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 3

6. Utilities Required 4

7. Experimental Procedure 4

8. Observations & Calculations 5

9. Nomenclature 6

10. Precautions & Maintenance Instructions 7

11. Troubleshooting 7

12. References 7

Combined Flow Reactor

 COMBINED FLOW REACTOR

1. OBJECTIVE:
Study of the effect of non-catalytic homogeneous reaction in a series arrangement of
PFTR and CSTR.

2. AIM:
To determine the conversion in both reactors connected in series (CSTR connected to
PFTR), for Saponification of ethylacetate with NaOH at ambient conditions.

3. INTRODUCTION:
When a single reactor cannot reaches the desired conversion then more reactors are
required to reach up to that level. To enhance the conversion we can arrange the two
reactors PFTR & CSTR in series. In this way the reactants well mixed .In an ideal
plug flow reactor (PFTR) 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. But 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. This type of reactor is also known as
Mixed Flow

4. THEORY:
When a single reactor cannot reaches the desired conversion then more reactors are
required to reaches the level. To enhance the conversion we can arrange the two
reactors PFTR & CSTR in series.
The optimum size ratio for two mixed flow reactors in series is found in general to be
dependent on the kinetics of the reaction & on the conversion level. For special case
of first order reactions, equal size reactors are best. For the reaction when n>1 the
smaller reactors will come first & then larger reactor. When n<1 larger will come first
In this way the reactors are chosen depending upon the reaction characterstics.
FOR CSTR
REACTION:
NaOH + CH3COOC2H5
CH3COONa + C2H5OH

Combined Flow Reactor 1

 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, = , min
Vo
The performance equation for the mixed flow reactor at steady state is:
VR C Ao X A C Ao C A
= = =
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
dC A
rA = = KC A2
dt
Hence,
VR C Ao X A C Ao C A C Ao C A
= = = =
Vo rA rA kC A2

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

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

C Ao X A
the rate constant, rA = , g mol/l min

FOR PFTR
For steady state rate operation:

XA
V dX
FAo
= r
0 A

For the reaction

K
CH3COOC2H5 + NaOH CH3COONa + C2H5OH
(B) (A)

rA = K C A C B Where, A = NaOH

B = CH3COOC2H5

Combined Flow Reactor 2

 For the condition:
C Ao = C Bo

rA = K C A2 .

C A = C Ao (1 X A )

X AF
V 1 dX
FAo
= 2
KC Ao (1 X )
0
2
A

Where, FAo = Vo C Ao
FAo = Molar flow rate of NaOH
Vo = Volumetric flow rate of feed, LPM
VR = Volume of the PFTR, L
X AF
VR 1 dX A
or
Vo
=
KC Ao (1 X )
0
2
A

1 X AF
or =
KC Ao (1 X AF )

When CAo, CBo are differ, then,

1 (C Bo / C Ao ) X A
= ln
KC Ao [(C Bo / C Ao ) 1] (C Bo / C Ao )(1 X A )

C Ao C A
XA =
C Ao
CA = Concentration of unreacted NaOH at steady state.
k = Reaction rate constant.

5. DESCRIPTION:
The set up consists of two feed tanks through which two reactants are fed to the
reactors fitted in series. Rotameters are provided to measure the individual flow of
chemicals. The flow rate can be adjusted by operating the needle valve provided on
respective Rota meter. The compressed air is used for circulation of feed. 1st is a
helical coil tube type reactor made up of SS pipe. Reactants enter at lower end
coming out of the top of coil from where it is fed to a MFR fitted with stirrer for
proper mixing. Pressure gauge, pressure regulator, & safety valve are fitted in the air

Combined Flow Reactor 3

 compressed line. The concentration of feed and the product coming out from the
reactor are analyzed by chemical titration and check the effect and the performance
of the reactor.

