DRYING

CONTENTS

Introduction of Drying

Applications of Drying

Theory of Drying

Classification & Types of Dryers

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 Drying

It is defined as” the removal of small amounts of

water or other liquid from a material by the application of
heat”. It also includes removal of volatile liquids or water
from another liquid or gas or suspension.

Drying is possible when the environment is unsaturated

with water vapour. Hence humidity is an important
determinant for drying of solids.

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The product obtained from an evaporator is either
concentrated solutions or suspensions or a wet slurry,
whereas that from a dryer is substantially dry solid.

Method of drying
 Thermal drying – application of heat
 Non thermal drying (freeze drying)

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Non thermal drying

Expression
The expression of solid to remove liquid.
e.g. Squeezing of wetted sponge

Extraction
The extraction of liquid from solid by use of solvent.

Adsorption
By use of desiccants such as anhydrous calcium chloride .

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 •Absorption
The absorption of moisture from gases by passage through a
sulfuric acid column.

•Desiccation
Desiccation of moisture from a solid by placing it in a sealed
container with a moisture-removing material
e.g. silica gel in bottle.

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Applications of Drying

Preparation of Bulk drugs

Ex. Dried aluminium hydroxide
Spray dried lactose
Powdered extracts
Preservation of drug product
Drying is necessary to avoid deterioration.
Ex.1. Crude drugs of animal & vegetable origin, synthetic &
semi synthetic drugs, aspirin & penicillin's tablets are
undergo chemical decomposition process.
2. Blood products,skin & tissue undergo microbial
decomposition
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• Improved characteristics
Drying produces material of spherical shape, uniform Size, free
flowing & enhanced solubility. Ex. Granules are dried to improve the
fluidity & Compression characteristics.

• Improved handling
Removal of moisture makes the material light in weight &
reduces the bulk thus the cost of transportation will be less & storage
will be efficient.

•Stability enhancement
By removal of moisture significantly reduces rate of chemical
reactions, chances of microbial attack or enzymatic actions and thus
improves stability.

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 Theory of Drying
In a wet solid mass, moisture is present in two forms,
a) Bound moisture
It is the minimum water (moisture) held by the material that
exerts an equilibrium vapor pressure less than the pure water at the
same temperature. Substances containing bound water are often
called hygroscopic substances.
b) Unbound moisture
It is the amount of water held by the material that exerts an
equilibrium vapor pressure equal to that of pure water at the same
temperature.

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Unbound water exists mostly in the voids of the solids. Thus, in a
non hygroscopic material, all the liquid is unbound water.

In a hygroscopic material, the unbound moisture is the liquid in

excess of the equilibrium moisture content.

Measurement of the moisture in a wet solid is referred as moisture

content , or MC:

weight of dry sample

% MC = X 100
weight of water in sample

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 TRAY DRYER
Principle
In the tray dryer, hot air is continuously circulated.
Forced convection takes place to remove moisture from the
solids placed in trays. Simultaneously, the moist air is
removed partially. This is also called as shelf, cabinet or
compartment dryer.

Construction
It consist of rectangular chamber whose walls are
insulated. Trays are placed inside the heating chamber.

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• Laboratory dryers contains 3 trays minimum & in
industry 20 tray.

• Each tray is rectangular or square & about 1.2 to 2.4

meters square in area. Trays are usually loaded from10 to
100 mm deep.

• Distance between bottom of upper tray & surface of the

substance loaded in the subsequent tray must be 40mm.

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Dryer is fitted with a fan for circulating air over the trays in
the corner of chamber, direction vanes are placed to direct
air in the expected path.

fig: Tray Dryer 15

Working :-

• Wet solids is loaded into trays. Fresh air is introduced

through inlet, which passes through the heaters & gets
heated up.

• Hot air is circulated by means of fans at 2 to 5 meter

per second.
Turbulent flow lowers the partial vapour pressure in the
atmosphere & also reduces the thickness of air boundary
layer.

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•As water evaporates from the surface, the water diffuses
from the interior of solid by capillary action. These occur
in single pass of air.

• The time of contact is short & amount of water is picked

up in a single pass is small. Therefore discharged air to the
tune of 80 – 90% is circulated back through fans. only
10-20% of fresh air is introduced.

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Advantages

1. Handling of materials can be done without losses

2. It can be operated batch wise, for following reasons:
a) each batch can be handled as separate entity.
b) equipment is readily adjusted for use in drying of variety of
materials.
c) valuable products can be handled efficiently.

Disadvantage
It requires more labour to load & unload, Time consuming

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Uses

Following substances can be dried,

1. Sticky materials
2.Plastic substances
3.Precipitates
4.Chemicals
5. Tablet granules & powders

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Principle DRUM DRYER
A heated hallow metal drum rotates on its longitudinal axis,
which is partially dipped in the solution to be dried.
The solution is carried as a film on the surface of the dryer & Dried
to form a layer. A suitable knife scraps the dried material, while drum
is rotating.

