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UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA


REACTION ENGINEERING LABORATORY
(CHE506)

NAME : MOHAMAD SAIFULLAH BIN ABD HAMID


STUDENT NO. : 2017632158
GROUP : EH2205H / GROUP 1
EXPERIMENT 1 : CONTINUOUS STIRRED TANK REACTORS
DATE PERFORMED : 24.10.2018
SEMESTER :5
PROGRAMME / CODE : EH220 / CHE506
SUBMIT TO : MADAM MIRADATUL NAJWA BINTI MUHD
RODHI

No. Title Allocated Marks (%) Marks


1.0 Abstract/Summary 5
2.0 Introduction 5
3.0 Objectives/Aims 5
4.0 Theory 5
5.0 Materials and Apparatus 5
6.0 Procedures/Methodology 10
7.0 Results 10
8.0 Sample of Calculations 10
9.0 Discussion 20
10.0 Conclusion 10
11.0 Recommendations 5
12.0 References 5
13.0 Appendices 5
TOTAL MARKS 100

Remarks:

Checked by:

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Date:
1.0 ABSTRACT

The experiment is to study the effect of temperature and space reaction time and to
determine the relationship between reaction rate with conversion, reactor volume and feed rate.
The reaction started when Ethyl Acetate and Naoh were mixed with equal volume by using
continuous stirred tank reactor at 30°C (room temperature). After 5 minutes the first 5mL
sample of solution is collected. This sample will undergo the titration process with 0.1M NaoH.
The sample is taken again for minutes 10, 15, 20, and 25 respectively. The amount of NaoH
been used in that titration has been recorded in the result. The same procedures were repeated
for different temperature which are 40°C and 50°C. All the result has been recorded, thus
calculation is made and the graphs were plotted based on the results.
2.0 INTRODUCTION
Chemical kinetics and reactor design are important in producing almost all industrial
chemicals. The selection of a reaction system that operates in the safest and most efficient way
is the key to the success or failure of a chemical plant. Reactor is the equipment that changes
the raw material to the product that we want. A good reactor will give a high production and
economical. One of criteria to design or to choose a reactor knows the effectiveness of the
reactor itself. There are many reactors depending on the nature of the feed materials and
products. One of the most important we need to know in the various chemical reaction is the
rate of reaction. By combining endothermic and exothermic reactions in one reactor, a mutual
utilization of thermal energy involved in reactions is expected to produce a saving energy and
a cost-down for running in industrial reaction process.
The reactors, in which chemicals are made in industry, vary in size from a few cm3 to
the vast structures that are often depicted in photographs of industrial plants. For example, kilns
that produce lime from limestone may be over 25 metres high and hold, at any one time, well
over 400 tonnes of materials.
The design of the reactor is determined by many factors but of particular importance
are the thermodynamics and kinetics of the chemical reactions being carried out.
The two main types of reactor are termed batch and continuous.
In adiabatic reactor, no interchange of heat occurs between the system and
surroundings. Thus no heating and cooling medium are required. A chemical reactor is a vessel
where reactions are carried out purposely to produce products from reactants by means of one
or more chemical reactions. A chemical reactor may be characterized by the mode operation
according to the flow condition. In this experiment, the Continuous Stirred Tank Reactor has
been used to conduct a chemical process.

3.0 OBJECTIVES
EXPERIMENT A
To determine the effect of reaction rate at constant temperature
EXPERIMENT B
1. To determine the order of reaction
2. To determine the effect of temperature on reaction rate constant, k
3. To determine the activation energy of saponification
4.0 THEORY

Continuous stirred-tank reactors (CSTRs) are open systems, where material is free to
enter or exit the system that operate on a steady-state basis, where the conditions in the reactor
don't change with time. Reactants are continuously introduced into the reactor, while products
are continuously removed.
CSTRs are very well mixed, so the contents have relatively uniform properties such as
temperature, density, etc. throughout. Also, conditions in the reactor's exit stream are the same
as those inside the tank. Pictured below is a CSTR that has yet to be fitted with a stirring system.
A CSTR is normally used for a homogeneous liquid-phase reaction. In the laboratory,
it may also be used for a gas-phase reaction for experimental measurements, particularly for a
catalyzed reaction. The CSTR is used for gas-liquid reaction when a gas reacts with a liquid in
the liquid phase. The gas molecules move from the gas phase into the liquid phase. The gas is
introduced below the impeller. Gas-Liquid reaction will covered in later Section.
General mole balances:

Assumptions in CSTR:
1) Operate at steady state therefore,

(Steady state is a situation, in which all the state variables remain constant despite parallel
processes trying to change them.)
2) Well mixed therefore rA is the same throughout the reactor
3) Rearranging the generation

4) In terms of conversion

Reactor Sizing
Given –rA as a function of conversion, -rA = f(X), one can size any type of reactor. It can be
done by constructing a Levenspiel Plot which FAo / -rA or 1 / -rA as a function of X. For FAo
/ -rA vs. X, the volume of a CSTR can be represented as the shaded area in the Levenspiel Plots
shown below:
Equipment Design
CSTRs consist of a tank, usually of constant volume, and a stirring system to mix reactants
together. Feed and exit pipes are present to introduce reactants and remove products. Pictured
below is a CSTR that has had a portion of its side removed to show the interior.

