1600
1400
1200
y = 0.8025x - 193.72
1000 R² = 0.5277
Axis Title

800
600
400
200
0
-200 0 200 400 600 800 1000 1200
Time (s)
0.05NaOH and 0.1CH3COOC2H5 at 30oC

Conductivity Concentration Ratio

Time (s) a1 (M) c1 (M) Xa Xc
(mS/cm) (a0-a1)/(a0. a1) (M-1)

0 10.63 0.05000 0.0000 0.00000 0.0000 0.0000

45 9.54 0.03302 10.2830 0.01698 0.3396 0.3396
90 8.95 0.02383 21.9608 0.02617 0.5234 0.5234
135 8.64 0.01900 32.6230 0.03100 0.6199 0.6199
180 8.45 0.01604 42.3301 0.03396 0.6791 0.6791
225 8.31 0.01386 52.1348 0.03614 0.7227 0.7227
270 8.21 0.01231 61.2658 0.03769 0.7539 0.7539
315 8.11 0.01075 73.0435 0.03925 0.7850 0.7850
360 8.03 0.00950 85.2459 0.04050 0.8100 0.8100
405 7.97 0.00857 96.7273 0.04143 0.8287 0.8287
450 7.91 0.00763 111.0204 0.04237 0.8474 0.8474
495 7.86 0.00685 125.9091 0.04315 0.8629 0.8629
540 7.81 0.00607 144.6154 0.04393 0.8785 0.8785
585 7.77 0.00545 163.4286 0.04455 0.8910 0.8910
630 7.73 0.00483 187.0968 0.04517 0.9034 0.9034
675 7.70 0.00436 209.2857 0.04564 0.9128 0.9128
720 7.67 0.00389 236.8000 0.04611 0.9221 0.9221
765 7.65 0.00358 259.1304 0.04642 0.9283 0.9283
810 7.62 0.00312 301.0000 0.04688 0.9377 0.9377
855 7.60 0.00280 336.6667 0.04720 0.9439 0.9439
900 7.58 0.00249 381.2500 0.04751 0.9502 0.9502
945 7.56 0.00218 438.5714 0.04782 0.9564 0.9564
990 7.54 0.00187 515.0000 0.04813 0.9626 0.9626
1035 7.53 0.00171 563.6364 0.04829 0.9657 0.9657
1080 7.52 0.00156 622.0000 0.04844 0.9688 0.9688
1125 7.50 0.00125 782.5000 0.04875 0.9751 0.9751
1170 7.49 0.00109 897.1429 0.04891 0.9782 0.9782
1215 7.48 0.00093 1050.0000 0.04907 0.9813 0.9813
1260 7.47 0.00078 1264.0000 0.04922 0.9844 0.9844
1305 7.46 0.00062 1585.0000 0.04938 0.9875 0.9875
1350 7.45 0.00047 2120.0000 0.04953 0.9907 0.9907
1395 7.44 0.00031 3190.0000 0.04969 0.9938 0.9938
1440 7.43 0.00016 6400.0000 0.04984 0.9969 0.9969
1485 7.42 0.00000 - 0.05000 1.0000 1.0000
 Graph of Concentration Ratio (M-1) against Time (s) at
30oC
7000
6000
Concentration Ratio (M-1)

5000
4000
3000 y = 1.8815x - 677.1
R² = 0.4383
2000
1000
0
0 200 400 600 800 1000 1200 1400 1600
-1000
Time (s)

Graph of NaOH Concentration (M) against Time

(s) at 30oC
0.06
NaOH Concentration (M)

0.05

0.04

0.03

0.02

0.01

0
0 200 400 600 800 1000 1200 1400 1600
Time (s)
0.05NaOH and CH3COOC2H5 at 37oC

Conductivity Concentration Ratio

Time (s) a1 (M) c1 (M) Xa Xc
(mS/cm) (a0-a1)/(a0. a1) (M-1)

