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ABSTRACT

The experiment involves a continuous stirred tank reactor (cstr). This experiment is to
determine the effect of temperature onto the reaction extent of conversion and to determine
the reactions activation energy. Firstly the reactor is filled with sodium hydroxide, NaOH
and Ethyl acetate, Et(Ac) until achieved 10 L. The flow rate of both solutions must same at
0.20 L/min. The solution is stirred and speed of 200 rpm. The water temperature is set at 50
C. The steady state conductivity and temperature values is recorded and then find the
concentration of NaOH in reactor and the extent of conversion from calibration curve. The
50ml sample is collected then carried out the back titration procedure immediately. The
experiment is repeated with different temperature; 55 C, 60 C and 75 C.

OBJECTIVES
-To carry out a saponification reaction between NaOH and Et(Ac) in CSTR 40 litre.
-To determine the effect of residence time onto the reaction extent of conversion.
-To determine the rate constant.
-To determine the reaction rate.

INTRODUCTION
Reactor is one of equipment used mostly in the industrials sector. It changes the raw material
into the desired product. A good reactor will give a high production and economical. One of
criteria to choose or to design a good reactor is to know the effectiveness of the reactor itself.
There a many types of reactor depending on the nature of the feed materials and products.
One of the most important we need to know in the various chemical reaction was the rate of
the reaction. The continuous stirred-tank reactor (CSTR) which is also known as vat- or backmix reactor usually is a common ideal reactor type in chemical engineering. A CSTR often
refers to a model used to estimate the key unit operation variables when using a continuous
agitated-tank reactor to reach a specified output. This reactor works for all fluids, liquids,
gases, and slurries. The behaviour of a CSTR is always modelled by that of a Continuous
Ideally Stirred-Tank Reactor (CISTR). All calculations performed with CISTRs assume
perfect mixing. In a perfectly mixed reactor, the output composition is identical to
composition of the material inside the reactor, which is a function of residence time and rate
of reaction. CSTR used in this experiment, (model: BP 143) is designed for students
experiments on chemical reaction in liquid phase under adiabatic and isothermal conditions.
CSTR consists of two tanks of solutions and one reactor. The reactor is modelled in order to
perform the saponification reaction between the sodium hydroxide and ethyl acetate.
Saponification reaction of ethyl acetate and sodium hydroxide produced sodium acetate in a
batch and the continuous stirred tank reactor evaluate the rate data needed to design a
production scale reactor.

THEORY
Reaction Kinetics
Reaction kinetics is the branch of chemistry that quantifies rates of reaction. An elementary
chemical reaction is a chemical reaction whose rate corresponds to a stoichiometric equation.
In symbols:
A+BC+D
and the reaction rate will be defined as:
-r = k (cA) (cB)
where k is referred as the specific reaction rate (constant). The overall order of reaction is
defined as:
n = +
The Mass Balance
Mass is a conservative entity, hence given a control volume V the sum of mass flows entering
the system will equal the sum exiting minus (plus) the consumed (generated) or accumulated
fractions:
Rate of mass in- rate of mass out+ rate of mass generated- rate of mass consumed = rate of mass
accumulation
shortly:
IN OUT + PROD CONS = ACC

Residence Time
The reactors residence time is defined as the reactor volume divided by the total feed flow
rates.

Residence time, =

Conversion
The conversion (or fractional conversion), denoted X, is a frequently used measure of the
degree of reaction. It i s defined as

X=

EXPERIMENTAL PROCEDURES
General Start-Up Procedures
1) The following solution is prepared:
a) 40 L of sodium hydroxide, NaOH (0.1 M)
b) 40 L of ethyl acetate, Et(Ac) (0.1M)
c) 1 L of hydrochloric acid, HCl (0.25M), for quenching
2) Ensure that all valves are initially closed
3) The feed vessels are charged as follow.
a) The charge port caps for vessels B1 and B2 is opened.
b) The NaOH is carefully poured into vessel B1 and Et(Ac) into B2.
c) The charge port for both vessels is closed.
4) The power for the control panel is turned on.
5) Check that there is sufficient water in thermostat T1 tank. Refilled is necessary.
6) Cooling water valves, V13 is opened and let the cooling water flow through the
condenser W1.
7) Adjust the overflow tube to give a working volume of 10 L in reactor.
8) Valves V2, V3, V7, V8 and V11 were opened.
9) The unit was ready to run the experiment.

General Shut-Down Procedures


1) Keep the cooling water valve V13 open to allow the cooling water to continue
flowing
2) Pumps P1 and P2 is switched off. Stirrer M1 is switch off.
3) The thermostat T1is switched off. Let the liquid in the reaction vessel R1 cool down
to room temperature.
4) Cooling water valve V13 is closed.
5) Valves V2, V3, V7, and V8 were closed. Valves V4, V9 and V12 to drain the liquid
from unit.
6) The power for the control panel is turned off.

Preparation of calibration curve for conversion versus conductivity


1) The following solutions is prepared
a) 1L of sodium hydroxide, NaOH (0.1 M)
b) 1L of sodium acetate, Et(Ac) (0.1M)
c) 1L of deionised water, H2O
2) Determine the conductivity and NaOH concentration 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 Et(Ac)


c) 50% conversion : 50 mL NaOH + 50 mL Et(Ac)
d) 75% conversion : 25 mL NaOH + 75 mL Et(Ac)

e) 100% conversion : 100 mL Et(Ac)

Back Titration Procedures for manual Conversion Determination


1) A burette is filled up with 0.1 M NaOH solution.
2) 10 mL of 0.25 M HCl is measured in a flask
3) 50 mL sample is obtained from the experiment and immediately add the sample to the
HCl in the flask to quench the saponification reaction.
4) 3 drops of phenolphthalein is added into the mixture.
5) The mixture is titrated with NaOH solution from the burette until the mixture is
neutralized. The amount of NaOH is recorded.

