TABLE OF CONTENTS

1.0 OBJECTIVES ....................................................................................... 2

2.0 SUMMARY ........................................................................................... 2

3.0 INTRODUCTION .................................................................................. 3

4.0 DATA AND RESULTS .......................................................................... 4

5.0 ANALYSIS AND DISCUSSION ............................................................. 7

6.0 CONCLUSIONS AND RECOMMENDATIONS ..................................... 9

7.0 TUTORIAL .......................................................................................... 11

8.0 REFERENCES ................................................................................... 13

9.0 APPENDICES..................................................................................... 14

1
1.0 OBJECTIVES

The objectives of this experiment were:

 To study for batch conditions the reaction between an ester (ethyl acetate) and sodium
hydroxide.
 To conduct mass balance and energy balance in batch process system.

2.0 SUMMARY

This experiment was conducted by using batch reactor system between reaction of ethyl
acetate and sodium hydroxide. Mass balance and energy balance in batch process system need
to be constructed at the end of the experiment. The experiment was begun by preparing 3L of 0.1
M sodium hydroxide, NaOH and 3L of 0.1M ethyl acetate, Et(Ac) solution. After that, these two
solutions were mixed into reactor R1 and the stirrer was switched on. With an interval of 5 minutes,
a sample was retrieved from valve 1 to conduct a conductivity measuring using conductivity meter
and stopped when the reading of conductivity remains constant. Based on result obtained, the
table 2.0 showed the conductivity against concentration of NaOH. Concentration of NaOH
decreases when the conductivity of solution decreases. It can be said that the results obtained
obeys the theory of calibration curve as it decreases at 0.015143 M with conductivity of 6.12
mS/cm to 0.003071 M at conductivity of 4.43 mS/cm. Based on the graph, conversion increases
as time increase. Conversion begun at minute 5 with 33.96% conversion and continuously
increase until minute 30 with 78.3% conversion. Reaction of batch process started to stabilize at
minute 35 with conversion of 79.72%. The whole process of conversion can be said that NaOH
solution has being converted during the reaction of time. To conclude, this experiment achieved
its objectives.

2
3.0 INTRODUCTION

The Batch reactor is the type of vessel widely used in the process industries. In a batch reactor
the reactants and the catalyst are placed in the reactor and the reaction is allowed to proceed for
a given time whereupon the mixture of unreacted material together with the products is withdrawn.
Provision for mixing may be required. In an ideal batch reactor, the concentration and temperature
are assumed to be spatially uniform. In practice, the condition can be approximately realized by
vigorous agitation or stirring. All the elements of the fluid spend the same amount of time in the
reactor, and hence have the same residence time (Matthew, 2008). From the viewpoint of
thermodynamics, a batch reactor represents a closed system. The steady states of the batch
reactor correspond to states of reaction equilibria.

Batch reactors are often used in the process industry. Batch reactors also have many
laboratory applications, such as small scale production and inducing fermentation for beverage
products. They also have many uses in medical production. Batch reactors are generally
considered expensive to run, as well as variable product reliability (Fogler, 2010). They are also
used for experiments of reaction kinetics, volatiles and thermodynamics. Batch reactors are also
highly used in waste water treatment. They are effective in reducing BOD (biological oxygen
demand) of influent untreated water.

A typical batch reactor consists of a tank with an agitator and integral heating/cooling system.
Liquids and solids are usually charged via connections in the top cover of the reactor. Vapors and
gases also discharge through connections in the top. Liquids are usually discharged out of the
bottom. The advantages of a batch reactor lies in its versatility. A single vessel can carry out a
sequence of different operations without the need to break containment. This is particularly useful
when processing, toxic or highly potent compounds.

