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Drying: Drying Is Commonly The Last Stage in A Manufacture Process. .Non
Drying: Drying Is Commonly The Last Stage in A Manufacture Process. .Non
Purposes of drying
1- The method gives rapid drying, the thin film spread over a large area
resulting in rapid heat and mass transfer.
2- The equipment is compact, occupying much less space than other
dryers.
The spray dryer provides a large surface area for heat and mass
transfer by atomizing the liquid to small droplets. These are sprayed
into a stream of hot air, so that each droplet dries to a solid particle.
• The drying chamber resembles the cyclone ensuring good
circulation of air, to facilitate heat and mass transfer, and that dried
particles are separated by the centrifugal action.....
• The character of the particles is controlled by the droplet form;
hence the type of atomizer is important.
• Rotary atomizer is preferable than jet which is easily blocked. Liquid
is fed to the disc of the atomizer which is rotated at high speed (up
to 20,000 rpm), a film is formed and spread as uniform spray. In
addition, the rotary atomizer is effective with suspensions. It can be
operated efficiently at various feed rates.
• 1-The droplets are small, giving a large surface area for heat
transfer, so that evaporation is very rapid. The actual drying
time of a droplet is only a fraction of a second, and the overall
time in the dryer is only a few seconds.
• Thus a liquid –to-vapour transition takes place, but here three states
of matter involved: liquid to solid, then solid to vapour
The phase diagram for water
• This will only happen if the pressure is prevented from rising above
the triple point pressure .
• 2-Sublimation can only occur at the frozen surface and is slow process (1mm
thickness of ice per hour). So, the surface area must therefore be increased and
• 3-the liquid thickness prior to freezing be reduced in order to reduce the thickness
of ice to be sublimated.
• 4-At low pressure large volumes of water vapour are produced which must be
removed to prevent the pressure rising above the triple point pressure.
• 5-The dry material often needs to be sterile, and it must also be prevented from
regaining moisture prior to the final packaging.
Stages of the freeze drying process
• 1- Freezing stage:
• The liquid material is frozen before the application of vacuum to
avoid frothing, and several methods are used to produce a large
frozen surface.
• a- Shell freezing : This is employed for large volumes such as blood
products. The bottles are rotated slowly and almost horizontally
in a refrigerated bath. The liquid freezes in a thin shell around the
inner surface of the bottle.
• Freezing is slow and large ice crystals form, which is a drawback
of this method.
• In vertical spin freezing the bottles are spun individually in a
vertical position , centrifuged and cooled by a blast of cold air. The
solution super cools and freezes rapidly, with the formation of small
ice crystals.
• b- Centrifugal evaporative freezing: The solution is spun in small
containers within a centrifuge. This prevents the foaming when a
vacuum is applied. The vacuum causes boiling at room temperature.
About 20% of the water is removed prior to freeze drying and there
is no need for refrigeration. Ampoules are usually frozen in this way
• 2 - Vacuum application stage: The containers and the frozen material
must be connected to a vacuum source sufficient to drop the pressure
below the triple point and remove the larger volumes of low – pressure
vapour formed during drying.
• 3 - Sublimation stage:
• Heat of sublimation must be supplied. Under these conditions the ice slowly
sublimes, leaving a porous solid which still contains about 0.5% moisture
after primary drying .
• Primary drying: It can reduce the moisture content of a freeze-dried solid
to around 0.5%. Further reduction can be affected by secondary drying .
• Heat transfer: Insufficient heat input prolongs the process, which is already
slow, and excess heat will cause melting.
• Vapour removal: The vapour formed must be continually removed to avoid
a pressure rise that would stop sublimation.
• Rate of drying: The rate of drying in freeze drying is very slow, the ice
being removed at a rate of about only 1mm depth per hour.
Advantages of freeze drying
• 4- Secondary drying:
• The removal of residual moisture at the end of primary drying is performed by
raising the temperature of the solid to as high as 50 or 60 C .
• 5- Packaging:
• Attention must be paid to packaging freeze-dried products to ensure protection
from moisture. Containers should be closed without contacting the atmosphere.
• Disadvantages:
• Unbound water: This water exists as a liquid and exerts its fully
vapour pressure, it can be removed readily by evaporation. During a
drying process this water is easily lost but the resulting solid is not
completely free from water molecules.
• Equilibrium moisture content:
• Bound water :
• Part of the moisture present in a wet solid may be adsorbed on
surfaces of the solid or be adsorbed within its structure to such an
extent to prevent it from developing its full vapour pressure and from
being easily removed by evaporation. Such moisture is described as
“bound” and is more difficult to remove than unbound water.
