Professional Documents
Culture Documents
CSTR Lab Report
CSTR Lab Report
The experiment is to study the effect of temperature and 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. After 1 minute the first 50mL sample of solution is collected and thus
undergo the titration process with 0.1M NaoH. The sample is taken again for minutes 5, 10, 15,
20, and 25 consecutively. 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. All the
result has been recorded, thus calculation is made and the graphs were plotted based on the
results. By the graph we can determine the rate of the reaction which is 2.1359L/mol.min and
1.0987L/mol.min respectively for 30°C and 40°C.
1
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.
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.
OBJECTIVE
To determine the effect of temperature on reaction rate constant, k for batch reaction and
determine the activation energy of saponification.
2
THEORY
The continuous stirred tank reactor or back mix reactor is a very common processing unit in
chemical and polymer industry. Its names suggest, it is a reactor in which the contents are well
stirred and uniform throughout. The CSTR is normally run at steady state, and usually quite well
mixed. The CSTR is generally modeled as having no spatial variations in concentrations,
temperature, or reaction rate throughout the vessel. Since the temperature and concentration are
identical everywhere within the reaction vessel, they are the same at the exits point as they are
elsewhere in the tank.
Assumptions in CSTR:
(Steady state is a situation, in which all the state variables remain constant despite
parallel processes trying to change them.)
3
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:
4
Effect of temperature on rate of reaction
Increasing the temperature can cause the rate of reaction also increase. An increase of 10 oC
typically doubles the rate of a reaction. In a chemical reaction, at low temperatures the molecules
collide with each other, but bounce apart. If, however, molecules collide at high temperatures,
bonds may be broken and new are molecules formed. Collision theory states that three conditions
must be met for a reaction to occur:
Molecules must collide with one another
Molecules must have the right orientation
Molecules must have sufficient energy
Every reaction has an energy barrier. The fact that a reaction increases with increasing
temperature suggests that only molecules with sufficient energy are able to react. The energy
barrier or minimum energy a molecule must possess to overcome this barrier is called activation
energy (Ea) which is can be shown in Arrhenius Law Equation:
k = A * e-Ea/RT
k = The rate constant
Ea = The activation energy
R = The gas constant
T = Temperature in Kelvin
A = Frequency factor constant or also known as pre-exponential factor or Arrhenius
factor.
5
Motor
stirrer Control
Panel
CSTR
V1
Drain
valve V2
Tank 1
Tank 2
Pump 1
Pump 2
V3
V4
PROCEDURE
General Start-up Procedure
6
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 tubings 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 . The timer was
started.
4. After 1 minute of reaction, 50 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 5, 10, 15, 20, and 25 minutes.
6. The experiment was repeated for temperature of .
Titration Procedures
7
2. 50 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.
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 tubings were cleaned properly as NaOH and Et(Ac)
are corrosive and could damage the tubings.
RESULTS
For temperature 30oC
8
Figure 1: graph of 1/CA vs time
Value of k based on the slope = 2.1359 L/mol.min and the order of reaction is 2nd order.
9
Figure 2: graph of 1/CA vs time
Value of k based on the slope = 1.0987 L/mol.min and the order of reaction is 2nd order.
10
Figure 3 : Graph of ln k vs 1/T
SAMPLE OF CALCULATIONS
To calculate CA at 30OC at 1 min
= 6.4 mL
V2 = VHCl - V1
= 10 mL - 6.4 mL
= 3.6 mL
11
n1 = CHCl x V2
= 0.0009 mol
N 2 = n1
= 0.0009 mol
= 0.018 mol/ L
= 55.556
12
- Ea/R = 6730K
Ea = -6730 K (8.314 J/mol.K)
= -55953.22 J/mol
DISCUSSION
NaOH + Et(Ac) →Na(Ac) + EtOH
The experiment was carried out by using special NaOH and Et(Ac). Order of the reaction
is referring to the powers of the concentration which are raised in the kinetic law. Moreover, 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 zero, first or second order. The rate law equation
of -rA can be modified into straight line equation y= mx+c.
