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FREEZE DRYER
Principle
Spray
Dryer
Construction
It consist of a large cylindrical drying chamber with a
short conical bottom, made up of stainless steel.
Diameter of 2.5- 9.0 meters & height 25.0 meters or
more.
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An inlet for hot air is placed in the roof of the chamber &
another inlet carrying spray disk atomizer is set in the
roof.
spray disk atomizer is about 300 mm in diameter &
rotates at a speed of 3000 to 50,000 rpm. Bottom of the
dryer is connected to a cyclone separator.
Working
Drying of material in spray dryer involves three stages.
a) Atomization of liquid
The feed is introduced through the atomizer
either by gravity or by using suitable pump to form fine
droplets. The properties of final product depends upon
the droplet form. Atomizer of any type:
1. pneumatic atomizer
2. pressure nozzle type
3. spinning disc atomizer
Rate of feed adjusted in a such a way that droplets
should be completely dried before reaching walls of
drying chamber.
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Advantages
1.
Disadvantages
1. It is very bulky & expensive.
2. Such huge equipment is not always easy to operate.
3. The thermal efficiency is low, as much heat is lost in
the discharged gases.
Uses
Spray dryers are used compulsorily, if :
1. The product is better form than that obtained by any other
dryer.
2. The quantity to be dried is large.
3. The product is thermolabile, hygroscopic or undergo chemical
decomposition.
Calcium sulphate
Acacia
Borax
Fruit juices
Sulphur
Blood
Pancreatin
Hormones
Chloramphenicol
Sodium
phosphate
Extracts
Milk
Lactose
Plasma
Vitamins
Serum
Starch
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Freeze Dryer
It is also known as lyophilization i.e. system is made solvent
loving for removing the same.
Principle
In freeze drying, water is removed from the frozen state by
Sublimation i.e. direct change of water from solid into vapour
without conversion to liquid phase. Solid-liquid- vapour equilibrium
phase diagram of water is useful to decide the experimental
conditions. The drying is achieved by subjecting material to
temperature & pressure below the triple point. Under these
conditions, any heat transferred is used as latent heat & ice sublimes
directly into vapour state. The water vapour is removed from the
system by condensation in a cold trap maintained at a temperature
lower than frozen material.
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Construction
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Working
The working of freeze dryer consist of following steps.
1. Preparation & pretreatment
The volume of solution introduced into the container is
limited by its capacity. Therefore pretreatment is essential. The
solutions are preconcentrated under the normal vacuum tray
drying. This reduces the actual drying by 8 to 10 times.
2. Prefreezing to solidify water
Vials, ampoules or bottles in which the aqueous solution is
packed are frozen in cold shelves (- 50C). The normal cooling
rate is about 1 to 3 Kelvin/ minute so that large ice crystals with
relatively large holes are formed on sublimation of ice. This is
also responsible for giving a porous product.
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3. Primary Drying
It means sublimation of ice under vacuum. The temp. &
pressure should be below the triple point of water i.e. 0.0098C
& 4.58 mmHg for sublimation, when water is alone present.
When a Solution of a solid is dried, the depression of
freezing point of water occurs. Hence, it is essential that the
temperature be brought below the eutectic point. The pressure
& temp. at which the frozen solid vaporizes without conversion
to liquid is referred to as the eutectic point. Depending on the
drug substances dissolved in water, the eutectic point is
determined. The usual range is from -10C to -30C.
The conditions of 1 to 8 K below eutectic point is sufficient.
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4. Secondary Drying
It is removable of residual moisture under high Vacuum.
The temp. of solid is raised to as high as 50 to 60 C but
vacuum is lowered below that is used in primary drying.
The rate of drying is very low & it takes about 10 to 20 hrs.
5. Packing
After vacuum is replaced by inert gas, the bottles &
vials are closed.
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Uses
It is used for drying of number of product,
1. Blood plasma & its fractionated product.
2. Bacterial & viral culture.
3. Antibiotics & plant extracts.
4. Steroids, vitamins & enzymes.
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Advantages
1.
2.
3.
4.
5.
6.
7.
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Disadvantages
1. The product is prone to oxidation, due to high porosity & large
surface area. Therefore, the product should be packed in vacuum
or using inert gas.
2. Equipment & running cost is very high.
3. The period of drying is very high. Time can not be shortened.
4. It is difficult to adopt the method for solutions containing nonaqueous solvents.
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