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Scope
Definition
Purpose
Theory of drying
Drying of solids

Drying

Assoc.Prof.Jomjai Peerapattana
Faculty of Pharmaceutical Sciences
Khon Kaen University
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Loss on drying
Moisture content
Behavior of solids during drying

Classification of dryers

Static bed dryers

Tray and truck dryers

Tunnel and conveyor dryers

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Definition

Moving bed systems

Turbo tray dryers

Pan dryers

Fluidized bed systems

Pneumatic systems

Specialized drying methods

Removal of liquid from material by application of

heat, by transfer of liquid from surface into
unsaturated vapor phase
Removal of small amount of water from
moisture-bearing table salt as well as to
recovery of salt from sea by evaporation
Drying and evaporation are distinguishable by
relative quantities of liquid removed from the
solid

Spray dryers
Freeze dryers
Microwave drying

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Purpose
Nonthermal methods of drying

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Unit process in preparation of granules

Processing of materials, e.g., preparation of
dried aluminum hydroxide, spray drying of
lactose, and preparation of powdered extracts
Reduce bulk and weight, lowering cost of
transportation and storage
Preservation of animal and vegetable drugs by
minimizing mold and bacterial growth in
moisture-laden material
Facilitating comminution, dried substance more
friable than original

expression of solid to remove liquid (squeezing of a

wetted sponge)
extraction of liquid from solid by use of solvent
adsorption of water from solvent by use of desiccants
(such as anhydrous CaCl2)
absorption of moisture from gases by passage
through sulfuric acid column
desiccation of moisture from solid by placing it in
sealed container with moisture-removing material
(silica gel in bottle)

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Theory of Drying
Rate of evaporation of liquid film at material
surface related to rate of heat transfer
Driving force is humidity differential,
for heat transfer, it is temp differential
Coefficient of mass transfer is varies with
velocity of air stream passing over surface

Drying involves both heat and mass transfer

operations
Heat transferred to material to supply latent
heat required for vaporization of moisture
Mass transfer involved in diffusion of water
through material to surface, evaporation of
water from surface, and diffusion of vapor into
passing air stream

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Foregoing discussion holds true as long as

there is a film of moisture on surface of material

Rate of drying may be accelerated by

Increasing

air flow rate and raising inlet air

temp
Introducing a high-temp radiating heat
source into drying chamber

Reducing

thickness of material and

allowing it to come in contact with raisedtemp surfaces
Increasing air velocity
Dehumidifying inlet air

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Drying of Solids

When drying surface causes a shrinkage of

solid, process becomes complicated

When surface becomes partially or completely dry,

heat and mass transfer equations become more
complex
Rate of drying is controlled by rate of diffusion of
moisture from interior of material
This diffusion is greatly influenced by molecular and
capillary structure of solid

This phenomenon can cause blocking and distortion

of capillary structure and interfere transfer of internal
water to material surface
This is so-called case hardening phenomenon, in
which solid surface becomes harder than interior
and less permeable to transmission of interior
moisture

Loss on Drying (LOD)

Moisture in a solid can be expressed on wet or dryweight basis

On wet-weight basis, water content is calculated as
percentage of weight of wet solid
On dry-weight basis, water is expressed as
percentage of weight of dry solid
In pharmacy, LOD, is expression of MC on a wetweight basis
% LOD = (wt of water in sample/total wt of wet sample) x 100 (6)

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Moisture Content (MC)

LOD values can vary from slightly above 0% to

slightly below 100%
MC values can change from slightly above 0%
and approach infinity
Small change in LOD value, from 80% to 83%,
represents and increase in MC of 88%, or a
22% increase in the amount of water that must
be evaporated per pound of dry product
% MC is far more realistic value than LOD in
determination of dryer load capacity

Calculated on dry-weight basis

Referred to as MC :
% MC = (wt of water in sample/wt of dry sample) x 100

(7)

5 g of moist solid is brought to constant dry

weight of 3 g :
MC = (5-3)/3 x 100 = 66.7%
LOD = (5-3)/5 x 100 = 40%

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Behavior of Solids During Drying

The changes may be easily seen if plotted rate

of drying against MC
When a wet solid is first placed in drying oven, it
begins to absorb heat and increases in temp

Rate of drying can be determined by

suspending wet material on a balance in
drying cabinet and measuring weight of
sample as it dries as a function of time
Plotted drying rate as MC vs time

