DRYING
CONTENT-
• Introduction
• Purposes
• Period of drying
• Classification of dryers
• Special types of dryers
• references
INTRODUCTION TO DRYING PROCESS
Drying can be described by three processes
operating simultaneously:
1. Energy transfer from an external source to the water or
organic solvent
Direct or Indirect Heat Transfer
2. Phase transformation of water/solvent from a liquid-like
state to a vapour state
Mass Transfer (solid characteristics)
3. Transfer vapour generated away from the API and out of
the drying equipment
Drying APIs is an important operation for the
production of consistent, stable, free-flowing
materials for formulation, packaging, storage and
transport
Particle attrition or agglomeration can result in major
differences in particle size distribution (PSD),
compressibility and flow characteristics
Equipment selection
Drying specifications
Purpose: To reduce the moisture level of wet granules
What are the problems What are the Why do it
equipment
Over drying (bone dry) Direct Heating Static To keep the residual
Solids Bed Dryers moisture low enough
Excess fines (preferably as a range) to
Direct Heating Moving prevent product
Possible fire hazard Solids Bed Dryers deterioration
Fluid Bed Dryer Ensure free flowing
Indirect Conduction properties
Dryers
PERIODS OF DRYING
••Warm
Warm up
up period
period :A-B
:A-B
••Constant
Constant Rate
Rate Period
Period (B-C)
(B-C)
HTHT dependent
dependent
••Falling
Falling rate
rate period
period (C-D)
(C-D)
MT
MT dependent
dependent
DRYERS IN THE PHARMA INDUSTRY
Dryers can be classified according to:
Heat transferring methods
Direct: Fluidised, Tray, Spray, Rotary Dryers, etc..
Indirect: Cone, Tumble, Pan Dryers, etc…
Continuous/ Batch processing
Continuous: large quantities/small residence time
Batch: small quantities/ long residence time
TRAY DRYERS
a batch tray dryeR consists of a stack of trays or
several stacks of trays placed in a large insulated
chamber in which hot air is circulated with
appropriately designed fans and guide vanes.
It is possible to convert the
batch tray dryer into a
continuous unit. Figure
shows the so-called Turbo
dryer, which consists of a
stack of coaxial circular trays
mounted on a single vertical
shaft. The product layer fed
onto the first shelf is leveled
by a set of stationary blades,
which scratch a series of
grooves into the layer surface.
The blades are staggered to
ensure mixing of the material.
ROTARY DRYERS
The cascading rotary dryer is
a continuously operated direct
contact dryer consisting of a
slowly revolving cylindrical
shell that is typically inclined
to the horizontal a few
degrees to aid the
transportation of the wet
feedstock which is introduced
into the drum at the upper end
and the dried product
withdrawn at the lower end.
VACCUM DRYERS
For drying of granular solids or slurries, vacuum dryers of
various mechanical designs are available commercially.
They are more expensive than atmospheric pressure
dryers but are suited for heat-sensitive materials or
when solvent recovery is required
FLUID-BED DRYERS (FLUIDIZED-BED DRYERS
•Concept of fluidization
•Gas velocity realizing the change from
stationary(fixed) bed into fluidized bed is
called the critical fluidized velocity
ucritical.
•When gas velocity is increased to the
particle free setting velocity u0 , the
particle will be carried over, u0 is called the
carried over velocity ucarried.
ucritical<uoptimum<ucarried
7
•CHARACTERISTICS OF FLUID-BED
to Dust Collector
Feed
Hot Air
Distributo r Plate
Dry product disch arg e
DRYERS: ADVANTAGES:HIGH HEAT
AND MASS TRANSFER RATES; SIMPLE product
discharge
STRUCTURES; LOW FABRICATING to Dust Collector
Feed
Hot Air
Distributo r Plate
COSTS; CONVENIENT MAINTENANCE;
Dry product disch arg e
HIGHER THERMAL EFFICIENCY THAN to Dust Collector
PNEUMATIC CONVEYING DRYERS;
Feed
Hot Air
Distributor Plate
to Dust Collector Dry product disch arg e
to Dust Collector
Feed Feed
DRYING TIME CAN BE CHANGED;
Hot Air
Hot Air
Distributo r Plate
Distributo r Plate
Dry product disch arg e
Dry product disch arg e
APPLIED TO DRYING OF GRANULAR
MATERIALS. Horizontally separately
fluidized compartments (Fig. 5-
•DISADVANTAGES: STRICT OPERATION 25) can get even drying and
AND CONTROL REQUIREMENTS; relatively low flow resistance.
MULTI-SEPARATELY FLUIDIZED
COMPARTMENTS(PLUG FLOW DRYERS)
HAVE COMPLEX STRUCTURES AND
GREAT FLOW RESISTA
8
(3)PNEUMATIC CONVEYING DRYERS
Characteristics: 1)Great
Feed
First Section
Second Section
Room for separating solids
Cleaned air
Feed Exhaust air
contacting area between air and
First Section
Second Section
Room for separating solids
Cleaned air
Exhaust air
solids;Higher heat transfer and Feed
mass transfer rates; Short drying
First Section
Feed
Second Section
First Section
Room for separating solids
Second Section Cleaned air
Room for separating solids Exhaust air
Cleaned air Feed
time(0.5~2s).
