UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA

REACTION ENGINEERING LABORATORY
(CHE506)
NAME : MUHAMMAD ROZAHIR BIN YAHYA (2015209108)
MOHAMMAD AIDIL BIN ALI (2015104137)
NUR ALEEYA BINTI ZAHARDI (2015263478)
NUR AQILAH BINTI MOHD ALI (2015218226)
NUR HAZREEN ATIQAH BINTI HARUN (2015259026)
NUR SYAHIRAH BINTI MAT DENG (2015298504)
GROUP : EH220 5B
EXPERIMENT : TUBULAR FLOW REACTOR (BP101-B)
DATE PERFORMED : 26TH SEPTEMBER 2017
SEMESTER :5
PROGRAMME / CODE : EH220
SUBMIT TO : SUFFIYANA BINTI AKHBAR

No. Title Allocated Marks (%) Marks

1 Abstract/Summary 5
2 Introduction 5
3 Aims 5
4 Theory 5
5 Apparatus 5
6 Methodology/Procedure 10
7 Results 10
8 Calculations 10
9 Discussion 20
10 Conclusion 10
11 Recommendations 5
12 Reference 5
13 Appendix 5
TOTAL MARKS 100

Remarks:

Checked by : Rechecked by:

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Date : Date :
 TABLE OF CONTENT
ABSTRACT

INTRODUCTION

THEORY

OBJECTIVES

APPARATUSES AND MATERIALS

METHODOLOGY

RESULT

CALCULATION

DISCUSSION

CONCLUSION

RECOMMENDATION

REFERENCE

APPENDICES
 ABSTRACT

This experiment was broken down into three sub-experiments: the plug flow reactor experiment,
the titration experiment, and the construction of calibration curve. The first experiment was done
using SOLTEQ Plug Flow Reactor (model BP101). The second experiment was done using a
laboratory scale set up for titration, and the third one was conducted by simple neutralization and
pH computation experiment. This experiment was conducted with the intention of calculating the
reaction rate constant for the saponification reaction between sodium hydroxide (NaOH) and
ethyl acetate (CH3COOCH2CH3) in the previously mentioned PFR. This experiment is also
conducted to study the effect of residence time on the reaction. With the flow rate being varied
and thus resulting in different residence time, the titration was done to inspect the extent of reaction
for each respective flow rates. Following the completion of the earlier part of the experiment, the
reaction rate constant is then computed using mathematical formulae.
 INTRODUCTION

Plug Flow Reactor (PFR) is used to describe the chemical reactions in continuous processes, where
flowing systems of cylindrical and operate at steady state.

Plug flow conditions means that all the material processed through the reactor must have the same
residence time so that the chemicals exiting the reactor have witnessed the same reaction
conditions of reactive species contact-time aging-temperature history. PFR can be used to predict
the behaviour of chemical reactors of such design. As known, reactors has been used widely in
chemical processes industry whereby it uses to produce desired product. There are many types of
reactor where product produced are based on specific specification, and condition.

A PFR typically has a higher efficiency than a CSTR of the same volume. That is, given the same
space-time (or residence time), a reaction will typically proceed to a higher percentage completion
in a PFR than in a CSTR. This is not always true for reversible reactions. Since a PFR is an
idealized reactor, it does not truly exist in the real world. It is impossible to have no mixing at all
during a reaction, but the amount of mixing in the reactor can be minimized.

There are several advantages to minimizing the amount of mixing so that the reactor closely
resembles a PFR. These advantages will be explained in further detail later. The plug flow reactor
has an inlet flow composed of the reactants. The reactant flows into the reactor and is
then converted into the product by a certain chemical reaction. The product flows out of the reactor
through the outlet flow.
 THEORY

In chemical kinetics a reaction rate constant or reaction rate coefficient, k, quantifies the rate of
a chemical reaction.

Next, residence time distribution (RTD) of chemical reactor is a probability distribution function
that describe amount time where fluid element inside the reactor. The RTD can be characterized
where the mixing and flow within reactors and to compare between real reactor and ideal models.

, =
0

A calibration curve is also known as a standard curve, where a general method for determining the
concentration of a substance in an unknown sample, then from the results comparing the unknown
to a set of standard samples of known concentration.

