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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 …………………………………… 2

7. Experimental Procedure …………………………………… 2

8. Observation & Calculation …………………………………… 3

9. Nomenclature …………………………………… 5

10. Precautions & Maintenance Instructions …………………………………… 5

11. Troubleshooting …………………………………… 6

12. References ……………………………………. 6

Spinning Basket Reactor


SPINNING BASKET REACTOR
1. OBJECTIVE:
Catalytic hydrolysis of ethyl acetate in Spinning Basket Reactor.

2. AIM:
To determine the reaction rate constant.

3. INTRODUCTION:
Reaction:
Liquid phase hydrolysis of Ethyl Acetate to ethanol and Acetic Acid.:
CH 3COOC 2 H 5+ H 2 O 
→ CH 3COOH + C 2 H 5 OH

4. THEORY:
Let the reaction be represented by:
A  B+D (1)
Rate = K CA (2)
Let V be the volume of the reaction mixture.
Let C be the concentration of Ethyl Acetate in the reactor at any time, t
Mass balance around the reactor is:
d (V C )
= − (k C )V (1)
dt
at t= 0, C = C0
Integration of the above equation yields:
C
ln = − kt (2)
C0
The apparent rate constant, k can be obtained from the above equation by using
observed time concentration data. This apparent constant will be true for the known
weight of catalyst used at a particular value of shaft speed, N.
C =C o −C B
Where
CB = Effluent concentration of Acetic Acid.
Co = Feed concentration of Ethyl Acetate.

Spinning Basket Reactor 1


5. DESCRIPTION:

Any catalytic liquid-liquid reaction involving the use of a catalyst placed in basket
can be studies in this set-up. The set-up consists of a reactor centrally having one
spinning basket derived through a variable speed motor. The reactant from feed tank
is fed to the reactor at the bottom. Flow rate of the feed is measured by the Rota
meter. Sampling points are provided for analysis.
Catalyst used in the reactor is Amberlyst 15 (Rohm - Haas or Aldrich) that can be
converted to acid form by continuous leaching of the catalyst with 10 % HCl solution
and then dry the rinsed resin with air to moisture content in equilibrium with the
atmosphere. The average size of catalyst particle in 0.5 mm.

6. UTILITY REQUIRED:

1. Electricity Supply: Single Phase, 220 V AC, 50 Hz, 5-15 amp combined socket
with earth connection.
2. Compressed air supply @ 2 CFM at 1 Bar.
3. Water Supply: (Initial fill).
4. Floor Drain Required.
5. Floor Area Required: 1 m x 0.75 m.
6. Laboratory Glassware Required : -
Conical flasks (250ml) : 05 Nos.
Measuring cylinder (50 ml) : 02 Nos.
7. Chemicals Required:
N/10 Ethyl Acetate : 10 L
N/10 NaOH : 200 ml
Phenolphthalein : Few drops

7. EXPERIEMNTAL PROCEDURE:

STARTING PROCEDURE
1. Prepare 4-5 % Ethyl Acetate solution in distilled water.
2. Based on the ambient temperature, note the density of Ethyl Acetate (ρ).
3. Fill the feed solution in the feed tank.
4. Fill water bath 3/4th with water.

Spinning Basket Reactor 2


5. Ensure that ON/OFF switch given on the panel is at OFF position.
6. Switch ON the mains supply.
7. Set the temperature of bath with increment / decrement and set button of DTC and
switch ON heater. Wait till desired temperature achieved.
8. Switch ON the pump and allow water to pass through reactor jacket.
9. Connect compressed air supply to the set up and set the air pressure 0.5 to 1
kg/cm2 by pressure regulator and pressure gauge.
10. For batch mode operation, fill the reactor 3/4th with feed solution.
11. Switch ON agitator motor and set the RPM of basket by variac.
12. Collect the 10-20 ml sample after every two minutes in measuring cylinder.
13. Put the sample in conical flask, add few drops of indicator and titrate it against
N/10 NaOH from burette.
14. Record the volume of NaOH used for titration.
15. For continuous mode allow feed to pass through the reactor at a fix flow rate by
Rota meter and flow control valve.
16. At steady state collect the 10-20 ml sample from the outlet of the reactor in
measuring cylinder.
17. Put the sample in conical flask, add few drops of indicator and titrate it against
N/10 NaOH from burette.
18. Repeat the experiment for different flow rate.
19. Repeat the experiment for different RPM.

8. OBSERVATION & CALCULATION:

DATA:
ρ = 895 kg/m3
MW = 88.11
N1 = 0.1 gmeq/L
VR = ----- L

OBSERVATIONS
VEA = ----- L
VW = ----- L
T = ----- oC

Spinning Basket Reactor 3


OBSERVATION TABLE (Batch mode)
S.N. N, RPM t, min VSamp VNaOH

OBSERVATION TABLE (Continuous mode)


S.N. N, RPM Vo, LPH VSamp VNaOH

CALCULATION (For Batch mode):


V EA×ρ
Co = , mole/L
MW ×V W

V NaOH × N 1
CB = , mole /L
V Samp

C F =C o −C B , moles/L

1 C 
k =   × ln o  , min-1
t   CF 
CALCULATION TABLE:
S.N. N, RPM t, min CF, mole/L k, min-1

CALCULATION (For Continuous mode):


V EA×ρ
Co = , mole/L
MW ×V W

V NaOH × N
CB = , mole /L
V Samp

C F =C o −C B , moles/L

Spinning Basket Reactor 4


VR * 60
τ= , min
Vo

1 C 
k = ln o  , min-1
τ  CF 

CALCULATION TABLE:

S.N. N, RPM τ, min CF, mole/L k, min-1

9. NOMENCLATURE:

ρ = Density of Ethyl Acetate at ambient condition, kg/m3


τ = Residence time, min.
CO = Initial feed concentration of Ethyl Acetate, mole/L
CB = Concentration of Acetic Acid, mole/L
CF = Concentration of Ethyl Acetate at out let, mole/L
k = Rate constant, min-1.
MW = Molecular Weight of Ethyl Acetate.
N = RPM of the shaft of Bucket.
N1 = Normality of NaOH, gmeq/L.
Vo = Flow rate of feed, LPH.
VR = Volume of reactor, L.
VEA = Volume of Ethyl Acetate taken for feed preparation, L.
VW = Volume of Distilled water taken for feed preparation, L.
T = Reaction temperature, oC.

10. PRECAUTION & MAINTENANCE:

1. Use clean water for making feed solutions.


2. Do not switch on the bath heater before filling the water into it.
3. Drain it properly after use.
4. Wash the reactor with hot water after use.

Spinning Basket Reactor 5


11. TROUBLESHOOTING:

1. If the fluid is coming without changing their concentration slow down the feed
rate.
2. If the fluid coming out at higher rate than feed decrease the RPM.
3. If electric panel is not showing the input on the mains light, check the main
supply.

12. REFERENCES:

1. Octave Levenspiel, “Chemical reaction engineering”, 3rd ed., John Wiley &
Sons, NY, 2001, Page 137-138.

Spinning Basket Reactor 6

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