3
4.0 DATA AND RESULTS

Table 1.0 Table of Calibration Curve

Concentration of NaOH (M) Conductivity (mS/cm)

0.0500 10.7

0.0375 9.7

0.0250 7.5

0.0125 5.6

0.0000 4.0

Concentration of NaOH (M) vs Conductivity (mS/cm)

12
y = 140x + 4
10
Conductivity (mS/cm)

R² = 0.9898
8

6 Conductivity
Power (Conductivity)
4
Linear (Conductivity)
2

0
0 0.02 0.04 0.06
Concentration of NaOH (M)

Figure 1.0 Graph of Calibration Curve of Concentration of NaOH (M) vs Conductivity (Ms/cm)

4
Volume of NaOH = 3L

Volume of Et(Ac) = 3L

Temperature = 30 °C

Table 2.0 Table of Results

Concentration of
Conversion, X
Time Temperature Conductivity NaOH, CNaOH (M)
(%) (Self
(min) (°C) (mS/cm) (From calibration
calculation)
curve)
0 30 6.12 0.015143 0
5 30 5.40 0.01 33.96
10 30 4.58 0.004143 72.64
15 30 4.54 0.003857 74.53
20 30 4.50 0.003571 76.42
25 30 4.50 0.003571 76.42
30 30 4.46 0.003286 78.3
35 30 4.43 0.003071 79.72
40 30 4.43 0.003071 79.72
45 30 4.43 0.003071 79.72
50 30 4.43 0.003071 79.72
55 30 4.43 0.003071 79.72
60 30 4.43 0.003071 79.72

5
 Conductivity (mS/cm) vs Concentration of NaOH, M
0.016
y = 0.0071x - 0.0286
Conductivity (mS/cm) 0.014 R² = 1
0.012
0.01
0.008
0.006
0.004
0.002
0
4 4.5 5 5.5 6 6.5
Concentration of NaOH, M

Figure 2.0 Graph of Conductivity (ms/cm) vs Concentration of NaOH, M

Conversion, X vs. Reaction Time, t

100
y = 0.8362x + 43.422
90 R² = 0.46
80
Conversion (%)

70
60
50
40
30
20
10
0
0 10 20 30 40 50 60 70
Reaction Time (min)

Figure 3.0 Graph of Conversion, X vs. Reaction Time, T

6
5.0 ANALYSIS AND DISCUSSION

The objective of the experiment is to conduct mass balance and energy balance in batch
process system.

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. They were 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 experiment was begun by preparing 3L of 0.1 M sodium hydroxide, NaOH and 3L of
0.1M ethyl acetate, Et(Ac) solution. After that, these two solutions were mixed into reactor R1
through the charge port on the vessel cover. With an interval of 5 minutes, a sample was retrieved
from valve 1 to conduct a conductivity measuring using conductivity meter until the reading
constant. The conductivity values were continuously recorded until minute 60. Trend graphs were
plotted to represent the trend of results obtained.

Based on the results obtained, a table of calibration curve of concentration of NaOH (M)
against conductivity (mS/cm) was plotted from Table 1.0. Then, from the calibration graph, a linear
equation y = 140x + 4 were obtained. From the equation, the data for concentration of NaOH was
calculated while conversion (%) was calculated based on formulation stated in Appendix A. Next,
the value obtained through calculation of conversion were used to plot a graph of Conversion (%)
against reaction time, min.

7
 Table 2.0 showed the Conductivity against Concentration of NaOH. Concentration of
NaOH decreases when the conductivity of solution decreases. It can be said that the results
obtained obeys the theory of calibration curve as it decreases at 0.015143 M with conductivity of
6.12 mS/cm to 0.003071 M at conductivity of 4.43 mS/cm. Figure 2.0 illustrated the trend of results
of conductivity which is directly proportional to concentration of NaOH. The concentration of
NaOH decreases when conductivity of solution decreases. It shows that the result obtained obeys
the calibration curve.

Next, based on Figure 3.0 showed the plotted graph of Conversion (%) against the
reaction time, min. The value of conversion (%) were then calculated and were being plotted
against reaction time, min and the linear equation obtained from the graph is y = 0.8362x + 43.422.
At minute 0, conversion of solution is 0% while at minute 60, the conversion of solution is 79.72%.
Based on the graph, conversion increases as time increase. Conversion begun at minute 5 with
33.96% conversion and continuously increase until minute 30 with 78.3% conversion. Reaction
of batch process started to stabilize at minute 35 with conversion of 79.72%. The whole process
of conversion can be said that NaOH solution has being converted during the reaction of time. A
theory proved that as conductivity decrease, conversion increase (Ain, 2013). This can be clearly
seen in the graph.

