DEPARTMENT OF CHEMICAL AND ENVIRONMENTAL

ENGINEERING

UNIVERSITI PUTRA MALAYSIA

ECH3905

CHEMICAL ENGINEERING LABORATORY III

Experiment Week 12 (Replacement for Week 5)

CONTINUOUS STIRRED TANK 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 required to to study the saponification reaction ethyl acetate and
sodium reaction to form sodium acetate in a batch reactor. The objective of the experiment is
to determine the order of saponification reaction and to determine the reaction rate constant.
This experiment consists of two parts. The first part is we would like to study the reaction
occur when different reaction time being introduced while the feed concentration and mixing
speed inside the CSTR is constant. the feed concentration is set to be 0.05 M NaOH and 0.05
M Ethyl Acetate while the mixing speed is 4.5 rpm. The reaction is taken at minutes of
5,10,15,20,25 and 30. For the second part, we would like to study the reaction occur when the
mixing speed is manipulated to 3,5,6 and 7 rpm while the feed concentration and time is keep
constant. The time interval is 5 minutes. The data was recorded and it will be used to calculate
the reaction constant, k, rate of reaction, order of reaction and activation energy. The expected
result from this experiment is the reaction is first order reaction.
 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 continuous stirred tank reactor (CSTR) is a batch reactor designed with an impeller
or other mixing device to ensure efficient mixing. In chemical engineering, CSTR is often
used to refer to an idealised agitated tank reactor used to model operation variables required to
attain a specified output. CSTRs offer wide applications in the areas of food, chemical and the
pharmaceuticals due to good blending and scale-up attribute. CSTRs – as a single reactor or,
constantly, configured as reactors in series or parallel are practically always operated under
steady state conditions. It is used primarily for liquid phase reactions and is assumed to be
perfectly mixed. The temperature and concentration (consequently, the rate of reaction) are
independent of time and position inside the CSTR. The outlet streams from a CSTR have the
same concentrations as the reaction mixture within the reactor. Agitator vessels are generally
used throughout the chemical process industries for various applications such as storing,
blending and reacting materials. In addition to this, most agitated vessels use baffles, and the
design of baffles system must satisfy process objectives economically. On the other hand,
presence of baffles in the reactor system has some other consequences- like abolishing the
formation of vortex, increase the power input, and to enhance the mechanical strength. The
existence of baffles in the reactor system yields axial type flow.

The saponification process is a process that produces soap and occurs between an ester
and alkali. In technical terms, saponification involves base (NaOH) hydrolysis of triglycerides,
which are esters of fatty acids, to form the sodium salt of a carboxylate. The reaction of the
process is as below:

𝐶𝐻3𝐶𝑂𝑂𝐶𝐻2𝐶𝐻3 + 𝑁𝑎𝑂𝐻 → 𝐶𝐻3𝐶𝑂𝑂𝑁𝑎 + 𝐶𝐻3𝐶𝐻2𝑂𝐻

The reactants are Ethyl Acetate and Sodium Hydroxide, reacts to form Sodium Acetate and
Ethanol. The reaction was carried out at constant temperature, volume, flowrate and
concentration of the reactants under perfect mixing in CSTR to achieve optimal conversion.
 3.0 MATERIALS & METHODS

Material
1. 0.05M Sodium Hydroxide
2. 0.05M Ethyl Acetate
3. 0.10M Hydrochloric Acid
4. Burette
5. Beaker
6. Volumetric flask
7. Beaker
8. Phenolphthalein
9. Tripod stand
10. CSTR complete set