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At the same time, moisture begins evaporating and

thus tends to cool the drying solid

After a period of initial adjustment, rates of

heating and cooling become equal and temp
of the material stabilizes

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This period of initial adjustment is shown as

segment AB
At point B, temp is stabilized and remains
constant as long as there is a film of moisture
remaining at surface of solid
Between points B and C, moisture evaporating
from surface is replaced by water diffusing
from interior of solid at a rate equal to rate of
evaporation
Rate of drying is constant, and time BC is
constant rate period
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At point C, surface water is no longer replaced

at a rate fast enough to maintain continuous
film
Dry spots appear, and rate of drying begins to
fall off
MC at this point is CMC
Between points C and D, number and area of
dry spots continue to grow, and rate of drying
falls steadily
Time CD is first falling rate period or period of
unsaturated surface drying

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At point D, film of surface water is completely

evaporated, and rate of drying depends on rate
of diffusion of moisture to solid surface
Point D is second critical point
Between points D and E, rate of drying falls
more rapidly than first falling rate, and time DE
is called second falling rate period
When drying rate equal to zero, starting at
point E, EM period begins, and solid is in
equilibrium with its surroundings, i.e., its temp
and MC remain constant

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Equilibrium Relative Humidity (ERH)

Continued drying after this point is waste of

time and energy
Equilibrium Moisture Content (EMC)

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RH surrounding material at which material neither

gains nor loses moisture is called ERH

MC of material that is in equilibrium with

atmosphere
MC at which material exerts water vapor pressure
equal to vapor pressure of atmosphere; no driving
force for mass transfer
EMC values of various materials may differ greatly
under same conditions, despite that they are in
equilibrium with their environment
These differences are due to the manner in which
water is held by material

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Classification of Dryers

Two useful classifications are based on either

method of heat transfer or method of solids
handling
Type of heat transfer is important in
demonstrating gross differences in dryer design,
operation, & energy requirements
Method of solids handling is suitable when
special attention must be given to nature of
material to be dried

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major criterion is presence or absence of agitation

Excessive agitation is contraindicated when the dried
material is friable and subject to attrition
drying time can be reduced, if dried product is
intended to be pulverized, and process made more
efficient, by use of a dryer that produces intense
agitation during drying cycle

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Classification based on
method of solids handling
Static-bed dryers

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No relative movement among solid particles,

May be bulk motion of entire mass
Only fraction of total number of particles is directly
exposed to heat sources
Exposed surface can be increased by decreasing
thickness of the bed and allowing drying air to flow
through it

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Static-Bed Systems
Tray and Truck Dryers
Most

commonly used in pharmaceutical

plant operations
Called shelf, cabinet, or compartment dryers
Cabinet in which material is spread on tiers
of trays
Number of trays varies with size of dryer

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Truck

dryer: trays are loaded on trucks

(racks equipped with wheels), which can be
rolled into and out of drying cabinet
In plant operations, truck dryer is preferred
over tray dryer because of greater
convenience in loading and unloading
Batch procedure

Each batch of material can be handled as separate entity

Batch sizes of pharmaceutical industry are small (500 or less
pounds per batch) compared with chemical industry (2000 or
more pounds per hour)
Same equipment is readily adjusted for use in drying a wide
variety of materials

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Batch drying is used extensively in manufacture of

pharmaceuticals:

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Tray dryers may be classified as direct or indirect

Most tray dryers are of direct type, heating is
accomplished by forced circulation of large volumes
of heated air
Indirect tray dryers utilize heated shelves or radiant
heat sources inside drying chamber to evaporate
moisture, which is then removed by either a vacuum
pump or small amount of circulated gas
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Tunnel and Conveyor Dryers

Tunnel dryers are adaptations of truck dryer

Trucks are moved progressively through drying tunnel
by moving chain
Trucks are loaded on one side of dryer, allowed to
reside in heating chamber for a time sufficiently long
to effect desired drying, and then discharged at exit
Operation may be described as semicontinuous,
because each truck requires individual loading and
unloading before and after drying cycle
Conveyor dryers are an improvement over tunnel
dryers because they are truly continuous

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Moving-bed dryers

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Moving-bed

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Atmospheric pan drying allows moisture to escape,

whereas in vacuum dryers, solvents are recoverable if
evacuated vapors are passed through condenser
Dried material is discharged through a door on bottom
of pan

Fluidized-bed dryers

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Fluidized-Bed Systems

is allowed to flow upward through a bed

of particulate solids at a velocity greater than
velocity of particles and less than velocity for
pneumatic conveying, solids are buoyed up
and become partially suspended in gas
stream
Mixture of solids and gas behaves like liquid,
and solids are said to be fluidized
Solid particles are continually caught up in
eddies and fall back in a random boiling
motion

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Solid particles are partially suspended in an upwardmoving gas stream

Particles are lifted and fall back in a random manner
so that the mixture of solid and gas acts like a boiling
liquid
Gas-solid contact is excellent and results in better
heat and mass transfer than in static and moving
beds
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Gas

