1.

Abstract

The purpose of conducting this experiment were to carry out saponification reaction between
Sodium Hydroxide, NaOH and Ethyl Acetate, Et (Ac), to determine the reaction rate constant
and to determine the effect of residence time on the conversion. Plug flow reactor (Model: BP
101) was used in this experiment. Feed flow rate of the NaOH and the Et(Ac) was set to be the
manipulated variable where the flow rates were varied to 50 ml/min, 100 ml/min, 150 ml/min,
200 ml/min, 250 ml/min and 300 ml/min. General start up procedure was performed before
conducting the experiments. Initially, P1 and P2 were adjusted to give a constant flow rate of 300
ml/min. Then, the flow rates were recorded. Both inlet and outlet conductivity were monitored
until they constant did not change with time in order to ensure that the plug reactor has reached
steady state. 50 ml sample was collected. The sample was mixed with 10 ml Hydrochloric acid,
HCl and three drop of phenolphthalein. Volume of titrated NaOH was recorded and tabulated in a
table. Then, the procedures were repeated for each different flow rates. From the data collected,
the value of reaction rate constant and rate of reaction is calculated. Then, a graph of conversion
factor against residence time is also plotted. From the graph we can see that the conversion factor
is directly proportional to the residence time where, as the residence time increased, the
conversion factor also increased. Besides that, the result also showed that as the feed flow rates
decreased, the volume of titrated NaOH and the percentage of conversion were increased while
the reaction rate constant decreased.

1.2

Introduction

In chemical engineering, a chemical reactor design deals with multiple aspects of chemical
engineering and chemical reactions. As designers they will always ensure that the reaction held
in the reactor proceeds with the highest efficiency towards the desired output product and
producing the highest yield of product that required the least amount of money to purchase and
operate (Schmidt & Lanny, 1998).
Chemical reactors are vessels that contain chemical reaction. Different types of chemical,
biological and physical processes take place in reactors and the degree of mixing and residence
time in reactors affect the degree of completion of reactions within the reactor (Dey, Herzog, &
Srinivasan, 2007). The plug flow reactor model (PFR) is one of the chemical reactors that used to
describe chemical reactions in continuous, flowing system of cylindrical geometry. According to
Mann (2009), it is used mostly to predict the behaviour of chemical reactors of such design, so
that the key reactor variables, such as the dimension of the reactor can be estimated.
A plug flow reactor (PFR) is a type of chemical reactor where the influent is pumped into the
pipe. The feed enters at one end of a cylindrical tube and the product stream will leaves at the
other end. In ideal plug flow reactor, there is no mixing and the fluid elements will leave in the
same order they arrived (Denbigh & Turner, 1984). So that, the fluid entering the reactor at time
t will exit the reactor at time t + 1 , where

is the residence time of the reactor.

Figure 1 Schematic Diagram of Plug Flow Reactor

Plug flow reactors are usually operate in adiabatic or nonisothermal condition where water at
controlled temperature is circulated through the tank to maintain constant reactant temperature
(Fogler, 2014). Besides that, plug flow reactor also usually operated at steady state where the
reactants are continually consumed as they flow down the length of the reactor.
There are some features of a plug flow reactor such that the flow of the reactor is laminar, the
properties of the reaction medium like pressure temperature, reactant and product concentrations
are the same throughout the entire cross section of flow. All the elemental volumes of the
reaction medium remain in the reactor for the same period of time and the change in
concentration, temperatures and pressure with time are identical for each elemental volume.
Besides that, there are also temperatures and reactant concentration gradients along the length of
the reactor and the rate of chemical reactions vary along the length of the reactor.

1.3

Aims

The objectives of this experiment are to:

i.
ii.
iii.

To carry out a saponification reaction between NaOH and Et(Ac)

To determine the reaction rate constant
To determine the effect of residence time on the conversion

1.4

Theory

Plug flow reactor (PFR) consist in a long, straight pipe in which the reactive fluid transits at
steady-state where no accumulation occur. The feed will enters at one end of a cylindrical tube
and the product stream leaves at the other end. The long tube and the lack of provision for
stirring prevent complete mixing of the fluid in the tube. Therefore, the properties of the flowing
stream will be different from one point to another in both radial and axial directions.

