School of Chemical Engineering & Advanced Materials

Module title: Engineering Practice (CME2121)

Laboratory experiment: Continuous Stirred Tank Reactor

Group no.: 27
Group members:
Darren Tang (140661602)
Jacqueline Tan (140661200)
Tan Zi Xiu (140661222)
Submission Date: January 2015

Summary

Safety
Hazard identification is important before starting any experiment. The hazards will be circled
out and recorded down. These, along with the COSHH form and Risk Assessment form are to
be assessed and verified by the lab technician, before deciding whether it is safe to carry on
with the experiment.
Hazard Identification and Mitigation

S/N

Work Activity

Type of
Hazard

Spill, Fire

Possible
consequences to
user if not
mitigated

Preparation of
solutions

Inhalation/Ingestio
n to user

Operation of PC,
equipment

Electrical

Ensure all drain

points are closed

Electrical shock,
Spills, electrical
possible inhalation
hazard
of vapor fumes

Adding/Refilling
solution into CSTR
tank

Spills

Taking readings
using the probes

Spills, electrical Irritation to skin,

hazard
electrical shock

Electric Shock to
user

Irritation to skin,
electrical shock to
user

Table 1.1: The identified hazards for the CSTR experiment.

Refer to Appendix G for detailed Risk Assessment table.

Risk Controls
Ensure that
proper PPE such
as gloves are
worn and avoid
contact
No liquids to be
handled near
them
Check that drain
points are closed
before
commencing
experiment
Ensure pouring
and introduction
of material into
tank is done
slowly
Ensure no
exposed wires
and ensure gloves
are worn.

Risk Assessment
The two solutions used for this experiment are Sodium Hydroxide and Ethyl Acetate. Taking
them together will form sodium acetate.
Sodium hydroxide is an irritant and hazardous in the case of skin contact. It is easily soluble
in water however it is hygroscopic in nature, in which it generates heat upon contact with
water. In the case of a spill, use appropriate tools such as acetic acid to neutralize and dispose
of it, and avoid water contact at all costs.
Ethyl Acetate is a clear, colourless liquid that is flammable in nature. Prolonged exposure to
this chemical may cause irritation to the eyes and respiratory tract. The vapours given off are
denser than air, hence it is at a risk of travelling to an ignition source and flashback. In the
event of a spill, use a non-combustible absorbent to absorb the residue and dispose of it. The
equipment was operated under 1atm (atmospheric pressure) and at room temperature
(25degC).
Risk Estimation Matrix

Severity of
Harm

High

Medium

Low

Severe

High

High

Medium

Moderate

High

Medium

Medium/Low

Minor

Medium/Low

Low

Low

Negligible

Effectively
Zero

Effectively
Zero

Effectively
Zero

Table 1.2: Risk estimation matrix

Negligible
Effectively
Zero
Effectively
Zero
Effectively
Zero
Effectively
Zero

Table of Contents
1. Introduction and Theoretical Background ...............................................1
2. Experimental Design and Method .......2
3. Equipment........................................................................................................3
4. Results .........................................................................................................4
5. Discussion .......5
6. Conclusion6
7. Data and Error Analysis...7
8. References....8
9. Nomenclature ..9
10. Appendix10

1. Introduction and Theoretical Background

1.1 REACTION IN CSTR
Continuous Stirred Tank Reactor (CSTR) is the most fundamental continuous reactor used in
chemical processes. During the operation, reactants are fed continuously into the reactor and
the contents of the tank are assumed to be well mixed by the agitator. The products are then
removed continuously from the reactor. The CSTR is commonly used in industrial
processing, mainly in homogenous liquid-phase flow reactions where agitation is required. In
this experiment, the reaction occurring within the reactor is saponification which is given by
the following first order reaction:
NaOH +
a

H3C2OOC2H5

H2COONa

C2H5OH

The reactants are Sodium hydroxide (a) and Ethyl Acetate (b), react to form Sodium Acetate
(c) and Ethyl Alcohol (d).

