Foreword

Welcome to value-conscious company. We are proud of the advanced engineering and

quality construction of each equipment we manufacture.

This manual explains the working of equipment. Please read it thoroughly and have all
the occupants follow the instructions carefully. Doing so will help you enjoy many years
of safe and trouble free operation.

When it comes to service remember that K.C. Engineers knows your equipment best
and is interested in your complete satisfaction. We will provide the quality maintenance
and any other assistance you may require.

All the information and specifications in this manual are current at the time of printing.
However, Because of K.C. Engineers policy of continual product improvement we
reserve the right to make changes at any time without notice.

Please note that this manual explains all about the equipment including options.
Therefore you may find some explanations for options not installed on your equipment.

You must follow the instructions and maintenance instructions given in the manual
carefully to avoid possible injury or damage. Proper maintenance will help ensure
maximum performance, greater reliability and longer life for the product.

K.C. Engineers
 Contents

1. Objective …………………………………… 1

2. Aim …………………………………… 1

3. Introduction …………………………………… 1

4. Theory …………………………………… 1

5. Description …………………………………… 2

6. Utilities Required …………………………………… 3

7. Experimental Procedure …………………………………… 3

8. Observation & Calculation …………………………………… 4

9. Nomenclature …………………………………… 5

10. Precautions & Maintenance Instructions …………………………………… 6

11. Troubleshooting …………………………………… 6

12. References ……………………………………. 6

Isothermal Continuous Stirred Tank Reactor

 ISOTHERMAL CONTINUOUS STIRRED TANK REACTOR

1. OBJECTIVE:
To study of a non-catalytic homogeneous reaction in a CSTR under isothermal
conditions.

2. AIM:
To determine the reaction rate constant for saponification of ethylacetate with NaOH
at a fixed temperature.
To study the effect of temperature on the reaction rate constant, k and determine the
activation of energy, (E) for this reaction.

3. INTRODUCTION:
In an ideal CSTR (that is an ideal steady state flow reactor) the contents in the reactor
are well mixed and have uniform composition throughout. Thus the exit stream has
the same composition as the fluid within the reactor. These types of reactors are
known as MIXED FLOW REACTOR.

4. THEORY:
REACTION:
NaOH + CH3COOC2H5
CH3COONa + C2H5OH
Reactor volume (volume of fluid in the reactor) = VR, Liters
Volumetric feed rate (volumetric feed rate of A + volumetric feed rate of B) = Vo,
LPM
VR
Residence time, τ = , min
Vo
The performance equation for the mixed flow reactor at steady state is:
VR C Ao X A C Ao − C A
τ = = =
Vo − rA − rA
XA and rA are evaluated at exit stream conditions, which are the same as the
conditions within the reactor.
For a second order reaction:
A+B
C+D
With CAo = CBo and negligible change in density of reaction mixture

Isothermal Continuous Stirred Tank Reactor 1

 − dC A
− rA = = KC A2
dt
Hence,
VR C Ao X A C Ao − C A C Ao − C A
τ = = = =
Vo − rA − rA kC A2

(C Ao − C A )
Degree of conversion, X A =
C Ao

and rate of reaction, -rA = CAo XA/ τ, g mol/l min

C Ao − C A
the rate constant, K= , L/g mole min
τ C A2
For nth order reaction, − rA = KC An
log( − rA ) = log k + n log C A
The order of the reaction, n, can be obtained from a plot of log (-rA) vs. logCA, that
yields a straight line with slope = n, and intercept (at CA= 1 or at log CA=0) shall give
the value of log (k).
Also, a plot of τ vs. XA/ (1-XA) 2 shall yield a straight line for an assumed second
order reaction with slope = 1/ (k CAo). From this slope rate constant, k can be
obtained.
Effect of temperature on reaction rate constant is expressed in terms of Arrheniu’s
law:
k = k o e − E / RT
ko is the frequency factor and E is called the activation energy of reaction.
A plot of k vs.1/T yields a straight line with slope = -E/R
From this slope, activation energy, E can be estimated.

5. DESCRIPTION:
The set up consists of two feed tanks through which two reactants are fed to the
reactor. Rotameters are provided to measure the individual flow of chemicals. The
flow rate can be adjusted by operating the needle valves provided on respective
Rotameter. The compressed air is used for circulation of feed. The CSTR is fitted with
stirrer for proper mixing. From top outlet of it samples are collected for analysis.
Constant temperature water bath arrangement is provided to conduct the experiment is
provided to conduct the experiment at various temperatures. Pressure Regulator,
Pressure gauge and Safety Valve are fitted in the compressed air line.

Isothermal Continuous Stirred Tank Reactor 2

6. UTILITIES REQUIRED:
Electricity Supply: Single Phase, 220 V AC, 50 Hz, 0.5 kW with earth connection.
Water Supply.
Drain.
Compressed Air Supply at 2 Bar, 0.5 CFM.
5 conical flasks.
Measuring cylinder
Stopwatch.
Burette.
CHEMICALS: QUANTITY:
NaOH Pellets. 100 gm
N/10 HCl. 100 ml
Ethyl acetate 200 ml
Indicator (phenolphthalein). Few drops

