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DEPARTMENT OF CHEMICAL AND ENVIRONMENTAL

ENGINEERING

UNIVERSITI PUTRA MALAYSIA

ECH3905

CHEMICAL ENGINEERING LABORATORY III

Title: The Effect of Temperature in a Plug Flow Reactor

Group: 5

Lecturer’s name: Dr. Faizah Md Yasin

Group members:
NAME MATRIC NO
CONSTANTINE EMPARIE ANAK TUJAH 188709
MOHD SAIFUL RIDZUAN BIN MOHD ALI 190418
INTAN NURANISSA BT MOHAMAD ZAILANI 187412
1.0 ABSTRACT

In this experiment, we are going to determine the effect of temperature to the conversion
of reactants inside a plug flow reactor (PFR). The reactants used in this experiment are sodium
hydroxide, NaOH and ethyl acetate, EtAc. Both the solutions have molarity of 0.1 M and placed
into two separate tank as much as 55 L each. The flowrate is keep constant at 1 L/min. After
the reactor is ready to use, the temperature is set at three different value which are at 40℃,
45℃ and 50℃ with time interval of 10 min, 7 min and 5 min respectively. The sample is then
taken and titrated with NaOH to observe their concentration exiting the reactor. Results
obtained is tabulated in a table.
2.0 INTRODUCTION

Every chemical reaction takes place in a chemical reactor. Chemical reactor is basically
an enclosed vessel where chemical reaction will happen inside of it. It is the role of a chemical
engineer to design an efficient reactor according to the specifications needed and ensure the
output product is high in quality. There are many types of reactor exists for example, batch
reactor, continuous stirred tank reactor (CSTR), catalytic reactor and plug flow reactor (PFR).

A plug flow reactor (PFR) also known as continuous tubular reactor is a type of reactor
where it is arranged as one long reactor or many short reactors in a tube bank ; no radial
variation in reaction rate (concentration); concentration changes with length down the reactor.
The plug flow type continuous reactors offer large volumetric reaction conversion due to lower
yield of undesired product. According to Cunningham et al. (2010), it is assumed to be no
mixing in an ideal plug flow reactor although there may be some mixing at any point in the
reactor.

This type of reactor is commonly used for large scale reaction, a fast reaction and for
continuous production at high temperature. PFR is known to withstand high temperature. A
PFR is preferable in most chemical reactions because it has high conversion per unit volume,
low operating cost and good heat transfer.

Figure 1: Diagram of Plug Flow Reactor


3.0 METHODS AND MATERIALS
Equipment and Material

Equipment

1. Plug flow reactor


2. Analytical balance

Labware

1. Spatula
2. Conical flask
3. Beaker
4. Retort stand

Material/Chemical

1. Hydrochloric acid solution (0.1M)


2. Ethyl acetate (0.05M)
3. Sodium hydroxide solution (0.1M)
4. De-ionized water

Experimental Procedure

General Start-up Procedures

1. The solutions were prepared by following:


a) 55 liter of sodium hydroxide, NaOH (0.1M)
b) 55 liter of ethyl acetate, Et(Ac) (0.05M)
c) 100 mL of hydrochloric acid, HCL (0.1M), for quenching
2. The feed tank B1 was filled with the NaOH solution and followed by tank B2 with the
Et(Ac) solution.
3. The water jacket B4 was filled and pre-heater with clean water.
4. The power for the control panel was turn on.
5. Both pumps P1 and P2 were switch on. Both valves V1 and V2 were adjusted to obtain
flow rates approximately 1.0 liter/min at both flow meters FI-01 and FI-02.
6. The solutions were allowed to flow through the reactor R1 and overflow into the waste
tank B3.
7. The unit was now ready for experiment.
General Shutdown Procedures

1. Both pumps P1 and P2 were switched off. The valves V1 and V2 were closed.
2. The heaters were switched off.
3. The cooling water was kept to circulating through the reactor while the stirred motor is
running to allow the water jacket to cool down to room temperature.
4. The power for the control panel was turned off.

Experiment 4: Effect of Temperature on the Reaction.

