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The experiment involves a continuous stirred tank reactor (cstr). This experiment is to
determine the effect of temperature onto the reaction extent of conversion and to determine
the reactions activation energy. Firstly the reactor is filled with sodium hydroxide, NaOH
and Ethyl acetate, Et(Ac) until achieved 10 L. The flow rate of both solutions must same at
0.20 L/min. The solution is stirred and speed of 200 rpm. The water temperature is set at 50
C. The steady state conductivity and temperature values is recorded and then find the
concentration of NaOH in reactor and the extent of conversion from calibration curve. The
50ml sample is collected then carried out the back titration procedure immediately. The
experiment is repeated with different temperature; 55 C, 60 C and 75 C.
OBJECTIVES
-To carry out a saponification reaction between NaOH and Et(Ac) in CSTR 40 litre.
-To determine the effect of residence time onto the reaction extent of conversion.
-To determine the rate constant.
-To determine the reaction rate.
INTRODUCTION
Reactor is one of equipment used mostly in the industrials sector. It changes the raw material
into the desired product. A good reactor will give a high production and economical. One of
criteria to choose or to design a good reactor is to know the effectiveness of the reactor itself.
There a many types of reactor depending on the nature of the feed materials and products.
One of the most important we need to know in the various chemical reaction was the rate of
the reaction. The continuous stirred-tank reactor (CSTR) which is also known as vat- or backmix reactor usually is a common ideal reactor type in chemical engineering. A CSTR often
refers to a model used to estimate the key unit operation variables when using a continuous
agitated-tank reactor to reach a specified output. This reactor works for all fluids, liquids,
gases, and slurries. The behaviour of a CSTR is always modelled by that of a Continuous
Ideally Stirred-Tank Reactor (CISTR). All calculations performed with CISTRs assume
perfect mixing. In a perfectly mixed reactor, the output composition is identical to
composition of the material inside the reactor, which is a function of residence time and rate
of reaction. CSTR used in this experiment, (model: BP 143) is designed for students
experiments on chemical reaction in liquid phase under adiabatic and isothermal conditions.
CSTR consists of two tanks of solutions and one reactor. The reactor is modelled in order to
perform the saponification reaction between the sodium hydroxide and ethyl acetate.
Saponification reaction of ethyl acetate and sodium hydroxide produced sodium acetate in a
batch and the continuous stirred tank reactor evaluate the rate data needed to design a
production scale reactor.
THEORY
Reaction Kinetics
Reaction kinetics is the branch of chemistry that quantifies rates of reaction. An elementary
chemical reaction is a chemical reaction whose rate corresponds to a stoichiometric equation.
In symbols:
A+BC+D
and the reaction rate will be defined as:
-r = k (cA) (cB)
where k is referred as the specific reaction rate (constant). The overall order of reaction is
defined as:
n = +
The Mass Balance
Mass is a conservative entity, hence given a control volume V the sum of mass flows entering
the system will equal the sum exiting minus (plus) the consumed (generated) or accumulated
fractions:
Rate of mass in- rate of mass out+ rate of mass generated- rate of mass consumed = rate of mass
accumulation
shortly:
IN OUT + PROD CONS = ACC
Residence Time
The reactors residence time is defined as the reactor volume divided by the total feed flow
rates.
Residence time, =
Conversion
The conversion (or fractional conversion), denoted X, is a frequently used measure of the
degree of reaction. It i s defined as
X=
EXPERIMENTAL PROCEDURES
General Start-Up Procedures
1) The following solution is prepared:
a) 40 L of sodium hydroxide, NaOH (0.1 M)
b) 40 L of ethyl acetate, Et(Ac) (0.1M)
c) 1 L of hydrochloric acid, HCl (0.25M), for quenching
2) Ensure that all valves are initially closed
3) The feed vessels are charged as follow.
a) The charge port caps for vessels B1 and B2 is opened.
b) The NaOH is carefully poured into vessel B1 and Et(Ac) into B2.
c) The charge port for both vessels is closed.
4) The power for the control panel is turned on.