Figure 2 Flow direction in plug flow reactor

Specific assumptions are mode about the extent of mixing in plug flow reactor. First, there is no
mixing in the axial direction or in the direction of flow. Second, complete mixing occur in the

radial direction and the last one is a uniform velocity profile is across the radius. The special
characteristic of this reactor is there is an absence of longitudinal mixing.
But, the validity of the assumptions will depend on the geometry of the reactor and the flow
conditions. There is two type of deviation for these assumptions:
i.
ii.

Mixing in longitudinal direction due to vortices and turbulence

Incomplete mixing in radial direction in laminar flow conditions

1.4.1 Rate of Reaction

Rate of reaction can be roughly defined as the rate of disappearance of reactants or the rate of
formation of products. When a chemical reaction is said to occur, a reactant (or several)
diminishes and a product (or several) produced. This is what constitutes a chemical reaction. For
example
aA + bB cC + dD

(Equation 1.1)

Where A and B are reactants and C and D are products. In this reaction, A and B is being
diminished and C and D is being produced. Rate of reaction is related with how fast the reactants
diminish or how fast the product is formed. Rate of reaction of each species corresponds
respectively to their stoichiometric coefficient. Such that:
r A
a

r B
b

rC
c

rD
d

(Equation 1.2)

Rate of equation for reactant A is:

r A

= k CA CB

(Equation 1.3)
6

Where,
k

=rate constant
CA

= concentration of A species

CB

=concentration of B species

=stoichiometric coefficient of A

=stoichiometric coefficient of B

The rate expression can be shown to be

-rA = k [A] [B]

(Equation 1.4)

1.4.2 Conversions
Taking species A as the basis, the reaction expression can be divided through the stoichiometric
coefficient of species A, hence the reaction expression can be arranged as follows:
b
c
d
A + B+ C + D
a
a
a

(Equation 1.5)

Conversion is an improved way of quantifying exactly how far has the reaction moved, or how
many moles of products are formed for every mole of A has consumed. Conversion X A is the
number of moles of A that have reacted per mole of A fed to the system. As seen below:
X A=

moles of A reacted
moles of A fed

(equation 1.6)

1.4.3 Residence time distribution function

The residence-time distribution (RTD) of a reactor is a characteristic of the mixing that occurs in
the chemical reactor. This omission is reflected in the RTD since there is no axial mixing in a
plug flow reactor. The residence time is determined experimentally by injecting an inert
chemical, molecule or atom called a tracer into the reactor at some time t = 0 and then the tracer
concentration, C is measured in the effluent stream as a function of time. The tracer should have
physical properties similar to those of the reacting mixture and be completely soluble in the
mixture. Besides that, it also should not adsorb on the walls or other surfaces in the reactor. In an
ideal plug-flow reactor, all the atoms of material leaving the reactor have been inside it for
exactly the same amount of time. The time the atoms have spent in the reactor is called the
residence time of the atoms in the reactor.

1.5

Apparatus

1.5.1 Apparatus:
1)
2)
3)
4)
5)
6)

Solteq plug flow reactor (Model: BP101)

Burrete
Conical flask
Measuring cylinder
Beakers
pH indicator

Figure 3 SOLTEQ Plug Flow Reactor (Model: BP101)

1.5.2 Materials:
1)
2)
3)
4)

1.6

0.1M sodium hydroxide, NaOH

0.1M ethyl acetate, Et(Ac)
0.1M hydrochloric acid, HCl
De-ionised water

Procedure

1.6.1 General Start-up Procedures

1

All the valves were ensured closed except V4, V8 and V17.

The following solutions were prepared: 20 liter of NaOH (0.1M) 20 liter of Et(Ac)
(0.1M)1 liter of HCL (0.25M) for quenching

Feed tank B1 was filled with NaOH while feed tank B2 was filled with the Et(Ac).

The water jacket B4 was filled with water and pre-heater B5 was filled with clean
water.
9

The power for the control panel was turned on.

Valves V2, V4, V6, V8, V9 and V11 were opened.

Both pumps P1 and P2 were switched on. P1 and P2 were adjusted to obtain flow rate
approximately 300mL/min at both flow meters Fl-01 and Fl-02. Both flow rates were
made sure to be equal.

