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This document contains the results of experiments conducted to study a batch reaction process in a batch reactor. Temperature was varied at 40°C, 50°C and 60°C. Samples were taken at regular intervals to measure conductivity which was then used to calculate concentration, conversion and kinetic parameters. Graphs were plotted and reaction order and rate constants were determined. The results show that increasing temperature leads to higher reaction rates as predicted by collision theory. Sources of error are also discussed.

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0% found this document useful (0 votes)
31 views21 pages

NO. Elements Page No

This document contains the results of experiments conducted to study a batch reaction process in a batch reactor. Temperature was varied at 40°C, 50°C and 60°C. Samples were taken at regular intervals to measure conductivity which was then used to calculate concentration, conversion and kinetic parameters. Graphs were plotted and reaction order and rate constants were determined. The results show that increasing temperature leads to higher reaction rates as predicted by collision theory. Sources of error are also discussed.

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andrias
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TABLE OF CONTENTS

NO. ELEMENTS PAGE NO.


1 SUMMARY 2
2 DATA & RESULTS 3 – 14
3 ANALYSIS & DISCUSSION 15-16
4 CONCLUSION 17
5 RECOMMENDATIONS 18
6 TUTORIALS 19
7 REFERENCES 20
8 APPENDICES

1
SUMMARY
The experiments of batch reaction process was to study the liquid phase reaction
kinetics in a batch reactor, to study the operation of a batch reactor at different operating
conditions in terms of conversion, to study the effect of temperature on the reaction in CSTR .
The variables involved in this experiment are time (min), temperature (C), conductivity
(mS/cm), concentration (M), and conversion (%).The experiment was begun by preparing the
chemicals 9L of 0.1 M Et (Ac) solution and 9L of 0.1 M NaOH solution. Then, necessary
steps were made to ready the batch reactor unit. 3L of 0.1 M Et (Ac) solution and 9L of 0.1 M
NaOH solution were poured into the reactor R1 through the charge port on the vessel cover.
Then, with intervals of 5 minutes, a sample was retrieved in order to determine the
conductivity value at temperature of 40 C, until the conductivity readings stabilized. The
experiment was then repeated with temperatures of 50 C and 60 C. The conductivity
values were continuously recorded until minute 30. Based on the result obtained, the
temperature and conductivity for each of temperature, 40C, 50C, and 60 C at 0
minutes till 30 minutes were recorded in each table respectively. Based on the figure 1 and 2,
it was a standard calibration curve of Concentration (M) against Conductivity (mS/cm) (figure
1) and Conversion (%) against Conductivity (mS/cm) (figure 2) was plotted. Then, from the
calibration graph, a linear equation were obtained. From the equation, the data for
Concentration of NaOH and Conversion (%) was calculated. Next, the values for -dCa/dt, ln
(-dCa/dt), ln (Ca), 1/Ca, and 1/T were obtained through calculations using the raw data from
the results table and related trend graphs were generated to portray the trend.As closure, based
on the collision theory, for a reaction to take place, the particles of the substances that are
reacting have to collide. If they collide with the enough energy then the particles will reacts.
When the temperature in the reaction was increases, the particles will move faster. Thus, the
collision take place will become higher .This will cause the molecules to collide with each
other producing more energy, in relation to higher reaction rate. Therefore, as the temperature
increases, the rate of conversion is higher too. There were possible errors that may occur.
Firstly, the chemical preparation of dilution NaOH and Ethyl Acetate may not accurate.
Secondly, the Batch may be contaminating with other chemicals. Other than that, the wires or
other equipment involved may be faulty. Other than that, time may be insufficient, causing
required data to not be obtained.

2
RESULTS
Experiment 1: Batch Saponification Reaction
Temperature : 400C
Table 1: Results of experiment 1

Time Temperature Conductivity Concentration of Conversion, X (-dCa/dt) ln (-dCa/dt) ln (Ca) 1/Ca


(min) (K) (mS/cm) NaOH (M) (%)

0 310.9 5.84 0.013464 73.4724 0 0 -4.307735822 74.2721331

5 309.4 5.18 0.008778 82.8048 0.0009372 -6.9726 -4.735506688 113.9211666

10 309.7 5.08 0.008068 84.2188 0.000142 -8.8596835 -4.819849659 123.9464551

15 310.2 4.93 0.007003 86.3398 0.000213 -8.454218392 -4.96141665 142.7959446

20 310.7 4.78 0.005938 88.4608 0.000213 -8.454218392 -5.126382903 168.406871

25 311.2 4.65 0.005015 90.299 0.0001846 -8.597319236 -5.295321858 199.4017946

30 311.5 4.53 0.004163 91.9958 0.0001704 -8.677361944 -5.481519311 240.211386

3
Experiment 2: Effects Of Temperature on the Batch Saponification Reaction
Temperature : 500C

Time Temperature Conductivity Concentration of Conversion, X (-dCa/dt) ln (-dCa/dt) ln (Ca) 1/Ca