From the result and calculations, the data was fitted to second order reaction. Hence the
rate law for both experiments is -rA= kCA2.The slopes of the graphs which represent the specific
reaction rate constant, k could also be obtained. All the calculated values as shown in table 3. For
the first temperature of 30oC, the value of k is 2.1359 L/mol/min whereas 1.0987 L/mol.min for
temperature 40oC. Furthermore, the value of -rA that we calculated also decreasing as temperature
increasing which is 0.0007 mol/L/min at 30oC and 0.0002 mol/L.min at 40oC.
Based on the equation, the value of rate constant should be increasing as the temperature
increasing. The errors in result is probably due to reading error at time 5 to 10 minutes at 30 oC
due to miscalculation or error that occurred during titration process. During titration, the volume
of NaOH needed to neutralize should be taken as soon as the sample turns into pink color. Result
could be affected if volume taken is slightly late than it should be.
Arrhenius Equation has been use to give the temperature behavior of the most reaction
rate constant within experimental accuracy over temperature range. A graph (Figure 3) was
plotted to find the value of -E/R. From the graph, the slope shown a straight line. The slope
13
indicated value of -E/R. The value of ln k 2 is higher that ln k1 which cause the positive value of
slope. Based on the equation obtained from the graph ln k vs 1/T , y = 6730x - 21.442, the value
of activation energy, E could also be calculated. Activation energy is important for the molecules
to use energy to complete the reaction. The value of activation energy obtained from this
experiment is -55.953 kJ/mol. Another way could also be used to calculate activation energy, by
By using from Arrhenius Equation which is ln (k 2/k1) = E/R (1/T1 - 1/T2). The E value calculated
is -52.415 kJ/mol. Both amount of activation energy are not too large for a reaction. The larger
the activation energy, the more temperature sensitive in the rate of reaction. Thus this shows that
the temperature is not too sensitive in the rate of reaction.
CONCLUSION
After all experiment has been done, first conclusion that can be made from this experiment was
this reaction was elementary and it is 2nd order. We concluded this by the graph 1/Ca versus
t(time) that has been plotted in Figure 1, 2 and 3. We get straight line graph that has a positive
slope value. Our second conclusions is the value of k is dependent on temperature and the rate
constant will only constant for a constant temperature. When the temperatures increase the value
of reaction rate also increase. This satisfied with the Arhenius’s Equation. We also conclude that
activation energy is constant for reactions that have a same concentration but different
temperatures. This has been proven by the equation ln (k2/k1)= E/R (1/T1-1/T2) and the graph
that we have plotted and we get almost the same values for both experiments. For overall
experiment, it can be considered as succeed because the effect of temperature and reaction can be
determined. This is because, the k values obtained were in positive values.
RECOMMENDATION
1. This experiment should be done in 4 different temperatures in order to get more accurate
results. Yet ours just in 3 different temperatures due to the maintenance problem occurred
during the experiment.
2. The apparatus should be clean thoroughly by using deionized water to avoid
contamination or defect in titration process.
3. The color of light pink that obtained in titration must be same for entire experiment to
avoid any variation in result.
REFERENCE
14
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) Aliff, (2006). Continuous Stirred Tank Reactor. Retrieved May 13, 2015 from
http://www.scribd.com/doc/36549783/Continuous-Stirred-Tank-Reactor-Cstr-2#scribd
4) Reaction kinetic studies in a mixed flow reactor. Retrieved May 13, 2015 from
http://solve.nitk.ac.in/dmdocuments/theory_Mixed%20Flow%20Reactor.pdf
5) Zarif, M. (2010). Continuous Stirred Tank Reactor. Retrieved May 13, 2015 from
http://www.scribd.com/doc/181148523/CONTINUOUS-STIRRED-TANK-REACTOR-
LAB-REPORT#scribd
APPENDIX
15