The reaction was carried out at constant temperature, volume,

flow rate and concentration of reagents under perfect mixing in CSTR to achieve steady state
and optimal conversion.

1.2 CONCENTRATIONS OF EACH SPECIES

The conversion that is associated with the solution conductivity can be achieved through the
use of following equations:
The inlet concentration of each reactant is calculated by the following equations:

[ a ] 0=

Fa
[ a ]
F a+ F b
(1)

[ b ] 0=

Fb
[ b ]
F a+ F b

(2)

The outlet concentration of the species is as follows:

[ c ]1 =[ b ] 0 X b

(3)

[ a ] 1=[ a ]0 [ b ] 0 X 0

(4)

for [ b ] 0< [ a ] 0

[ c ]1 =[ a ] 0 X a

(5)

[ a ] 1=[ a ]0 ( 1X a )

(6)

for [ a ] 0< [ b ] 0
Note that the equations to use depends on which reactant is limiting reagent.

1.3 CONDUCTIVITY
The equations (3), (4), (5) and (6) are combined to give an equation that solves for X a from a
measured value of conductivity. The conductivity of the solution is used to obtain conversion
within the reactor. From the reaction, the conductivity of the mixture is contributed by
sodium hydroxide (a) and sodium acetate (c). There is no conductivity for ethyl acetate and
ethyl alcohol as the contents do not contain ions. The conductivities of pure solutions (a) and
(c) with their concentrations are given by:
k a =0.195 [ 1+ 0.0184 ( T 294 ) ][ a ]
k c =0.07 [ 1+ 0.0284 ( T 294 ) ][ c ]

(7)
(8)

When T > 294

The conductivity of mixture is determined by the sum of equations 7 and 8:
k =k a + k c

1.4 CONVERSION AND RATE CONSTANT

Using the following equations to obtained the optimal conversion:

(9)

X a , 1=

k 10.195 [ 1+ 0.0184 ( T 294 ) ] [ a ] 0

{0.070[1+0.0284 ( T 294 ) ]0.195 [ 1+0.0184 ( T 294 ) ] } [ a ] 0

(10)
Equation 10 is formed by manipulating the equations 7, 8 and 9. The concentration terms is
written in terms of conversion, Xa and Xb depending on which reactant is the limiting reagent.
d ( V [ a ]1 )
=F [ a ]0 F [ a ] 1Vk [ a ] 1 [ b ]1
dt

(11)

Since the continuous reactor runs under steady state condition, there is no change to the
volume and hence, the equation 11 is rearrange to find the rate constant K.
k=

F ( [ a ]0 [ a ] 1 )
V [ a ]1 [ b ] 1

(12)

2. Experimental Design and Method

Continuous Stirred Tank Reactor (CSTR) was used to conduct pilot scale experiment on the
reaction of sodium hydroxide and ethyl acetate. The flow rates were chosen to be 32ml/min,
52ml/min and 72ml/min for both the pump settings. At flow rate 32ml/min, the conductivity
and temperature were recorded at every 3 minutes interval and at 52ml/min and 72ml/min,
the readings were taken down at every 1 minute interval. Each run took about 30 minutes for
at least 10 readings.

2.1 PREPARATION OF STOCK SOLUTIONS

As the conductivity sensor should not be exposed to concentrations that exceed 0.05M of
NaOH and 0.1M of H3C2OOC2H5, the reagent concentrations of 0.03M and 0.05M for
NaOH and H3C2OOC2H5 are used respectively. The NaOH and H3C2OOC2H5 stock
solutions were prepared by adding 2.4g of NaOH solids and 9.76ml of H3C2OOC2H5
solutions with the deionised water into 2L volumetric flask. Similarly, the H3C2OOC2H5
stock solution was made by transferring 9.76ml of H3C2OOC2H5 solution with deionised
water into 2L volumetric flask.