A CSTR can also function as a loop reactor when a heated, pressurized fluid is injected into
the system to facilitate the stirring. This allows for higher heat and mass transfer rates while
simplifying maintenance because there is no agitator.

Usage Examples
Continuous stirred-tank reactors are most commonly used in industrial processing,
primarily in homogeneous liquid-phase flow reactions, where constant agitation is required.
They may be used by themselves, in series, or in a battery. CSTRs are also used in
the pharmaceutical industry as a loop reactor.
5.0 MATERIALS AND APPARATUS

1. Continuous-stirred Tank Reactor


2. Conical flask
3. 50 mL burette
4. 50 mL measuring cylinder
5. 0.25 M Hydrochloric Acid
6. 0.1 M Sodium Hydroxide
7. 0.1 M Ethyl Acetate
8. Phenolphthalein
9. Clamp burette holder
10. Dispenser

Figure 1: CSTR Figure 2: Phenolphthalein and


0.25M Hcl
6.0 PROCEDURES

General Start-up Procedure


1. The following solutions were prepared:
a) 20 L of sodium hydroxide, NaOH (0.1 M).
b) 20 L of ethyl acetate, Et(Ac) (0.1 M).
c) 1 L of hydrochloric acid, HCl for quenching (0.25 M).
2. All valves were initially closed.
3. Feed tanks were charged:
a) Charge port caps were opened for tanks T1 and T2.
b) NaOH solution was carefully poured into vessel T2 and Et(Ac) solution into vessel
T1.
c) The charge port caps were closed for both tanks.
4. The power was turned on for the control panel.
5. The heater was not switched on until it was fully submerged in the liquid. Liquid level
was maintained above the heater to avoid damage to the heater.
6. The stirrer assembly was secured properly to avoid damage to the mechanical seal.
7. All tubing’s were inspected periodically for leakage and worm out. Leakage might
cause damage to equipment by corrosive reactants

Experimental Procedures

1. Pump P1 was switched on to pump 1.25 L of 0.05 M Ethyl Acetate, Et(Ac), from the
feed tank into reactor. Pump P1 was switched on.
2. Pump P2 was switched on to pump 1.25 L of 0.05 M Sodium Hydroxide, NaOH, into
the reactor. Pump P2 was stopped when 2.5 L of total volume was reached.
3. The stirrer and the heater were switched on and temperature was set to be 30°C. The
timer was started.
4. After 5 minute of reaction, 5 mL of sample was collected from the reactor. The
sample was titrated with sodium hydroxide, NaOH.
5. Step 4 was repeated for reaction times of 10, 15, 20, and 25 minutes.
6. The experiment was repeated for temperature of 40°C and 50°C.
Titration Procedures

1. 10 mL of 0.25 M hydrochloric acid, HCl, was prepared in a conical flask.


2. 5 mL sample collected was added to the conical flask to quench the saponification
reaction.
3. 3 drops of phenolphthalein were added to the conical flask as indicator.
4. The mixture was then titrated with 0.1 M NaOH until it turned light pink
(neutralized).
5. The volume of NaOH used was recorded

General Shut-down Procedures

1. The cooling water valve from main pipe was kept open to allow the cooling water to
continue flowing.
2. Both pumps P1 and P2 were switched off. The stirrer and heater were switched off to
let the equipment to cool down to room temperature.
3. Cooling water valve from main pipe was closed.
4. The power for control panel was turned off.
5. After each experiments, the reactor tubing’s were cleaned properly as NaOH and
Et(Ac) are corrosive and could damage the tubing’s.
7.0 RESULTS
For temperature 30°C

Time (min) Volume of Volume of CA (mol/L) 1/CA (L/mol)


sample (mL) NaOH
used for
titration (mL)
0 5 20 0.100 10.00
5 5 20 0.100 10.00
10 5 19 0.020 8.33
15 5 21.4 0.072 13.89
20 5 20.4 0.092 10.87
25 5 20.8 0.084 11.90
Table 1: Volume of NaOH used for titration (mL) for 30°C

1/ CA vs Time
16
13.89
14
11.9
12 10.87
10 10
10 8.33 y = 0.101x + 9.5695
R² = 0.2459
1/CA