0 5.23 0.05000 0.0000 0.00000 0.0000 0.0000

45 4.68 0.03697 7.0513 0.01303 0.2607 0.2607
90 4.27 0.02725 16.6957 0.02275 0.4550 0.4550
135 4.00 0.02085 27.9545 0.02915 0.5829 0.5829
180 3.79 0.01588 42.9851 0.03412 0.6825 0.6825
225 3.64 0.01232 61.1538 0.03768 0.7536 0.7536
270 3.51 0.00924 88.2051 0.04076 0.8152 0.8152
315 3.41 0.00687 125.5172 0.04313 0.8626 0.8626
360 3.34 0.00521 171.8182 0.04479 0.8957 0.8957
405 3.27 0.00355 261.3333 0.04645 0.9289 0.9289
450 3.24 0.00284 331.6667 0.04716 0.9431 0.9431
495 3.21 0.00213 448.8889 0.04787 0.9573 0.9573
540 3.18 0.00142 683.3333 0.04858 0.9716 0.9716
585 3.16 0.00095 1035.0000 0.04905 0.9810 0.9810
630 3.15 0.00071 1386.6667 0.04929 0.9858 0.9858
675 3.14 0.00047 2090.0000 0.04953 0.9905 0.9905
720 3.14 0.00047 2090.0000 0.04953 0.9905 0.9905
765 3.13 0.00024 4200.0000 0.04976 0.9953 0.9953
810 3.13 0.00024 4200.0000 0.04976 0.9953 0.9953
855 3.12 0.00000 - 0.05000 1.0000 1.0000
900 3.12 0.00000 - 0.05000 1.0000 1.0000
945 3.12 0.00000 - 0.05000 1.0000 1.0000

Graph of Concentration Ratio (M-1) against Time

(s) at 37oC
5000
Concentration Ratio (M-1)

4000 y = 4.3444x - 850.64

R² = 0.6761
3000

2000

1000

0
0 100 200 300 400 500 600 700 800 900
-1000
Time (s)
 Graph of NaOH Concentration (M) against Time
(s) fat 37oC
0.06
NaOH Concentration (M)

0.05

0.04

0.03

0.02

0.01

0
0 200 400 600 800 1000
Time (s)
 CHAPTER 5: DISCUSSION OF RESULTS

. Effect of Temperature on Conversion

Comparing Table 4.1 and Table 4.2, the effect of decreasing the concentration of
NaOH from 0.1M to 0.05M can be observed. That is the conversion of reactant
reaches 1 at 1035sec for the 0.1M NaOH (equimolar) reaction but reaches 1 at
1485seconds for the 0.05M NaOH (non-equimolar) reaction. This shows that
increasing the concentration of reactant will increase the speed of conversion and
hence rate of reaction. This happens because the higher concentration of a reactant
causes more collisions of the reactant.
The observation of Table 4.2 and Table 4.3 shows the effect of temperature on
conversion and conversion rate. Conversion is higher (0.339564) at 45 seconds for
the reaction at 30ºC. Conversion is lower (0.260664) at 45 seconds for the reaction
at 37ºC. Which shows the rate of conversion increases drastically at a higher
temperature. That is conversation of reactant reaches 1 at 855seconds for 37 and 1
at 1485seconds for 30ºC. Therefore conversion occurs faster with increase in
temperature.
Effect of Temperature on Conductivity
Throughout the experiment, it was observed that as reaction time increased the
conductivity decreases. By referring to all the table of values, it can be seen that
the conductivity of the reaction mixture decreases with time. The reaction therefore
goes by measuring the conductivity. Moreover, Table 4.2 and Table 4.3 show the
comparison of conductivity with temp it shows that the conductivity of the reactant
at 30ºC is higher than 37ºC. This implies that when temperature increases, the
conductivity decreases. The temperature increase leads to an intensification of
thermal movement of ions. In exothermal reactions, ions have enough energy to
surmount the potential barrier and undergo reaction. This means that the number of
ions which contribute to conductivity is reduced. Hence conductivity is inversely
proportional to temperature.
Plots of Concentration against Time
Figures 4.1.1 and 4.2.1 shows plots obtained for the concentration of reactant
against time. All plots obtained are downward sloping. This indicates that
concentration of the reactant (NaOH) decreases with time regardless of equimolar
or non-equimolar reaction conditions. Also, temperature makes the difference in
the timing, at Figure 4.1.1 the curve is longer than that of Figure 4.2.1 because at a
higher temperature the process finishes faster.
Plots of Concentration Ratio against Time
𝑎0 −𝑎𝑖
Figures 4.4-4.6 show the plots obtained for the concentration ratio against
𝑎0 ×𝑎𝑖
time. Plots obtained are upward sloping, indicating concentration ratio increases
with time.
From Figures 4.4 and Figure 4.6, Equations of the curve were obtained to be and
respectively. These equations were used to obtain the slope which gives the
specific rate constants. This rate constant value is 𝑘1 = 1.8815𝑀−1 𝑠 −1 at 30ºC; and
𝑘2 = 4.3444𝑀−1 𝑠 −1 at 37ºC. The rate constant obtained is therefore increasing as
temperature is increased. This experiment is obeying the Arrhenius theory.
Activation Energy
According to the Arrhenius Equation, increasing the temperature of a reaction
generally speeds up the process (increases the rate) because the rate
−𝐸
constant increases. In the equation 𝑘 = 𝐴𝑒 𝑅𝑇 , as T increases, the value of the
exponential part of the equation becomes less negative thus increasing the value of
k.
𝑎0 −𝑎𝑖
Rate constants 𝑘1 and 𝑘2 were gotten by taking the slope of plots of against
𝑎0 ×𝑎𝑖
time t for 30ºC and 37ºC respectively. Using a variation of the Arrhenius equation
(see equation 2.), the activation energy was determined. The analysis of the
experimental data showed that the activation energy is 93.357kJ/mol.
 CHAPTER 6: RECCOMENDATION AND CONCLUSION

