Assignment on

Application of drying in various pharmaceutical products

COURSE TITLE: Pharmaceutical Engineering and Technology

COURSE CODE: BPH-312
Name: NUR HOSSEN
ID: BPH-05807096
Batch: BPH-58

COURSE TEACHER: Md. Kamaluddin

Associate Professor
Stamford University Bangladesh
CONTENT

Introduction of Drying
Purpose
Method of Drying
Applications of Drying
Mechanism of Drying
Theory of Drying
Classification & Types of Dry
Introduction of 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 a Suspension. Drying is possible when the environment is unsaturated with
the water vapor. Hence humidity is an important determinant for drying of solid. 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. The process of evaporation involves
removal of much more quantity of liquid per hour than in drying.

Drying is a mass transfer process consisting of the removal of water moisture or moisture
from another solvent, by evaporation from a solid, semi-solid or liquid (hereafter product).
To be considered "drying", the final product must be a solid, either as a continuous sheet
(e.g., paper), as long pieces (eg. wood), particles (cereal grains, corn flakes) or in powder
form (sand, salt, washing powder, milk powder). To achieve this, there must be a source of
heat, and a sink of the vapor thus produced. In byproducts (food, grains, vaccines), and
pharmaceuticals, the solvent to be removed is almost invariably water.

Purpose of drying
Reduction of transportation cost

To make the material more suitable for handling

Prevention from corrosion
Drying inhibits the growth of bacteria, yeasts, and mold through the removal of water.

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

Thermal Drying:
Application of heated air (convective or direct drying). Air heating reduces air relative
humidity, enlarging the driving force for drying. Besides, higher temperatures speed up
diffusion of water inside the solids, so drying becomes even faster. However, product
 quality considerations limit the applicable rise to air temperature. An excessively hot air
almost completely dehydrates the solid surface, its pores shrink and almost close,
leading to crust formation or "case hardening", which is usually undesirable.

Indirect or contact drying (heating through a hot wall), as drum drying, vacuum drying.
Dielectric drying (radiofrequency or microwaves being absorbed inside the material) It is
the focus of intense research nowadays. It may be used to assist air drying or vacuum
drying. Researchers have found that microwave finish drying speeds up the otherwise
very low drying rate at the end of the classical drying methods.
Freeze drying is increasingly applied to dry foods, beyond its already classical
pharmaceutical or medical applications. It keeps biological properties of proteins, and
retains vitamins and bioactive compounds. Pressure can be reduced by a high vacuum
pump (though freeze drying at atmospheric pressure is possible in dry air). If using a
vacuum pump, the vapor produced by sublimation is removed from the system by
converting it into ice in a condenser, operating at very low temperatures, outside the
freeze drying chamber.

Natural air drying takes place when materials are dried with unheated forced air, taking
advantage of its natural drying potential. The process is slow and weather dependent,
so a wise strategy "fan off-fan on" must be devised considering the following conditions:
Air temperature, relative humidity and moisture content and temperature of the
material being dried. Grains are increasingly dried with this technique, and the total
time (including fan off and on periods) may last from one week to various months, if a
winter rest can be tolerated in cold areas.

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
 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.

Application of Drying
Preparation of bulk drugs
Examples: Dried aluminum hydroxide
Spray dried
Lactose Powdered extracts

Preservation of drug product

Drying is necessary to avoid deterioration.
Examples:
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.

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.
 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

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

Mechanism of drying

Drying involves two process

Heat Transfer: It takes place from the heating medium to the solid; except in dielectric or high
frequency electric drying, where heat is generated within the solid & flows to exterior surface.

Mass Transfer
It involves movement of the moisture to the surface of the solid & its subsequent evaporation from the
surface. The transfer of vapors from the surface to the surrounding is affected by external conditions like
temperature, humidity, air flow rate, pressure & evaporating surface exposed.
Equilibrium Moisture Content (EMC)
It is the amount of water present in the solid which exerts a vapor pressure equal to the vapor pressure
of the atmosphere surrounding it. EMC in a wet mass is shown below.

Depending upon temperature and humidity conditions, solids may absorbs or lose moisture.
Desorption

When air is continuously passed over the solid containing moisture more than EMC, then solid loses
water continuously till EMC is reached. This phenomenon is known as desorption

Sorption
When air is continuously passed over the solid containing moisture less than EMC, then solid absorbs
water continuously till EMC is reached. This phenomenon is known as sorption.
Measurement of EMC
The solid samples are placed in a series of closed chambers such as desiccators.
Each chamber consist of solutions which maintain a fixed relative humidity in the enclosed air
spaces.
Solid samples are exposed to several humidity conditions, the exposure is continued until the
material attains a constant weight.
The difference in the final & initial weights gives the moisture content.

Factors Affecting EMC

Nature of material
Nonporous insoluble solids have an EMC zero

EX. Talc
For fibrous or colloidal organic substances, EMC values are high.
For porous solids, EMC values are much higher & variable

Nature of Air
For air of zero humidity, EMC of all materials is zero.

As the temperature of air increases, the EMC of solid decreases.