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Drying particles are partially separated so that they

flow over each other
Motion may be induced by gravity or mechanical
agitation
The resultant separation of particles and continuous
exposure of new surfaces allow more rapid heat and
mass transfer than in static beds

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Pan Dryers
dryers of indirect type
Operate under atmospheric pressure or
vacuum
Generally used to dry small batches of
pastes or slurries
Shallow, circular jacketed pan with flat
bottom and vertical sides
Heat is supplied by steam or hot water
Set of rotating plows in the pan that revolve
slowly, scraping moisture-laden mass from
the walls and exposing new surfaces to
contact with heated sides and bottom

Individual trucks of the tunnel are replaced with an

endless belt or screen that carries wet material
through drying tunnel

Efficient for drying of granular solids, because each

particle is completely surrounded by drying gas
Intense mixing between solids and gas results in
uniform conditions of temp, composition, particle
size distribution
Only requirements are granules are not so wet that
they stick together on drying, and dried product is not
so friable as to produce excessive amounts of fine
particles through attrition
Twofold to sixfold advantage in thermal efficiency
over tray dryer
Faster in drying and handling time than tray dryer

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Types of Fluidized-Bed Dryers

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Vertical and horizontal

Fluidizing air stream is induced by a fan mounted in
upper part of apparatus
Air is heated to required temp and flows upward
through wet material, which is in drying chamber
fitted with a wire mesh support at bottom
Bag collector filter is at the top of drying chamber to
prevent carryover of fine particles
The unit is batch-type dryer, and drying chamber is
removed from the unit to permit charging and
dumping
Dryer capacities: 5 kg to 200 kg and average drying
time is 20 to 40 min

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Because of the short drying time and excellent mixing

action of the dryer, no hot spots are produced, and
higher drying temps can be employed than are used
in conventional tray and truck dryers
Designed for direct preparation of tablet granulations,
drying of conventionally produced wet granulations
As a granulator, dry ingredients are placed in
chamber and fluidized while granulating liquid is
sprayed into the bed, causing particles to
agglomerate into granules
At the end of granulating cycle, granules are dried by
heating the fluidizing air

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A continuous dryer is more suitable than a batch type

for the drying of larger volumes of materials
A fluidized-bed dryer of this type, is a horizontal
vibrating conveyor dryer
The heated air is introduced into a chamber below the
vibrating conveying deck and passes up through the
perforated or louvered conveying surface, through the
fluidized bed of solids, and into an exhaust hood
A fluidized bed of uniform density and thickness is
maintained in any given drying zone by the vibration
Residence time in any drying zone is controlled by the
length of the zone, the frequency and amplitude of the
vibration, and the use of dams

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Dryer

can be divided into several different

zones with independent control of airflow and
temp, so that drying can take place at the
maximum desirable rate in each stage without
sacrificing efficiency or damaging heatsensitive materials
Dryer capacity is limited only by retention time
produced by conveying speeds
In pharmaceutical operations, capacities
range as high as 1 to 2 tons per hour.

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Pneumatic Systems

Pneumatic dryer

Drying particles are entrained and conveyed in

high-velocity gas stream
Pneumatic systems further improve on fluidized
beds
Each particle is completely surrounded by an
envelope of drying gas
Heat and mass transfer are extremely rapid; drying
times are short

Spray Dryers

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Surface liquid is quickly evaporated, and a tough shell

of solids may form
As drying proceeds, liquid in interior of droplet must
diffuse through this shell
Diffusion of liquid occurs at much slower rate than
transfer of heat through the shell to interior of droplet
The resultant buildup of heat causes the liquid below
the shell to evaporate at greater rate than it can
diffuse to surface
The internal pressure causes the droplet to swell, and
the shell becomes thinner, allowing faster diffusion

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Handle only fluid materials such as solutions, slurries,

and thin pastes
Fluid is dispersed as fine droplets into a moving
stream of hot gas, where they evaporate rapidly
before reaching the wall of drying chamber
The product dries into a fine powder, which is carried
by the gas current and gravity flow into a collection
system
When the liquid droplets come into contact with hot
gas, they quickly reach a temp slightly above temp of
the gas
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If the shell is nonelastic or impermeable, it ruptures,

producing either fragments or budlike forms on the
original sphere
Thus, spray-dried material consists of intact spheres,
spheres with buds, ruptured hollow spheres, or
sphere fragments
Rate of feed is adjusted so that each droplet of
sprayed liquid is completely dried before it comes in
contact with the walls of drying chamber, and the
dried powder is not overheated in the drying process

