ISOTHERMAL PLUG FLOW TUBULAR REACTOR

(Coiled Tube Type)

1. OBJECTIVE:
To study of a non-catalytic homogenous reaction in a coil tube type plug flow reactor
under isothermal condition.

2. AIM:

2.1 To determine the reaction rate constant, (K) for saponification of ethylacetate
with sodium hydroxide at a fixed temperature.

2.2 To study the effect of temperature on the reaction rate constant, (K) and
determine the activation energy, (E) for this reaction.

3. INTRODUCTION:

Real reactors do not satisfy the idealized flow patterns, back mix flow or plug flow
deviation form ideality can be due to channeling of fluid through the vessel, recycling of
fluid within the vessel or due to the presence of stagnant region or pockets of fluid in
the vessel.

In an ideal plug flow reactor (PFR) there is no mixing in the direction of flow and
complete mixing perpendicular to the direction of flow. Concentration of the reactant
varies along the length of the reactor but not in the radial direction.

4. THEORY:

In case of a coil, turbulence is introduced due to frequent change in direction of flow and
presence of secondary flow, So higher value of, K is expected in case of a coil type PFR.

REACTION:

NaOH + CH3COOC2H5 CH3COONa + C2H5OH

(A) (B) (C) (D)

The above reaction is second order reaction (n = 2)

For second order reaction

 − RA = dCA
dt

− RA = KCA2 …………….. (1)

Where − RA is rate of disappearance of A, CA is concentration of A at any time t, K is Rate

constant.

5. DESCRIPTION:
The reactor is made up of SS tube and formed a helical coil. 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 rate of chemicals. The flow rate can be adjusted by the
needle valves provided on respective rotameter. The compressed air is used for
circulation of feed. Constant temperature water bath arrangement is provided to
conduct the experiment at various temperatures. Pressure regulator, pressure gauge
and safety valve are fitted in the compressed air line. Product coming out from the
reactor are analyzed by chemical titration.

6. UTILITIES REQUIRED:

6.1 Electricity supply: single phase, 220 V AC, 50 Hz, 5-15 Amp combined socket
with earth connection.

6.2 Compressed air supply continuous @ 0.5 CFM at 1 Bar.

6.3 Water supply (Initial fill)

6.4 Floor drain required.

6.5 Laboratory glass ware:-

Conical flasks (250 ml) : 01 No.

Measuring cylinder (50 ml) : 01 No.

 Burette (50 ml) : 01 No.

6.6 Chemicals:-

Distilled water : 40 Lit

NaOH Pellets : 100 gm

N/10 NaOH : 100 ml

N/10 HCl : 100 ml

Ethyl acetate : 200 ml

Indicator (phenolphthalein) : Few drops

7. EXPERIMENTAL PROCEDURE:

7.1 STARTING PROCEDURE:

7.1.1 Prepare 20L of N/10 NaOH solution by dissolving 80 gm of sodium

hydroxide in 20L of distilled water.

7.1.2 Prepare 20L of N/10 ethyl acetate solution by mixing 176 gm (or 196 ml)
of ethyl acetate in 20L of distilled water.

7.1.3 Take 20 ml of N/10 hydrochloric acid in measuring cylinder.

7.1.4 Fill the burette by N/10 sodium hydroxide (Standard Solution).

7.1.5 Close all the valves V1-V11.

7.1.6 Open valve V4 and V6 , fill sodium hydroxide solution in feed tank A.

7.1.7 Close valve V4 and V6.

7.1.8 Open valve V5 and V7 , fill ethyl acetate solution in feed tank B.

7.1.9 Close valve V5 and V7.

7.1.10 Fill water in the water bath.

7.1.11 Ensure that ON/OFF switches given on the panel are at OFF position.

o
7.1.12 Set the reaction temperature (ambient to 70 C) by increment, decrement
and set button of DTC.

7.1.13 Connect electric supply to the set-up.

 7.1.14 Start the heater and stirrer of the bath and wait till constant temperature
is attained.

7.1.15 Connect compressed air supply to the set-up at valve V1.

2
7.1.16 Open valve V1 and set air pressure 0.5 to 1 kg/cm by pressure regulator
and pressure gauge.