Both solutions then were allowed to flow through the reactor R1 and overflow into
waste tank B3.

Valves V13 and V18 was opened. Pump P3 then was switched on in order to circulate
the water through pre-heater B5. The stirrer motor M1 was switched on and set up to
speed about200 rpm to ensure homogeneous water jacket temperature.

1.6.2 Experiment Procedures

1. The general starts up procedures were performed.
2. Valves V9 and V11 were opened.
3. Both the NaOH and Et(Ac) solutions were allowed to enter the plug reactor R1 and
empty into the waste tank B3.
4. P1 and P2 were adjusted to give a constant flow rate of about 300 ml/min at flow
metersFI-01 and FI-02. Both flow rates were ensured same. The flow rates were
recorded.
5. The inlet (QI-01) and outlet (QI-02) were started to monitor the conductivity values
until they do not change over time. This is to ensure that the reactor has reached
steady state.
6. Both inlet and outlet steady state conductivity values were recorded. The
concentration of NaOH exiting the reactor and extent of conversion from the
calibration curve.

10

7. Optional: Sampling was opened from valve V15 and 50ml of sample was collected. A
back titration procedure was carried out manually to determine the concentration of
NaOH in the reactor and extent of conversion.
8. The experiment was repeated from step 4 to 7 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 were made sure to be equal.
1.6.3 Titration Procedures
1. The burette was filled up with 0.1 M NaOH solution.
2. 10 mL of 0.25 M HCl was poured in a flask.
3. 50 mL samples that were collected from the experiment at every controlled flow
rate (300,250, 200, 150, 100 and 50 mL/min) were added into the 10mL HCl to quench
the saponification reaction.
4. 3 drops of phenolphthalein were dropped into the mixture of sample and HCl.
5. The mixture then was titrated with NaOH until it turns light pink.
6. The amount of NaOH titrated was recorded.

11

1. 1.7

Result

2.
6.

9.

12.

15.

21.

18.
19.

5.

7.

10.

13.

16.

22.

23.

26.

29.

27.

30.

28.

31.

RE

24.

20. V
O

OUTLET
CONDUCTIVITY
(ms/cm)

25. C
O

8.

11.

14.

17.

FL

32.

(m

O
N

O
H

(
%

T
R
I
12

T
A
T
E
D
(
m
L

55.

66.

34.

35.

36.

37.

)
38.

39.

40.

41.

42.

43.

45.

46.

47.

48.

49.

50.

51.

52.

53.

54.

Q1

60. 2

61.

62.

63. 9

64.

65.

6.8

52.

4.0

75.

76.

6.1

1.7

56.

57.

58.

59.

30

30

60

6.

67.

68.

69.

70.

25

25

50

8.

13

0
71. 1

72.

73.

6.5

%
74. 8
3

0
77.

88.

78.

79.

80.

81.

20

20

40

89.

90.

91.

92.

15

15

30

82. 1

83.

84.

6.2

85. 8

86.

87.

6.4

1.1

97.

98.

5.5

7.9

108.

109.

6.4

3.3

119.

120.

9.6

0
93. 1

94.

95.

5.9

%
96. 8
8
%

0
99.

110.

100.

101.

102.

103.

0
104.

10

10

20

21.

105.

106.

5.5

111.

112.

113.

114.

115.

116.

117.

50

50

10

23.

5.2

0
0
121. Table 1.7

14

107. 9

%
118. 9
6
%

122. 1.8

Calculations

123.

Volume of sample, Vs

124.

Conc. NaoH in feed vessel, CNaOH,r : 0.1 mol/L

125.

Vol. HCl quenching, VHCl,s

126.

Conc. HCl standard soln, CHCl,s

: 0.25 mol/L

127.

Conc. NaOH for titration, CNaOH,s

: 0.1 mol/L

128.

: 50 mL

: 10 mL

129.

(A) Sample: flowrate

=
300 mL/min of NaOH

130.
&
131.
300 mL/min of Et(Ac)
132.
134.

133.
(B) Volume of titrating NaOH

=
23.50 mL = 0.02360 L

135.
137.

