EXPERIMENT NO: 10
BATCH
CRYSTALLIZER
AIM:
1. To study the crystallization of C 7 H 6 O 2 (benzoic acid) in batch crystallizer.
2. To verify the material balance around the crystallizer.
3. To determine the yield of C 7 H 6 O 2 crystals.
INTRODUCTION TO CRYSTALLIZATION:
Crystallization is the process where by a solid separates from a solution because
conditions have been imposed on the solution so as the solid phase to form particles of
crystalline character to grow to a size sufficiently large to allow separation by physical
methods.
A saturated solution containing the solute is altered by either cooling, evaporation
of solvent, or addition of another substance so that the ability of the solvent to dissolve
the solute is lessened, and a fraction of the solute forms a solid phase, which may be
removed from the mixture.
From the solubility or phase diagram, the effect of changes in the temperature and
solute and solvent concentrations can be seen.
Based on the material balance, the yield of crystals resulting from cooling and/or loss of
solvent due to evaporation can be estimated from:
Y= WR [C1-C2 (1-V)] / [1-C2 (R-1)]
where,
Y= yield of crystal, kg.
W= Initial wt. of solvent (e.g. Water), (1b, kg)
R= Ratio of molecular wt. of hydrated and anhydrous salt.
C1= Initial solution concentration, (1b of anhydrous salt/1b of solvent, kg of anhydrous
salt/kg of solvent.)
C2= Final solution concentration
V= Solvent lost by evaporation (1b/1b of original solvent)
The physical properties of saturated solution and slurry may be obtained from:
𝑃𝑝𝑃𝑟
Density = Ps =
𝑃𝑟𝑋+(1−𝑋)𝑃𝑝
Where,
Ps = Slurry density
Pp = Solid particle density
Pґ = Fluid density
X = Wt. Fraction of solid in slurry
Viscosity:
µs = µ ґ e 4.1 (1- ∈) (0.64 +∈)
Where,
µs = Viscosity of slurry (in CP)
µґ = Viscosity of saturated solution (in CP)
∈ = Fraction of liquid in slurry
(In many cases slurries have ≈ 20% solids, ∴∈ = 0.8)
𝜇𝑠
= 1.8 (according to the value of ∈ = 0.8, it should be equal to 3.25)
𝜇𝑟
SATURATED SOLUTION:
A saturated solution is a solution which is in equilibrium with a solid phase of the
dissolved material. A saturated solution has in it the maximum quantity of the solute at
that temperature.
If the saturated solution is cooled or solvent evaporated, a non-equilibrium condition is
established which can be remarkably stable. That is, a solid phase will not immediately
precipitate in order to re-establish the equilibrium. This non-equilibrium solution where
in the liquid has dissolved more than the equilibrium quantity of solute is called
super saturated solution.
The super saturated of a given solution cannot become infinity large .There is a limit.
This limit is encountered when there occurs a spontaneous formation and the system
reverts to the equilibrium state.
The process of crystallization is shown in
figure:
1. A saturated solution can be made
super-saturated by a change of
temperature (cooling) or a
reduction in solvent content. This
super-saturated solution can
remain in a metastable equilibrium
for every long period of time.
2. In the metastable zone crystal
growth can occur if there are seed
crystals upon which the solids may
deposit, but spontaneous
nucleation will not take place.
3. In the liable zone there will be a sudden spontaneous formation of crystal nuclei
that will produce so many very small particles.
BATCH CRYSTALLIZATION:
Batch crystallization is characterized by the fact that the system is always in the unsteady
state. The initial super-saturation at which crystallization starts will drop quickly from
relatively high value to the saturation value. If crystal growth is to continue, the solution
must be maintained in the metastable region. As a consequence, cooling must continue
and the batch temperature must continue to drop during the growth period. In batch
crystallization, it is comparatively easy to penetrate the liable zone producing a fine
crystal. By using controlled seeding the solution will not become liable thereby
aiding crystal growth.
PROCEDURE:
1. Prepare a saturated solution of benzoic acid in water at 50 oC by dissolving the
given amount of benzoic acid in 2 liter of solution. The crystallizer should be filled
to 3/4th of its capacity. During mixing, the agitator should be used for effective
mixing. After uniform mixing has been achieved, stop the electric supply to the
electric heater.
2. Now fix the agitator speed (N) at some value and observe slow agitation speed.
3. Allow the flow of cold water (at less than 5oC) to pass through the jacket at a pre-
fixed flow rate with help of rotameter. Record the calibrated Rotameter reading
(flow rate may be fixed such that the rise in cooling water temperature is maximum
with the help of respective sensors.
4. Record the temperature of inlet water, outlet water and solution temperature with
the help of respective sensors.
5. Carry out the crystallization process for about 2 hrs.
6. After two hours, stop the cooling water supply, open the valve fixed at the cone of
the crystallizer and collect the slurry in the bottom receiving tank that is fixed with
a mesh at the top. The crystals shall be collected on the mesh and liquid in the tank.
7. Collect all the crystals from the mesh on a filter paper and weigh. Let the weight of
the product crystals be P (kg). (The crystals may be screened for size distribution if
desired).Steps 1-7 may be repeated with the addition of known weight of seed
crystals at step 5.
OBSERVATION AND CALCULATIONS:
1. Initial amount of benzoic acid taken ……………(in gms)
2. Initial amount of water taken ……………….(in ml/ litre)
3. Amount of mother liquor left ………………..(in ml/litre)
Material balance for water:
Water in solution = water evaporated + water in mother liquor
Solubility of benzoic acid at final temp. When crystals were separated out ……(to
be taken from solubility data )
say for example if x gm per liter of water , then amount of benzoic acid left in mother
liquor = (x/100)*water in mother liquor
Material balance for benzoic acid:
Benzoic acid in feed solution = benzoic acid in solution at final temp. + benzoic
acid produced as crystals
Time Cooli Solution
o
T(min) Inlet, Twng
o Outlet, Tw o Temp.T s C
T. water
min
Amount of crystal of collected after 2 hrs. =P (gm/kg).
Wt. of mother liquor = M ( g m / k g ) .
Finally calculate the yield of benzoic acid crystals.