Effect of Residence Time of The Reaction in a CSTR


1) Perform the general start-up procedures.
2) Switch on both pumps P1 and P2 simultaneously and open valves V5 and V10 to
obtain the highest possible flow rate into the reactor.
3) Let the reactor fill up with both the solution until it is just about to overflow.
4) Readjust the valves V5 to V10 to give a flow rate of about 0.1 L/min. Make sure that
both flow rates are the same. Record the flow rate.
5) Switch on the stirrer M1 and set the speed to about 200 rpm.
6) Start monitoring the conductivity value at Q1-401 until it does not change over time.
This is to ensure that the reactor has reached steady state.
7) Record the steady state conductivity value and find the concentration of NaOH in the
reactor and extent of conversion from the calibration curve.

8) Open sampling valve V12 and collect 50 mL sample. Carry out a back titration
procedure to manually determine the concentration of NaOH in the reactor and extent
of conversion.

APPARATUS
1)
2)
3)
4)
5)
6)

Continuous stirrer tank reactor Model: BP 143


50 mL burette
200 mL beaker
Conical flask
Conductivity probe
Solution :
a) Sodium hydroxide (NaOH) 0.1M
b) Ethyl Acetate (Et(Ac)) 0.1 M
c) Deionised water
d) Phenolphthalein
7) 100 mL Measuring cylinder

RESULTS
Reactor volume

= 10 L

Concentration of NaOH in feed vessel = 0.1 M


Concentration of Et(Ac) in feed vessel = 0.1 M
Temp

Flow rate

Of NaOH

(( C)

(ml/min)

Flow
rate
Of
Et(Ac)
(ml/min
)

Vol. of
NaOH
Titrate
d

Total flow
rate of
sol. F0
(ml/min)

Residenc
e time,

Conductivity

(min)

(mS/cm
)

(mL)

28.9

100

100

23.1

200

28.9

150

150

26.0

300

28.9

200

200

25.7

400

28.9

250

250

28.2

500

28.9

300

300

30.6

600

50
33
25
20
17

Exit
conc.
NaOH,
CNaOH,
(M)

Vol. of
unreacte
d
quenchin
g HCl
(mL)V2

Vol of H
reacted
with Na
in sam
(ml),V3

5.50

0.0038

9.24

0.76

5.09

-0.0020

10.40

-0.4

5.05

-0.0014

10.28

-0.2

5.03

-0.0064

9.28

-1.2

4.92

-0.0112

12.24

-2.2

Preparation of Calibration Curve


Conversion

Solution Mixture

Concentration Conductivity
Of NaOH (M) (mS/cm)

0.1 M NaOH

0.1 M Et(Ac)

H2O

0%

100 mL

100 mL

0.0500

12.83

25%

75 mL

25 mL

100 mL

0.0375

7.29

50%

50 mL

50 mL

100 mL

0.0250

3.42

75%

25 mL

75 mL

100 mL

0.0125

5.75

100%

100 mL

100 mL

0.0000

16.09

Rate Constant, k
k (M-1s-1)

ln k

1/T (C-1)

133.24

4.89

0.035

772.73

6.65

0.035

20.44x103

9.93

0.035

129.88

4.87

0.035

52.15

3.95

0.035

No

Rate Constant, k (M-1s-1)

Reaction rate, -rA (M/s)

133.24

1.92 x 10-3

772.73

3.10 x 10-3

20.44x103

0.04

129.88

5.32

52.15

6.54 x 10-3

Graph of Calibration Curve

SAMPLE CALCULATIONS

NaOH + HCl NaCl + H2O

Unknown quantity:
Concentration of NaOH in the reactor

CNaOH

mol/L

Volume of sample

Vs

50 mL

Concentration of NaOH in the feed vessel

CNaOH,f

0.1 mol/L

Known quantities:

Volume of HCl for quenching

VHCl,s

Concentration of HCl in standard solution

CHCl,s

Volume of titrated NaOH

V1

Concentration of NaOH used for titration

CNaOH,s

10 mL
=

0.25 mol/L
mL

0.1 mol/L

Calculations:
Conc. of NaOH entering the reactor, CNaOH,0 =
Vol. of unreacted quenching HCl, V2

CNaOH,f

mol/L

x V1

mL

Vol. of HCl reacted with NaOH in sample, V3

VHCl,s - V2

mL

Moles of HCl reacted with NaOH in sample, n1

(CHCl,s x V3)/1000

mol

Moles of unreacted NaOH in sample, n2

n1

mol

Conc. of unreacted NaOH in the reactor, CNaOH

n2/ Vs x 1000

mol/L

Conversion of NaOH in the reactor, X

(1-

Residence time, =

= 10 L/(0.1+0.1) Lmin-1
= 50 min
Exit concentration of NaOH
CNaOH,0 =

CNaOH,f

0.05 mol/L

) x 100%

V2

V3

n1

x V1

0.1/0.25 x 23.1

9.24 mL

VHCl,s - V2

10 - 9.24

0.76 mL

(CHCl,s x V3)/1000

0.25 x 0.76/1000

1.9x10-4

n2

n1

1.9x10-4 mol

CNaOH

n2/ Vs x 1000

1.9x10-4/50x1000

0.0038 M

(1-

) x 100% =
=

Rate constant

k1

(0.1-0.0038)/50(0.0038)2

133.24 M-1s-1

Reaction rate
-rA

kCA2

k= 133.24
-rA

kCA2

(133.24)(0.0038)2

1.92 x 10-3 M/s

[1-(3.8x10-3/0.05)]x100%
92.4%

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