Drying rate curve

It is obtained by plotting a graph of FMC on X- axis & drying rate On Y- axis. Depending on
external conditions & internal mechanism of fluid flow, solids show different drying patterns.
A typical drying cycle of a solid can be divided into three distinct zones,

1. Initial Adjustment Period

2. Constant Rate Period
3. Falling Rate period
1. Initial Adjustment Period
It is time corresponding to AB curve, which is also called as Heating up Period. During this
period, solids absorbs heat & temperature is increase i.e. An wetted substance when kept for
drying it absorbs heat from surrounding & vaporization of moisture takes place which cools the
surface. Heat flows to the cooled surface at higher rates, leads to rise in temperature &
evaporation again .This continues & after some time heating & cooling rate becomes equal.
This temperature is equal to wet bulb temperature of drying air & is referred by the point B on
graph.

2. Constant rate period

It is time corresponding to BC curve in graph. The temperature remains constant & rate of drying is
constant. During this period, there is a continuous liquid film over the surface of solid. Moisture
evaporating from the surface is replace by the water diffusing from the interior of the solid. Also the
drying rate remains constant as show in curve by region BC
Rate of diffusion = Rate of evaporation

As drying proceeds, the coarse capillaries are completely depleted of water & solid fails to maintain
uniform film. The area over which moisture film is not present is known as dry spot. Such dry spot start
appearing & drying rate start falling & point (point C) at which decrease in drying rate start is referred to
as the critical moisture content (CMC).

CLASSIFICATION OF DRYERS
 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.
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.
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 vapor pressure in the
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. Atmosphere & also reduces the thickness of air boundary layer.

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

Uses Following substances can be dried,

1. Sticky materials
2. Plastic substances
 Drum Dryer
Principle
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 such way that the drum dips partially into the feed.
On one side of the drum a spreader is placed & on other side a doctors knife is placed to
scrap the dried material.
A storage bin is placed connecting the knife to collect the material

1. Sticky materials

2. Plastic substances

3. Precipitates
4. Chemicals
5. Tablet granules & powders
 Drum dryer

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

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

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
7. Malt & glandular extracts
8. Insecticides.
9. Calcium & barium carbonates.

Spray Dryer
Principle
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.
 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.

Spray dryer

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.
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.

Uses
Spray dryers are used compulsorily, if
1. The product is a better form than that obtained by any other dryer.
2. The quantity to be dried is large.
3. The product is thermo labile, hygroscopic or undergo chemical decomposition.

Fluidized 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.

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.
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, profiler & heat exchanger are connected serially to heat the air to the required
temperature. The temp. Of hot air & exit air are monitored.
Bag filters are placed above the drying bowl for the recovery of fines.

Fluidized bed dryer

 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 profiler, 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.
The granules rise in the container because of high velocity gas & later fall back in a random
boiling motion. This condition said to be Fluidized 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.

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.
6. Hot spots are not observed in the dryer.
7. It facilitates the drying of thermo labile 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.
Disadvantages
1. Many organic powders develop electrostatic charge during drying. To avoid this, efficient
earthling 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.

Vacuum 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.
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.

Vacuum dryer

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 25-30C, on account of
lowering of boiling point. Water vapor passes into the condenser where condensation takes
place.
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.

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 overheating as the material is in contact with steam heated surface for
longer period.

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.
 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 vapor without conversion to liquid phase. Solid-liquid- vapor 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 vapor state. The water
vapor is removed from the system by condensation in a cold trap maintained at a temperature
lower than frozen material.

Construction
Freeze dryer consist of
Drying chamber in which trays are locked.
Heat supply in the form of radiation source, heating coils.
Vapor condensing or adsorption system.
Vacuum pump or steam ejector or both.
Freeze dryer
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 pre-concentrated under
the normal vacuum tray drying. This reduces the actual drying by 8 to 10 times.
2. Refreezing 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.
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.
Vacuum is applied to the tune of about 3 mmHg on the frozen sample and the temperature is
linearly increased about 30 C in a span of 2 hrs. Heat (About 2900 kilojoules/ Kg) is supplied
which transfer as latent heat & ice sublimes directly into vapor state. As the drying proceeds,
thickness of dried solids increases. Primary drying stage removes easily removable water, about
98% to 99%.
4. Secondary drying it is removable of residual moisture under high Vacuum. The temp. Of solid
is raised to as high as 50 to 60C but vacuum is lowered below that be 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.

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.

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 dos

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 cannot be shortened.
4. It is difficult to adopt the method for solutions containing no aqueous solvents.

Conclusion
Drying is an essential unit operation used in various process industries. The mechanism of drying
is well understood as a two-stage process and depends on the drying medium and the moisture
content of the product being dried.

Batch dryers are common in chemical and pharmaceutical industries, while continuous dryers are
routinely used where large production is required. Since the cost of drying is a significant portion
of the cost of manufacturing a product, improving efficiency or finding alternative drying routes
is essential.
 Reference

1. Slide share .com

2. Scribd.com
3. Chemical Engineering Science
4. Serve.me.nus.edu.sg
5. www.ncbi.nlm.nih.gov
6. www.chemengonline.com

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