7. EXPERIMENTAL PROCEDURE:
1. Prepare 20L of N/10 NaOH solution by dissolving 80 gm of NaOH in 20L of
water.
2. Prepare 20L of N/10 ethylacetate solution by mixing 176 ml of ethylacetate in 20L
of water.
3. Fill the respective tanks with these solutions.
4. Set the reaction temp. Start the heater and stirrer of the bath and wait till steady
state temp. in the water bath is attained. Record the reaction temperature, T.
5. Adjust the flow rate of the two streams so that in the feed mixture CAo = CBo (i.e.
have equal flow rates (e.g. 10 LPH each, you may use the flow range 16LPH to 2.5
LPH for each stream) using calibrated rotameters.
6. Pass equimolar feed rates of ethyl acetate and NaOH into the CSTR by allowing
equal volumetric feed rates of reactants in to the reactor
7. After about 10 min or time equal to twice the residence time of the reactor (which
ever is greater) i.e when steady state is achieved, collect exact 20ml of the sample
of the liquid at the out let, in a graduated cylinder that already contains 20 ml of
(chilled) N/10 HCl. Transfer this solution (40 ml) in a 250ml or 100 mL titration
flask.

Isothermal Continuous Stirred Tank Reactor 3

 8. Using phenolphthalein as indicator, titrate this solution (i.e excess HCl) against
N/10 NaOH (add NaOH from burette). & note the volume of N/10 NaOH used (
VNaOH)
9. For calculating the conversion at equilibrium condition, collect the sample 10 ml,
in an empty conical flask and allow the reaction to proceed for completion for two
hours. After two hours titrate the solution with N/10 HCl using phenolphthalein as
indicator. Note the volume of N/10 HCl used.
10. Repeat all the steps for four different reaction temperatures (25, 30, 35, 40 oC) at a
single flow rate of feed, or you may use four different flow rates at a constant
temperature.

8. OBSERVATION & CALCULATIONS:

DATA:
VR = ------------ L
CAo = ------------ g mole/L
VHCl = ------------ ml
VSAMP = ------------ ml
NNaOH = ---------- g mole/L
NHCL = ---------- g mole/L
OBSERVATION:
Vo = --------- LPH
VNaOH = ---------- ml
Run. T,K VNaOH,ml Vo, LPH
No

CALCULATIONS:
V HCL N HCL
HCLO = , g mole = ---------------- g mole
1000

Isothermal Continuous Stirred Tank Reactor 4

 (V NaOHN NaOH )
HCLR = HCLO − , g mole = ----------------- g mole
1000
HCLR
CA = × 1000 , g mole/L = ----------------------- g mole/L
VSAMP

(C Ao − C A )
XA= = ---------------
C Ao

VR * 60
τ= = ---------------------- min
Vo

C Ao − C A
K= , L/g mole min = ------------------- L/g mole min
τ C A2
Plot τ vs. XA/ [1-XA]2 on a simple graph, the slope is = 1/ (K CAo); from the slope
find k and report k at the reaction temp.
CACLULATION OF ACTIVATION ENERGY (E):

Run. T,K 1/T , K-1 K , L/g

No molmin

Plot Plot k vs 1/T on a semi-log graph. Draw a smooth line (best fit line) through all
the data points and measure the slope and intercept of the straight line.
−E
Slope = = -------------
R
E = slope × R , cal/mol = ---------------

9. NOMENCLATURE:
CA = Conc. of unreacted NaOH in the reactor, g mole/L
CAo = Initial concentration of NaOH in feed, g mole/L
E = Activation energy, cal/mol
HCLO = Amount of HCL taken as quench, g mole
HCLR = Amount of HCL reacted with NaOH, g mole

Isothermal Continuous Stirred Tank Reactor 5

 K = Rate constant, L/g mole min
NHCL = Number of moles of HCL used, g mole/L
NNaOH = Number of moles of NaOH used, g mole/L
R = Real gas constant, cal/mol K
T = Reaction temperature, K
VR = Volume of the reactor, L
VSAMP = Volume of sample collected, ml
VHCL = Volume of HCL, ml
VNaOH = Volume of NaOH, ml
Vo = Volumetric flow rate, LPH
XA = Fractional conversion
τ = Residence Time, min

10. PRECAUTIONS & MAINTENANCE INSTRUCTIONS:

1. Measure the exact volume of water and weigh the chemicals.
2. Always use clean water and good quality chemicals and standard solution for
titration.
3. Use electronic balance for weighing of chemicals. Don’t mix the droppers of
different chemicals.
4. Keep close all the drain valves and vent valve should open while filling the
reactant in feed tanks.
5. Flow should not be disturbed during the experiments.
6. Handle the chemicals carefully.
7. Don’t ON heater switch before filling the water in the bath.
8. There should be no air in the flow during experiment.

11. TROUBLESHOOTING:
1. If any type of suspended particles are come in the Rotameter. Remove the
Rotameter clean the tube and fit that at its place.
2. If there is any leakage tight that part or remove that and fix that again after
wrapping Teflon tape.
3. If Rotameter fluctuating more than average tight control knob of that.
4. If D.T.C display ‘1’ on display board it means sensor connection is not OK tight
that.

Isothermal Continuous Stirred Tank Reactor 6

 5. If switch ON the heater but temperature can’t rise but panel LED is ON it means
bath heater had burned replace that.

12. REFERENCES:
1. Octave Levenspiel, “Chemical reaction engineering,”3rd ed., John Wiley & Sons,
NY, 2001, Page 27, 90-97.
2. Coulson & Richardson, “Chemical Engineering Vol-3” 4th ed, Asian Books
Pvt.Lt, ND, 1991, Page 17-18, 43-45, 61, 64-65.

Isothermal Continuous Stirred Tank Reactor 7