Method
Experiment 1: Reaction time
1. The 5L solution such as 0.05M NaOH, 0.05M Ethyl Acetate and 1L of 1.0M
Hydrochloric Acid are prepared using dilution method.
2. The 5L feed solution 0.05M NaOH and 0.05M Ethyl Acetate are put into the tank
vessel.
3. The pump 1 is turned on the fill the CSTR with 1L of 0.05M NaOH, after that, pump
2 is turned on to fill the CSTR with 1L of 0.05M Ethyl Acetate.
4. The mixing speed is set 4.5rpm.
5. For every 5minutes, take 50ml sample from the CSTR and quenched it as soon as
possible with 10ml of HCl.
6. The phenolphthalein is added into the taken sample.
7. The titration process is carried out in order to determined how much NaOH is left at
the end of the reaction.
8. The data is recorded when the first pink solution occurs.
Experiment 2: Mixing Speed
1. The 5L solution such as 0.05M NaOH, 0.05M Ethyl Acetate and 1L of 1.0M
Hydrochloric Acid are prepared using dilution method.
2. The 5L feed solution 0.05M NaOH and 0.05M Ethyl Acetate are put into the tank
vessel.
3. The pump 1 is turned on the fill the CSTR with 1L of 0.05M NaOH, after that,
pump 2 is turned on to fill the CSTR with 1L of 0.05M Ethyl Acetate.
4. The mixing speed is set at 3rpm.
5. After 5minute mixing, 50ml sample is taken and left are being drained from the
CSTR.
6. The phenolphthalein is added into the taken sample.
7. The titration process is carried out in order to determined how much NaOH is left
at the end of the reaction.
8. The data is recorded when the first pink solution occurs.
9. Refill the tank again with 1L of 0.05M NaOH and 1L of 0.05M Ethyl Acetate.
10. Repeat the step 4 to 9 by varying the mixing speed at 5rpm, 6rpm and 7rpm.
 4.0 RESULT AND DISCUSSION
Preparation of Feed
Sodium Hydroxide Ethyl Acetate
Volume of feed tank, Vtank= 5L Volume of feed tank, Vtank= 5L
Initial concentration of NaOH, CNaOH= Initial concentration of EtAc, CEtAc=0.05M
0.05M Relative Molecular Weight of EtAc,
Relative Molecular Weight of NaOH, MVEtAc=88.11 g/mol
MWNaOH=40g/mol Density of EtAc, pEtAc=902 g/L
Mass of NaOH required= Volume of EtAc, M1V1=M2V2
CNaOH X 40g/mol x 5L= 10g NaOH (902 g/L/ 88.11 g/mol) x V1= 0.05 mol/L x
5L, V1= 0.0244L=24.4mL

Preparation of Titrant Solution

Mass of NaOH required Volume of HCL needed
=CNaOH x MWNaOH x VNaOH = CHCL x 1L x MWHCL x pHCL
=0.1 mol/L x 40 g/mol x 1L =0,25 mol/L x 1L x 36.46 g/mol x1.3 g/ml
=4 g NaOH =11.85 ml HCL

Volume of sample= 50ml Standard concentration of NaOH,

CNaOH,standard= 0.1 mol/L
Volume of reactor=2.5L Standard concentration of HCL,
CHCL,standard= 0.25 mol/L
Volume of HCL=10ml Feed concentration of NaOH, EtAc
= 0.05 mol/L
Temperature of reactor: 31oC
Time VNaOH VHCL VHCL Mole of Mole of CNaOH lnCNaOH 1/ 1/ Rate of
2
(min) Titrate Unreacted reacted HCL NaOH unreacted CNaOH (CNaOH) reaction,r
(ml) with with used to used in in sample (L/mol) (mol.L-
1
NaOH in NaOH quench the (mol/L) .min-1)
sample in the sample
(ml) sample reaction (mol)
(ml) (mol)
5 5.90 2.36 7.64 0.00191 0.00191 0.0382 -3.265 26.178 686.29 0.0001259
10 6.85 2.74 7.26 0.00182 0.00182 0.0364 -3.313 27.473 754.74 0.0001143
15 7.85 3.14 6.86 0.00172 0.00172 0.0344 -3.370 29.070 845.05 0.0001021
20 7.55 3.02 6.98 0.00175 0.00175 0.0350 -3.352 28.571 816.33 0.0001057
25 7.40 2.96 7.04 0.00176 0.00176 0.0352 -3.347 28.409 807.08 0.0001069
30 7.65 3.06 6.94 0.00174 0.00174 0.0348 -3.358 28.736 825.74 0.0001045
Table 1. Effect of reaction time.
 Figure 1: CNaOH vs Time