First Section Feed
Exhaust air
Feed Second Section First Section
Room for separating solids Second Section
First Section
Cleaned air Room for separating solids
Second Section
Feed
Exhaust air Cleaned air
Room for separating solids
First Section Exhaust air
Cleaned air
2)Stable operation and fine
Second Section
Exhaust air Room for separating solids
Cleaned air
Exhaust air
Feed
product quality.
First Section
Second Section
Room for separating solids
Cleaned air
Exhaust air Feed
First Section
Second Section
Room for separating solids
Cleaned air
Exhaust Feed
air
First Section
Second Section
Room for separating solids
Cleaned air
Exhaust air
3)Applying to thermally sensitive and easily oxidized materials .
Defects: Materials easily broken; great flow resistance; high drying
duct. (about 30m)
5
FREEZE DRYER
Highly heat-sensitive solids, such as some certain
biotechnological materials, pharmaceuticals and foods with
high flavor content, may be freeze dried at a cost that is at
least one order-of-magnitude higher than that of spray
drying – itself not an inexpensive drying operation. Here,
drying occurs below the triple point of the liquid by
sublimation of the frozen moisture into vapor, which is then
removed from the drying chamber by mechanical vacuum
pumps or steam jet ejectors. Generally, freeze drying yields
the highest quality product of any dehydration techniques
2. Primary drying (sublimation drying)
are performed at low temperature and vacuum.
The drying progresses gradually from the surface to the center
of the products.
The pores or channels formed by the sublimation ice become
the ways of vapor to escape.
The boundary between drying layer and frozen layer is known
as the sublimation interface.
The temperature of the sublimation interface is a critical
parameter to be controlled in primary drying process.
90% water in drugs is removed after primary drying.
In primary drying process, the temperature of frozen layer
must be lower than Te or Tg’.
The temperature of dried layer must is lower than the collapse
temperature (Tc).
The temperature of the heater in the drying chamber should be
controlled strictly.
3. Secondary drying (desorption drying)
purpose : to remove a portion of the bound water.
The moisture content of drugs is lower than 3% after
secondary drying.
Because of large absorption energy, the product
temperature in secondary drying must be increased
high enough to remove the bound water, and on the
other hand, this temperature cannot induce
denaturation of proteins and deterioration of biological
drugs.
The Tg of the products increases gradually with the decrement
of water in secondary process.
So the drying temperature of the products can be increased
gradually, but cannot be higher than Tg.
4. Encapsulation process
When the secondary drying process is complete, plugging
system in the chamber is used directly to plug the vials in
order to prevent the freeze dried drugs from oxidation and
water absorption.
The encapsulation can also be completed after filling
nitrogen gas into the chamber.
7.1.5 CRITICAL PROBLEMS OF FREEZE-DRYING IN
DRUGS
1. Temperature Control and identification of
drying procedures
Frozen drugs will melt, collapse or crimple if the temperature is higher
than the optimum temperature.
if the temperature is too low, refrigeration load will causing excessive
energy consumption and the sublimation rate will be decreased greatly
2. Cooling Rate in freezing process
freezing process determines the drying rate and the
quality of freeze-dried product.
The optimum cooling rates vary with different
biological agents.For instance,
slow freezing is usually beneficial to protein polypeptide-
type drugs.
Fast freezing is usually beneficial to the virus and vaccine.
DRYER FOR SLURRY AND SUSPENSION
SPRAY DRYER
DRUM DRYERS
In drum dryers, slurries or pasty feedstocks are dried on the
surface of a slowly rotating steam-heated drum. A thin film of
the paste is applied on the surface in various ways. The dried
film is doctored off once it is dry and collected as flakes
(rather than powder).
BAND DRYER
For relatively free-flowing granules and extrudates that may undergo
mechanical damage if they are dispersed, band dryers are a good
option. It is essentially a conveyor dryer wherein the band is a
perforated band over which the bed of drying solids rests. Drying air
at rather low velocities flows upwards through the band to
accomplish drying.
TUNNEL DRYER
In this simple dryer concept, cabinets, trucks or trolleys containing the
material to be dried are transported at an appropriate speed through a long
insulated chamber (or tunnel) while hot drying gas is made to flow in
concurrent, countercurrent, cross-flow or mixed flow fashion. In the
concurrent mode, the hottest and driest air meets the wetted material and
hence results in high initial drying rates but with relatively low product
temperature (wet-bulb temperature if surface moisture is present).
MICROWAVE (MW) AND RADIO FREQUENCY (RF) DRYING
Unlike conduction, convection or radiation, dielectric heating
heats a material containing a polar compound volumetrically, i.e.,
thermal energy supplied at the surface does not have to be
conducted into the interior, as limited by Fourier's law of
heatconduction. This type of heating provides the following
advantages:
· Enhanced diffusion of heat and mass
· Development of internal pressure gradients which enhance
drying rates
· Increased drying rates without increasing surface temperatures
· Better product quality
