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Journal andand
of Engineering Applied Sciences
Applied , Vol.
Sciences, 3, 3,
Vol. Issue (1)(1)
Issue November, 2016
May, 2016
Abstract
This work presents an experimental study of the saponi cation reaction of ethyl acetate by so-
dium hydroxide in a tubular reactor at 1 atmosphere (atm) of pressure. The objective of this study
is to analyze the effect of operating conditions on the rate constant and conversion in order to ex-
plore the tubular reactor performance. The temperature, reactant flow rate, and residence time are
the parameters considered for analyzing the reactor performance. The steady-state conversion is
achieved after a period of 30 minutes. Conversion decreases with the increased reactant flow rate,
owing to the resulting decrease in residence time. The rate constant rst decreases and then in-
creases with feed flow rate. The rate constant and conversion increase with increased temperature
within the studied temperature range. The residence time declines with increased reactants flow
rates leading to decreased NaOH conversion. The obtained NaOH conversion values at different
temperatures have been compared with literature data. The outcomes of this study may be useful
in maximi ing the conversion of ethyl acetate saponi cation reaction for industrial scale synthesis
.of sodium acetate and ethanol synthesis in a tubular reactor
Keywords Saponi cation; Plug flow reactor (PFR); Conductivity; Conversion; Hydrolysis.
Article history Received May 04, 2016, Accepted November 08, 2016
Al Mesfer, M.K. and Danish, M. Experimental Study of the Influence of Process Conditions on Tubular Reactor Performance
17
Journal of Engineering
Journal andand
of Engineering Applied Sciences
Applied , Vol.Vol.
Sciences, 3, Issue (1) (1)
3, Issue November, 2016
May, 2016
Al Mesfer, M.K. and Danish, M. Experimental Study of the Influence of Process Conditions on Tubular Reactor Performance
18
Journal of Engineering
Journal andand
of Engineering Applied Sciences
Applied , Vol.
Sciences, 3, 3,
Vol. Issue (1)(1)
Issue November, 2016
May, 2016
Al Mesfer, M.K. and Danish, M. Experimental Study of the Influence of Process Conditions on Tubular Reactor Performance
19
Journal of Engineering
Journal andand
of Engineering Applied Sciences
Applied , Vol.Vol.
Sciences, 3, Issue (1) (1)
3, Issue November, 2016
May, 2016
concentration 98.0 -100 were utili ed to temperature, the reactor coil is immersed
conduct the experiments. The distilled water in water, which is maintained at a xed
generated using distilled water unit (Type temperature by temperature controller. Water
2008,GFL) was used to prepare the solutions enters the reactor through non-return valve
of sodium hydroxide NaOH ( 0.1 M) and and this valve prevents water draining back
ethyl acetate CH3COOC2H5 ( 0.1 M). from reactor when pump is under switch off
position.
2.2 Experimental Setup The reactants i.e. NaOH and CH3COOC2H5
The tubular reactor (reactor coil enter the reactor coil from one end and leave
length—20.9 m; internal diameter—5.0x10-3 the reactor vessel through the other end of the
m; total volume of reactor V—0.41x10-3 m3) coil. The conductivity probe housing allows
obtained from Arm eld (U.K.) has been used the conductivity probe to be xed in the
for the experiments for the investigation stream of products mixture coming out from
as shown in Fig.1 and designed properly to the reactor coil. The progress of the hydrolysis
facilitate the detailed study. reaction is recorded by conductivity probe
The tubular reactor in which the chemical as the conductivity of solution varies with
reaction takes place made up of a pliable conversion. The conductance of the reaction
coil. The volume of the reactor in the form mixture varies with conversion. Priming
of coil is 0.41x10-3 m3. The conductivity vessel attached with reactor service unit is
and temperature sensors are inserted into used to ll the reactor coil and returned back
the gland for online data acquisition. In into the hot water circulator system. The
order to conduct an experiment at a xed reactants flow rates from the storage vessel
Al Mesfer, M.K. and Danish, M. Experimental Study of the Influence of Process Conditions on Tubular Reactor Performance
20
fixed using peristaltic pumps. Solutions of 0.1M m3 sec)
NaOH and 0.1M CH3COOC2H5 were used for performa
conducting the experiments; and the saponification fixed tem
reaction were performed at a fixed temperature of data were
30°C. Conductance of reaction mixture was recorded shows th
at 5-minute intervals until steady-state condition was with vario
Journal of Engineering
Journal andand
of Engineering Applied
Applied reached.
Sciences , Vol.