2.2 START-UP EXPERIMENT

At the start of the experiment, the taps for the feed tanks and CSTR were closed to prevent
leakage of solutions. Then, 2L of each sodium hydroxide and ethyl acetate solutions were
poured into the respective tanks. Next, the default readings for conductivity and temperature
were recorded by placing the probe and thermocouple into the feed tanks for measurement.
Once the readings were taken down, the probe and thermocouple was placed back into the
reactor. The main power was switched on followed by the pumps A and B as well as the
impeller. The temperature control was turned on only after the solution has filled up the
thermocouple. Then, the pumps were adjusted to desired flow rates that had achieved a
minimum of 10 readings per run as the temperature reached 30 oC. Each reading was recorded
at an interval of at least 1 minute interval for the system to reach steady-state. The procedure
is repeated for other flow rates. Feed tanks were refilled with reactant solutions twice.

2.3 SHUTDOWN EQUIPMENT

After collecting all the experiment data, the pumps and impeller switches were turned off
follow by the main power switch. The recorded data will be used for discussion on the
discrepancies between the published values and experimental values.

3. Equipment
[Insert Picture here]

The reactor is made up of several components:

i)

Two feed tanks: To store the solutions.

ii)

Two peristaltic pumps A and B: To pump the chemicals into the reactor with individual manual
speed controls.

iii)

Reactor vessel: Consist of impeller that ensure good mixing of reactants.

iv)

Thermocouple: To control the reactor temperature.

v)

Conductivity probe: To measure the solution conductivity.

vi)

Hot/Cold Water circulation: Fluid that flows through heating/cooling coils.

vii)

Conductivity meter: To display the conductivity measured by the probe

viii)

Temperature meter: To display the temperature measured by the thermocouple

4. Results

5. Discussion
5.3 RATE CONSTANT K
The rate constants are calculated by the following equation:
k=

F ( [ a ] 0[ a1 ] )
V [ a ] 1 [ b ]1

No. of runs
Average Flow rate
(L/s)
Average
Temperature (oC)
Rate Constant, k

(5.3.1)

Run 1

Run 2

Run 3

0.000533

0.000859

0.00118

32.9

33.4

32.3

(L/mol. s)
0.0165
0.0286
Table 5.3.1: Experimental rate constant at various average flow rates

0.0507

Refer to appendix C for detail calculation of rate constant k.

Source

Smith et al. [Ref]

Rate Constant, k (L/mol. s)

0.11
Table 5.3.2: Rate constant at steady state extracted from the literature

The experimental rate constants are obtained through the calculation using the equation 5.3.
From table 5.3.1, an increasing trend of experimental rate constants is observed as the
average flow rates increase. During steady-state, the experimental rate constants are expected
to be constant for the 3 runs however, the values deviate from each other due to several
experiment errors. The fluctuation of flow rates could be due to the inconsistent of peristalsis
pumps as it might affect the actual set point of flow rates. The inaccurate flow rates will
indirectly affect the concentrations which in turn cause the rate constants to deviate. Besides,
the settings for the pumps and impeller may have transportation lags in the system which
occurs after every new setting is made. Therefore, the instrument readings will lag behind and
fluctuate through a range of values. Due to these inevitable experimental errors, it can be
used to explain the experimental rate constants are different from those found in literature.

However, the theoretical rate constant only depends on the temperature therefore, the value is
more reliable. According to the literature, the theoretical rate constant is abstracted to be 0.11
L/mol.s at steady state. The theoretical rate constant is correlated to temperature and the
relationship is represented by Arrhenius law:
k =Ae

Ea
RT

(5.3.2)

The exponential term that consists of the ratio of activation energy E to the average kinetic
energy has significant influence on the rate constant. As the rate constant depends on the
temperature, it can be infer that high temperature and low activation energy favour larger rate
constant, and thus increase the rate of reaction. Theoretically, the rate constant can be derived
by Arrhenius law. The deviation between the experimental k value and theoretical k value is
due to the different equations (5.3.1 and 5.3.2) being used. The experimental k value is
calculated based on the concentrations whereas the theoretical k value is derived based on
temperature. Both dependencies are different which produce contrasting results.