6. UTILITIES REQUIRED:
1. Electricity Supply: Single Phase, 220 V AC, 50 Hz, 0.5 kW with earth
connection.
2. Compressed Air Supply : 2 Bar, 0.5 CFM.
3. Water Supply.
4. Drain.
5. 5 conical flask
6. measuring cylinder
7. Stop watch
8. Burette
9. CHEMICALS: QUANTITY:
NaOH pellets 100 gm
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. Connect compressed air line to the apparatus and adjust the pressure in the tanks
with the help of pressure regulator and pressure gauge.
5. The outlet coming from P.F.T.R is the inlet feed mixture for the C.S.T.R.
6. After about 10 min i.e. when steady state is achieved, collect exact 10ml of the
sample of the liquid at both CSTR & PFTR outlets, in a graduated cylinder that
already contains 20 ml of N/10 HCl. Transfer this solution (30 ml) in a 250ml or
100 ml titration flask.
7. Titrate this solution (i.e excess HCl) against N/10 NaOH (add NaOH from
burette) using phenolphthalein as indicator.

Combined Flow Reactor 4

 8. 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.

8. OBSERVATION & CALCULATIONS:

DATA:
FOR CSTR
VR = --------- L
CAo = ---------g mole/L
VHCl = --------- ml
VSAMP = --------- ml
NNaOH = ---------- g mole/L
NHCL = ---------- g mole/L
FOR PFTR
VR = --------- L
CAo = --------- g mole/L
VHCl = --------- ml
VSAMP = --------- ml
NNaOH = ---------- g mole/L
NHCL = ---------- g mole/L

OBSERVATIONS:

FOR CSTR
Vo = ------------ LPH
VNaOH = -------- ml
FOR PFTR
Vo = ------------ LPH
VNaOH = -------- ml
CALCULATIONS:
FOR CSTR:
VHCL N HCL
HCLO = , g mole = ---------------- g mole
1000

Combined Flow Reactor 5

 (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
= = ---------------------- min
Vo

C Ao C A
k= , L/g mole min = ------------------- L/g mole min
C A2
Plot 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.
FOR PFTR:
VHCL N HCL
HCLO = , g mole= ------------------ g mole
1000
(V NaOH N 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
= , min= ------------------ min
Vo

C Ao C A
k= , L/g mole min = ----------------- L/g mole min
C Ao C A
Plot vs [1/CA 1/CAo] on a simple graph, the slope is = 1/K; from slope find K and
report K at the reaction temp.

9. NOMENCLATURE:
CA = Conc. of unreacted NaOH in the reactor, g mole/L
CAo = Initial Conc. of NaOH in the feed mixture, g mole/L
HCLO = Amount of HCL taken for quench, g mole
HCLR = Amount of HCL reacted with NaOH, g mole
K = Rate constant, L/g mol min

Combined Flow Reactor 6

 NHCL = Number of moles of HCL used, g mole/L
NNaOH = Number of moles of NaOH used, g mole/L
VR = Reactor volume, L
Vo = Volumetric feed rate, LPH
VHCl = Volume of N/10 HCl taken for quench, ml
VSAMP = Volume of sample taken, ml
VNaOH = Volume of NaOH used for neutralizing, ml
XA = Degree of conversion,
= Residence time, min

10. PRECAUTIONS & MAINTENANCE INSTRUCTIONS:

1. Measure the exact volume of water and weigh the chemicals carefully.
2. Always use clean water and good quality chemicals and standard solution for
titration.
3. Use electronic balance for weighing of chemicals. Dont 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. There should be no air in the flow during experiment.
8. Always drain and clean the feed tanks and reactors after conducting the
experiment.

11. TROUBLESHOOTING:
1. If any type of suspended particles are come in the Rota meter. Remove the Rota
meter 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 Rota meter fluctuating more than average tight control knob of that.

12. REFERENCES:
1. Octave Levenspiel, Chemical reaction engineering,3rd ed., John Wiley & Sons,
NY, 2001, Page 90-97, 101-103, 111-112.

2. Coulson & Richardson, Chemical Engineering Vol-3 4th ed, Asian Books
Pvt.Lt, ND, 1991, Page 34-37, 43-45, 61, 64-65.

Combined Flow Reactor 7