Sciences, The
3,
Vol. steady-state
Issue
3, (1)(1)
Issue May,condition
November, 2016 was reached after
2016
30 minutes as shown in Fig.2.
0.9
are controlled by using two peristaltic pumps; 0.85
Conductivity λt ( Siemens m)
Conductivity λt (Siemeens m)
reactants flow rate can be adjusted. 0.83 0.85
0.82
0.81
2.3 Experimental Procedure 0.8 0.8
0.76
conditions. Two peristaltic pumps were used
0.75
to pump the reactant from feed tanks and enter 0 3 6 9 12 15 18 0.7
6.5
the reactor vessel. The reactants pass through Time t x10-2 (sec)
Conductance of reaction mixture was recorded were obtained under steady state conditions.
Al Mesfer, M.K. and Danish, M. Experimental Study of the Influence of Process Conditions on Tubular Reactor Performance
21
Journal of Engineering
Journal andand
of Engineering Applied Sciences
Applied , Vol.Vol.
Sciences, 3, Issue (1) (1)
3, Issue November, 2016
May, 2016
280
6. Result
Conversion X
(m3 mol.sec)
0.8 0.5
260 0.18
reactor
0.17
conversio
240 higher (8
0.75 0.45 0.16 obtained
220 be due t
0.15
lower re
200 0.14 time incr
18 0.7 0.4
6.5 7 7.5 8 8.5 9 9.5 10 10.5 6.5 7.5 8.5 9.5 10.5 to increa
Reactants flow rate F x 107 (m3/sec) Reactants flow rate F x 107 (m3 sec)
The effec
OC2H5
Fig. 4: Variation of residence time and rate constant with performa
Fig.3: Effect of reactant flow rates on conductivity and reactants flow rate
iconversion
Effect of reactant flo rates on conducti ity Fig. 4: Variation of residence time and rate constant researche
and conversion suggested
ith3.3 Temperature
reactants flo rate temperat
The conductivity increases with reactant flow rate ijayara
contributed The experiment was conducted at a flow rate of
upto 0.818 Siemens m at flow rates of both reactants
n the other The toconductivity increases with with
reactant 3.3 Temperature
10.0x10 -7
m3 sec for both reactants i.e., NaOH and
equal 10.0x10-7 m3 sec as compared 0.773
o not. The -7 3 CH3COOC2H5. Concentration of both reactants was 0. 5
at a given flow rate upto 0.818 Siemens m at flowA
Siemens m at a flow rate of 6.67x10 m /sec. The experiment was conducted at a flow
adjusted e ual to 0.1 M NaOH and 0.1 M
decrease of conductivity with an increased feed flow 0.
l to that of rate of 10.0x10
CH3COOC -7
m3/sec for
2H5. Variation of both
rate reactants
constant i.e.,
and
rates of both the
rate signifies reactants equal
formation to desired
of less 10.0x10 -7
m3/
products.
tration and conversion with temperature is shown in Figure 5. It is 0. 5
The conversion curve shows a decline with increased
sec as compared with 0.773 Siemens45m at NaOH and
found that theCH COOC
reaction H . Concentration
conversion of
is a strong function
flow rate. Conversion reaches a value of at a 3 2 5
0.
a flow
flowrate
rate
of of 6.67x10
10.0x10 -7
m3in/sec.
m3 -7sec A decrease
comparison with a of reaction temperature, and variation
both reactants was adjusted e ual to 0.1 Mis almost linear.
Conversion X
0.4
0.5 Fig.6: Com
0.3 temperatu
(Wijayara
0.2 0.45
5 0 5 40 45
Fig. 4: Variation of residence time and rate constant with performance have not been explored by the
reactants flow rate
researchers (Ahmed et al. 2013) although it was
3.3 Temperature suggested that conversion increases with increased
temperatures of reaction mixtures (Ullah et al., 2015;
The experiment was conducted at a flow rate of ijayarathne et al., 2014).
10.0x10-7 m3 sec for both reactants i.e., NaOH and
CH3COOC2H5. Concentration Journal
Journal ofEngineering
both reactants
of Engineering
of andand
Applied
Applied
temperature
was Sciences 0.Vol.
, Vol.
Sciences,
isIssue
53, 3,
Issue
more
(1)(1)
profound
November,
May, 2016
than the change with
2016
320
adjusted e ual to 0.1 M NaOH and 0.22
0.1 M specific rate constant.
Residence time vs.reactant 0.