5.1

Nomenclature
Fa

Volume feed rate of sodium hydroxide

L/s

Fb

Volume feed rate of ethyl acetate

L/s

[]

Sodium hydroxide concentration in Feed Vessel

mol/L

[b]

Ethyl acetate concentration in Feed Vessel

mol/L

Temperature

Volume of the reactor

Ni

Number of moles of species i in the reactor

moles

vi

Stoichiometric Coefficient

ri

Reaction rate

Residence Time

Rate Constant

L/mol.s

Pre-Exponential factor

Ea

Activation energy

kJ/mol

Gas Constant

J/mol.K

11. Appendix A: Experimental Design Calculation

11.1 CALCULATION FOR THE MASS OF NAOH PELLET FOR STOCK SOLUTION

Molar Concentration of NaOH=0.03 mol/ L

Molecular weight of NaOH =40 g/mol

Mass of NaOH pellet=40 0.03 2=2.4 g

11.2 CALCULATION FOR THE VOLUME OF H3C2OOC2H5 FOR STOCK SOLUTION

Molar Concentration of H 3C 2OOC 2 H 5=0.05 mol / L

Molecular weight of H 3 C 2 OOC 2 H 5=88 g /mol

Concentration of H 3 C 2 OOC 2 H 5 solution=0.05 88=4.4 g /L

Density of H 3C 2OOC 2 H 5 solution=0.901 g / L

Volume of H 3 C 2 OOC 2 H 5=

mass
4.4
=
2=9.76 ml
density 0.901

11. Appendix B: Results

11.1 RAW DATA
Time
(min)

Conductivity
(mS/cm)

Temperature
(C)

Run 1
Flowrate (ml/min)
Pump A: 32
Pump B: 32

0
3
6
9
12
15
18
21
24
27
30

3.72
3.63
3.39
3.26
3.20
3.17
3.13
3.10
3.12
3.07
3.07

Time
(min)

Conductivity
(mS/cm)

Temperature
(C)

Run 2
Flowrate (ml/min)
Pump A: 52
Pump B: 51

26.0
31.1
30.6
30.1
29.9
30.5
30.2
30.0
30.5
30.2
30.0

0
1
2
3
4
5
6
7
8
9
10

Table 11.1: Raw Data

11.2 CONCENTRATION OF A VERSUS TIME

3.08
3.15
3.16
3.16
3.15
3.13
3.10
3.08
3.07
3.03
3.03

Time
(min)

Conductivity
(mS/cm)

Temperature
(C)

Run 3
Flowrate (ml/min)
Pump A: 72
Pump B: 70

29.8
30.5
30.7
30.7
30.6
30.4
30.3
30.3
30.2
30.1
30.0

0
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15

3.02
3.05
3.06
3.05
3.07
3.04
3.03
3.01
2.99
2.97
2.94
2.93
2.93
2.96
2.96
2.95

30.0
29.9
30.1
30.5
30.7
30.5
30.5
30.3
30.2
30.1
30.0
29.8
29.9
29.6
29.6
29.5

12. Appendix C: Sample Calculations

12.1 CALCULATE THE CONCENTRATION OF SPECIES IN FEED VESSELS
Initial conductivity of sodium hydroxide (NaOH): 7.53mS/cm = 0.00753 S/cm
Initial Temperature (T0) = 26.4C = 299.4K
Concentration of NaOH:
ka 0.195[1 0.0184(T 294)][a]
0.00753 0.195[1 0.0184(299.4 294)][a]
[a] 0.035mol /L

Concentration of ethyl acetate in feed vessel: 0.05mol/L=0.05mol/dm3

[b] 0.05mol /dm 3

Flow rates
Run 1
Pump A (NaOH)
Pump B (Ethyl acetate)
Run 2
Pump A (NaOH)
Pump B (Ethyl acetate)
Run 3
Pump A (NaOH)
Pump B (Ethyl acetate)
Table 12.1: Average flow rates.

ml/min
32
32

L/s
0.000533
0.000533

Average (L/s)