5) Check that there is sufficient water in thermostat T1 tank. Refilled is necessary.
6) Cooling water valves, V13 is opened and let the cooling water flow through the
condenser W1.
7) Adjust the overflow tube to give a working volume of 10 L in reactor.
8) Valves V2, V3, V7, V8 and V11 were opened.
9) The unit was ready to run the experiment.
: 100 mL NaOH
8) Open sampling valve V12 and collect 50 mL sample. Carry out a back titration
procedure to manually determine the concentration of NaOH in the reactor and extent
of conversion.
APPARATUS
1)
2)
3)
4)
5)
6)
RESULTS
Reactor volume
= 10 L
Flow rate
Of NaOH
(( C)
(ml/min)
Flow
rate
Of
Et(Ac)
(ml/min
)
Vol. of
NaOH
Titrate
d
Total flow
rate of
sol. F0
(ml/min)
Residenc
e time,
Conductivity
(min)
(mS/cm
)
(mL)
28.9
100
100
23.1
200
28.9
150
150
26.0
300
28.9
200
200
25.7
400
28.9
250
250
28.2
500
28.9
300
300
30.6
600
50
33
25
20
17
Exit
conc.
NaOH,
CNaOH,
(M)
Vol. of
unreacte
d
quenchin
g HCl
(mL)V2
Vol of H
reacted
with Na
in sam
(ml),V3
5.50
0.0038
9.24
0.76
5.09
-0.0020
10.40
-0.4
5.05
-0.0014
10.28
-0.2
5.03
-0.0064
9.28
-1.2
4.92
-0.0112
12.24
-2.2
Solution Mixture
Concentration Conductivity
Of NaOH (M) (mS/cm)
0.1 M NaOH
0.1 M Et(Ac)
H2O
0%
100 mL
100 mL
0.0500
12.83
25%
75 mL
25 mL
100 mL
0.0375
7.29
50%
50 mL
50 mL
100 mL
0.0250
3.42
75%
25 mL
75 mL
100 mL
0.0125
5.75
100%
100 mL
100 mL
0.0000
16.09
Rate Constant, k
k (M-1s-1)
ln k
1/T (C-1)
133.24
4.89
0.035
772.73
6.65
0.035
20.44x103
9.93
0.035
129.88
4.87
0.035
52.15
3.95
0.035
No
133.24
1.92 x 10-3
772.73
3.10 x 10-3
20.44x103
0.04
129.88
5.32
52.15
6.54 x 10-3
SAMPLE CALCULATIONS
Unknown quantity:
Concentration of NaOH in the reactor
CNaOH
mol/L
Volume of sample
Vs
50 mL
CNaOH,f
0.1 mol/L
Known quantities:
VHCl,s
CHCl,s
V1
CNaOH,s
10 mL
=
0.25 mol/L
mL
0.1 mol/L
Calculations:
Conc. of NaOH entering the reactor, CNaOH,0 =
Vol. of unreacted quenching HCl, V2
CNaOH,f
mol/L
x V1
mL
VHCl,s - V2
mL
(CHCl,s x V3)/1000
mol
n1
mol
n2/ Vs x 1000
mol/L
(1-
Residence time, =
= 10 L/(0.1+0.1) Lmin-1
= 50 min
Exit concentration of NaOH
CNaOH,0 =
CNaOH,f
0.05 mol/L
) x 100%
V2
V3
n1
x V1
0.1/0.25 x 23.1
9.24 mL
VHCl,s - V2
10 - 9.24
0.76 mL
(CHCl,s x V3)/1000
0.25 x 0.76/1000
1.9x10-4
n2
n1
1.9x10-4 mol
CNaOH
n2/ Vs x 1000
1.9x10-4/50x1000
0.0038 M
(1-
) x 100% =
=
Rate constant
k1
(0.1-0.0038)/50(0.0038)2
133.24 M-1s-1
Reaction rate
-rA
kCA2
k= 133.24
-rA
kCA2
(133.24)(0.0038)2
[1-(3.8x10-3/0.05)]x100%
92.4%