Figure 2: ln CNaOH vs Time

 Figure 3: 1/CNaOH vs Time

Figure 4: 1/ (CNaOH)2 vs Time

Speed VNaOH VHCL V HCL reacted Mole of HCL Mole of CNaOH Rate of
(rpm) titrate, unreacted with NaOH in used to NaOH unreacted in reaction,r
(ml) with NaOH sample quench the unreacted in sample (mol.L-
1
in sample (ml) reaction sample (mol/L) .min-1)
(ml) (mol) (mol)
3 3.55 1.42 8.58 0.00215 0.00215 0.0430 0.0001596
5 7.50 3.00 7.00 0.00175 0.00175 0.0350 0.0001057
6 8.10 3.24 6.76 0.00169 0.00169 0.0338 0.0000986
7 7.10 2.84 7.16 0.00179 0.00179 0.0358 0.0001106
Table 2. Effect of stirrer speed.

Figure 5: CNaOH vs stirrer speed

 SAMPLE CALCULATION

Reaction Rate Constant, k

1/CA = kt + 1/CA0 which is equivalent to y=mx+c.
Hence, from figure 3 the reaction rate constant is 0.0863 L/mol.min.

Rate of Reaction, -rA

Since CNaOH = CEtAc
-rA = kCACB = kCA2
0.0863𝐿 (0.0382 𝑚𝑜𝑙)2 0.0001259 𝑚𝑜𝑙
−𝑟 − 𝑟𝐴 = 𝑥 =
𝑚𝑜𝑙 ⋅ min 𝐿 𝐿. 𝑚𝑖𝑛

Activation Energy, EA
In this experiment, temperature cannot be manipulated. So, the activation energy for the
reaction cannot be calculated.
Initial moles of NaOH in sample
Concentration of NaOH, CNaOH =
0.05mol/L Volume of sample, Vs =
50ml
Initial moles of NaOH in sample = 0.05mol/L x (50/1000) L
= 0.0025 mol
Unreacted VHCl
Concentration of EtAc, CEtAc = 0.05 mol/L
Concentration of HCl, CHCl (quenching solution) = 0.25
mol/L Volume of HCl added to sample, VHCl = 10ml
Concentration of NaOH, CNaOH (titrating solution) =
0.1 mol/L VNaOH used for titrating = 5.9ml
Volume of quench HCl unreacted with NaOH in sample, VHCl unreacted
= CNaOH/CHCl x VNaOH titrated
= 0.1/0.25 x 5.9ml
= 2.36ml

Unreacted CNaOH
Volume of HCl reacted with NaOH in sample, VHCl reacted
= VHCl - VHCl unreacted
= (10 – 2.36) ml
= 7.64 ml
Mole of HCl reacted with NaOH in sample
= CHCl x VHCl reacted
= 0.25 mol/L x (7.64/1000) L
= 0.00191mol
Mole of NaOH unreacted in sample = Mole of HCl reacted with NaOH in sample
= 0.00191mol
Concentration of NaOH unreacted with EtAc, Unreacted CNaOH
= mole of unreacted NaOH in sample / Vs
= 0.00191mol/ (50/1000) L
= 0.0382 mol
DISCUSSION