The result obtained during this process was not fully obeyed the collision theory because
the temperature obtained is 30oC during the whole experiment. This is because the temperature
indicator at the batch reactor is malfunction. Based on the collision theory, particles of the
substances that are reacting have to collide in order for a reaction to take place. If they collide
with enough energy, then the particles will reacts. When the temperature of the reaction
increases, the particles will move vigorously. Thus, higher collision activity will take part. It will
then cause the molecules in the solution to collide with each other producing more energy, in
relation to higher reaction rate. Therefore, as temperature increase, rate of conversion is higher.

For every system, they must have their own advantages and disadvantages. The
advantage of using batch reactor are that it has high conversion per unit volume for one pass and
it has the flexibility of operation for the same reactor where same reactor can produce one product
at one time and a different product the next. Lastly, this reactor is easy to clean. The
disadvantages of using batch reactor are it has high operating cost and the product quality is more
variable than with continuous operation.

8
 During the experiment, there were some possible errors that may occur. Firstly, the
chemical preparation of dilution of NaOH and Ethyl Acetate may not accurate that may be disrupt
the results. Secondly, the reactor itself may be contaminated with other chemical causing
abnormal results. Lastly, the malfunctioned of temperature indicator may lead to slightly different
result from theory.

6.0 CONCLUSIONS AND RECOMMENDATIONS

The objective of the experiment is to conduct mass balance and energy balance in batch
process system. Based on result, concentration of NaOH decreases when the conductivity of
solution decreases. It can be said that the results obtained obeys the theory of calibration curve
as it decreases at 0.015143 M to 0.003071 M. The trend of results of conductivity showed in
graphs is directly proportional to concentration of NaOH. This is because, the concentration of
NaOH decreases when conductivity of solution decreases. Thus, the result obtained obeys the
calibration curve. Based on the graph, conversion increases as time increase. Conversion begun
at minute 5 and continuously increase after 30 minutes. Reaction of batch process started to
stabilize at minute 35 and the whole process of conversion can be said that NaOH solution has
being converted during the reaction of time. A theory proved that as conductivity decrease,
conversion increase. The result obtained during this process was not fully obeyed the collision
theory because the temperature obtained is 30oC during the whole experiment. This is because
the temperature indicator at the batch reactor is malfunction. Based on the collision theory,
particles of the substances that are reacting have to collide in order for a reaction to take place.
If they collide with enough energy, then the particles will reacts. When the temperature of the
reaction increases, the particles will move vigorously. Thus, higher collision activity will take part.
It will then cause the molecules in the solution to collide with each other producing more energy,
in relation to higher reaction rate. Therefore, as temperature increase, rate of conversion is higher.
The advantage of using batch reactor are that it has high conversion per unit volume for one pass
and it has the flexibility of operation for the same reactor where same reactor can produce one
product at one time and a different product the next. To conclude, this experiment achieved its
objectives.

9
 During the experiment, there were some possible errors that may occur. Firstly, the
chemical preparation of dilution of NaOH and Ethyl Acetate may not accurate that may be disrupt
the results. In order to minimize the errors that might happen while conducting the experiment,
students need to dilute NaOH and Ethyl Acetate accurately. The eye’s level must be in
perpendicular to the reading of the solution. Besides, the reactor itself may be contaminated with
other chemical causing abnormal results. So, the reactor need to be clean before conducting this
experiment to prevent any contaminants exists while reaction happens. Lastly, the malfunctioned
of temperature indicator may lead to slightly different result from theory. Thus, before conducting
any experiment, students need to ensure all the glassware or equipment in ready state which can
be used in order to prevent any inaccurate reading for that experiment.

10
7.0 TUTORIAL

1. Describe an example of industrial applications other than saponification that utilized batch
reactors in its process. Discuss the advantages and the disadvantages of using batch reactors in
chemical reaction.

Batch chemical reactors may be used to manufacture a variety of products. One of it

includes the margarine manufacturing process in which the production of fatty base for edible
margarines by the hydrogenation of vegetable oil is carried out in high temperatures.

But there are advantages and disadvantages of using batch reactors in chemical reaction.
The ultimate advantages of the batch reactor are the simplicity of the design that allows
tremendous flexibility, and integration of the performance equation over time. The simplicity of
design, usually a stirred tank, makes operation and monitoring easy for the majority of reactions.
The integrated form of the performance equation has variety of significance depending on the
particular reaction procedure being performed. This also makes the batch reactor to be cleaned
easily. Other than that, batch reactors can be used to produce small amount of products while still
in testing phase.

One of the disadvantages that are usually detected of the batch reactor has been the
labour required between runs for emptying and filling the tank. But this disadvantage is no longer
the main issue since the recent advances in computer control that was being added to it. Due to
computer control, the batch reactor should no longer be looked upon as something to be avoided.
The major disadvantage of batch reaction now is the hold-up time between batches. Although the
actual reaction time necessary to process a given amount of feed may be substantially less than
for a time-averaged reactor such as a CSTR, when the hold-up time is added, the total process
time may be greater. Other disadvantages of the batch reactor are dependent on the particular
type of reaction being considered, such as whether the reaction is in parallel or series.

11
2. Write a one-paragraph summary of any journal article that studies chemical reaction in a batch
reactor. The article must have been published within the last 5 years. Explain on the batch reactor
used in the study and its significance to the study done.

Reactor runaway occurs when an exothermic reaction takes place in a reactor with
insufficient heat transfer area. Designers need to know how they can choose the right criterion,
and the results can help with it. Selectivity and profit can be decreased if runaway occurs in a fed-
batch reactor. Fed-batch reactors are commonly used in chemical plants, where many products
are prepared through exothermic reaction steps, so mainly in pharmaceutical plants. These
reactors are stirred vessels, which are operated fed-batch. In fed-batch operation, at least one of
the reagents is fed continuously to the others, which already in the reactor to control the
temperature and selectivity of the operation. To reach high selectivity, temperature has to be
controlled, which is difficult if a highly exothermic reaction is carried out and the heat transfer is
limited, so a careful design of feeding trajectory are necessary. Optimal feeding trajectory can be
calculated to avoid runaway (causing high temperature and low selectivity) based on a specific
criteria. The reaction rate increases due to the temperature rise, causing a further increase in
reaction rate and temperature. Without any safety action, only the reactant consumption limits the
maximum temperature. One of the safety actions can be the application of runaway criteria to
characterize the safe operating regimes where the optimal operating conditions can be found.
The optimal feeding trajectory is determined in case a pilot plant fed-batch reactor using different
runaway criteria as a non-linear constraint based on particle swarm optimization and sequential
quadratic programming.

12
8.0 REFERENCES

Ain, N. (2013). Chemical reaction engineering. Retrieved March 4, 2018, from

https://www.slideshare.net/NurulAin45/chemical-reaction-engineering-28330576

Fogler, H. S. (2010). Scilab Code for Elements of chemical Reaction Engineering Book Details
Title: Elements of chemical Reaction Engineering. Retrieved from
https://scilab.in/files/textbooks/SantoshKumar/Fogler.pdf

Foutch, G. L., & Johannes, A. H. (2003). Reactors in Process Engineering. In Encyclopedia of

Physical Science and Technology (pp. 23–43). Elsevier. http://doi.org/10.1016/B0-12-
227410-5/00654-2

Kummer, A., & Varga, T. (2017). Feeding Trajectory Optimization in Fed-Batch Reactor with
Highly Exothermic Reactions. Computers & Chemical Engineering, 98, 1–11.
http://doi.org/10.1016/J.COMPCHEMENG.2016.12.008

Levenspiel, O. (1999). Chemical Reaction Engineering. Industrial & Engineering Chemistry

Research, 38(11), 4140–4143. https://doi.org/10.1021/ie990488g

Matthew, P. (2008). "Sensing Change in Batch Reactors. Chemical Engineering, 56-59.

13
9.0 APPENDICES

APPEDIX A: FORMULATION AND SAMPLE CALCULATION

1. Concentration of NaOH, CNaOH (M) (From Calibration Curve)

y = mx + c

y = 140x + 4

5.58 = 140x + 4

X = 0.012

2. Fractional Conversion, X (%)

𝐶𝑁𝑎𝑂𝐻 (𝑡=0)− 𝐶𝑁𝑎𝑂𝐻(𝑡)

X= 𝑥 100%
𝐶𝑁𝑎𝑂𝐻(𝑡=0)