8
6
4
2
0
0 5 10 15 20 25 30
Time (min)

Graph 1: 1/CA vs Time (30°C)

Based on the slope, the k value is 0.101 L/mol.min and the order of reaction is second order .
For temperature 40°C

Time (min) Volume of Volume of CA (mol/L) 1/CA (L/mol)


sample (mL) NaOH
used for
titration (mL)
0 5 20 0.100 10.00
5 5 20 0.100 10.00
10 5 20.2 0.096 10.42
15 5 20.8 0.084 11.90
20 5 20.7 0.086 11.63
25 5 20.6 0.088 11.36
Table 2: Volume of NaOH used for titration (mL) for 40°C

1/CA vs Time
11.9
12
11.63

11.5 11.36

y = 0.0753x + 9.9443
11 R² = 0.6895
1/CA

10.42
10.5
10 10
10

9.5
0 5 10 15 20 25 30
Time (min)

Graph 2: 1/CA vs Time (40°C)

Based on the slope, the k value is 0.0753 L/mol.min and the order of reaction is second order.
For temperature 50°C

Time (min) Volume of Volume of CA (mol/L) 1/CA (L/mol)


sample (mL) NaOH
used for
titration (mL)
0 5 20.5 0.090 11.11
5 5 21.3 0.074 13.51
10 5 21.3 0.074 13.51
15 5 20.3 0.094 10.64
20 5 20.5 0.090 11.11
25 5 20.6 0.088 11.36
Table 3: Volume of NaOH used for titration (mL) for 50°C

1/CA vs Time
16
13.51 13.51
14
11.11 11.11 11.36
12 10.64
10
y = -0.0504x + 12.503
1/CA

8
R² = 0.1338
6
4
2
0
0 5 10 15 20 25 30
Time (min)

Graph 3: 1/CA vs Time (50°C)

Based on the slope, the k value is -0.0504 L/mol.min and the order of reaction is second
order.
Temperature, Specific Rate of ln k 1/T (K-1)
T reaction rate reaction, -rA (L/mol.min)
(K) constant, k (mol/min.L)
(L/mol.min)
303 0.1010 0.00101 -2.2926 0.003300
313 0.0753 0.00075 -2.5863 0.003195
323 0.0504 0.00041 -2.9878 0.003097

Table 4 : Calculated values of k, -rA, ln k and 1/T

ln k vs 1/T
0
0.00305 0.0031 0.00315 0.0032 0.00325 0.0033 0.00335
-0.5

-1

-1.5
ln k

y = 3417.2x - 13.548
-2 R² = 0.9881 -2.2926
-2.5863
-2.5
-2.9878
-3

-3.5
1/T (1/min)

Graph 4: ln k vs 1/T
8.0 SAMPLE OF CALCULATIONS

SAMPLE OF CALCULATION
i) To calculate volume of quenching HCl, V1 at minute 0:
V1 = (CNaOH / CHCl) x /Volume of titrated NaOH
= (0.1 mol L-1 / 0.25 mol L-1) x 20 mL
= 8 mL
ii) Volume of HCl reacted, V2 :
V2 = VHCl - V1
= 10 mL - 8 mL
= 2 mL
iii) Moles of reacted HCl, n1 :
n1 = CHCl x V2
= 0.25 mol/L x 2 mL x 1 L / 1000 mL
= 0.0005 mol
iv) Moles of unreacted NaOH in sample, n2:
N2 = n1
= 0.0005 mol
v) Concentration of unreacted NaOH, CNaOH:
CNaOH unreacted = n2 / volume sample
= 0.0005 mol/ 0.005 L
= 0.100 mol/ L
vi) 1/CA = 1/0.1 L/mol
= 10
vii) To find specific reaction rate constant, k
From the slope of the graph

viii) To calculate the rate of reaction, -rA


-rA = kCA2
= (0.101 L/mol.min) x (0.100 mol/L)2
= 0.00101 mol/L.min

ix) To calculate the activation energy from the reaction Ea


Temperature 303K and 313K
From the graph ln k vs 1/T, the equation for the best fit of the data between temperature 303
K and 313 K is
y = 2797.1x – 11.523 (calculated manually using the result because the graph shows the line
equation between 303 K to 323 K)
ln k = 2797.1 (1/T) - 11.523
and the slope of the line given is
- Ea/R = 2797.1K
Ea = -3417.2K (8.314 J/mol.K)
= -23255.09 J/mol