This experiment was conducted to investigate the saponification process of ethyl acetate and
sodium hydroxide. There were two manipulated variables. First was the residence time of the
saponification process, at 5 minutes interval, while the speed of stirrer was kept constant. The
other manipulated variable was speed of the stirrer while the residence time, 5 minutes, was
kept constant. The responding variables for this experiment were reaction constant (k), rate of
reaction and order of reaction. Although, activation energy is also an important data for any
reaction, our experiment did not permit as we had a limited technology to figure it out. The
reaction started when sodium hydroxide and ethyl acetate were mixed in the CSTR. The
reaction between the sodium hydroxide and ethyl acetate are saponification process which
produced sodium acetate and ethyl alcohol. This reaction is the main reaction in the
manufacturing of soap. The general equation of this reaction is

CH3COOC2H5+NaOH  CH3COONa + C2H5OH

Volume of sodium hydroxide used for titration was used to calculate the volume of
hydrochloric acid remained unreacted. The theoretical trend for the sodium hydroxide used
increases as the residence time increases. However, between minute 15th and 25th the value
fluctuated from the trend. Also, the value of sodium hydroxide used for titration should be
increasing as the speed of the stirrer increasing. In actuality, the experiment data had general
inclination to follow the theory but at 7 rpm the value deviated.

The order of reaction was determined by using graphical method where Figure 3 fitted
the criteria the best where it showed a plot of 1/concentration of NaOH against time. Second-
order reaction is one whose rate is proportional to the square of the concentration of one
reactant. Moreover, the rate constant was also discovered from said graph; 0.0863 L/mol.min.
From the acquired data in Table 1, the first rate was 0.0001259 mol/L.min. The value of the
rate of reaction decreased as the time increased until it reached the value of 0.0001045
mol/L.min at minute 30th. According to the theory, as the time increases, the rate of reaction
also increases as longer contact time between reactants. For the stirrer speed experiment, the
first value of rate of reaction was 0.0001596 mol/L.min at 3 rpm and ended with 0.0001106
mol/L.min with a speed of 7 rpm. Theoretically, the reaction rate should be increase as the
mixing speed increases. This is because mixing speed helps the Sodium hydroxide to react and
contact with Ethyl acetate easily and frequently which directly develop the chemical reaction.
 The data that we procured did not obey the theories fully because of several mistakes
that we did during the experiment. The major error was during titration where our group could
not reach the endpoint which was indicated by the change of colour of phenolphthalein.
 5.0 CONCLUSION

From the experiment, we are able to carry out the saponification reaction between ethyl
acetate and sodium reaction to form sodium acetate in a Continuous Stirred Tank Reactor
(CSTR). The effect of residence time for the saponification reaction is studied as he
concentration of unreacted NaOH in sample was decreasing for the 1st 15 minutes and
increasing for the following 10 minutes and reduce back for the last 5 minutes. For the 1 st 15
minutes, the results follow the theory of rate of reaction where less NaOH can be reacted with
ethyl acetate when the reaction time increases. For the 1st 15 minutes, the results follow the
theory of rate of reaction where less NaOH can be reacted with ethyl acetate when the reaction
time increases. There might be errors occur in the reactor that disrupt the process causing the
value between minute 15th and 25th fluctuated from the trend. Besides, by manipulating the
mixing speed of batch CSTR with constant reaction time and reaction temperature, the
concentration of unreacted NaOH in sample was reducing when the mixing speed is increasing
and decrease at last. Again, it showed positive results at the beginning and there might have
technical errors occurred during the experiment which affect the last reading. The order
saponification reaction then determined which is 2nd order reaction with reaction rate constant,k
of 0.0863 L/mol.min.

There are some recommendations which can be done to reduce errors and to improve
the accuracy and consistency of the data collecting. First, the feed tank should be cleaned
thoroughly to prevent inaccuracy of initial molar concentration of feed. Second, eyes must be
parallel to the scale of measuring instruments like measuring cylinder, conical flask and more
to get more accurate readings. Third, during the titration, NaOH has to be titrate carefully to
the sample carefully until the solution turns from colourless to light pink. Last, the reactor is
suggested to cover with insulation layer to prevent the loss of heat to the surrounding.