From the experiment carried out, the following have been concluded after thorough
calculation and observations;
1. Increasing the concentration of reactant will increase the speed of conversion and
hence rate of reaction.
2. Conversion occurs faster when the temperature is increased.
3. Conductivity of the reactant is inversely proportional to the temperature.
4. The effect of temperature on the time taken to complete the reaction is massive, the
higher the temperature, the faster the reaction gets completed.
5. From the graphs of the concentration ratio, the concentration ratio increases with
time, so they’re directly proportional. The rate constant increases as temperature
increases concluding that this experiment obeys Arrhenius Theory.
 CHAPTER 7: REFERENCES

1. "The Sequencing Batch Reactor as a Powerful Tool for the Study of

Slowly Growing Anaerobic Ammonium-oxidizing Microorganisms -
Springer." The Sequencing Batch Reactor as a Powerful Tool for the
Study of Slowly Growing Anaerobic Ammonium-oxidizing
Microorganisms - Springer. N.p., 01 Nov. 1998. Web. 26 Feb. 2014.>
2. ^ "Aerobic Granulation in a Sequencing Batch Reactor." Aerobic
Granulation in a Sequencing Batch Reactor. N.p., n.d. Web. 26 Feb. 2014.
3. ^ "Water Science & Technology 27:5-6 (1993) 241-252 - T. Kuba Et Al. -
Biological Phosphorus Removal from Wastewater by Anaerobic-Anoxic
Sequencing Batch Reactor." Water Science & Technology 27:5-6 (1993)
241-252 - T. Kuba Et Al. - Biological Phosphorus Removal from
Wastewater by Anaerobic-Anoxic Sequencing Batch Reactor. N.p., n.d.
Web. 26 Feb. 2014.
4. ^ "Aerobic Granular Sludge in a Sequencing Batch Reactor." Aerobic
Granular Sludge in a Sequencing Batch Reactor. N.p., n.d. Web. 26 Feb.
2014.
 CHAPTER 8: APPENDIX

Time (s) Conductivity ai Conc. Ratio C1 (M) Xa XC

(mS/cm) (a0-a1)/(a0*a1)
0 9.98 0.10 0 0 0 0
45 9.16 0.07248 3.796 0.02752 0.27517 0.27517
90 8.72 0.0577… 7.3…… 0.04……. 0.04……. ……

[1] This table will be done at 30 and 37 ℃ for both equimolar and non-equimolar reaction.
[2] To get a1 use the eqn. below for all tempt.

At 45 seconds
A1 = 9.16ms/cm
A0 = 9.98 [PLS CHECK THE TABLE SENT]
A0 = 0.1M
A (infinity) = 0
A (infinity) = 7.00 mS/cm [Check the table sent for the values at steady state]
C (infinity) = 0.1M

Concentration ratio
(a0-a1)/(a0*a1) = [0.1 – a1(obtained above)] ……..

= 0.1 [9.98 -9.16 / 9.98 – 7.00]

Xa = 0.1 – 0.0725 / 0.1 = 0.2752

Xc = 0.02752 / 0.1 = 0.2752

Arrhenius eqn.
In (k2/k1) = Ea/R (1/T1 – 1/T2)
Pls check internet for proper placement of parameters.
K = slope of graph of concentration ratio against time.
T1 = 30 = 30 + 273 = 303
T2 = 37 + 273 = ………..
K2 for slope of graph at 37 and K1 at 30 slope
Ea = ………………
Summary of today’s class.
Follow the example pls
All the best.