Year 2

Chemical Engineering Laboratory

Short Report

Student Name Ng Joe Wei

Group Number 8

Experiment Title Reaction – Tubular Flow Reactor

Date of Experiment 28/09/2020

Demonstrator Dr Wong Voon Loong

Declaration Form

I, < Ng Joe Wei > have read and understand the Guidelines on student discipline
procedures:

(https://www.hw.ac.uk/students/studies/record/discipline.htm and Regulation 50 of

http://www1.hw.ac.uk/ordinances/regulations.pdf )

I, < Ng Joe Wei >, confirm, that this work submitted for assessment is my own and
is expressed in my words. Any uses made within it of the works of other authors in
any form (e.g. ideas, equations, figures, drawings, text, tables, other forms of data,
programs) are properly acknowledged and referenced at the point of their use. A
list of the references employed is included.

Signature Ng Joe Wei

Date 28/09/2020

Date Saved: 5-Oct-20 Page 1 of 6

Discussion
The main objective of this experiment is to find out the effect of residence time and the
temperature on a reaction in a Tubular Flow Reactor.

Conductivity (ms/cm) 14
12
10
8 y = -0.094x + 11.64
6 R² = 0.9984
4
2
0
0 20 40 60 80 100 120
Conversion (%)

Figure 1: Calibration graph obtained by plotting conductivity against conversion

An experiment is carried out to prepare a calibration curve to determine the conversion from
the conductivity obtained. Based on figure 1, it shows that the conductivity decreases linearly
as the conversion increases. A best fit line of y= -0.094x +11.64 is obtained from the graph
with a gradient of -0.094 and a y intercept of 11.64 ms/cm. As the experiment proceeds, more
products are formed from the reactant and this increases the conversion. At 0%, it shows a
high conductivity of 11.6 ms/cm due to large number of hydroxide ions present in the NaOH
solution. But as the reaction proceeds, more sodium acetate is formed from sodium
hydroxide and ethyl acetate and the concentration of hydroxide ion falls. The hydroxide ions
are replaced by same number of acetate ions which has a lower conducting level (Das,
2011). Consequently, the overall conductivity decreases. The graph obtained deviates slightly
from the best fit line as the calibrating experiment has only been carried out once due to time
limitation. As a result, it lowers down the accuracy of the experimental data.

60.0 57.0
48.7
50.0 41.9
Conversion (%)

37.7
40.0 33.9 y = 1E-06x3 - 0.0011x2 + 0.361x + 19.543
32.6 R² = 0.9992
30.0

20.0

10.0

0.0
0 50 100 150 200 250 300
residence time (s)

Figure 2: Graph showing conversion against residence time

The experiment is carried out by varying the total flowrate of solutions at a range of 0.1-0.6
L/min to obtain different residence time. The volume of reactor and the stirring speed was
fixed at 0.4L and 200rpm respectively. According to figure 2, it shows that the conversion
goes up as the residence time increase. At a residence time of 40s, it shows that the
conversion is 32.6%, while at 240s, the conversion increases up to 57%. The increase in
conversion proves that more products are formed with every mole of NaOH consumed in the
!
reaction. Based on the equation t = !"# !
, where 𝑉"#$ is the volume of reactor and 𝑉% is the
$
total flowrate of solutions, the residence time is inversely proportional with total flowrate of
solutions. A lower flowrate gives a longer residence time. At high residence time, it gives
more time for molecules to be reacted to form product. Thus, giving higher conversions. This
proves that in practical application, it is preferably to use lower flowrates to have a higher
residence time. It is also shown that the gradient of the graphs becomes less steep as the

Date Saved: 5-Oct-20 Page 2 of 6

residence time increase. This is due to the conversion has slowly reached its maximum. The
concentration of reactants decreases as the reaction proceeds, hence not much reactants
are left to form additional products.