(min) (K) (mS/cm) NaOH (M) (%)

0 311.6 7.84 0.027664 45.1924 0 0 -3.58762335 36.14806246

5 310.6 7.58 0.025818 48.8688 0.0003692 -7.904172055 -3.656683356 38.73266713

10 312.7 7.25 0.023475 53.535 0.0004686 -7.665761032 -3.751819254 42.59850905

15 313.9 7.2 0.02312 54.242 7.1E-05 -9.552830681 -3.767057235 43.25259516

20 315.6 7.16 0.022836 54.8076 5.68E-05 -9.775974232 -3.779417041 43.79050622

25 316.6 7.1 0.02241 55.656 8.52E-05 -9.370509124 -3.798247991 44.62293619

30 318.5 6.99 0.021629 57.2114 0.0001562 -8.764373321 -3.833720272 46.23422257

Table 2: Results of experiment 2 when the temperature was 500C

4
Temperature : 600C

Time Temperature Conductivity Concentration of Conversion, X (-dCa/dt) ln (-dCa/dt) ln (Ca) 1/Ca


(min) (K) (mS/cm) NaOH (M) (%)

0 313.9 7.69 0.026599 47.3134 0 0 -3.626881658 37.59539832

5 312.5 7.58 0.025818 48.8688 0.0001562 -8.764373321 -3.656683356 38.73266713

10 314.7 7.19 0.023049 54.3834 0.0005538 -7.498706947 -3.770132894 43.38583019

15 317.9 7.1 0.02241 55.656 0.0001278 -8.965044016 -3.798247991 44.62293619

20 320.9 6.99 0.021629 57.2114 0.0001562 -8.764373321 -3.833720272 46.23422257

25 322.9 6.58 0.018718 63.0088 0.0005822 -7.448696527 -3.978269651 53.42451117

30 325 6.52 0.018292 63.8572 8.52E-05 -9.370509124 -4.001291473 54.66870763

Table 3: Results of experiment 2 when the temperature was 600C

5
GRAPHS

Figure 1 – Concentration of NaOH (M) vs Conductivity


Slope = 0.0071 , y-intercept= 0.0280

Figure 2 – Conversion vs Conductivity


Slope = -0.1414 , y-intercept= 1.5605

6
Figure 3 – ln [-dCa/dt] vs ln CA @ 40 C
Slope = -1.0313 , y-intercept= -3.0199
Order of Reaction, 
ln [-dCa/dt] =  [ln CA]+ ln k
 = slope, m
 = -1.0313
Rate Constant
ln [-dCa/dt] =  [ln CA] + ln k
ln k = C
k = ln-1 C
k = ln-1 [-3.0199]
k = 0.04881

7
Figure 4 – ln [-dCa/dt] vs ln CA @ 50 C
Slope = -1.1191 , y-intercept= -3.0991

Order of Reaction, 
ln [-dCa/dt] =  [ln CA]+ ln k
 = slope, m
 = -1.1191
Rate Constant
ln [-dCa/dt] =  [ln CA] + ln k
ln k = C
k = ln-1 C
k = ln-1 [-3.0991]
k = 0.045089

8
Figure 5– ln [-dCa/dt] vs ln CA @ 60 C
Slope =- 0.9552 , y-intercept= -3.4380

Order of Reaction, 
ln [-dCa/dt] =  [ln CA]+ ln k
 = slope, m
 = -0.9552
Rate Constant
ln [-dCa/dt] =  [ln CA] + ln k
ln k = C
k = ln-1 C
k = ln-1 [-3.4380]
k = 0.032129

9
Figure 6 - Conversion vs Time @ 40 C

Figure 7- Conversion vs Time @ 50 C

10
Figure 8- Conversion vs Time @ 60 C

11
Figure 9 – 1/CA vs Time @ 40 C
Slope =25.473, y-intercept= 49.959
k =25.473

Figure 10 – 1/CA vs Time @ 50 C


Slope =1.5440, y-intercept= 36.021
k=1.5440

12
Figure 11– 1/CA vs Time @ 60 C
Slope =2.9804, y-intercept= 33.602
k =2.9804

Figure 12 – ln k vs 1/T
Slope =-0.6157, y-intercept= 3.1241

Saponification Reaction’s Activation Energy, E


ln k = (-Ea/R)(1/T) + ln A

13
Y = mX +C
(-Ea/R) = Slope, m=-0.6157
Ea = -R  m
=5.1112

Arrhenius Constant, A
ln k = (-Ea/R)(1/T) + ln A
Y = mX +C
ln A = C
A = ln-1 C
A = ln-1 [3.1241]
A = 22.7394

