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1.0
Title of Experiment
Effect Of Residence Time For Hydrolysis Reaction Of Ethyl Acetate In Turbular Flow Reactor
2.0
3.0
Objective
Introduction
Catalytic Tubular Reactor has been designed for experiments on chemical reactions in liquid phase
under isothermal and adiabatic conditions. The unit comes complete with a jacketed tubular reactor,
reactant feed tank and pump, temperature sensors and conductivity measuring sensors. The reactor will
enable students to conduct the acid-catalysed liquid-phase hydrolysis of ethyl acetate (EtAC) to ethanol
(EtOH) and acetic acid (HAc), using an immobilized anion ion-exchange resin as catalyst:
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FKKSA/BKF2741/Module/Rev01/2/08/10
Module 5:
TT
02
Q
02
TT
04
Hot Circulator
Glass
Beads
Reactor
Catalyst
Packing
TT
03
V3
FI
01
Q
01
Heat
Exchanger
TT
01
V2
V1
Drain
Peristaltic
Pump
V4
V6
Drain
V5
Drain
Feed Tank
Product Tank
Figure 1: Process flow diagram for the catalytic tubular reactor unit.
FA0
FA
FA(y)
V
FA(y +
y)
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FKKSA/BKF2741/Module/Rev01/2/08/10
Module 5:
To develop the TFR design equation, the reactor volume shall be divided into a number of subvolumes
so that within each subvolume V, the reaction may be considered spatially uniform. Assuming that the
subvolume is located a distance y from the entrance of the reactor, then FA(y) is the molar flow rate of A
into volume V and FA(y + y) is the molar flow rate of A out of the volume. In a spatially uniform
subvolume V,
rAdV rA V
(1)
For a tubular reactor at steady state, the general mole balance is reduced to,
dN A
dt
FA ( y ) FA ( y y ) rA V
(2)
In the above expression, rA is an indirect function of y. That is, rA is a function of reactant concentration,
which is a function of the position, y down the reactor. The volume, V is the product of the crosssectional area, A of the reactor and the reactor length, y.
V Ay
(3)
F ( y y ) FA ( y )
A
ArA
y
(4)
F ( y y ) FA ( y ) dFA
lim A
dy ArA
y 0
y
(5)
It is usually most convenient to have the reactor volume, V rather than the reactor length, y as the
independent variable. Accordingly, the variables Ady can be changed to dV to obtain this form of the
design equation for a TFR,
dFA
rA
dV
(6)
Note that for a reactor in which the cross-sectional area, A varies along the length of the reactor, the
design equation remains unchanged. This means that the extent of reaction in a plug flow reactor does
not depend on its shape, but only on its total volume.
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FKKSA/BKF2741/Module/Rev01/2/08/10
Module 5:
If FA0 is the molar flow rate of species A fed to a system operated at steady state, the molar flow rate at
which species A is reacting within the entire system will be [FA0X]. The molar feed rate of A to the
system minus the rate of reaction of A within the system equals the molar flow rate of A leaving the
system, FA . This is shown in mathematical form to be,
FA
FA0 FA 0 X
FA0 (1 X )
(7)
The entering molar flow rate FA0 is just the product of the entering concentration C A0 and the entering
volumetric flow rate v 0 ,
FA0
C A 0v 0
(8)
Combining Equation [4-7] and Equation [4-6] yields the design equation with a conversion term for the
TFR,
FA0
dX
rA
dV
(9)
Rearranging and integrating Equation 9 with the limit V = 0 when X = 0, we obtain the plug-flow
reactor volume necessary to achieve a specified conversion X,
V FA 0
X
0
dX
rA
(10)
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FKKSA/BKF2741/Module/Rev01/2/08/10
Module 5:
4.0
Experimental Procedure
4.1
Equipment
4.3
4.4
1. TFR
2. Beakers
3. Measuring Cylinders
5. Ethyl Acetate
6. Deionised water
4. Stop Watch
2.
Prepare a 20 liter of ethyl acetate solution by adding 800mL of ethyl acetate into 19.2 L of
deionised water.
3.
4.
Connect the water de-ionizer to the laboratory water supply. Fill up feed tank B1 with the
19.2 L of de-ionized water. Then add in 800mL of ethyl acetate to prepare the feed solution.
5.
2.
3.
Keep the cooling water circulating through the reactor while the stirrer motor is running to
allow the water jacket to cool down to room temperature.
4.
If the equipment is not going to be used for long period of time, drain all liquid from the unit.
Rinse the feed tanks with clean water.
5.
4.5
Experiment Procedures
1.
2.
3.
4.
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FKKSA/BKF2741/Module/Rev01/2/08/10
Module 5:
5.
Start monitoring the inlet (QI-01) and outlet (QI-02) conductivity values until they do not
change over time. This is to ensure that the reactor has reached steady state.
6.
Record both inlet and outlet steady state conductivity values. Find the concentration of HAc
exiting the reactor and extent of conversion from the calibration curve.
7.
Repeat the experiment (steps 4 to 6) for different residence times by changing the feed flow
rates of EtAC to 30, 50 and 60 mL/min.
5.0
Data Collection
1.
2.
3.
VTFR
v0
For a first order reaction with initial reactant concentration C A0 , the rate law is shown to
be:
rA kCA kCA0 (1 X )
rA FA0
VTFR
where: X
v0
k
dX
dX
v 0C A 0
dV
dV
X
0
v0
dX
ln(1 X )
(1 X )
k
= extent of conversion
Reactor volume
= _____ L
_____ M
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FKKSA/BKF2741/Module/Rev01/2/08/10
Module 5:
No.
Flow rate of
Residence
EtAC
time, (min)
(mL/min)
Inlet
conductivity
(mS/cm)
Outlet
conductivity
(mS/cm)
Exit
concentration of
HAc (M)
Conversion,
X (%)
1
2
3
4
5
6
7
8
9
10
4. For constant TFR volume, flow rate and initial concentrations, the reaction rate
constant is,
v0
ln(1 x)
VTFR C A0
5. For different reactor residence times, calculate the value of the reaction rate constant, k
and the rate of reaction, r A .
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FKKSA/BKF2741/Module/Rev01/2/08/10
Module 5:
Conductivity (mS/cm)
2.00
1.50
y = -0.0003x6 + 0.0101x5 - 0.1161x4 + 0.6709x3 - 2.0634x2 + 3.2862x
R = 0.9635
1.00
0.50
0.00
0.00
1.00
2.00
3.00
4.00
5.00
6.00
7.00
8.00
9.00
10.00
Concentration (mol/liter)
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FKKSA/BKF2741/Module/Rev01/2/08/10