500
450 434
400 385
362
(mol^-1Ls^-1)
rate constant

350
325
300 285
250
200 199
y = 1987.5x-0.415
150
R² = 0.9894
100
50
0
0 50 100 150 200 250 300
residence time (s)

Figure 3: Graph showing rate constant against residence time

2.50
1.98
2.00 1.68
rate of reaction
( molL^-1s^-1)

1.41
1.50
1.10
1.00 0.75
0.37
0.50 y = 63.914x-0.935
R² = 0.9978
0.00
0 50 100 150 200 250 300
residence time (s)

Figure 4: Graph showing rate of reaction against residence time

Figure 3 shows a decreasing graph where the rate constant drops as the residence time
increase. At a residence time of 40s, it shows the highest rate constant at 434 𝑚𝑜𝑙&' 𝑙𝑠 &' and
it decreases to 199 𝑚𝑜𝑙&' 𝑙𝑠 &' when the residence time increases up to 240s. The rate
!$ )
constant was calculated using the formula 𝑘 = ∗ ( ) where 𝑉"#$ is the volume of
!!"# (%$ '&)
reactor, 𝑉% is the total flowrate of solutions, 𝐶*% is the initial concentration, and X is the extent
of conversion. From this formula, it is shown that the residence time is inversely proportional
!
to the rate constant k, where ! $ is the reciprocal of the residence time. This proves that the
!"#
trend of the experimental data collected is matches with the formula derived.

Figure 4 shows that the rate of reaction decreases as the residence time increases. At a
residence time of 40s, it has the highest rate of reaction at 1.98 𝑚𝑜𝑙 𝑙&' 𝑠 &' . However, the rate
of reaction decreases to 0.37 𝑚𝑜𝑙 𝑙&' 𝑠 &' when the residence time increases up to 240s. As
the residence time increases, the longer the reactant stays in the reactor. Hence, having
more time to react to form products. This leads to a higher conversion which decreases the
concentration of reactant. In this experiment, this is a second order reaction overall which is
first order with respect to reactants. With both the reactant having equal number of mols, the
rate law is written as −𝑟* = 𝑘𝐶* + . According to this equation, the rate of reaction is directly
proportional with the concentration of reactant. Hence, the rate of reaction decreases when
the concentration of reactant falls. In short, at long residence time, it gives a high conversion.
This leads to a lower concentration of reactant which decreases the rate of reaction.

Date Saved: 5-Oct-20 Page 3 of 6

 66.0 64.0
63.4
64.0 62.3

Conversion (%)
62.0
60.0 58.7
58.0
56.0 y = -0.0286x2 + 18.938x - 3074.1
54.4
R² = 0.9964
54.0
52.0
310 315 320 325 330 335
Temperature (K)

Figure 5: Graph showing conversion against temperature at a total flowrate of 0.3L/min

The experiment is carried out at a temperature range of 313K to 333K with an interval of 5K.
The total flow rate and residence time is fixed at 0.3 L/min and 80s respectively. According to
figure 5, the conversion increases with a rise of the temperature. It is shown that the gradient
of the graph becomes less steep as the temperature increases. From 313K to 318K, it shows
a significant increase in the conversion from 54.4% to 58.7%. However, it only shows a minor
increase in conversion from 63.4% to 64% when the temperature increase from 328K to 333K.
In this experiment, it is found that the forward reaction is an endothermic reaction where heat
is removed from surroundings. Hence, with an increase in temperature the equilibrium tends
to shift to the right which produces more products. With a rise in the concentration of the
products, also simply means that the conversion is high (Gary, n.d.). Moreover, a rise in
temperature increases the kinetic energy of the molecules of the reactants. The number of
collisions increases, the frequency of collisions increases. Consequently, molecules of
reactants collide more often and produce more products. It is observed that the conversion
reaches constant at higher temperature. This is because the conversion has slowly reaches
its maximum. There are not much reactants available anymore to form extra products. Hence,
giving a maximum conversion.

Conclusion
To summarise this experiment, the flowrate is inversely proportional to the residence time. An
increase in residence time shows a positive correlation with the conversion as they have more
time to react to give higher conversion. Next, the rate constant and rate of reaction calculated
shows a negative correlation with the residence time. Lastly, the conversion increases as the
temperature rises due to the endothermic forward reaction. It is recommended to repeat the
experiment for the preparation of the calibration curve for at least 3 times to improve the
accuracy of the experimental data collected.