PROCEDURES

1. The general start-up procedures were performed.


2. Both NaOH and Et(Ac) solutions were allowed to enter the plug reactor R1 and empty
into the waste tank B3.
3. Both valves V1 and V2 were adjusted to give the desired flow rate of 1.0liter/min at
flow meters FI-01 and FI-02.
4. The temperature of reaction was set to 40⁰C.
5. The inlet (QI-01) and outlet (QI-02) conductivity values were monitored until they do
not change over time to ensure that the reactor has reached steady state.
6. Sampling valve V15 was opened and 50 ml sample was collected.
7. The sample then added with 10ml of 0.25M HCL to quench the sample.
8. 1-2 drops of phenolphthalein were added into the sample,
9. A back-titration procedure was carried out to manually determine the concentration of
NaOH in the reactor.
10. The experiment (steps 2 to 6) was repeated with different temperature of 45⁰C and 50⁰C
while allowing the reaction to occur in the PFR with time interval of 7 minutes and 5
minutes.
4.0 RESULTS AND DISCUSSIONS

Reactor Volume: 60 L
Concentration of NaOH in the reactor, CNaOH = 0.1 M (55L)
Concentration of NaOH in the feed vessel, CNaOH.f = 0.1 M (55L)
Concentration of HCl quench, CHCl.s = 0.25 M (0.0215L)
Volume of sample, Vs =0.1 L

Temperature Residence Flowrate Flowrate Volume of


(˚C) time, of NaOH of Et(Ac) NaOH (L)
τ (min) (L/min) (L/min) (Titration)

45 10 1 1 0.0007
55 7 1 1 0.0002
60 5 1 1 0.00005

Table 1. Data acquired from the experiment.

Sample Calculations

• Temperature at 45 ˚C,

Residence Time, τ, (min)

𝑅𝑒𝑎𝑐𝑡𝑜𝑟 𝑉𝑜𝑙𝑢𝑚𝑒 (𝐿) 𝑣


Residence Time, 𝜏 = 𝐿 =𝑣
𝑇𝑜𝑡𝑎𝑙 𝐹𝑙𝑜𝑤 𝑅𝑎𝑡𝑒 ( 0
min)

Total flow rate, Vo = Flow rate of NaOH + Flow rate of Et(Ac)

= 1 L/min NaOH + 1 L/min Et(Ac)

= 2.0 L/min

Hence,

60𝐿
Residence Time, 𝜏 = = 30𝑚𝑖𝑛
2𝐿/𝑚𝑖𝑛
Conversion

For flow rates of 1 L/min, T=45 ˚C,


• Moles of reacted NaOH, n1 :
n1 = Concentration NaOH x Volume of NaOH titrated
= 0.1 M x 0.0007L
= 7x10-5 mol

• Moles of unreacted HCl, n2 :


Moles of unreacted HCl = Moles of reacted NaOH
n2 = n1
n2 = 7x10-5 mol

• Volume of unreacted HCl, V1 :


𝑛2
V1 = 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝐻𝐶𝑙 𝑄𝑢𝑒𝑛𝑐ℎ

7𝑥10−5 𝑚𝑜𝑙
= 0.25𝑀

= 2.8x10-4 L

• Volume of HCl reacted, V2 :

V2 = Total volume HCl – V1


= ( 0.0215– 2.8x10-4)L
= 0.02122L

• Moles of reacted HCl, n3 :

n3 = Concentration HCl x V2
= 0.25M x 0.02122L
= 5.305x10-3 mol

• Moles of unreacted NaOH, n4 :

n4 = n3
= 5.305x10-3 mol
• Concentration of unreacted NaOH :
𝑛
CNaOH unreacted = 𝑣𝑜𝑙𝑢𝑚𝑒 4𝑠𝑎𝑚𝑝𝑙𝑒
5.305𝑥10−3 𝑚𝑜𝑙
= 0.1𝐿

=0.05305M

𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑁𝑎𝑂𝐻 𝑢𝑛𝑟𝑒𝑎𝑐𝑡𝑒𝑑 0.05305𝑀


• Xunreacted = = = 0.5305
𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑁𝑎𝑂𝐻 0.1𝑀

• Xreacted = 1 - Xunreacted = 1 - 0.5305 = 0.4695 → 46.95%

Reaction Rate Constant, k

𝑣0 𝑋
𝑘= ( )
𝑉𝑇𝐹𝑅 𝐶𝐴𝑂 1 − 𝑋

For flow rate of 0.2 L/min :