The calibration curve is a plot of how the instrumental response, the so-called analytical signal,
changes with the concentration of the analyte (the substance to be measured). The operator
prepares a series of standards across a range of concentrations near the expected concentration of
analyte in the unknown. The concentrations of the standards must lie within the working range of
the technique (instrumentation) they are using.

Analyzing each of these standards using the chosen technique will produce a series of
measurements. For most analyses a plot of instrument response vs. concentration will show a linear
relationship. The operator can measure the response of the unknown and, using the calibration
curve, can interpolate to find the concentration of analyte.

OBJECTIVES

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.

APPARATUSES AND MATERIALS

1. BP101 Plug Flow Reactor

Figure: BP101 Plug Flow Reactor

2. Conductivity probe

Figure: Conductivity Probe

3. Sodium hydroxide NaOH

4. Ethyl acetate Et(Ac)
5. Feed tanks
6. Waste tank
7. Stopwatch
8. Phenolphthalein
9. Beaker
10. Conical flask
11. Burette
12. Retort stand

Figure: Retort Stand and Conical Flask

 METHODOLOGY

General Start-up Procedures

1. All valves are ensured to be initially closed except for valves V4, V8 and V17.
2. The following solutions are prepared:
a. 20 litre of sodium hydroxide, NaOH (0.1 M)
b. 20 litre of ethyl acetate, Et(Ac) (0.1 M)
c. 1 litre of hydrochloric acid, HCl (0.25 M), for quenching
3. Feed tank B1 is filled with NaOH solution and feed tank B2 with Et (Ac) solution.
4. Water jacket B4 is filled with water and pre- heater B5 with clean water.
5. The power for the control panel is turned on.
6. Valves V2, V4, V6, V8, V9 and V11 are opened.
7. Both pumps P1 and P2 are switched on. P1 and P2 are adjusted to obtain flow of
approximately 300 ml/ min at both flowmeters F1- 01 and F1- 02. Both flow rates are
ensured to be the same.
8. Both solutions are allowed to flow through the reactor R1 and overflow into waste tank
B3.
9. Valves V13 and V18 are opened. Pump P3 is switched on to circulate the water through
pre- heater B5. The stirrer motor M1 is switched on and the speed is set to about 200 rpm
to ensure homogeneous water jacket temperature.
10. The unit is ready for experiment.

General Shut-down Procedures

1. Pumps P1, P2 and P3 are switched off. Valves V2 and V6 are closed.
2. The heaters are switched off.
3. The cooling water is let to be circulating through the reactor while the stirrer motor is
running to allow the water jacket to cool down to room temperature.
4. If the equipment is not going to be used for long period of time, all liquid is drained from
the unit by opening valves V1 to V19. The feed tank is rinsed with clean water.
 5. The power for the control panel is turned off.

Experiment A: Preparation of Calibration Curve for Conversion vs. Conductivity

The reaction to be studied is the saponification reaction of ethyl acetate Et (Ac) and sodium
hydroxide NaOH. Since this is a second order reaction, the rate of reaction depends on both
concentrations of Et (Ac) and NaOH. However, for analysis purposes, the reaction will be carried
out using equimolar feeds of Et (Ac) and NaOH solutions with same initial concentrations. This
ensures that both concentrations are similar throughout the reaction.

+ () () +

The following procedures will calibrate the conductivity measurements of conversion values for
the reaction between 0.1 M ethyl acetate and 0.1 M sodium hydroxide:

Procedures:

1. The following solutions are prepared:

a. 1 litre of sodium hydroxide, NaOH (0.1 M)
b. 1 litre of ethyl acetate, Na(Ac) (0.1 M)
c. 1 litre of deionised water, H2O
2. The conductivity of NaOH concentration is determined for each conversion values by
mixing the following solutions into 100 ml of deionised water:
a. 0% conversion : 100 ml NaOH
b. 25% conversion : 75 ml NaOH + 25 ml Na(Ac)
c. 50% conversion : 50 ml NaOH + 50 ml Na(Ac)
d. 75% conversion : 25 ml NaOH + 75 ml Na(Ac)
e. 100% conversion : 100 ml Na(Ac)
Experiment B: Back Titration Procedures for Manual Conversion Determination

It is advisable to carry out manual conversion determination on experiment samples to verify the
conductivity measurement values. The following procedures will explain the method to carry out
back titration on the samples. It is based on the principle of quenching the sample with excess acid
to stop any further reactions, the back titrating with a base to determine the amount of unreacted
acid.