Relative humidity (RH) of air
• Air at a given temperature is capable of taking up water vapour until
it is saturated (at 100% RH ). If the temperature is raised then the
air will be able to take up more moisture and the relative humidity
falls.
• The RH of air is dependent not only on the amount of moisture in the
air , but also on its temperature, as the amount of water required to
saturate air is itself dependent on temperature.
• The EMC of a solid exposed to moist air varies with the relative
humidity (Fig 26.2, Aulton p.382). Ordinary atmospheric
conditions are of the order of 20 C and 70-75 RH
• , so that if exposed to atmosphere a material such as kaolin will
contain about 1% moisture, whereas a starch –based product may
have as much as 30% or more. Materials exposed to humid
conditions will regain moisture, and so there is no advantage in
drying to moisture content lower than that which the material will
have under the conditions of use
Loss of water from wet solids
• 2- Efficient heat transfer per unit area (to supply sufficient latent heat
of vaporization or heat of sublimation in case of freeze-drying)
• Tray drier:
• In Fig.26.4. tray drier. Air flows in direction of the arrows over each shelf
in turn. The wet material is spread on shallow trays resting on the shelves.
Electrical elements or steam-heated pipes are positioned as shown, so that
the air is periodically reheated after it has cooled by passage over the wet
material on one shelf before it passes on the next.
• The rate at which drying occurs has been found to show certain
phases (fig.26.5, Aul) in which the change in moisture content is
plotted against time. From A to B
the relationship is linear, which is
known as the constant-rate period,
whereas from B to C the rate of loss
of moisture decreases and is known
as the falling-rate period. The end
of the constant rate period, B,is referred
to as the critical moisture content.
- The first falling- rate period has
a linear relationship, that is , the
decrease in drying rate is uniform,
whereas in the second falling-rate
period there is a continuous decrease
in the rate of drying until the EMC is
reached.
• Good contact between the warm drying air and wet particles is found
in the fluidized – bed drier.
• Principles of fluidization. The particulate matter is contained in a
vessel, of which is perforated, enabling a fluid to pass through the
bed of solids from below.
• If the air velocity through the bed is increased gradually and the
pressure drop through the bed is measured, a graph of the operation
shows several distinct regions, as indicated in the fig.
• Fig.26.6..Effect of air velocity on pressure drop through a
fluidized bed........
- At first, when the air velocity is low, (point A) , flow takes place
between the particles without casing disturbance, but as the velocity is
increased e point (B), is reached (gravity = force of fluidization on that
particle). Rearrangement of the particles occurs to offer least resistance
(C), and they are suspended in the air and can move.
• At point (D), pressure drop through
the bed decreases slightly because of
the greater porosity. Further increase
in the air velocity causes the particles to
separate and move freely and the bed is
fully fluidized.
Any additional increase in
velocity separates the particles further,
that is, the expands without appreciable
change in the pressure drop, until (E),
when the air velocity is sufficient to transport
the particles to the top of the bed.
• In the region D---E fluidization is irregular , much of the air flowing
through in bubbles, the term boiling bed being commonly used to
describe it .
• The important fact is that to produces
conditions of great turbulence,
the particles mixing with good
contact between them and the air.
Hence if hot air is used the
turbulent conditions lead to
high heat and mass transfer
rates, the fluidized – bed technique
therefore offers a mean of rapid drying.
Advantages of fluidized-bed drying
• 1- Efficient heat and mass transfer give high drying rates, so that
drying times are shorter than with static-bed convection driers.
Economic, heat challenge to thermolabile materials is minimized.
• 2-The fluidized state of the bed ensures that drying occurs from
the surface of all the individual particles and not just from the
surface of the bed. Hence, most of the drying will be at constant
rate and the falling –rate period is very short.
• 3-The temperature of a fluidized bed is uniform and can be
controlled precisely.
• 3-The turbulence in a fluidized bed causes some attrition to the
surface of the granule. This produces a more spherical free-
flowing product.
• 5-The free movement of individual particles eliminates the risk of
soluble materials migrating, as may occur in static beds.
Disadvantages of fluidized-bed drying
• Infrared heating has been used to dry wet granules, but it suffers
from the disadvantage that it is absorbed very quickly and does
not penetrate far into the wet mass.
• The surface layers dry quickly and the absorption of further energy
then raises the temperature of the dry material to a high value. For
this reason infrared radiation is now seldom used as a heat source
in pharmaceutical manufacture.
The use of microwave radiation
• 2- The thermal efficiency is high, as the drier casing and the air
remain cool. Most of the microwave energy is absorbed by the
liquid in the wet material.