52
51

0.000867
0.000850

0.000859

72
70

0.00120
0.00117

0.00119

0.000533

12.2 CALCULATION K VALUE AND CONVERSION FOR RUN 1

Fa
[a]
Fa Fb
Fa 0.000533L / s
Fb 0.000533L / s
0.000533
[a]0
0.035 0.0175mol / L
0.000533 0.000533
Fb
0.000533
[b]0
[b]
0.05 0.025mol / L
Fa Fb
0.000533 0.000533
[a]0

[c]1 [a]0 X a
[a]1 [a]0 (1 X a )
kc 0.07[1 0.0284(T 294)][c]
ka 0.195[1 0.0184(T 294)][a]
L 0.07[1 0.0284(T 294)]
M 0.195[1 0.0184(T 294)]
kc L[a]0 X a
ka M[a]0 (1 X a ) M[a]0 M[a]0 X a
k kc ka
k L[a]0 X a M[a]0 M[a]0 X a
T 30.18C 273 303.18K
mS
1S
S
k 3.098

0.003098
cm 1000mS
cm
k M[a]0
Xa
L[a]0 M[a]0
0.003098 0.195[1 0.0184(303.18 294)] (0.0175)

(0.07[1 0.0284(303.18 294)]) (0.0175) (0.195[1 0.0184(303.18 294)]) (0.0175)

0.3644

0.364

[a]1 [a]0 (1 X a )
0.0175(1 0.3644)
0.0111mol /L
[b]1 [b]0 [a]0 X a
0.025 (0.0175 0.3644)
0.01862mol /dm 3
F [a] [a]1
k 0

V [a]1[b]1
0.000533 0.0175 0.0111

0.0111 0.01862
1
0.0165L / mol s

12.3 CALCULATION K VALUE AND CONVERSION FOR RUN 2

[a]0

Fa
[a]
Fa Fb

Fa 0.000867L /s
Fb 0.00085L /s
0.000867
0.035
0.000867 0.00085
0.01767mol /L
Fb
0.00085
[b]0
[b]
0.05
Fa Fb
0.000867 0.00085
0.0247mol/L
k M[a]0
Xa
L[a]0 M[a]0
[a]0

0.003062 0.195[1 0.0184(303.18 294)] (0.01767)

(0.07[1 0.0284(303.18 294)]) (0.01767) (0.195[1 0.0184(303.18 294)]) (0.01767)
0.3755

[a]1 [a]0 (1 X a )
0.01767(1 0.3755)
0.01103mol /L
[b]1 [b]0 [a]0 X a
0.0247 (0.01767 0.3755)
0.01806mol /dm 3
F [a]0 [a]1
k

V [a]1[b]1
0.0008585 0.01767 0.01103

0.01103 0.01806
1
0.02862L /mol s

12.4 CALCULATION K VALUE AND CONVERSION FOR RUN 3

[a]0

Fa
[a]
Fa Fb

Fa 0.00120L /s
Fb 0.00117L /s
0.00120
0.035
0.00120 0.00117
0.01772mol /L

[a]0

[b]0

Fb
0.00117
[b]
0.05
Fa Fb
0.00120 0.00117

0.0247mol /L
k M[a]0
Xa
L[a]0 M[a]0
0.002946 0.195[1 0.0184(302.68 294)] (0.01772)
(0.07[1 0.0284(302.68 294)]) (0.01772) (0.195[1 0.0184(302.68 294)]) (0.01772)
0.4238
[a]1 [a]0 (1 X a )
0.01772(1 0.4238)

0.01021mol /L
[b]1 [b]0 [a]0 X a
0.0247 (0.01772 0.4238)
0.01719mol /dm 3
F [a]0 [a]1
k

V [a]1[b]1
0.001185 0.01772 0.01021

0.01021 0.01719
1
0.05071L / mol s

The objectives are to understand the limitations in assuming ideal CSTR behaviour and how

these can be minimised by controlling the operating conditions. Also, issues related to the
scale up of a CSTR and deviations from the ideal CSTR will be investigate from the
experiment.