PLUG FLOW REACTOR

(COIL TYPE)
OBJECTIVE:
Study the effect of flow rate on the conversion of saponification reaction of ethyl acetate with
aqueous sodium hydroxide solution.

REACTION:
NaOH + CH3 COOC2H5 CH3COONa + C2 H5 OH
(A) (B) (C) (D)
CHEMICALS REQUIRED:
N/10 Ethyl acetate ------ 20 litre
N/10 NaOH ------ 20 litre
N/10 HCl ------500 ml
N/10 Oxalic acid ----- 100 ml
Phenolphthalein indicator

APPARATUS / GLASSWARE REQUIRED:

A five conical flasks (250ml), measuring pipette, burette, stop-clock.

INTRODUCTION:
Real reactors do not satisfy the idealized flow patterns, back mix flow or plug flow deviation
form ideality can be due to channeling of fluid through the vessel, recycling of fluid within the
vessel or due to the presence of stagnant region or pockets of fluid in the vessel.

In an ideal plug flow reactor (PFR) there is no mixing in the direction of flow and complete
mixing perpendicular to the direction of flow. Concentration of the reactant varies along the
length of the reactor but not in the radial direction.

THEORY:
In case of a coil, turbulence is introduced due to frequent change in direction of flow and
presence of secondary flow, So higher value of, K is expected in case of a coil type PFR.

In a plug 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 volume dV. Thus for reactant A,
= 0(for steady-state flow reactor)
input = output + disappearance by reaction + accumulation (1)

Let, input of A, moles/time = F A

output of A, moles/time = FA+d F A
disappearance of A by reaction=

1
 moles A reacting
( r A V = (volume of t h e reactor )
( time )( volume of t h e fluid )

Introducing these three terms into Eq. (1), we obtain

F A = (FA+d F A) + (-rA)dV
Noting that,
d F A= - F A 0 d X A
We obtain on replacement
F A 0 dX A= ( r A d V

Rearranging, we get,
dV dX A
=
F A 0 (r A )
On integration,
Xf C Af
V dX A 1 d CA
= = = (2)
F A 0 C A 0 0 (r A ) C A 0 C (r A )
A0

Eq. (2) is the desired performance equation for a plug flow reactor.
For a second order equimolar reaction with the same initial reactants concentration ( C A0 C B 0
), the rate law is shown to be:

rA kC A C B kC A2 kC A2 0 1 X 2 (3)
dX dX
rA F A 0 V0 C A 0
dV dV (4)
FA 0 X dX FA 0 X
V PFR
kC A0 0 1 X 2 kC A0 1 X (5)
where
X = extent of conversion
CA = exit concentration of reactant NaOH (M)
V0 = total inlet flow rate of solutions (L/hr)
CA0 = inlet concentration of reactant NaOH in the reactor (M)
=residence time.
VPFR = Volume of Plug flow reactor.
For constant PFR volume, flow rate and initial concentrations, the reaction rate constant is,
V0 X
k
V PFRC A0 1 X (6)

2
Subsequently, for different reactor residence times, calculate the value of the reaction rate
constant, k and the rate of reaction, -rA.
2
Rate of reaction rA kC A (7)

DESCRIPTION:
The reactor is made up of SS tube and formed a helical coil. The set up consists of two feed tanks
through which two reactants are fed to the reactor. Rotameters are provided to measure the
individual flow rate of chemicals. The flow rate can be adjusted by the needle valves provided on
respective rotameter. The compressed air is used for circulation of feed. Constant temperature
water bath arrangement is provided to conduct the experiment at various temperatures. Pressure
regulator, pressure gauge and safety valve are fitted in the compressed air line. Products coming
out from the reactor are analyzed by chemical titration.

EXPERIMENTAL PROCEDURE:
1. Prepare 20L of N/10 NaOH solution by dissolving 80 gm of sodium hydroxide in 20L of
distilled water.
2. Prepare 20L of N/10 ethyl acetate solution by mixing 176 gm (or 196 ml) of ethyl acetate in
20L of distilled water.
3. With the help of standard oxalic acid, determine the normality of the NaOH solution taken in
the tank.
4. Using this standardized sodium hydroxide solution, determine the normality of hydrochloric
acid solution
5. Take 10 ml of N/10 hydrochloric acid in measuring cylinder.
6. Fill the burette by N/10 sodium hydroxide (Standard Solution).
7. Open valve V4 and V6, fill sodium hydroxide solution in feed tank A.
8. Open valve V5 and V7, fill ethyl acetate solution in feed tank B.
9. Close all the valves.
10. Fill the water in water bath.
11. Set the reaction temperature 50 oC by increment, decrement and set button of DTC.
12. Start the heater and stirrer of the bath and wait till constant temperature is attained.
13. Connect compressed air supply to the set-up at valve V1.
14. Open valve V1 and set air pressure 0.5 to 1 kg/cm2 by pressure regulator and pressure gauge.
15. Pass sodium hydroxide and ethyl acetate into the reactor by adjusting the flowrates of A and
B to be equal.
16. Start the stirrer of the reactor.
17. After about 10 min or time equal to the residence time of the reactor (which ever is greater)
collect exact 10 ml of the sample from the outlet in measuring cylinder that already contain
10 ml of hydrochloric acid.
18. Note down the reaction temperature.
19. Repeat the experiment for different flow rates of feed.

3
OBSERVATIONS & CALCULATIONS
Preliminary titrations:

Standardization of NaOH : -
Volume of Oxalic acid taken = 10 ml
Normality of Oxalic acid = -------- (given)
Volume of NaOH run down = --------ml.(titre value)
Normality of NaOH =
Standardization of HCl:-
Volume of HCl taken ,V1 = 10 ml.
Volume of NaOH run down ,V3 = -------- ml.
Normality of HCl =

Tabulation:

Observation Table:
S. No. Feed flow rate (LPH) Volume of NaOH
A B rundown, VNaOH (ml)

Calculation Table:
CA0 CA XA k (-rA)
(mol/lt) (mol/lt) (%) (min) mol/lt.min

GRAPH:
Plot a graph of conversion vs. residence time. Compare the conversion effect at different
residence times.

Model calculations:

CAO = A NA / ( A + B ) = --------------------(mol/lt)

( ( NV )HCl ( NV ) NaOH )
CA= (mol /l t)
sample volume

4
 = V*60 / ( A + B ) , (min)

V0 X
k ( )
V PFRC A0 1 X , mol . min
2
(- rA) = k C A (mol/lt.min)

PRECAUTION & MAINTENANCE INSTRUCTIONS:

1) Measure the exact volume of water and weight of chemicals
2) Keep close all the drain valves V8-V11 and vent valves V6-V7 should be open while
filling the reactant in feed tanks.
3) Flow should not be disturbed during the experiment.
4) Handle the chemicals carefully.
5) Do not ON the switch of the heater switch before filling water in the water bath.

RESULT:
1. Calculate the concentration of unreacted NaOH (mol/lit).
2. Determine the fractional conversion of NaOH at the end of the reaction.
3. Plot the conversion vs residence time.

5
BLOCK DIAGRAM:

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