RXN in PFR Tube

PLUG FLOW REACTOR (STRAIGHT TUBE TYPE)
AIM:
⮚ To study of a non-catalytic homogeneous reaction in a straight type plug flow reactor
under ambient conditions.
⮚ To determine the reaction rate constant, (k) for saponification of ethyl acetate with
sodium hydroxide at ambient conditions..
APPARATUS:
Conical flask (250 ml) : 10 No.
Measuring cylinder (50 ml) : 01 No.
Burette (50 ml) : 01 No.
pipette (10 ml ) : 01 N0.
CHEMICALS:
Distilled water : 50 Lit
NaOH Pellets : 100 gm
N/20 NaOH : 100 ml
N/10 HCl : 100 ml
Ethyl acetate : 200 ml
Indicator (phenolphthalein) : Few drops

DESCRIPTION:
The set up consists of two feed tanks through which two reactants are fed to the reactor .Flow rate
can be adjusted and measured by using peristaltic pump. The concentration of feed and the product
coming out from the reactor are analyzed by chemical titration.
PROCEDURE:
Starting Procedure:
1. Prepare 20L of N/10 NaOH solution by dissolving 80 gm of sodium hydroxide in 20L of

distilled water.
2. Prepare 20L of N/10 ethyl acetate solution by mixing 176 gm (or 196 ml) of ethyl acetate
in 20L of distilled water.
3. Take 10 ml of N/10 hydrochloric acid in measuring cylinder.
4. Fill the burette by N/10 sodium hydroxide (Standard Solution).
5. Close all the valves.
6. Open lid, fill sodium hydroxide solution in feed tank A.
7. Open lid, fill ethyl acetate solution in feed tank B.
8. Pass sodium hydroxide and ethyl acetate into the reactor by allowing equal flow rate
controlled by rpm.
9. After about 10 min or time equal to the residence time of the reactor (whichever is greater)
collect exact 10 ml of the sample from the outlet in measuring cylinder that already contain
10 ml of hydrochloric acid.
10. Transfer the sample solution in a conical flask.
11. Titrate the solution, using phenolphthalein as an indicator against N/10 sodium hydroxide
(add NaOH from burette).
12. Repeat the experiment for different flow rates of feed.
Closing Procedure:
1. When experiment is over stop the flow of feed.

2. Drain the feed tanks and reactor by open the valve.
THEORY:
In plug flow, the concentration of reactant decreases progressively through the system
and in mixed flow the concentration drops immediately to a low value. Because of this
fact, a plug flow reactor is more efficient than the mixed flow reactors for reaction whose
rates increases with reactants condition. 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.
REACTION:
NaOH + CH3COOC2H CH3COONa + C2H5 OH

(A) (B) (C) (D)
The above reaction is second order reaction (n = 2)

For second order reaction.
 dC A
 rA 
dt
rA  kCA2 (1)
Where rA is rate of disappearance of A, CA , CB is concentration of A and B at any time t, k is
rate constant.
The performance
equation for the plug
flow reactor at steady
state is:
VR

vo (2)
In terms of concentration we can write

CA
dC A
  
C Ao
rA (3)
Where  is residence time , VR is volume of reactor , vo is a volumetric flow rate of reactants A
and B, CAo is the initial concentration of A.
Substitute the value of –rA in equation (3) from equation (1)

C
1 A dCA
k CAo CA2
 
(4)
On solving the above equation we get

CA
1 1 
  
k  C A  CA o
1  C Ao  C A 
  
k  C AC Ao 
𝐶𝐴𝑜 − 𝐶𝐴
Rate constant, 𝑘 = 𝐶𝐴0 𝐶𝐴
1 𝐶𝐴0 − 𝐶𝐴0 + 𝐶𝐴0 𝑋𝐴

= [ ]
𝑘 𝐶𝐴0 . 𝐶𝐴0 (1 − 𝑋𝐴 )
1 𝑋𝐴
= [ ]
𝑘𝐶𝐴0 1 − 𝑋𝐴
Degree of conversion,
C Ao  C A
XA = C Ao
XA
Also, a plot of τ vs. 1  X A shall yield a straight line for an assumed second order reaction with
1

slope (kC Ao ) . From this slope rate constant, k can be calculated.
OBSERVATION & CALCULATION:
DATA:
Working volume of reactor VR = Lit
Volume of HCl VHCl = 10 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
OBSERVATION TABLE:
S.No. NA (RPM) NB (RPM) V1 (ml) t(sec)

