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SUMMARY

In this experiment, we have to carry out a saponification reaction


between NaOH and ethyl acetate in tubular flow reactor. We also need to
determine the reaction rate constant and determine the effect of residence
time on the conversion in a tubular flow reactor. We run this experiment at
six different flow rates of sodium hydroxide and ethyl acetate which are at
300mL/min, 250mL/min, 200 mL/min, 150mL/min, 100mL/min and
50mL/min. We also collect the data of inlet and outlet conductivity for these
six flowrates. Each of the flowrate performed, we take a 50mL sample at the
exit stream and mix it with 10mL of 0.25M hydrochloric acid. Then, we carry
out the titration using 0.1M of NaOH with the sample that has been mixed
with hydrochloric acid. The volume of NaOH required to neutralize that
sample is recorded in other to determine what exactly the amount of NaOH
that is unreacted. Besides that, from the calculation to determine the
conversion of sodium hydroxide and residence time, we plot a graph of
conversion versus residence time. From that graph, we will know what is the
effect of residence time to the conversion of sodium hydroxide.

INTRODUCTION
Every industrial chemical process is designed to produce economically
a desired product from a variety of starting materials through a succession of
treatment steps. The raw materials undergo a number of physical treatment
steps to put them in the form in which they can be reacted chemically. Then,
they pass through the reactor. The products of the reaction must then
undergo further physical treatment like separations, purifications and others
for the final desired product to be obtained.
Design of the reactor is no routine matter and many alternatives can
be proposed for a process. In searching for the optimum, it is not just the
cost of the reactor that must be minimized. One design may have low reactor
cost but the materials leaving the unit may be such that their treatment
requires a much higher cost than alternative cost.
There are three types of ideal reactors which are batch reactor, plug
flow reactor and continuous stirred tank reactor. Plug flow and continuous
stirred tank reactors are characterized as continuous flow reactor. Plug flow
or tubular reactors are always used in a continuous flow mode with reagents
flowing in and products being removed. They can be the simplest of all
reactor designs. Tubular reactors are often referred to by other names like
packed-bed reactor and bubble column reactors.
Tubular reactors may be empty for homogenous reactions or packed
with catalyst particles for heterogeneous reactions. Packed reactors require
upper and lower supports to hold particles in place. Uppermost packing is
often of inert material to serve as a pre-heat section. Pre-heating can also be
done with an internal spiral channel to keep incoming reagents close to the
heated wall during entry, as shown above.

It is often desirable to size a tubular reactor to be large enough to fit 8


to 10 catalyst particles across the diameter and be at least 40-50 particle
diameters long. The length to diameter ratio can be varied to study the
effect of catalyst loading by equipping the reactor with spools to change
this ratio.

THEORY
In a tubular flow reactor the composition of the fluid varies from point
to point along a flow path, consequently the material balance for a reaction
component must be made for a differential element of the volume dV. Thus,
for reactant A which in this case is sodium hydroxide, NaOH solution
becomes:
input = output + disappearance of A +
accumulation
Accumulation = 0
Input of A (mol/s) = FA
Output of A (mol/s) = FA + dFA
Disappearance of A by reaction (mol/s) = (-rA ) dV
Therefore, the equation above becomes:
FA = (FA + dFA) + (-rA) dV
Noting that:
dFA = d [FA0 (1 - XA)] = -FAO dXA
We obtain on replacement :
FA0 dXA = (-rA ) dV

The equation of reaction we perform in this experiment is:


CH3CO2C2H5 + NaOH C2H5OH +
For second order equimolar reaction with the same initial reactants
concentration (CA0 = CB0), the rate law is shown to be:
-rA = k CA CB = k CA2 = k
2
CA02/dV)
(1- X)
-rA = FA0 (dX
= V0 CA0 (dX/dV)

VTFR =

where X = extent of conversion


CA = exit concentration of reactant NaOH
V0 = total inlet flowrate of solutions
CA0 = inlet concentration of reactant NaOH in the reactor
For constant PFR volume, flowrate and initial concentrations, the reaction
rate constant is :
k=

Formula for residence time, :

= VTFR / V0

OBJECTIVE
1. To carry out saponification reaction between sodium hydroxide and
ethyl acetate in a Tubular Flow Reactor.
2. To determine the reaction rate constant.
3. To determine the effect of residence time on the conversion of Tubular
Flow Reactor

APPARATUS
1.
2.
3.
4.
5.
6.

