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1. OBJECTIVE:
To study of a non-catalytic homogeneous reaction in a coil type plug flow reactor under
ambient conditions.
2. AIM:
To determine the rate constants for saponification of ethyl acetate with sodium hydroxide
(NaOH) at ambient temperature.
3. INTRODUCTION:
Real reactors do not satisfy the idealized flow patterns. Back mix flow or plug flow
deviation from ideality can be due to channeling of fluid through the vessel or due to the
presence of stagnant region or pockets of fluid in the vessel.
In the 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.
4. THEORY
In an ideal plug flow reactor (PFR) there is no mixing in the direction of flow(along the
length of the reactor) and complete mixing perpendicular to the direction of flow (in the
radial direction).
In case of a COIL, turbulence is introduced due to frequent change in direction of flow
and presence of secondary flow, so a higher value of k is expected in case of a COIL type
PFR.
PRODUCT
FEED V0,
CA0
V is the volume of the reactor; V0 is the volumetric feed rate,C A0 is the feed concentration
of A, and X is the degree of conversion .
XAF
dx
(1 X A )2
X AF
1
k C A 0 (1X AF )
When
CA 0
and
CB0
differ, then:
CB0
X A
C A0
( )
( )
1
ln
CB0
CB0
k C A0[
1]
(1 X A )
C A0
CA 0
X A=
( )
C A 0C A
CA 0
This experiment illustrates a bimolecular reaction (reacting species are ethyl acetate and
sodium hydroxide):
CH3COOC2H5 + NaOH CH3COONa + C2H5OH
(1)
(B)
(A)
-rA= k CACB
where A= NAOH and B = CH3COOC2H5
The initial concentrations of the reacting species are the same CA0= CB0 (neglecting
change in density)
-rA = kCA2
CA= CA0 (1- xA)
5. DESCRIPTION
The reactor is made up of SS tube. The tube is bent in the helical form. The air
compressed feed reactants are given through rotameters. The flow rate can be adjusted by
operating the needle valve provided on respective rotameter. The compressed air is used
for circulation of feed. The concentration of feed and the product coming out from the
reactor are analyzed by chemical titration and check the effect and the performance of the
reactor.
6. UTILITIES REQUIRED
Compressed Air Supply at 2 bar, 0.5 CFM
Water Supply
Drain
Electricity Supply: 1 Phase, 220 V AC, 0.5 kW
Apparatus: 10 and 20 ml pipettes, 50 cc burette, 6 No.100 cc titration flasks, 6 No. 50 cc
graduated cylinder, stop-watch
Chemicals:
Solution of ethyl acetate (N/10)
Solution of sodium hydroxide (N/10)
Solution of hydrochloric acid (N/10)
Indicator (phenolphthalein)
Quantity
10 L
10 L
1L
Few drops
7. EXPERIMENTAL PROCEDURE
1) Prepare 10 L of N/10 NaOH solution by dissolving 40 gm of NaOH in 10L of
water.
2) Prepare 10 L of N/10 ethylacetate solution by dissolving 88 gm of ethylacetate in
10L of water.
3) Check the drain valves of both feed tanks are closed and pressure regulator reads
zero pressure. Fill the tank A and B with appropriate reactants while keeping air
releasing valve open. Close the air releasing valves and tank feed inlet valves.
4) Open air inlet valve (from compressor), pull and adjust the pressure regulator to
1kg/cm2.
5) Adjust the rotameter A and rotameter B to adjust the flow rate of the two streams
in the feed mixture CA0 = CB0
6) Pass equimolar mixture of Ethylacetate and NaOH into the PFR by allowing equal
volumetric feed rates of reactant in to the reactor.
7) After about 10 min or time twice the residence time of the reactor (which ever is
greater) i.e. when steady state is achieved, collect exact 10 ml of sample of the
liquid at the outlet, in a graduated cylinder that already contains 10 ml of (chilled)
N/10 HCl. Transfer this solution (20 ml) in a 250 ml or 100 ml clean and dried
titration flask.
8) Titrate this solution against the N/10 solution of sodium hydroxide adding 1 drop
of phenolphthalein as indicator. When the endpoint of titration has been reached,
read the used volume of NaOH from the burette (VNaOH).
9) Note the volumetric flow rate of liquid at the end of the reactor. Note the reaction
temperature.
10) Repeat all the steps for five to seven for different flow rates of feed at the same
temperature.
8. SPECIFICATION
Reactor: Material stainless steel, capacity 0.7 liters (approx.) (Helical coiled tube type)
Feed Tank (2Nos.): Material stainless steel, capacity -20 liters
Feed Circulation: By Compressed air
Flow Measurement: Rotameter 2 Nos. (One Each for Reactants)
Piping: Material stainless steel and PVC
Pressure Regulator: 0-2 Kg/cm2
Pressure Gauge: Bourdon type 0-2 Kg/ cm2
Stop Watch: Electronic
9. FORMULAE
XA
a. Degree of Conversion :
b.
c.
V HCL
N HCLV
NaOH
K C A 0=
VR
Vo
N NaOH
Vsample
C A =
d. Rate constant
e.
Residence time
k=
gmol/L
C A 0C A
CA 0C A
C A 0 C A
XA
=
CA
1X A
CA 0CA
CA 0
V = L
CA0 = .. gmol/L
CB0 = .. gmol/L
VHCl = mL
Vsamp = mL
Observation Table:
S. No.
1
2
3
Vo, LPM
VNaOH
Calculation Table:
Run No.
, min
CA, gmol/L
k, l/(gmol.min)