136.

(C) Volume of quenching HCl

unreacted

with

NaOH

C NaOH ,std
C HCl ,std

in

sample

x Volume of NaOH

titrate
138.

=
0.1mol / L
0.25mol / L

139.

x 0.02360L
=

9.44 x 10-3 L
140.
142.

141.
15

(D) Volume of HCl reacted with

VHCl volume of quenching HCl

NaOH in sample

unreacted with
143.
NaOH in sample
144.

=
10 mL 9.44 mL

145.

=
0.56 mL

146.

=
0.56 x 10-3 L

147.
149.

148.
(E) Mole of HCl reacted with

=
CHCl,std x volume of HCl reacted with

NaOH in sample

NaOH in
150.
sample
151.

=
0.25 mol/L x (0.56 x 10-3) L

152.

=
140 x 10-6 mol

153.
154.
156.

155.
(F) Mole of NaOH unreacted in

=
Mole of HCL reacted with NaOH in

sample

sample
157.

=
140 x 10-6 mol

158.
159.
(G)

160.
Concentration

of

NaOH

unreacted with Ethyl Acetate,

CA
16

s
V

Mole of HCl reacted

161.

=
140 106 mol
0.05 L

162.

=
2.8 x 10-3 mol/L

163.
164.
(H)

165.
Steady

state

fraction

conversion of NaOH (XA)

CA
C AO

166.

=
1

2.8 103 mol/ L

0.1 mol/ L

167.

=
0.972 x 100%

168.

97.2%
169.
170.
172.

171.
(I)

Concentration

of

NaOH

=
CNaOH,O (G)

reacted with Ethyl Acetate

173.

=
0.05 mol/L (2.8 x 10-3) mol/L

174.

=
0.0472 mol/L

17

175.
177.

176.
(J) Mole of NaOH reacted with

=
(I) x Vs

Ethyl Acetate in sample

178.

=
0.0472 mol/L x 0.05 L

179.

=
2.36 x 10-3 mol

180.
181.
(K)

182.
Concentration

of

Ethyl
(J )
Vs

Acetate reacted with NaOH

183.

=
3

2.36 10 mol
0.05 L
184.

=
0.0472 mol/L

185.
187.

186.
(L)

Concentration

of

Ethyl

=
CEA,O (K)

Acetate unreacted, CB

188.

=
0.1 mol/L 0.0472 mol/L

189.

=
0.0528 mol/L

190.
194.

191.
(M) Residence time,

=
V CSTR
F0

192.
195.
193.
18

4.0 L
0.3 L/min +0.3 L/min
196.

=
6.6667 min

197.
198.
199.

V0 = Total inlet flow rate = 600 mL/min =

0.6 L/min
200.

VTFR = Volume for reactor = 4 L

201.

CAO = Inlet concentration of NaOH = 0.1 M

202.

203.

(N) Reaction rate constant, k

V0
X
(
)
V TFR C A 0 1X

204.

=
0.6 L/min
0.972
(
)
(4 L)(0.1 M ) 10.972

205.

=
52.07 L/mol.min

206.

207.

=
k(CA0)2 (1 X)2

(O) Rate of reaction, -rA

208.

=
52.07 (0.1)2 (1 0.972)2

209.
4.08 x 10-4 mol/L.min
The calculation above were repeated for all

210.
flow rates and graph was plotted.

19

211.