Construction
• It consist of a horizontally mounted hollow steel drum of 0.6 –
3.0 meters diameter & 0.6 – 4 meters in length, whose external
surface is polished.
• Below the drum, feed pan is placed in a such way that the drum
dips partially into the feed.

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• On one side of the drum a spreader is placed & on other
side a doctor’s knife is placed to scrap the dried material.
• A storage bin is placed connecting the knife to collect
the material.

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Fig: Drum Dryer
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Working

• Steam is passed inside the drum. Drying capacity is directly

proportional to the surface area of the drum. Heat is transferred by
conduction to the material.

• Drum is rotated at a rate of 1- 10 revolutions per minute. the liquid

material present in the feed pan adheres as a thin layer to the external
surface of drum during its rotation.

• Material is completely dried during its journey in slightly less than

one rotation. the dried material is scrapped by knife, which then falls
into a storage bin. The time of contact of the material with the hot
metal is 6-15 seconds only

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Advantages

1. Drying time is less only few seconds. Hence , heat

sensitive material can be dried.
2. Less space as compared to spray dryer.
3. Rates of heat & mass transfer are high.
4. Product obtained is completely dried & is in the final
form.
Disadvantages
1. Maintenance cost is higher than spray dryer.
2. Skilled operators required .
3. It is not suitable for solutions of salts with less
solubility.
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Uses
It is used for drying solutions, slurries, suspensions etc.
& also drying of products like,
1. Milk product
2. Starch product
3. Ferrous salt
4. Suspensions of zinc oxide & kaolin
5. Antibiotics
6. Yeast & pigments
Malt & glandular extracts
Insecticides.
Calcium & barium carbonates.

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Principle SPRAY DRYER

The fluid to be dried is atomized into fine droplets,

which are thrown radially into a moving stream of hot gas.
Temperature of droplets is immediately increased & fine
droplets get dried in the form of spherical particles. This
process completes in few seconds before the droplets reach
the wall of 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. 28
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 dia. & rotates at a
speed of 3000 to 50,000 rpm. Bottom of the dryer is
connected to a cyclone separator. Fig :- Spray dryer

Fig: Spray Dryer 29

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 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 such a way that droplets should
be completely drided before reaching walls of drying
chamber. 32
b) Drying of liquid droplets
•Surface of a liquid drop is dried immediately to form a tough shell.
Liquid inside must escape by diffusing through the shell at a
particular rate.

• Heat transfer from outside to inside takes place at a rate greater than
liquid diffusion rate. As a result, heat inside mounts up which allow
the liquid to evaporate. This leads to increase in internal pressure,
which causes droplets to swell.

•The shells thickness decreases where as permeability for vapour

increases. If the shell is neither elastic nor permeable it ruptures &
internal pressure escape.

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 c) Recovery of dried product
Centrifugal force of atomizer drives the droplet to follow
helical path. Particles are dried during their journey &
finally fall at the conical bottom.
All these processes are completed in a few seconds. Particle
size of the final product ranges from 2 to 500 mm.
Particle size depends upon solid content of the feed, liquid
viscosity, feed rate & disc speed.
Capacity of spray dryer – 2000 kg/hr

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Advantages
1. It is continuous process & drying completes within 3 to 300 sec.

2. Labour cost is low.

3. Product of uniform & controllable size can be obtained.

4. Fine droplets form provide large surface area for heat & mass
transfer. Product shows excellent solubility.

5. Either solution or suspensions or thin paste can be dried in one

step to get final product ready for package.

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6. Drying of sterile product & Reconstituted product.

7. Globules of an emulsion can be dried with the dispersed

phase inside & layer of continuous phase outside.

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.

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Uses
Spray dryers are used compulsorily, if :

1. The product is a better form than that obtained by any other

2. The quantity to be dried is large.

3. The product is thermolabile, hygroscopic or undergo chemical

decomposition.

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 FLUIDISED BED DRYER

Principle
Hot air is passed at high pressure through a perforated
bottom of container containing granules to be dried. The
granules are lifted from the bottom & suspended in the
stream of air. This condition is called Fluidized state. The
hot gas Surrounding every granule to completely dry them.
Thus, materials or granules are uniformly dried.

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 Construction
Two types of bed dryers are available

1. Vertical fluid bed dryer

2. Horizontal fluid bed dryer

• The dryer is made up of stainless steel or plastic. A

detachable bowl is placed at the bottom of the dryer, which
is used for charging & discharging.

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• The bowl has perforated bottom with a wire mesh support for
placing materials to be dried. A fan is mounted in the upper part of
circulating hot air.

• Fresh air inlet, prefilter & heat exchanger are connected serially to
heat the air to the required temperature. The temperature of hot air &
exit air are monitored.

• Bag filters are placed above the drying bowl for the recovery of
fines.

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42
Fluidized Bed Dryer DSM-FD200
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Working
• The wet granules to be dried are placed in the detachable bowl & it
is pushed into dryer.

• Fresh air is allowed to pass through a prefilter, which subsequently

gets heated by passing through a heat exchanger. The hot air flows
through the bottom of the bowl. The air velocity is gradually
increased.