0.015143−0.015143
= 𝑥 100%
0.015143

= 0%

14
APPENDIX B: Mass Balance

NaOH + C4H8O2 C2H3O2Na + C2H6O

0.6 mol

3L, 0.1M n1 NaOH n3 C2H3O2Na = 0.11916 mol

3L, 0.1M n2 C4H8O2 REACTOR n4 C2H6O = 0.18252 mol

n5 NaOH = 0.06084 mol

n6 C4H8O2 = 0.02916 mol

𝑛𝑜.𝑜𝑓 𝑚𝑜𝑙𝑒
Molarity =
𝑙𝑖𝑡𝑒𝑟𝑠 𝑜𝑓 𝑠𝑜𝑙𝑣𝑒𝑛𝑡

1) No. of mole = 3L x 0.1 M/L

= 0.3 mol of NaOH

2) No. of mole = 3L x 0.1 M/L

= 0.3 mol of C4H8O2

15
Determine the limiting reactant and excess reactant.

Sodium Hydroxide (NaOH) Ethyl Acetate, Et(Ac)

𝑚𝑎𝑠𝑠 𝑚𝑎𝑠𝑠
n= P=
𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 𝑣𝑜𝑙𝑢𝑚𝑒

Given, Given,

Mass = 12 g P = 1000 kg/m3

MW = 40 g/mol 1 𝑚ᶟ
V = 30 ml x = 0.00003 m3
10⁶ 𝑚𝑙
12 𝑔
n=
40 𝑔/𝑚𝑜𝑙 Mass = (1000 kg/m3)(0.00003 m3)
n = 0.3 mol Mass = 0.03 kg x (1000 g/1 kg)
Mass = 30 g
𝑚𝑎𝑠𝑠
n=
𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡

m = 30 g
MW = 88.11 g/mol
30 𝑔
n=
88.11 𝑔/𝑚𝑜𝑙

n = 0.34 mol

0.3 mol NaOH/ 0.3 mol 0.34 mol Et(Ac)/ 0.3 mol
=1 = 1.133

Thus, Sodium Hydroxide, NaOH is the limiting reactant while Ethyl Acetate, Et(Ac) is the excess
reactant.

16
 𝐧𝐍𝐚𝐎𝐇(𝐟𝐞𝐞𝐝)− 𝐧𝐎𝐮𝐭
3) Fractional conversion,f =
𝐧𝐍𝐚𝐎𝐇(𝐟𝐞𝐞𝐝)

0.3𝑚− 𝑛𝑜𝑢𝑡
0.7972 =
0.3𝑚

nOut = 0.06084 mol

n5 = 0.06084 mol

4) C balance

(0.3 mol)(0.6 mol)(4 mol C/1 mol C4H8O2) = (n3)(2 mol of C/1 mol C2H3O2Na) + (n4)(2 mol of
C/1 mol C2H6O) + (n6)(4 mol C/1 mol C4H8O2)

0.72 mol = 2n3 + 2n4 + 4n6

5) H balance

(0.3 mol)(0.6 mol)(1 mol H/1 mol NaOH) = (n3)(3 mol of H/1 mol C2H3O2Na) + (n4)(6 mol of
H/1mol C2H6O) + 0.06243(1 mol of H/1 mol NaOH) + (n6)(8 mol of H/1 mol C4H802)

0.18 = 3n3 +6n4 + 0.06084 + 8n6

6) O balance

(0.3)(0.6)(1 mol of Na/1 mol of NaOH) + (0.3)(0.6)(2 mol of O/1 mol of C4H8O2) = (n3)(2 mol of
O/1 mol of C2H3O2Na) + (n4)(1 mol O/1 mol C2H6O) + 0.06243 + (n6)(2 mol of O/C4H5O2)

0.9 mol = 2n3 + n4 + 0.06084 + 2n6

7) Na balance

(0.3)(0.6)(1 mol of Na/1 mol of NaOH)=(n3)(1 mol of Na/1 mol of C2H3O2Na)+0.006243

0.18 = n3 + 0.06084

n3 = 0.11916

17
From C balance,

0.72 mol = 2(0.11916) + 2(n4) + 4(n6)

0.72 mol = 0.23832 + 2(n4) + 4(n6)
0.48168 = 2n4 + 4n6 Equation 1

From H balance,

0.18 mol = 3(0.11916) + 6(n4) + 0.06084 + 8(n6) Equation 2

By using elimination method,

n4 = 0.18252
n6 = 0.02916

18