CH 3 COOC
reaction H Variation
2temperature,
5. of rate
flow rate and variation constant and
0.21is almost study (73.4 at 40atoC) and ittemperatures
may be due
conversion
300 with temperature is reactant
shownflow in Figure 5. It is The 0.results
5 obtained different of
Rate constant vs.
linear.
found that the reaction conversion is a strong
rate 0.2 function
reaction mixture have been compared
to the large volume of reaction mixture and with findings
of reported0.by Wijayarathne et al. 2014 as shown in Fig.
280reaction temperature, and variation is almost linear.
Residence time tR (sec)
Conversion X
6. Results reported by were
(m3 mol.sec)
260
1.2
0.18
0.75
Residence time increases with decreased
1.1 Rate constant vs. reactor 0.6volume of 0.44x 10-3 m3. The NaOH
Rate constant k x103 (m3 mol.sec)
temperature
0.17 0.7 flow rate
conversion
0.55
and this by
reported leads to increased
Wijayarathne al.reaction
et work
Current
V 0.41 L)
2014
(Volumeis
1
240 higher (80 at 40 oC) compared ijayarathne
with theet al.value
0.9 Conversion vs. 0.16
conversion.
obtained in
0.5 present study (73.4 at 40 o
VolumeC)Vand
0.44it
L)
2014 (
may
temperature 0.65
220 0.8 be due toThe effect
the large volume of of reaction
reaction mixturemixture and
0.15 0.45
lower reactant flow rate compared with. Residence
Conversion X
0.7 0.6
temperatures
time increases
0.4 ondecreased
with reactor flowperformance
rate and this haveleads
200 0.14
0.6 25 30 35 40 45
6.5 7.5 8.5 9.5 10.5
0.55
to increased
not been reaction
explored conversion
by the researchers
. (Ahmed
0.5 Temperature T (oC
Reactants flow rate F x 107 (m3 sec)
0.4 et effect
The al. 2013)
of reactionalthough it was suggested
mixture temperatures on reactor
Fig. 4: Variation of residence time and rate constant with 0.5 Fig.6: Comparison
performance have of NaOH conversion
not been at different
explored by the
reactants0.3
flow rate thattemperatures
conversion
researchers (Ahmed increases
of reaction
et
mixture withwith
al. 2013) although increased
literature data
it was
(Wijayarathne et al. 2014)
0.2 0.45 suggested that conversion increases with increased
3.3 Temperature
5 0 5 40 45
temperatures of reaction mixtures (Ullah et
temperatures of reaction mixtures (Ullah et al., 2015;
4. Conclusions
Temperature T (0C) al., 2015; etijayarathne
ijayarathne al., 2014). et al., 2014).
ture is more profoundThe experiment
than the change was conducted
with at a flow rate of
rate constant. 10.0x10 -7
m 3
sec for both reactants i.e., NaOH and In this investigation, hydrolysis of ethyl acetate ( 0.1
Fig.5:
Fig.5: RateRate constantconstant
and conversion andversusconversion versus
temperature curves
CH3COOC2H5. Concentration of both reactants was M)
0. 5 with sodium hydroxide ( 0.1 M) has been studied.
volume of 0.44x 10 -3
m 3
. The NaOH 10.65
atmosphere (atm) and a concentration of 0.1 M of
respectively.
1.2 The change in conversion 0.75 with both reactants. The influence of operating conditions
temperatureet of
on reported by Wijayarathne al. 40
2014°C. is The rate constant of 0.6
80 o
at 40 C) 1.1 compared with Rate constant vs.
the value
Rate constant k x103 (m3 mol.sec)
the
in present study (73.41
saponi
at 40 oC) cation
temperature
and it mayreaction increased 0.7 from 0.55
Current work (Volume
V 0.41 L)
to the large volume 0.9
of reaction
0.228x10 -3 mixture
vs. and
m3 mol.sec
Conversion to 1.081x10-3 m3/ 0.5
ijayarathne et al. 2014 (
0.65 Volume V 0.44 L)
eactant flow rate compared with. Residence
temperature
mol.sec
0.8 with
reases with decreased flow rate and this leads an increased temperature from 0.45
Conversion X
Al Mesfer, M.K. and Danish, M. Experimental Study of the Influence of Process Conditions on Tubular Reactor Performance
5 30 35 40 45 23
Temperature T (oC
Al Mesfer, M.K. and Danish, M. Experimental Study of the Influence of Process Conditions on Tubular Reactor Performance
24
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Vol. Issue (1)(1)
Issue November, 2016
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Al Mesfer, M.K. and Danish, M. Experimental Study of the Influence of Process Conditions on Tubular Reactor Performance
25