Tubular Flow Reactor Apparatus


Beaker
Burette
Magnetic stirrer
Dropper
Retort stand

REAGENTS
1. Hydrochloric acid, HCL solution
2. 0.1M Sodium hydroxide, NaOH solution
3. Phenolphthalein

PROCEDURES
1. All valves are ensured to initially closed except valves V4, V8, and V17.
2. The following solutions are prepared:
a) 20 litre of sodium hydroxide, NaOH (0.1M)
b) 20 litre of ethyl acetate, Et(Ac) (0.1M)
c) 1 litre of hydrochloric acid, HCl (0.25M) for quenching
3. The feed tank B1 is filled with the NaOH solution and feed tank B2 with
the Et(Ac) solution.
4. The water jacket B4 and preheater B5 are filled with clean water.
5. The power of control panel is turned on.
6. Valves V2, V4, V6, V8, V9 and V11 are opened.
7. Both pumps P1 and P2 are switched on. P1 and P2 are adjusted to
obtain flow of approximately 300ml/min at both flow meters FI-01 and
FI-02. Both flowrates must be same.
8. Both solutions are allowed to flow through the reactor R1 and overflow
into the waste tank B3.
9. Valves V13 and V18 are opened. Pump P3 is switched on to circulate
water through pre-heater B5. The stirrer motor M1 is switched on the
speed is set to about 200rpm to ensure homogenous water jacket
temperature.
10.
To start experiment, valves V9 and V11 are opened.
11.
Both NaOH and Et (Ac) solutions are allowed to enter the plug
reactor R1 and empty into waste tank B3.
12.
P1 and P2 are adjusted to give constant flowrate of about
300ml/min at flow meters FI-01 and FI-02. The flowrates are recorded.
13.
The inlet (QI-01) and outlet (QI-02) conductivity values are start
monitoring until they do not change over time. This is to ensure that
the reactor has reached steady state.
14.
Both inlet and outlet steady state conductivity values are
recorded. The concentration of NaOH exiting the reactor and extent of
conversion are found from the calibration curve.
15.
Sampling valve V15 is opened and 50mL sample is collected. A
back titration procedure is carried out to manually determine the
concentration of NaOH in the reactor and extent of conversion.
16.
Steps 4-7 are repeated for different residence times by reducing
the feed flow rates of NaOH and Et(Ac) to about 250, 200, 150, 100
and 50 ml/min. Both flow rates are make sure to be the same.

RESULTS
Volume of Reactor, V = 400 mL
Concentration of NaOH in feed tank, CAO = 0.1 M
Concentration of Et (Ac) in feed tank, CB0 = 0.1 M

Total flowrate of
solution, V0

Residence Time, (min)

Inlet Conductivity
(mS/cm)

Outlet conductivity
(mS/cm)

Conversion, X

(mL/min)

Reaction Rate constant,


K (L/mol.min)

Rate of Reaction,
(mol/L.min)

Flowrate of
NaOH
300
250
200
150
100
50

Flowrate of Et(Ac)
(mL/min)

1
2
3
4
5
6

(mL/min)

No

Volume of 0.25M HCl = 10 mL

300
250
200
150
100
50

600
500
400
300
200
100

0.67
0.80
1.00
1.33
2.00
4.00

9.0
8.9
8.8
8.7
8.5
7.9

7.1
6.8
6.5
6.4
5.7
4.9

1.60
0.98
0.87
0.69
0.52
0.21

-40.0
612.5
66.9
16.7
5.42
0.7

-0.144
0.002
0.011
0.016
0.012
0.004

Flowrate of NaOH
(mL/min)
300
250
200
150
100
50

Volume of NaOH (mL)


9.50
12.60
13.40
14.80
16.40
20.60

Concentration of NaOH,
CAO (M)
0.260
0.198
0.187
0.169
0.152
0.121