14
DISCUSSIONS
The purpose of the experiment Batch Reaction Process were to study the liquid phase
reaction kinetics in a batch reactor, to study the operation of a batch reactor at different
operating conditions in terms of conversion and to study the effect of temperature on the
reaction in CSTR.
The experiment was begun by preparing the chemicals 9L of 0.1 M Et (Ac) solution and
9L of 0.1 M NaOH solution. Then, necessary steps were made to ready the batch reactor unit.
3L of 0.1 M Et (Ac) solution and 9L of 0.1 M NaOH solution were poured into the reactor R1
through the charge port on the vessel cover. Then, with intervals of 5 minutes, a sample was
retrieved in order to determine the conductivity value at temperature of 40 C, until the
conductivity readings stabilized. The experiment was then repeated with temperatures of 50
C and 60 C. The conductivity values were continuously recorded until minute 30. Trend
graphs were plotted to represent the trend of results obtained.
Based on the result obtained, the temperature and conductivity for each of temperature,
40C, 50C, and 60 C at 0 minutes till 30 minutes were recorded in each table respectively.
Based on the figure 1 and 2, it was a standard calibration curve of Concentration (M) against
Conductivity (mS/cm) (figure 1) and Conversion (%) against Conductivity (mS/cm) (figure 2)
was plotted from the Appendix A. Then, from the calibration graph, a linear equation y =
0.0071x – 0.028 and y = -0.1414x + 1.5605 were obtained. From the equation, the data for
Concentration of NaOH and Conversion (%) was calculated. Next, the values for -dCa/dt, ln
(-dCa/dt), ln (Ca), 1/Ca, and 1/T were obtained through calculations using the raw data from
the results table and related trend graphs were generated to portray the trend.
Basically , from the graphs in for – ln [-dCa/dt] Vs ln CA for 40 C, 50 C and 60C in
figure 3, figure 4 and figure 5 respectively ,the slope of the graph showed value at -1.0313,
-1.1191 and -0.9552 respectively. Meanwhile the value for y-intercept showed was -3.0199,
-3.0991 and -3.4380 respectively. From the slope and y-intercept of the graph for all the
temperatures, the value of order of reaction, and rate constant, k can be determined. The
value for order of reaction,  for 40 C, 50 C and 60C were -1.0313, -1.1191 and -0.9552
respectively while the rate constant ,k value were 0.04881,0.045089 and 0.032129
respectively.

15
Besides that, from the graph for Conversion against Time at 40C,50C and 60C in
figure 6,figure 7 and figure 8 respectively, it can observe that the value for the conversion for
all the three temperatures was increasing with time where the value in 40C start to increase
from 73.4724% to 91.9958%. Meanwhile for 50C, the conversion starts to increase from
45.1924 % to 57.2114 %. For the temperature 60C, the conversion starts to increase from
47.3134% to 63.8572 %. Based on the collision theory, for a reaction to take place, the
particles of the substances that are reacting have to collide. If they collide with the enough
energy then the particles will reacts. When the temperature in the reaction was increases, the
particles will move faster. Thus, the collision take place will become higher .This will cause
the molecules to collide with each other producing more energy, in relation to higher reaction
rate. Therefore, as the temperature increases, the rate of conversion is higher too.
Next , based on the graph plotted in figure 9, figure 10 and figure 11 for 1/Ca against
time for 40C,50C and 60C, the rate constant, k was determine from the slope value. It was
then, the saponification reaction’s activation energy, Ea and Arrhenius constant, A was
calculated from the slope and intercept values by using Arrhenius equation. From the graphs
generated in figure 12, the value for Activation Energy, Ea calculated was 5.1112 and a value
of 22.7394 was obtained for the Arrhenius Constant.
There were several advantages of using the batch reactors in chemical reaction. The
batch reactor has high conversion per unit volume for one pass. Furthermore, the flexibility of
the operation same reactor can produce one product at one time and a different product for the
next. It is also easy to clean compare to the other reactors. However, the batch reactor also has
its own disadvantages such as high operating cost. Besides that, the product quality was more
variable than with continuous operation.