7.1.17 Pass sodium hydroxide and ethyl acetate into the reactor by allowing
equal flow rate controlled by valve V2-V3.

7.1.18 After about 10 min or time equal to the residence time of the reactor
(which ever is greater) collect exact 10 ml of the sample from the outlet in
measuring cylinder that already contain 20 ml of hydrochloric acid.

7.1.19 Note down the reaction temperature.

7.1.20 Transfer the sample solution in a conical flask.

7.1.21 Titrate the solution, using phenolphthalein as an indicator against N/10

sodium hydroxide (add NaOH from burette).

7.1.22 Repeat the experiment for different flow rates of feed.

7.1.23 Repeat the experiment for different reaction temperature.

7.2 CLOSING PROCEDURE:

7.2.1 When experiment is over stop the flow of feed by close the valve V2-V3.

7.2.2 Switch OFF the heater and stirrer of the water bath.

2
7.2.3 Reduce air pressure to 0 kg/cm by pressure regulator and pressure
gauge.

7.2.4 Close the valve V1.

7.2.5 Drain the feed tanks, reactor and water bath by open the valve V8-V11.
8. OBSERVATION & CALCULATIONS:

GIVEN DATA:

Real gas constant R = 1.987 cal/mole K

Working volume of reactor VR = ______ Lit
Volume of HCl VHCl = 20 ml
Volume of sample VSAMP = 10 ml
Normality of NaOH in feed solution NNaOH = 0.1 g eq/L
Normality of NaOH used for titration N1 = 0.1 g eq/L
Normality of HCl NHCl = 0.1 g eq/L
9. NOMENCLATURE:

Nom Column Headings Units Type

CA Concentration of unreacted NaOH in the reactor mole/L Calculated

CAo Initial concentration of NaOH in the feed mixture mole/L Calculated
E Activation energy of the reaction Cal/mol Calculated
HClO Amount of HCl taken for quench mole Calculated
HClR Amount of HCl reacted with NaOH mole Calculated
K Rate constant for individual run L/ mole min Calculated

K
T Rate constant obtained from slope L/ mole min Calculated
N1 Normality of NaOH used for titration g eq /L Given
NHCl Normality of HCl g eq /L Given
NNaOH Normality of NaOH in feed solution g eq /L Given
R Real gas constant Cal/mole K Given
S1 Slope of graph (τ vs. XA/ [1-XA]) min Calculated
S2 Slope of graph (ln K vs 1/T’) K Calculated
T Reaction temperature oC Measured
T’ Reaction temperature K Calculated
V1 Volume of NaOH used for titration ml Measured
VA Volumetric flow rate of NaOH LPH Measured
VB Volumetric flow rate of CH3COOC2H5 LPH Measured
VHCl Volume of N/10 HCl taken for quench ml Given
VSAMP Volume of sample ml Given
VR Working volume of reactor Lit Given
XA Degree of conversion * Calculated
τ Residence time min Calculated

* Symbols are unitless

10. PRECAUTION & MAINTENANCE INSTRUCTIONS:
10.1 Measure the exact volume of water and weight of chemicals.

10.2 Always use distilled water, good quality chemicals and standard solution for
titration.

10.3 Keep close all the drain valves V8-V11, and vent valves V6-V7 should be open
while filling the reactant in feed tanks.

10.4 Flow should not be disturbed during the experiments.

10.5 Handle the chemicals carefully.

10.6 Do not ON the switch of heater, before filling the water in the water bath.

11. TROUBLESHOOTING:

11.1 If any type of suspended particles are come in the rotameter, remove the
rotameter clean the tube and fit it at its place.

11.2 If there is any leakage tight that part or fix it again after wrapping teflon tape.

11.3 If rotameter fluctuating more than average tight control knob.

11.4 If DTC do not display temperature on display board it means sensor connection is
not proper (tight computer jacket).

11.5 If switch of the heater is ON, the heater but temperature can’t rise but panel LED
is ON it means bath had burned replace it

12. REFERENCES:
rd
12.1 Levenspiel, Octave (2001). "Chemical Reaction Engineering" 3 Ed. NY: John
Wiley & Sons. pp 27-28, 44, 72, 111.

th
12.2 Fogler H. Scoot (2008). "Elements of Chemical Reaction Engineering" 4 Ed.
ND: Prentice-Hall of India Pvt. Ltd. pp 172-174.
13. PHOTOGRAPH:
14. BLOCK DIAGRAM: