EXPERIMENT 6

CONTINUOUS STIRRED TANK REACTOR (CSTR)

AIM:

To study of a non catalytic homogeneous second order liquid phase reaction in a CSTR under
ambient conditions.
To determine the reaction rate constant for saponification of ethylacetate with NaOH at ambient
conditions
Reaction : NaOH + CH3COOC2H5 CH3COONa + C2H5OH

THEORY:

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 REACTOR.

REACTANT A REACTANT B

Con. of A, CAO Conc. of B, C BO

Feed rate, FAO, Mixer Feed rate, F BO
moles/min A + B = C +D moles/min

VR

Product

CSTR

Reactor volume (volume of fluid in the reactor) = VR , L

Volumetric feed rate (volumetric feed rate A + = VO, LPM

Volumetric feed rate B)

Space time, τ = VR / VO

The performance equation for the mixed flow reactor at steady state is:

VR CAO XA CAO - CA
τ = ------- = ----------- = ------------
VO -rA -rA

XA & 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.

The reaction rate (rate of disappearance of A) = -rA = k CA2

Hence,
VR CAO XA CAO – CA CAO – CA
τ = ------- = ------------ = ------------ = ------------
VO -rA -rA k CA2

Degree of conversion, XA = (CAO – CA) / CAO

Rate of reaction, -rA = CAO XA / τ

Rate constant, k = (CAO – CA) / τ CA2

For nth order reaction, n, can be obtained from a plot of log(-rA) vs log CA, 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.

DESCRIPTION
The reactor is made up of SS – 304. The air compressed feed reactants are given through
Rotameter. The concentration of feed and the product coming out from the reactor is analyzed by
chemical titration and check the effect and the performance of the reactor.
A continuous stirred tank flow reactor (CSTR) required. 6 no. 50cc graduated cylinder, 100cc
titration flask, 50cc burette and one stop watch.

CHEMICALS

1. N / 10 NaOH
2. N / 10 HCl
3. N / 10 ethylacetate (8.8 gms of ethylacetate in 1L of water)
4. Indicator (phenolphthalein)

UTILITIES REQUIRED

1. Compressed air supply at 2 Bar, 0.5 CFM

2. Water Supply
3. Drain
4. Electric supply: 1 phase. 220 V AC. 0.5 kW
5. Instruments. Laboratory Glassware and chemicals required for analysis as per the system
adopted.

PROCEDURE

1. Prepare 20L of N/10 NaOH solution by dissolving 80gm of NaOH in 20L of water.
2. Prepare 20L of N/10 ethylacetate solution by mixing 176 gms of ethylacetate in 20L
water.
3. Filled the respective tanks with these solutions.
4. Adjust the flow rate of the two streams so that in the feed mixture C AO = CBO i.e have
equal flow rates (eg: 2 LPH each you may use the flow range : 2 LPH to 16 LPH for each
stream) using caliberated rotameters.
 5. Pass equimolar feed rates of ethylacetate and NaOH into the CSTR by allowing equal
volumetric feed rates of reactants into the reactor and simultaneously start the mixer of
the CSTR. Ensure constant stirring through out the experiment.
6. After about 10min or time equal to residence time of the reactor i.e when steady state is
achieved, collect exact 10ml of the sample of the liquid at the outlet, in a graduated
cylinder that already contains 20ml of N/10 HCl. Transfer this solution (30ml) in a 250ml
or 100ml titration flask.
7. Titrate this solution (ie. Excess HCl) against N/10 NaOH (add NaOH from burette)
8. Using phenolphthalein as indicator, note the volume of N/10 NaOH used (VNaOH).
9. Note the volumetric flow rate of liquid at the end of the reactor.
10. For calculating the conversion at equilibrium condition, collect the sample 10ml, 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.
11. Repeat all the step for four to six different flow rate of feed.

RESULT:

The non catalytic homogeneous second order liquid phase reaction (saponification of ethyl
acetate with NaOH) at ambient condition was studied.

The rate constant for the above reaction was found to be

k = _________ L/gmol.min (from graph)

k = _________ L/gmol.min (from calculation)

STANDARD DATA

Effective volume of the reactor, VR = 2.649 L

Initial conc. of NaOH, CAO = 0.0455gmol/L

Reaction temp, T = 30O C

Volume of HCl used for quenching, VHCl = 20ml

Normality of quench HCl used, NHCl = 0.1N

Volume of reaction sample added, VSAMP = 10ml

Normality of std. NaOH, NNaOH = 0.1N

OBSERVATIONS & CALCULATIONS

Standardization of NaOH

0.1N Oxalic acid x NaOH ----- Phenolphthalein indicator

Volume of Oxalic acid Titre value
(ml) 1 2 3

Standardization of HCl

0.1N Na2CO3 x HCl -------- Phenolphthalein indicator

Volume of Na2CO3 Titre value

(ml)
1 2 3

Total volume of feed rate to

Run no Volume of std. NaOH
the reactor
 used for titration
LPH LPM, VO
(ml)

Run τ CA k -rA
HClR XA XA
no. (min) (gmol/L) (L/gmol.min) (gmol/min) (1-XA)2

Plot τ vs. [XA / (1 – XA)2]

τ vs. [XA / (1 – XA)2]

τ
Slope = 1 / k CAO

XA
(1 – XA)

CALCULATION FOR EACH RUN

Amount of HCl taken as quench (HCLO) = VHCl x NHCl / 1000
= 20 x 0.1 x 10-3
= 2 x 10-3 gmol

Amount of HCl reacted with the unreacted NaOH of reaction sample (HClR)
HClR = HClO (VNaOH x NNaOH / 1000)
= ________ gmol

Concentration of unreacted NaOH in the reaction mixture (CA)

CA = [HClR / VSAMP] x 1000
= ______ gmol/L

Conversion, X = [CAO – CA] / CAO

= _______

Residence time, τ = VR / VO
= _____ min

Rate of reaction, -rA = [VO x CAO x X] / VR

= _______ gmol/L.min

Rate constant, k = [CAO – CA] / [τ x CA2]

= ________ L/ gmol.min

Average k = [k1 + k2 + ------ + kn] / n

= _______ L/gmol.min