Procedures:

1. A burette is filled up with 0.1 M NaOH solution.

2. Ten ml of 0.25 M HCl is measured in a flask.
3. A 50 ml sample is obtained from experiment and immediately is added to the HCl in the
flask to quench saponification reaction.
4. A few drops of pH indicator are added to the mixture.
5. The mixture is titrated with NaOH solution from the burette until the mixture is neutralized.
The amount of NaOH titrated is recorded.

Experiment 3: Effect of Residence Time on the Reaction

Procedures:

1. General start- up procedures is performed.

2. Valves V9 and V11 are opened.
3. Both NaOH and Et (Ac) are allowed to enter the plug reactor R1 and empty into the waste
tank B3.
4. P1 and P2 are adjusted to give constant flow rate of about 300 ml/ min at flow meters F1-
01 and F1- 02. Both flow rates are ensured to be the same. The flow rates are recorded.
5. The conductivity values for inlet (QI- 01) and outlet (QI- 02) are started to be monitored.
The values are ensured to be monitored until they do not change over time. This is to ensure
that the reactor has reached steady state.
 6. The steady state conductivity values for both inlet and outlet are recorded. The
concentration of NaOH exiting the reactor and the extent of conversion is determined from
calibration curve.
7. Sampling valve V15 is opened to collect 50 ml sample. Back titration is carried out based
on procedure on Experiment B.
8. Steps 4 to 7are repeated 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. The flow rates are ensured
to be the same.

RESULT AND CALCULATION

Solution Mixtures Concentration Conductivity,

Conversion 0.1 M NaOH 0.1 M H2O of NaOH (M) (mS/cm)
Na(Ac)
0% 100 mL - 100 mL 0.0500 11.45
25% 75 mL 25 mL 100 mL 0.0375 7.52
50% 50 mL 50 mL 100 mL 0.0250 5.83
75% 25 mL 75 mL 100 mL 0.0125 1.95
100% - 100 mL 100 mL 0.0000 0.1195
Table 1 - Calibration curve data

Conductivity vs Conversion
14
12
Conductivity(mS/cm)

10
8
6
4 y = -0.1129x + 11.02
R = 0.9832
2
0
0 20 40 60 80 100 120
-2
Conversion(%)

Table 2 - Conductivity vs conversion

 2 2
0 11.95 0 0 131.1025
0.25 7.52 0.0625 1.88 56.5504
0.5 5.83 0.25 2.915 33.9889
0.75 1.95 0.5675 1.4625 3.8025
1.00 0.1195 1 0.1195 0.0143
TOTAL 2.5 26.8695 1.875 6.377 225.4586
Table 3 - Linear regression table

0
[ ] [ ] = [ ]
2 1

0 1
[ ] = [ ] [ ]
1 2

1
=[ ] [ ]
2
5 2.5 -1 26.8695
=[ ] [ ]
2.5 1.575 6.377
11.0201
=[ ]
11.2927
= 11.0201 11.2927
5(6.377) (2.5)(26.8695)
= =
( 2 ( )2 ( 2 ( )2 ) 9.375 6.75)(1127.293 721.9700)
35.2888
=| | = 0.9915
35.5898
Therefore, since R2 = 0.9832, the calibration curve is still reliable as it suffers only 1.6843%
deviation from perfect unity.
From the table above also, conversion and concentration are related by equation C = 0.0125 +
0.0625
 No Flow rate of Flow rate Total flow Residence Outlet Volume
NaOH of Et(Ac), rate of time, conductivity(mS/cm) of
(mL/min) (mL/min) solution, (min) NaOH
0 (mL/min) titrated
( mL)
1 300 300 600 0.667 7.3 30.4
2 250 250 500 0.800 7.7 31.3
3 200 200 400 1.000 7.8 29.9
4 150 150 300 1.333 7.3 30.0
5 100 100 200 2.000 6.8 29.5
6 50 50 100 4.000 6.2 30.7

