EXPERIMENT 5

PLUG FLOW REACTOR ( PFR )

OBJECTIVE:

To study non catalytic homogeneous reaction in a plug flow reactor.

To determine the reaction rate constant for saponification of ethyl acetate with NaOH at ambient
conditions.

THEORY

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

Product

ΔV

r
Z

Feed

VO , CAO

For steady state rate operation:

For the reaction,

k
CH3COOC2H5 + NaOH CH3COONa + C2H5OH
(B) (A)
 -rA = k CA CB A = NaOH
B = CH3COOC2H5

For the condition:

CAO = CBO and neglecting change in density
-rA = k CA2
CA = CAO ( 1 – xA )

Therefore

FAO = Molar flux rate of NaOH

FAO = VO CAO
VO = Volumetric flow rate of feed, LPM
VR = Volume of PFTR, L

Or

Or
1 xA
τ = -------- ---------- ------------- (1)
kCAO (1 – xA)

When CAO = CBO, then,

1 (CBO/CAO) - xA
τ = --------------------------- ln ------------------------- --------------- (2)
kCAO [(CBO/CAO) – 1] (CBO/CAO) (1 – xA)

CAO - CA
τ = -----------
CAO

CA = Concentration of unreacted NaOH at steady state

K = Reaction rate constant

DESCRIPTION:

The reactor is glass tube. The air compressed feed reactants are given through
Rotameters. 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 plug flow reactor, required 6 No. 50 cc graduated cylinder. 6 No. 100 cc titration
flasks, 50 cc burette and one stopwatch.

CHEMICALS:

1. N/10 NaOH,
2. N/10 HO,
3. N/10 Ethylacetate (8.8 gms of ethylacetate in 1 L of water),
4. Indicator (Phenolphthalein)

UTILITIES REQUIRED:

1. Compressed Air Supply at 2 Bar, 0.5 CFM.

2. Water Supply.
3. Drain.
4. Electricity 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 of
water.
3. Fill the respective tanks with these solutions.
 4. Adjust the flow rate of the two streams so that in the feed mixture C AO = CBO ie. have
same volumetric flow rates (eg. 2 LPH each you may use the flow range: 3 LPH to 15
LPH for each stream) using calibrated rotameters.
5. Pass equimolar feed rates of ethyl acetate and NaOH into the PFTR by allowing equal
volumetric feed rates of reactants in to the reactor
6. After about 10 min or time equal to the residence time of the reactor (which ever is
greater) i.e when steady state is achieved, collect exact 10 ml of the sample of the liquid
at the out let, in a graduated cylinder that already contains 20 ml of N/10 HCL. Transfer
this solution (30 ml) in a 250m1 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 (V NaOH)

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 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 HCI using phenolphthalein as indicator. Note the

volume of N/10 HCI used.

11. Repeat all the steps for four to six different flow rates of feed.

RESULT:

The rate constant for the given second order reaction (non catalytic homogeneous reaction-
saponification of ethyl acetate with NaOH at ambient conditions) in PFR is obtained as

From calculation, k = ______ L/gmol.min

From graph, k = ______ L/gmol.min

OBSEVATION AND CALCULATIONS:

Run No.

Reaction temperature, T = 20OC

Reactor diameter, d = 3.5 cm

Reactor length, L = 130 cm

Vol. of reactor, VR = (π / 4) x d2 x L = 0.866 L

Volumetric feed rate of feed, VO = ______ L/min

Initial conc. of NaOH in feed mixture, CAO = 0.049 gmol/L

Initial conc. of ethylacetate in feed, CBO = 0.049 gmol/L

Volume of HCl for quenching, VHCl = 20ml

Standardization of NaOH

0.1 N Oxalic acid x NaOH phenolphthalein indicator

Titre volume
Vol. of Oxalic acid
1 2 3
20ml
NNaOH =

Standardization of HCl

0.1 N Na2CO3 x HCl phenolphthalein as indicator

Titre volume
Vol. of Na2CO3
1 2 3
20ml

NHCl =

Flow rate Reaction mixture Volume of NaOH

Sl.no
LPH LPM (ml) (ml)

CA -rA k
Run no τ, min XA 1/CA – 1/CAo
gmol/L gmol/L.min L/gmol.min
Plot τ vs. [1/CA – 1/CAO] on a simple graph, the slope is = 1/k. from slope calculate k

τ vs. [1/CA – 1/CAO]

τ
(min) Slope = 1/k

1 1
---- - ------ , L/gmol
CA CAO

CALCULATION STEPS FOR EACH RUN:

RUN NO. 1

Amount of HCl taken as quench (HClO) = VHCl x NHCl / 1000 gmol

= 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 NHCl /1000) gmol
= 2 x 10-3 – ( ____ x 0.1 x 10-3)
= _____ gmol

Concentration of unreacted NaOH in the reaction mixture (CA)

CA = ( HClR / VSAMP) x 1000, gmol
= ( ____ / 10 ) x 1000, gmol
= _____ gmol/ L

Conversion, X = (CAO – CA) / CAO

= (0.049 - ____ ) / 0.049
= ______
Residence time, τ = VR / VO min
= 0.866 / _____
= _____ min

Rate of reaction, -rA = X x (1-X) x CAO / τ, gmol/L.min

= ________ gmol/L.min

Rate constant, k = X x (1-X) x CAO x τ, L/gmol.min

= _______ L/gmol.min

Average k = (k1 + k2 + ---- + kn) / n