• When the velocity of the air is greater than settling velocity of

granules,the granules remain partially suspended in the gas stream.

• A point of pressure is reached at which frictional drag on the

particle is equal to the force of gravity.
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• The granules rise in the container because of high velocity gas &
later fall back in a random boiling motion. This condition said to be
Fluidised State.

• The gas surrounds every granule to completely dry them. The air
leaves the dryer by passing through bag filters.

• The entrained particles remain adhered to the inside of the bags.

Periodically the bags are shaken to remove the entrained particles.

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Advantages
1. It requires less time to complete drying i.e. 20 to 40 min.
compared to 24hr of tray dryer.

2. Different sizes with different drying capacity from 5 to 200 kg/hr.

3. Handling simple & low labour cost.

4. Thermal efficiency is 2 to 6 times than tray dryer.

5. Mixing efficiency is also high as compared to other dryers.

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6. Hot spots are not observed in the dryer.

7. It facilitates the drying of thermolabile substances, as contact time

is short.

8. It can be used for batch type or continuous type.

9. It has high output from a small floor space.

10. The free movement of individual particles eliminates the risk of

soluble material migrating as may occur in static bed.

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Disadvantages
1. Many organic powders develop electrostatic charge during
drying. To avoid this, efficient earthing of dryer is essential.
2. The turbulence of the fluidized state of granules may cause
attrition of some materials resulting in the production of fines. but
using a suitable binding agent this problem can be solved.
3. Fine particles may become entrained & must be collected by bag
filters.
Uses
1. It is popularly used for drying of granules in the production of
tablets.
2. It can be used in three operations like mixing, granulation &
drying.
3. It is modified for coating of granules.
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 VACCUM DRYER
Principle
In vacuum dryer, material is dried by the application of
vacuum. When vacuum is created, the pressure is lowered so that
water boils at a lower temperature. Hence, water evaporates faster.
The heat transfer becomes efficient i.e. rate of drying enhances
substantially.
Construction
• It is made up of a cast iron heavy jacketed vessel.
It is so strong that it can withstand high vacuum within the oven &
steam pressure in the jacket.
• The enclosed space is divided into a number of portions by means of
20 hollow shelves, which are part of jacket. These shelves provide
large area for conduction of heat.
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•Over the shelves, metal trays are placed for keeping the
material.
•The oven door can be locked tightly to give an air tight
seal. oven is connected to a vacuum pump by placing
condenser in between.
• Fig : Vacuum Dryer

Fig: VACCUM DRYER 50

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Working

• Material to be dried is spread on trays. Trays are placed on the

shelves.

•Pressure is decreased up to 30 to 60 kilopascals by means of vacuum

pump. door is closed firmly.

•Steam or hot air is supplied into the hollow space of jacket &
shelves. heat transfer by conduction takes place.

•At this vacuum, evaporation of water from the material takes place
at 25-30°C, on account of lowering of boiling point. Water vapour
passes into the condenser where condensation takes place.
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Advantages

1. Large surface area for heat transfer.

2. Handling of material, trays & equipment is easy.

3. Easy to switching over to next material.

4. Hot water of desired temperature can be supplied.

5. Electrically heated hollow shelves can be used.

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 Disadvantages

1. Heat transfer coefficient are low.

2. Limited capacity & used for batch process.

3. More expensive than tray dryer. labour & running cost is also high.

4. There is danger of over heating as the material is in contact with

steam heated surface for longer period.

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Uses
1. Heat sensitive materials, which undergo decomposition.

2. Dusty & hygroscopic material.

3. Drugs containing toxic solvents. these can be separated into closed

containers.

4. Feed containing valuable solvents. These are recovered by

condensation.

5. Drugs which required as porous end products.

6. Friable dry extracts

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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 this
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
Freeze dryer consist of ,
• Drying chamber in which trays are locked.
• Heat supply in the form of radiation source, heating coils.
• Vapour condensing or adsorption system.
• Vacuum pump or steam ejector or both.

Fig: FREEZE DRYER 57

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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.

Prefreezing to solidify water

Vials, ampoules or bottles in which the aqueous solution is packed
are frozen in cold shelves (- 50ᵒC). 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. 0.0098ᵒC & 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 -10ᵒC
to -30ᵒC.

The conditions of 1 to 8 K below eutectic point is sufficient.

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Vacuum is applied to the tune of about 3 mmHg on the
frozen sample and the temperature is linearly increased
about 30 ᵒC in a span of 2 hrs. Heat (About 2900 kilojoules/
Kg) is supplied which transfer as latent heat & ice sublimes
directly into vapour state. As the drying proceeds, thickness
of dried solids increases. Primary drying stage removes
easily removable water, about 98% to 99%.

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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 60ᵒC 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. Thermo labile substances can be dried.

2. Denaturation does not occur.
3. Migration of salts & other solutes does not take place.
4. Moisture level can be kept as low as possible.
5. Product is porous & uniform.
6. Sterility can be maintained.
7. Material can be dried in its final container such as single
dose & multiple dose.

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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 non

aqueous solvents.

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