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OB JECTIVE
Mass transfer with Chemical reaction (Solid – Liquid System): Dissolution of benzoic acid in
aqueous NaOH solution is studied.
AIM
1. To study the dissolution of benzoic acid in aq. NaOH solution.
2. To compare the observed enhancement factor for mass transfer with those predicted by the
film and boundary layer models.
THEORY
Solid – liquid mass transfer plays an important role in some industrial operations. The
dissolution may occur with or without chemical reaction. In case dissolution is accompanied by
solid – liquid reaction, it is desirable to know the enhancement in the rate of mass transfer due to
chemical reaction.
The dissolution of a solid in a solution accompanied with instantaneous chemical reaction
can be expressed as:
A + nB B Product
where A is the solid and B is the liquid phase reactant. The reaction is assumed to be
instantaneous so that A and B don’t coexist. The mechanism of solid dissolution involves:
dissolution of A in liquid followed by its reaction with species B diffusing from the bulk liquid
phase at a reaction plane.
If the film model is applied to this situation, the enhancement factor, defined as the
ratio of the solid-liquid mass transfer coefficient with reaction, k r to the mass transfer coefficient
without reaction, k, given by:
kr D D [ Bo ]
film A B (1)
k DB DA nB [ A* ]
1/ 3 2/3
k D D [ Bo ]
b r A B (2)
k DB DA nB [ A* ]
DESCRIPTION OF APPARATUS
In the present experiment we aim at finding the enhancement in the rate of dissolution
due to simultaneous reaction and compare it with the enhancement predicted on the basis of the
film and boundary layer models. The system is: dissolution of benzoic acid in aq. NaOH
solution.
The set-up consists of a cylinder of benzoic acid mounted on a SS rod and with a D.C
motor. The operational range of rotation is between 100 to 250 rpm. The cylinder is immersed in
an aqueous solution of sodium hydroxide of known concentration in a vessel filled to 2/3 rd its
capacity. The position of the benzoic acid cylinder is so adjusted that the liquid level rises above
the top surface by about 3 cm. The dimensions of the benzoic acid cylinder may be fixed at
diameter 3 to 4 cm, length: 7 to 8 cm. The cylinder can be prepared by pouring powder benzoic
acid in the mould of desired dimensions with 4 to 6 mm SS rod located in the center of the
mould in a vertical position.
UTILITIES REQUIRED
Water Supply.
Drain.
Electricity Supply: 1 Phase, 220 V AC, 0.5 kW.
Laboratory Glassware
CHEMICALS REQUIRED
1. Benzoic acid
2. N/10 NaOH
3. N/10 HCl
4. Indicator
EXPERIMENTAL PROCEDURE
1. Prepare the benzoic acid cylinder first by using the die set provided with apparatus.
2. Record the dimensions of the benzoic acid cylinder (O.D, length and O.D of SS rod).
3. Fill the vessel with 0.1N NaOH solution of known concentration up to 2/3 of its volume.
Record the volume of aqueous 0.1N NaOH solution added (V).
4. Start the heater of water bath and fix the dissolution temperature (ambient to 50 oC), wait
till the aq. Solution attains the desired temperature. Record the temperature (T).
5. Now fix the benzoic acid cylinder inside the vessel containing aq. NaOH solution and start
the motor at a fixed rotational speed, (N, rpm)
6. Run the experiment for 10 minutes.
7. Stop the motor and remove the benzoic acid cylinder.
8. Mix thoroughly the contents of vessel and analyze it for un-reacted NaOH concentration
by titration against standard N/10 HCl solution.
9. Measure the benzoic acid cylinder dimensions again.
10. Repeat steps 1 to 9 for different concentrations of aq. NaOH solutions.
Repeat steps 1 to 7 using de-ionized water (1.6 litre). This run may be carried for about 45
to 60 minutes duration. During this period small samples (10 ml) should be withdrawn at
regular intervals of 10 minutes and analyzed for dissolved benzoic acid by titration against 0.1
kmol/m3 NaOH solution.
OBSERVATIONS
DATA REDUCTION
AS *D ar *L ar 2 * ( 2
( Dar d rod
2
))
4
7. The rate constant, KSL, for physical dissolution is obtained from the integrated material balance
equation for benzoic acid.
AS C
K SL* * t ln(1 A )
V C
OBSERVATION TABLES:
TABLE 1:
TABLE 2:
Volume of N/10
Concentration of
Time t, NaOH used for
Benzoic acid C=V2/100, 1-C/C* ln (1-C/C* ) K
min 10ml of Solution
kmol/m3
(V2) , ml
After plotting t vs ln [1 – C/C*] we record the slope of the line given by:
Slope = -k As / V;
knowing As and V, we get k
Enhancement factor,
R
exp
kxC *
For aq NaOH:
Cylinder dimensions:
Initial diameter = Di
Initial Length = Li
Final Diameter = Df
Final Length = Lf
S.S rod dia = drod
Operating Temp. = T
Motor speed = N
Volume of NaOH Taken in tank = V lt
Initial concentration of NaOH, C =
Volume of sample taken for titration = 10 ml
TABLE 1:
t , min R` , kmole / min R , kmole / min-m2
TABLE 2:
Volume of N/10
Time Concentration of
HCl used for 10ml
t, NaOH in Solution CA/CA0 ln (CA/CA0) k
of Solution (V2) ,
min C= V2 / 100
ml
Plot of ln(1-C/C*) vs. t and ln(CA/CA0) vs. t yields straight line with Slope =
For time t
As
-K x = Slope
V
-K = Slope x V / As
(at T = 0C and N = rpm.)
R
Effectiveness factor; exp
kxC *
The theoretical values for enhancement factor, , for the film model and boundary layer
model is obtained from Eq.1 and Eq.2 respectively.
The diffusivity of benzoic acid, DA, may be obtained from the literature = 1.04x10-9 m2/s at 300C
Value of DB may be taken as = 4.1x10-9 m2/s at 30oC.
kr D D [ Bo ]
film A B (1)
k DB DA nB [ A* ]
NOMENCLATURE
Di : Initial Diameter.
Li : Initial Length.
Df : Final diameter.
Lf : Final length.
drod : S.S.rod dia.
T : operating temperature.
N : Motor speed.
V : Volume of liquid taken in tank.
DA &DB : Diffusivity constant.
TROUBLE SHOOTING
In case of any problem regarding operation of the apparatus, the apparatus should be
quickly switched off and electric supply should be cut off.
Electrical:
1. Electric shock: It means that either earth wire inside the panel is loose or there is
no earth provided in the socket to which the equipment is plugged. So, make it
sure that the equipment is earthed properly.
2. Display of ‘1’ on D.T.C: It means sensors connections are loose. Locate the point
of loose connection and solder it properly
3. No rise in temperature despite heater is On: It means there is some loose
connection. Check out for the same and then either solders it or tight it, whatever
is applicable.
General:
Leakage: The point of leakage should be detected and the concerned part is tightened
properly. If the problem still persists then the part is removed and Teflon tape is wrapped on the
threads properly and the part is then refitted carefully.
REFERENCES
Mass transfer with chemical reaction by G.Astarita