SAMPLE OF CALCULATION

Information :
Flowrate of NaOH and Et(Ac) = 300 mL/min
Volume of the reactor = 0.4 L
Concentration of NaOH in feed tank = 0.1M
Concentration of Et(Ac) in feed tank = 0.1M
Volume of HCI ,(VHCI,S) = 10ml,

()
Residence time, = ()

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

= 300 mL/min NaOH + 300 mL/min Et(Ac)

= 600 mL/min

= 0.6 L/min

0.4
Residence time, =
0.6/

= 0.667min
Other residence times were calculated by the same way, and varies the flow rates.

For flow rate 300mL/min

Mole of NaOH reacted, ni = CNaOH volume of NaOH titrated
= 0.1 M 0.0304 L
= 0.00304mole
Moles of HCI unreacted ,n2 = moles of reacted NaOH ,n1
n2=n1
n2=0.00304moles.
2
volume of HCI unreacted ,V2 =

0.00304
=
0.25
=0.01216L
Volume of HCI reacted ,V1= total volume of HCI volume of unreacted HCI,V2
= (0.01 0.01216)L = -2.1610-3L
Moles of HCI reacted,n3 = CHCI titrated, V1
n3 = 0.25mole (-2.1610-3L)
n3 =-5.4 10-4mole/L
Moles of NaOH unreacted, n4= Moles of HCI reacted,n3
n4 = -5.4 10-4mole/L
n4
Concentration of NaOH unreacted = ()
5.4 104mole/L
= 0.05

= -0.0108 M

Xunreacted =

0.0108
= 0.1

= -0.108

Xreacted = 1- Xunreacted
 = 1-(-0.108)

=1.108

Find the reaction rate constant,

0
= 0 = 0 2 = 0 2 2
= ( )
0 0 0 0 (1 ) 0 1

0 1 0.6 1.108
= ( )= ( )= ( ) = 153.89
0 1 0 1 0.4 0.1 1 1.108

Calculating rate of reaction:

2 (1
mol
= 0 )2 = 0.166
L min

Residence time, Conversion, X Reaction rate Rate of reaction,

(min) (%) constant, (mol.L/min)
(L.mol/min)
0.667 110.8 -153.890 0.166
0.800 112.6 -111.710 0.141
1.00 109.8 -112.041 0.110
1.333 110.0 -82.500 0.083
2.000 109.0 -60.560 0.055
4.000 111.4 -24.430 0.028
Table 4 - Calculated data for conversion
 Conversion,x(%) versus residence time, (min)
120

Conversion,(%)

110

100
0 1 2 3 4 5
Resindence time,(min)

Table 5 - conversion vs time

DISCUSSION

In this experiment, we able to carry out the saponification experiment of NaOH and Et(Ac)
in plug flow reactor. The main objective in this experiment is to study the effect of residence time
on the performance of this plug flow reactor(PFR). 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. As the experiment is done, we
collected few data consist of concentration of NaOH and conductivity, k. We then plotted a graph
conductivity vs concentration of NaOH using all the data that we have collected. From the graph
we can observed that the conductivity decreased along with the decreasing concentration of NaOH
when taking a best fit line out of the graph.

After that, we determined the value of residence time, conversion of the reactions, reaction
rate constants and rate of reactions. The reaction rate constant we get for flow rate of 300 ml/min
is -153.890 L/mol.min, for flow rate of 250 mL/min reaction rate constant is -111.710 L/mol.min
, for flow rate of 200 mL/min reaction rate is -112.041 L/mol.min, for flow rate of 150 mL/min
reaction rate is -82.500 L/mol.min , for flow rate of 100 mL/min reaction rate is -60.560 L/mol.min
and for flow rate of last which is for the 50 mL/min reaction rate constant is -24.430 L/mol.min.
From the reaction rate constant we determined, we can see that the value of reaction rate constant
is increased as the flow rate is decrease. Thus, these shows that the reaction rate constant is depend
to the flow rate flow in the plug flow reactor. However, we do get a negative reaction rate constant
which is invalid as the value of reaction rate constant will always be positive. It is maybe due to a
few error while taking reading on the conductivity value that lead to this error or maybe the device
not functioning well enough.