212. Graph 1.8 Conversion VS Residence Time

213.
214.
215.
216.
217.
218.
219.
220.
221.
222.
223.
20

224.
225.
226. 1.9
Discussion
227.
228. In this experiment, saponification reaction between NaOH and Et(Ac) were
carried out in the plug flow reactor. These two solutions react together in the plug
flow reactor to complete saponification reaction. The main objective is to study the
effect of residence time on the conversion and to determine the reaction rate
constant. Plug Flow Reactor (PFR) was used in this experiment where it is a type
of reactor that consists of a cylindrical pipe and is usually operated at steady state.
The feed which is NaOH and Et(Ac) enter at one end of a cylindrical tube and
leaves product from the end of cylindrical tube. At the end of the experiment, we
are able to calculate the reaction rate constant by using specific formula and can
determine the effect of residence time on the conversion in the plug flow reactor.
229.
230. The experiment is started by running up the equipment in order to start the
saponification process. For this experiment we set the flow rate of both solutions
as the varying components while the flow rate of both solutions is controlled by
the temperature of the reactor. We set the flow rate to 300mL/min, 250mL/min,
200mL/min, 150mL/min, 100mL/min and 50mL/min for both components.
231.
232. Based on the result obtained, in order to determine the reaction rate constant and
the rate of the reaction for the saponification process we used this following
formula:
233.
234. The rate of reaction can be determined by applied this formula:235.
236. -rA = k CA2(1-X)2
237.
238. While, the reaction rate constant can be calculated using this formula:239.
v0
X
k
=
240.
V TFR C AO 1X

241.

21

242. The residence time and conversion of NaOH are calculated and tabulated in table
1.7. For the residence time,

, of 6.6667 min, the conversion of NaOH is

97.2%. For the next 8th minute of residence time, the conversion of NaOH
dropped to 83.0%. As for the 10.0000 minute of residence time, the conversion of
NaOH increased for 3.6% from 83.0% at 8.0000 minute to 86.6% at 10 th minute.
As the residence time increases to 13.3333 min, conversion of NaOH has a sudden
increase to 88%. The conversion of NaOH was further increased to 92.8% at the
residence time of 20.0000 minute. Lastly, at 40.0000 min of residence time, the
final conversion of NaOH obtained was at 96.0%. All these data of conversion and
residence time was plotted into graph and shown in graph 1.8.
243.
244. By analyzing the graph plotted, we can say that the conversion factor is inversely
proportional from 6.6667 minute of residence time to 8.000 minute of residence
time and directly proportional from 10 minute residence time to 40 minute
residence time. Initially, it shows a drop of NaOH conversion from 6.6667 minute
to 8.000 minute of residence time. This is due to error while performing the
experiment where the sample might be exposed to long before titration is
performed. As for the rest of the graph chart, the conversion of NaOH show that it
is gradually increases with residence time. Residence time was defined as the
length of time the fluid would stay in the reactor while conversion is a property
that shows how much of the reaction has taken place. The longer the reactants
would stay in the reactor, more products would be formed. The data mainly shows
that the longer the residence time, the percentage of conversion increases and this
obey the expected result where the longer time left in the reactor, more reaction
occurs between NaOH and Et(Ac).
245.
246. The reaction rate constant for total flow rate 600ml/min is 52.07 Lmol/min while
flow rate 500 ml/min is 6.10 L.mol/min. Next, for flow rate 400ml/min, 300
ml/min and 200 ml/min the rate constant are 6.46 L.mol/min, 5.5 L.mol/min and
6.4 L.mol/min respectively. The reaction rate constant is 6.0 L.mol/min for flow
rate 100 ml/min. From the reaction rate constant we determined, we can see that
the value of reaction rate constant is decreased as the flow rate is decrease. These
22

shows that the reaction rate constant is depend to the flow rate flow in the plug
flow reactor.
247.
248. 1.10

Conclusion

249. As a conclusion, the objective of this experiment is successfully achieved.

Saponification reaction between NaOH and Et(Ac) was obtained in the reactor. By
using a plug flow reactor, these two substances were flowed into the reactor and
mixed together for a certain period of time to complete the saponification process.
Both reaction rate constant and effect of residence time on the conversion was also
determined. Graph of residence time vs conversion was plotted based on the result
obtained. The relationship between residence time and conversion was successfully
studied and graphed in graph 1.8. By analysing the graph, is shows that the longer
the residence time, the greater the percentage of conversion. This is due to the
longer the reactants stay in the reactor, more products would be formed. From the
data obtained also it can be concluded that the reaction rate constant is depend on
the flow rate in the plug flow reactor where, as the flow rate decrease, the reaction
rate constant increased.
250. The plug flow reactor is employed in industrial application where high
exothermic or explosive application involved in carrying the chemical reaction. It
ensures safe heat transfer between the instrument and the surrounding and
commonly used to ensure static mixing of the components.
251.
252.
253.
254.
255.
256.