CALCULATIONS :
N NaOH
C Ao = 2 (mol/L)
VHCl N HCl
MHCL = 1000 (mole)
M HCL 
V1 N1 
MHCLR = 1000 (mole)
M HCLR
CA   1000
VSAMP (mole/L)
C Ao  C A 
XA 
C Ao
VA = NA* 0.165
VB = NB* 0.157
VR * 3600

v A v B  (sec)
C Ao  C A
k
 C Ao C A (L/mole sec)
CALCULATION TABLE:1
S.No. XA k(L/mole min) XA/ [1-XA]

 (min)
Plot t vs. XA/ [1-XA] on a simple graph, and find slope S.

S= (min)
S1
kt  ( L / mole min)
C AO
NOMENCLATURE:
Nom Column Heading 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
MHCL Amount of HCl taken for quench mole Calculated
MHCLR Amount of HCl reacted with NaOH mole Calculated

k Rate constant for individual run L/ mole sec Calculated
kt Rate constant obtained from slope L/ mole sec 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
NA RPM of Peristaltic pump A * Measured
NB RPM of Peristaltic pump B * Measured
S Slope of the graph (τ vs. XA/ [1-XA]) sec-1 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 sec Calculated
t Time sec Measured
* Symbols are unitless quantity.
PRECAUTION & MAINTENANCE INSTRUCTIONS:

1. Measure the exact
volume of water
and weight of chemicals.
2. Always use distilled water, good quality chemicals and standard solution for titration.
3. Keep close all the drain valves V8-V10, and vent valve V6- V7 should be open while filling
the reactants in feed tanks.
4. Handle the chemicals carefully.
RELEVANT BACKGROUND READING:

Fogler, H. Scott, Elements of Chemical Reaction Engineering, 3rd Ed., PHI India Pvt. Ltd.
(1999).
(Chapters 3, 5)
Levenspiel, O., Chemical Reaction Engineering, 3rd Ed., John Wiley and Sons (1999).
(Chapter 3)
BLOCK DIAGRAM:

RXN in PFR Tube

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PLUG FLOW REACTOR (STRAIGHT TUBE TYPE)

Conical flask (250 ml) : 10 No.

Measuring cylinder (50 ml) : 01 No.

Burette (50 ml) : 01 No.

pipette (10 ml ) : 01 N0.

Distilled water : 50 Lit

NaOH Pellets : 100 gm

N/20 NaOH : 100 ml

N/10 HCl : 100 ml

Ethyl acetate : 200 ml

Indicator (phenolphthalein) : Few drops

1. Prepare 20L of N/10 NaOH solution by dissolving 80 gm of sodium hydroxide in 20L of

1. When experiment is over stop the flow of feed.

NaOH + CH3COOC2H CH3COONa + C2H5 OH

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

rA  kCA2 (1)

Where rA is rate of disappearance of A, CA , CB is concentration of A and B at any time t, k is

In terms of concentration we can write

Where  is residence time , VR is volume of reactor , vo is a volumetric flow rate of reactants A

and B, CAo is the initial concentration of A.

Substitute the value of –rA in equation (3) from equation (1)

On solving the above equation we get

1 𝐶𝐴0 − 𝐶𝐴0 + 𝐶𝐴0 𝑋𝐴

OBSERVATION & CALCULATION:

S.No. NA (RPM) NB (RPM) V1 (ml) t(sec)

S.No. XA k(L/mole min) XA/ [1-XA]

Plot t vs. XA/ [1-XA] on a simple graph, and find slope S.

Nom Column Heading Units Type

CAo Initial Concentration of NaOH in the feed mixture mole/L Calculated

MHCL Amount of HCl taken for quench mole Calculated

MHCLR Amount of HCl reacted with NaOH mole Calculated

kt Rate constant obtained from slope L/ mole sec 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

NA RPM of Peristaltic pump A * Measured

NB RPM of Peristaltic pump B * Measured

S Slope of the graph (τ vs. XA/ [1-XA]) sec-1 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 sec Calculated

t Time sec Measured

* Symbols are unitless quantity.

PRECAUTION & MAINTENANCE INSTRUCTIONS:

RELEVANT BACKGROUND READING:

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