The rate of reaction also can be determined after we had done find the reaction rate
constant. The rate of reaction we get for 300ml/min flow rate is 0.166 mol/L.min, for the
250mL/min the rate of reaction is 0.141mol/L.min, for the 200mL/min the rate of reaction is
0.110mol/L.min, for the 150mL/min the rate of reaction is 0.083mol/L.min, for the 100 mL/min
the rate of reaction is 0.055mol/L.min and for the 50mL/min the rate of reaction is 0.028mol/L.min.
After all value of rate of reactions has been calculated, a graph of conversion factor against
residence time is plotted. We used this formula to determine residence which is use for a function
of total flow rates of the feed by time before plotting the graph,

(),
Residence Time, =
( ),0

From the graph that had been plotted, we can say that the graph has no specific pattern
which increasing at certain point then decreasing at the other point. Supposedly, the result of
conversion factor is inversely proportional to the residence time. This maybe due to the error that
stated above. The value of conversion factor that we get is also invalid because it has a value which
more than 1. Conversion, xA is the number of moles of A that reacted per mole of A fed to the
system. This conversion error maybe due to the PFR that had problem with its stirring mechanism.
Thus, when the residence time increases, the conversion factor also decreases.

CONCLUSION

From this experiment, we are able to carry out the saponification reaction between NaOH
and Et(Ac) in plug flow reactor. The reaction between them is pass through the plug flow reactor,
mixed and react at certain period of time. In plus, we are able to determine the reaction rate constant
for the saponification process. The reaction rate constant we get for flow rate of 300 ml/min is -
153.890 L/mol.min, for flow rate of 250 mL/min reaction rate constant is -111.710 L/mol.min ,
for flow rate of 200 mL/min reaction rate is -112.041 L/mol.min, for flow rate of 150 mL/min
reaction rate is -82.500 L/mol.min , for flow rate of 100 mL/min reaction rate is -60.560 L/mol.min
and for flow rate of last which is for the 50 mL/min reaction rate constant is -24.430 L/mol.min.
By doing that, saponification process was completed. But the value of the rate constant is not
acceptable because all the values of the reaction rate constant that we get are negative which is
wrong because the values of reaction rate constant will always be negative. This is due to certain
error while conducting the experiment,which is maybe not taking the reading at the right time,
following a wrong procedure or the PFR had a problem with its mechanism. Besides that, from
this experiment we also are able to determine the reaction rate of this particular reaction. From
sample calculation done show the data get from result use for calculating to achieve our objective
. Moreover, from this experiment also, we can study the relationship between the residence time
and the conversion of the reactants. However, the graph that we plotted is invalid from its theory
which stated that the conversion must inversely proportional with residence time. This is due to
value of conversion which are bigger than one. Due to the objective of the experiment that we
failed to achieve, we can concluded that this experiment is failed .

RECOMMENDATION

1. This experiment should be repeated at various other temperatures to investigate the

relationship between the reaction rate constant and the rate of reaction.
2. It is further recommended that the experiment be repeated using dissimilar flow rates for
the NaOH solution and ethyl acetate solutions to investigate the effect that this will have
upon the saponification process.
3. For obtained more accurate results, run several trials on tubular flow reactor so we can take
the average value from each different molar rates.
4. During titration students should more alert and carefully because we only want the last
drop of NaOH that will convert the solution to light pale purple colour. Thus, the excess of
drop of NaOH will give effect on the result in the calculations.
5. During conducted experiment, the flow rates should be constantly monitored to prevent
any changes occur that can influence our result.
6. Titration should be immediately stopped when the indicator turned pink.
 REFERENCE

[1] https://en.wikipedia.org/wiki/Plug_flow_reactor_model

[2] https://en.wikipedia.org/wiki/Chemical_reactor

[3] http://www.stamixco-usa.com/plug-flow-reactors

[4] https://www.scribd.com/doc/29195386/Plug-Flow-Reactor

[5] http://www.chem.arizona.edu/~salzmanr/480a/480ants/chemkine.html