Temperature 313K and 323K


y = 4096.9x – 15.676 (calculated manually using the result because the graph shows the line
equation between 303 K to 323 K)
ln k = 4096.9 (1/T) - 15.676
- Ea/R = 4096.9K
Ea = -4096.9K (8.314 J/mol.K)
= -34061.63 J/mol

x) Activation energy from Arrhenius equation


Temperature 303K and 313K
ln (k2/k1) = E/R (1/T1-1/T2)
ln (0.0753/0.1010)/ (1/303 - 1/313) = E/(8.314)
E = -23153.29 J/mol
Temperature 313K and 323K
ln (0.0504/0.0753)/ (1/313 - 1/323) = E/(8.314)
E = -33746.63 J/mol
9.0 DISCUSSION

The experiment was carried out by using special NaOH and Et(Ac). Rate of reaction
for NaOH or any species as reactant could be found from the graph plotted using data. Firstly,
the order should be guess between zeros, first or second order. The rate law equation of -rA
can be modified into straight line equation y= mx+c. The order of reaction also can be
determined by the best fit line of graph.
From the data plotted, it shows that all the reaction is second order reaction because
the best fit line is plotted when using 1/CA vs Time. Hence the rate law for both experiments
is -rA= kCA2. The slope of the graph shows the rate constant of the reaction which is k value.
All the calculated values as shown in graph 1 which is for the first temperature of 30°C, the
value of k is 0.101 L/mol/min whereas 0.0753 L/mol.min for temperature 40°C. Furthermore,
based on graph 3, the k value for temperature 50°C is -0.0504 L/mol.min. The value of –rA is
decreasing as the temperature increasing which is 0.00101 mol/min.L for temperature 303 K,
0.00075 mol/min.L for temperature 313K and 0.00041 mol/min.L for temperature 323K.
Based on the theory, the –ra value should increasing when the temperature
increasing. This error is probably due to the miscalculation or the error occurred during the
titration process. The value of NaOH used must be taken as soon as the sample turn to light
pink during the neutralization process. If the sample turn to dark pink or pinky it show error
during the titration.
By using Arrhenius equation, the activation energy can be obtained. Based on the
slope of graph 4, it indicated the value of E/R. By using from Arrhenius Equation which is ln
(k2/k1) = E/R (1/T1 - 1/T2), the value of activation energy can be obtained. The activation
energy between the temperature 303K and 313K is -23153.29 J/mol while the activation
energy between the temperature 313K and 323K is -33746.63 J/mol so the total activation
energy for this reaction is -56899.92 J/mol. The larger the activation energy, the more
temperature sensitive in the rate of reaction.
10.0 CONCLUSION

As the conclusion, the reaction order for this reaction is second order reaction based
on the results obtained. This order of reaction is obtained by plotting the graph of 1/CA vs
Time at it shows the most best fit line when plotted. Furthermore, based on the results it shows
some error when the –ra value decreasing when the temperature increasing. Based on the theory
it should increasing due to temperature increasing. Its shows that the k value is dependent to
the temperature. Based on the activation energy calculated by using the Arrhenius law, it shows
not too large for the reaction and can be concluded that this reaction is not too sensitive to the
temperature. Arrhenius Equation has been use to give the temperature behavior of the most
reaction rate constant within experimental accuracy over temperature range. For overall
experiment, it can be concluded as successful experiment because all the objectives is fulfilled
which the order of reaction can be determined, the k value can be calculated and the activation
energy also can be calculated. By the results, it shows the effect of temperature and space
reaction time towards k value and order of reaction can be determined.

11.0 RECOMMENDATION

1. The color of light pink that obtained in titration must be same for entire experiment to
avoid any variation in result.
2. The experiment should be done in 4 or 5 temperature to get the accurate results.
3. The apparatus should be clean to avoid the contamination during the titration process.
4. The experiment should be done for a longer time to get the accurate results.
5. The CSTR should be cleaned monthly to avoid any error due to contamination during
the experiment.
12.0 REFERENCES

1. Stenstrom, M. K. (2003). Fundamentals of Chemical Reactor Theory. Los Angeles:


Civil and environmental Engineering Department.
2. Fogler, H. (2010). Continuous-Flow Reactors. In Essentials of Chemical Reaction
Engineering: Mole Balances (p. 4). Prentice Hall.
3. Reaction kinetic studies in a mixed flow reactor. Retrieved May 13, 2015 from
http://solve.nitk.ac.in/dmdocuments/theory_Mixed%20Flow%20Reactor.pdf
4. Chemical Reactors. Retrieved from:
http://www.essentialchemicalindustry.org/processes/chemical-reactors.html
5. Continuous Stirred Tank Reactors. Retrieved from:
http://encyclopedia.che.engin.umich.edu/Pages/Reactors/CSTR/CSTR.html
6. Zarif, M. (2010). Continuous Stirred Tank Reactor. Retrieved May 13, 2015 from
http://www.scribd.com/doc/181148523/CONTINUOUS-STIRRED-TANK-
REACTORLAB-REPORT#scribd
13.0 APPENDICES