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Proper feed rate is determined by observation of

outlet air temp and visual inspection of the walls of
drying chamber
If inlet air temp is kept constant, a drop in liquid feed
rate is reflected by a rise in outlet temp
Excessive feed rates produce a lowering of outlet
temp, and ultimately, a buildup of material on the
walls of chamber

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Separation of solid product from effluent gas is by

means of cyclone separator (as primary collector)

Product that reaches the walls of drying chamber,

chamber product, is removed at bottom of chamber

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cyclone product

coarser in size and subjected to heat longer (because of

increased retention time) than cyclone product

Final dried product is a mixture of both chamber and

cyclone products

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spray dryer

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Specialized Drying Methods

Spray Drying and Spray Congealing of

Pharmaceuticals

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Spray drying finds great utility in pharmaceutical

industry because of rapidity of drying and unique form
of final product
Three major uses :

Freeze Dryers

drying heat-sensitive materials

changing the physical form of materials for use in tablet and
capsule manufacture
encapsulating solid and liquid particles

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Many products lose their viability in liquid state and

readily deteriorate if dried in air at normal atmospheric
pressures
These materials may be heat-sensitive or may react
with oxygen, in order to be stabilized, they must be
dehydrated to a solid state
Material is first frozen and then subjected under a
high vacuum to heat (supplied by conduction or
radiation, or both) so that frozen liquid sublimes
leaving only solid, dried components

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Blood serum, plasma, antibiotics, hormones, bacterial

cultures, vaccines, and many foodstuffs are
dehydrated by freeze drying, also referred to as
lyophilization, gelsiccation or drying by sublimation
Dried product can be readily redissolved or
resuspended by addition of water prior to use,
reconstitution
Freeze drying depends on phenomenon of
sublimation, whereby water passes directly from solid
state (ice) to vapor state without passing through
liquid state
Schematic pressure-temp diagram for water,
sublimation can take place at pressures and temps
below triple point, 4.579 mm Hg absolute (4579
microns) and 0.0099C

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The water contains dissolved solids, resulting in a

different pressure-temp relationship for each solute

pressure and temp at which the frozen solid vaporizes

without conversion to liquid is referred to as eutectic point

Freeze drying is carried out at temps and pressures

well below this point to prevent frozen water from
melting, which would result in frothing, as liquid and
frozen solid vaporize simultaneously
In actual practice, freeze drying is carried out at
temps of - 10C to - 40C, and at pressures of 2000
to 100 microns

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freeze dryer

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Microwave Drying.

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The heating effect is produced by interaction of a

rapidly oscillating electric field (915 or 2450
megahertz) with polarized molecules and ions in
material

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Thus, moisture is mobilized as vapor rather than

liquid, and its movement to the surface can be
extremely rapid because it does not depend on mass
concentration gradients or on slow liquid diffusion
rates

Industrial microwave dryers are usually of static bed

continuous type
Materials are placed on conveyor belts and conveyed
through the microwave applicator
Generally, a stream of hot air is used simultaneously
with microwaves to sweep away moisture evolving
from surface of material

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The application of microwave energy to the drying of

solids represents a radical departure from
conventional means of drying
Instead of applying heat externally to a material,
energy in form of microwaves is converted into
internal heat by interaction with material itself
This permits extremely rapid heat transfer throughout
material, which in turn can lead to rapid drying

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Often, the microwave treatment is used in the last

stages of hot air drying (second falling rate period) to
remove last remaining portion of solvent, reducing
total drying time by 50% or more

Microwave drying can be used for drying of

pharmaceutical materials at low ambient temps,
avoiding high surface temps, case hardening, and
solute migration.
Microwave vacuum drying at low pressure (1 to 20
mm Hg) and moderate temp (30 to 40C) can be used
for drying thermolabile materials such as vitamins,
enzymes, proteins, and flavors

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The field imposes order on otherwise randomly

oriented molecules
As the field reverses polarity, it relaxes and allows
molecules to return to their random orientation, giving
up stored potential energy as random kinetic energy,
or heat
Interaction of alternating field with ions causes billiard
ball-like collisions with un-ionized molecules, and
impact energy is converted into heat
In microwave drying, mass transfer is primarily result
of a pressure gradient due to rapid vapor generation
inside material, that is, most of internal moisture is
vaporized before leaving the sample

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The rising cost of energy has generated a great

deal of interest in microwave drying
microwaves couple directly into solvent, and no
energy is used to heat air, walls of dryer, conveyor,
or trays

extremely efficient energy utilization, and energy savings of

as much as 70% have been realized in industrial
installations

References
The

theory and practice of industrial

pharmacy. Third edition. Chapter 3 drying.
Pharmaceutics the science of dosage form
design. Chapter 38 drying.
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