23

257.
258.
259.
260.
261. 1.11 Recommendations
262. In my point of view, there are a few recommendations and precautions that have
to be considered during the experiments in order to get an accurate value and
readings of data. Firstly, before started the experiment, make sure that all valves
are properly open to carry out the experiment. . Make sure to perform general startup and shut down procedure so that the equipment will run smoothly and is in the
best shape to operate. The pump also should never let to run dry. Besides that, the
temperature should be constantly monitored throughout the experiment so that it
will remain the same from start. Each flow rates of the feed also should be
constantly monitored so that it remains constant throughout the reaction to prevent
any changes that can affect the result. Run several trials on tubular flow reactor to
get more accurate results by taking the average value from each different molar
rates.
263. In order to avoid from any contaminants into the sample, the titration should be
done as soon as possible after taking the sample. Be extra careful when carry out
the titration where the titration should be stop as soon as the indicator turn into
pale pink color. The excess drop of NaOH from titration can effect on the solution
color hence effect the calculations and the result.
264.
265.
266.
267.
268.
269.
270.
271.
24

272.
273.
274.
275. 1.12

Reference

276.
277.

Denbigh, K., & Turner, J. C. (1984). Chemical Reactor Theory: An Introduction.

London: Cambridge University Press.

278.

Dey, D., Herzog, A., & Srinivasan, V. (2007). Tracer Studies In A Plug Flow
Reactor. 1-43.

279.

Fogler, H. S. (2014). Elements of Chemical Reaction Engineering (4th ed.).

London: Pearson Education.

280.

Green, D., & Perry, R. (1987). Perry's Chemical Engineer's Handbook. McGraw
Hill.

281.

Levenspiel, O. (1999). Chemical Reaction Engineering. John Wiley.

282.

Mann, U. (2009). Principles Of Chemical Reactor Analysis And Design (2nd

ed.). New Jersey: A John Wiley & Sons, Inc.

283.

Schmidt, & Lanny, D. (1998). The Engineering of Chemical Reactions. New

York: Oxford University Press.

284.

Smith, J. (1981). Chemical Engineer Kinetics. McGraw Hill.

285.

Tamir, A. (1998). Applications of Markov Chains in Chemical Engineering.

Elsevier Science B.V.

286.

Winterbottom, J., & King, M. (1999). Reactor Design for Chemical Engineers.
United Kingdom: Stanley Thornes Ltd.
287.

288.
289.
290.
25

291.
292.

293.
294.
295.
296. 1.13 Appendix

26

297.

27

298. Figure 4 SOLTEQ Plug Flow Reactor

299.
300.
301.
302.
303.
304.
305.
306.
307.

28

308.
309.
UNIVERSITI TEKNOLOGI MARA
310.
FAKULTI KEJURUTERAAN KIMIA
311.
CHEMICAL ENGINEERING LABORATORY iii (CHE 574)
312.
313. 314.
315.
NUR IZZATI BINTI AHMAD TARHIZI
N
:
(2014233914)

316.
G

317.

318.

EH200 4A

319.
EX

320.

321.

PLUG FLOW REACTOR

322.
D

323.

324.

15 MARCH 2016

325.
P

326.

327.

EH220

29

328.
S

329.

332.

330.
331.

333.

MADAM NURHASHIMAH BINTI ALIAS

MISS SITI KHATIJAH BINTI JAMALUDIN

Title

336.

337.

Abstract

340.

341.

Introduction

344.

345.

Objectives

348.

349.

Theory

352.
356.

353.
Procedures/Met
hodology
357.
Apparatus

360.

361.

Results

364.

365.

Calculation

368.

369.

Discussion

372.

373.

Conclusion

376.

Recommendati

380.

377.
ons
381.

384.

385.

Appendices

388.

334.
Allocate
d
Mark
s (%)
338.
5
342.
5
346.
5
350.
5
354.
10
358.
5
362.
10
366.
10
370.
20
374.
10
378.
5
382.
5
386.
5
389.
100

References

TOTAL
391.

392.

Remarks:
30

335.
Marks

339.
343.
347.
351.
355.
359.
363.
367.
371.
375.
379.
383.
387.
390.

393.
394.
Checked by:
Rechecked by:
395.
Date:
Date:
396.

31