Date Saved: 5-Oct-20 Page 4 of 6

References

1) Das, Kuheli & Sahoo, Parashuram & Magapu, Sai Baba & Murali, N. & Swaminathan,
Pradeep. (2011). Kinetic Studies on Saponification of Ethyl Acetate Using an
Innovative Conductivity-Monitoring Instrument with a Pulsating Sensor. International
Journal of Chemical Kinetics.
2) Gary, L. (n.d.). Lechatelier. Web.mst.edu. Available at:
<https://web.mst.edu/~gbert/LeChatelier/LeChatelier.html> (Accessed 4 October
2020).

Appendix

Table 1: Raw data obtained from experiment to prepare calibration curve

Solution Mixtures (mL)
Conversion, %
0.1 M 0.1 M Conductivity
Water
NaOH Na(Ac) (mS/cm)
0 100 - 100 11.6
25 75 25 100 9.2
50 50 50 100 7.2
75 25 75 100 4.5
100 - 100 100 2.2

Table 2 : Raw data obtained from the experiment by changing the flowrates to obtained different
residence time

Total flow
Flowrate Flowrate rate of Inlet Outlet
residence Conversion
No. of NaOH of Et(Ac) solutions, conductivity conductivity
time (s) (%)
(L/min) (L/min) V0 (ms/cm) (ms/cm)
(L/min)

1 0.30 0.30 0.6 10.14 8.58 40 32.6

2 0.25 0.25 0.5 10.29 8.45 48 33.9
3 0.20 0.20 0.4 10.12 8.10 60 37.7
4 0.15 0.15 0.3 9.84 7.70 80 41.9
5 0.10 0.10 0.2 9.60 7.06 120 48.7
6 0.05 0.05 0.1 8.72 6.28 240 57.0

Table 3: Raw data obtained from experiment by changing the temperature

Total flow
Flow
Temperature Flowrate rate of Inlet Outlet
rate of residence Conversion
(K) of NaOH solutions, conductivity conductivity
Et(Ac) time (s) (%)
(L/min) V0 (ms/cm) (ms/cm)
(L/min)
(L/min)
Inlet Outlet
313 9.37 6.53 54.4
318 9.05 6.12 58.7
323 298 0.15 0.15 0.3 8.59 5.78 1.33 62.3
328 8.24 5.68 63.4
333 8.50 5.62 64.0

Date Saved: 5-Oct-20 Page 5 of 6

Table 4: Rate constant and rate of reaction calculated for different residence time

Total flow
Rate rate of
rate of residence
constant, reaction
solutions, time (s)
(𝑚𝑜𝑙&' 𝑙𝑠 &' ) (𝑚𝑜𝑙 𝑙&' 𝑠 &' )
V0 (L/s)

36 40 434 1.98
30 48 385 1.68
24 60 362 1.41
18 80 325 1.10
12 120 285 0.75
6 240 199 0.37

Sample Calculations

1) Best fit line of calibration curve (conductivity vs conversion)

𝑦 = −0.094𝑥 + 11.64
8.58 − 11.64
𝑥=
(−0.094)
= 32.6%

2) Residence time, t

𝑉"#$
t=
𝑉%

0.4
=
0.6

= 0.667 mins

= 40 s

3) Rate constant, k

𝑉% 𝑋
𝑘= ( )
𝑉"#$ ∗ 𝐶*% 1 − 𝑋

0.6 0.326
= ( )
0.4 ∗ 0.1 1 − 0.326

= 7.26 𝑚𝑜𝑙&' 𝑙𝑚𝑖𝑛&'

= 434 𝑚𝑜𝑙&' 𝑙𝑠 &'

4) Rate of reaction

Both the reactants NaOH and Et(Ac) having the same concentration
−𝑟* = 𝑘𝐶* +
−𝑟* = 𝑘𝐶*% + (1 − 𝑋)+
−𝑟* = 434 ∗ (0.1)+ ∗ (1 − 0.326)+
= 1.98 𝑚𝑜𝑙 𝑙&' 𝑠 &'

Date Saved: 5-Oct-20 Page 6 of 6