There were several possibility errors that may contribute to the inaccurate result and
abnormal trend of graph throughout the experiment. Firstly, the chemical preparation of
dilution NaOH and Ethyl Acetate may not accurate that leads to disrupt results.Secondly, the
Batch may be contaminating with other chemicals that leads to abnormal results. Other than
that, the wires or other equipment involved may be faulty. When this happens, the panel will
not display the correct value and could even disrupt the whole process of the experiment.

16
Other than that, time may be insufficient, causing required data to not be obtained. With this
problem, current data will not be enough, and will affect the resulted trend graph.

17
CONCLUSIONS

The purpose experiments of batch reaction process was to study the liquid phase
reaction kinetics in a batch reactor, to study the operation of a batch reactor at different
operating conditions in terms of conversion, to study the effect of temperature on the reaction
in CSTR . Based on the result obtained, the temperature and conductivity for each of
temperature, 40 C, 50 C, and 60 C at 0 minutes till 30 minutes were recorded in each table
respectively. Based on the figure 1 and 2, it was a standard calibration curve of Concentration
(M) against Conductivity (mS/cm) (figure 1) and Conversion (%) against Conductivity
(mS/cm) (figure 2) was plotted. Then, from the calibration graph, linear equations were
obtained. From the equation, the data for Concentration of NaOH and Conversion (%) was
calculated. Next, the values for -dCa/dt, ln (-dCa/dt), ln (Ca), 1/Ca, and 1/T were obtained
through calculations using the raw data from the results table and related trend graphs were
generated to portray the trend.As closure, based on the collision theory, for a reaction to take
place, the particles of the substances that are reacting have to collide. If they collide with the
enough energy then the particles will reacts. When the temperature in the reaction was
increases, the particles will move faster. Thus, the collision take place will become higher
.This will cause the molecules to collide with each other producing more energy, in relation to
higher reaction rate. Therefore, as the temperature increases, the rate of conversion is higher
too.

18
RECOMMENDATIONS

There were few recommendations in order to overcome the possible errors. Firstly, the
chemical preparation of dilution NaOH and Ethyl Acetate should be prepared carefully so that
the disrupted results can occur. Secondly, the Batch must be cleaned before and after the
usage to prevent contaminations. Other than that, the wires or other equipment involved must
undergo frequent maintenance. Other than that, time must be sufficient to prevent required
data to not be obtained.

19
TUTORIALS
1. Describe an example of industrial applications other than saponification that
utilized batch reactors in its process.
Manufacture of margarine applied the utilized batch in its process. The production of the
fatty base for edible margarines by the hydrogenation of vegetable oils is carried out at
high temperatures and has serious disadvantages, among them the toxicity of the nickel
catalysts and afire-hazardous filtration stage. Here, a batch reactor and selective, low
loaded palladium catalyst was described which allow vegetable oil hydrogenation to take
place at lower temperatures producing high quality, pure hydrogenated fat, free of catalyst.
Under these milder conditions, the thermal decomposition of oils and fats does not form
secondary products, and heavy metals from the catalyst do not enter the final product. In
addition, even lower hydrogenation temperatures can be used with the palladium catalyst,
resulting in fat with low Transisomer content. The catalyst has been tested successfully in
full-scale production. Using an inertial separator in a batch reactor, catalyst loss has been
eliminated.

2. Write down the function of each following component in a batch reactor used in this
experiment.

Component Function
Stirrer To stir the mixture in the reactor so that the mixture composition was
homogenous and well mixed. Besides that, the function was to distribute the heat
to all the mixture and achieve thermal equilibrium.

Thermocouple It was a sensor to measure the temperature in the heater and reactor.

Temperature Temperature controller is a measurement device used on temperature control.


Controller Thermocouple-type and resistor-type temperature controllers measure
temperature electronically, obtaining the temperature change from the sensor
and sending the measured data to the electronic processor. The output device
will then control the temperature variation within a specific range.

REFERENCES

20
Batch Reactor. (2015) Wikipedia. [Online].[Accessed 31 March, 2015]. Available from
World Wide Web: http://en.wikipedia.org/wiki/Batch_reactor

Chemicals Reactor. (2014) Enzyme Technology. [Online].[Accessed 31 March, 2015].


Available from World Wide Web:
http://www.essentialchemicalindustry.org/processes/chemical-reactors.html

Chemicals Reactor. (2011) Chemical Wisc Online Library. [Online].


[Accessed 31 March, 2015]. Available from World Wide Web:
http://jbrwww.che.wisc.edu/home/jbraw/chemreacfun/ch4/slides-matbal.pdf

Rutherford Aris, Elementary Chemical Reactor Analysis, Butterworth-Heinemann, 2013,


p150

Smith,J.M, Chemical Engineering Kinetics, McGraw Hill, 1981

21

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