V0 = Total inlet flow rate


= 2 L/min
VTFR = Volume for reactor
= 60 L
CAO = inlet concentration of NaOH
= 0.1 M
• X = 0.5305

2 0.5305
𝑘 = (60)(0.1) (1−0.5305) = 0.3766 L/mol.min

Rate of Reaction

−𝑟𝐴 = 𝑘 (𝐶𝐴0 )2 (1 − 𝑋)2

−𝑟𝐴 = 0.00576(0.1)2 (1 − 0.6165)2

𝑚𝑜𝑙
−𝑟𝐴 = 8.3014 × 10−4
𝐿. 𝑚𝑖𝑛
Other data of different temperatures were calculated using above steps. All the values are
recorded in Table 2.

TEMPERATURE, RESIDENCE CONVERSION, REACTION RATE OF


C TIME, τ (min) X (%) RATE REACTION, -
CONSTANT, rA (mol/L.min)
k (L/mol.min)
45 10 53.05 0.3766 8.3014E-04
55 7 46.5 0.2897 8.2919E-04
60 5 46.3 0.2874 8.2877E-04
Table 2. Values obtained from calculations.

This experiment is conducted to determine the reaction rate constant and to study the
effect of temperature and residence time on the conversion in a continuous reactor. In this
discussion, we are able to carry out saponification reaction between NaOH and Et(Ac) in plug
flow reactor. These two solutions react together in the PFR to complete saponification reaction.
Plug Flow Reactor (PFR) is a type of reactor that consists of a cylindrical pipe and is usually
operated at steady state. The feed enters at one end of a cylindrical tube and leaves product
from the end of cylindrical tube. The long tube and the lack of provision for stirring prevent
complete mixing of the fluid in the tube.

At the end of the experiment, we are able to determine the reaction rate constant by
using formula and to determine the effect of temperature and residence time on the conversion
in the plug flow reactor. Residence times have to be manipulated throughout the experiment
and the effects of each one is studied. Residence time, in this particular experiment, is varied
by the means of changing the temperatures of the feed solutions.

After, the experiment is conducted, the data consisting inlet flow rates, temperature and
volume of NaOH used in the titration process are tabulated in Table 1. A series of calculation
were made based on the data tabulated that can see in Sample of Calculation section. After that,
the values of residence times, conversion of the reactions, reaction rate constants and rate of
reactions were determined. These values are tabulated in Table 2. The rate of reaction we get
for 45˚C is 8.3014x10-4 mol/L.min, for 55˚C the rate of reaction is 8.2919x 10-4 mol/L.min,
and for the 60˚C the rate of reaction is 8.2877x10-4 mol/L.min. After all values of rate of
reactions has been calculated, a graph of rate of reaction against temperature is plotted.
RATE OF REACTION VS
TEMPERATURE
8,31E-04
RATE OF REACTION (L/MOL.MIN)

8,30E-04

8,30E-04

8,29E-04

8,29E-04

8,28E-04
45 55 60
TEMPERATURE (C)

Figure 2: Graph of Rate of reaction vs Temperature.

CONVERSION VS TEMPERATURE
54

52
CONVERSION (%)

50

48

46

44

42
45 55 60
TEMPERATURE (C)

Figure 3. Graph of Conversion vs Temperature.

Based on the graph, as the temperature increases, the rate of reaction and conversion will
decrease. This proved that, to get more product, the saponification process is optimum at lower
temperature.
5.0 CONCLUSIONS

From the experiment, we are able to carry out the saponification reaction between the
NaOH and Et(Ac) in plug flow reactor. The reaction between them is pass through the plug
flow reactor and react at three different time which are 40⁰C, 45⁰C and 50⁰C. In conclusion, as
the temperature increases, the rate of reaction and conversion will decrease. This proved that,
to get more product, the saponification process is optimum at lower temperature.

There are several precaution steps to ensure the reading is accurate and reliable. Firstly,
the reading of equipment such as titration must be perpendicular to the eyes to prevent the
parallax error. Other than that, the reading should be repeated for at least 3 times for each
parameter to get average and consistent reading. Moreover, all the chemical must be handled
in the fume chamber to provide ventilation for the protection of lab occupants during chemical
manipulations. Last but not least, the titration process must be performed with correct technique
to determine the actual endpoint or equivalence point of the titration in order to get accurate
reading.