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Avinash Chandra
Mass Transfer
©Dr. Avinash Chandra
Drying
• Drying is commonly the last stage in a manufacture process.
• Drying is the final removal of water from material (usually by
heat)
5- Preservative.
Introduction
• Drying is the removal of small amounts of water
form the wet materials (solid).
also used to removed of other organic liquids, such as
benzene or organic solvent from solid.
Ls dx where :
R • R: drying rate in kg H2O /h.m2
A dt • Ls : weight of dry solid in kg
• A : exposed surface area in m2
W W • dx : change in water content in kg
Xt s H2O/kg dry solid
• dt : change in time in hour
Ws • x: water content in kg H2O/kg dry
solid
X Xt X * • Xt : Moisture content at time t (kg
water/kg dry solid).
• W : Weight of water (kg water).
• X* : is equilibrium water contents
•Xt = W/ LS
• Ws: Weight of dry solid (kg)
©Dr. Avinash Chandra
©Dr. Avinash Chandra
Schematic Diagram:
©Dr. Avinash Chandra
Equilibrium curve
©Dr. Avinash Chandra
Hysteresis
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Batch drying
©Dr. Avinash Chandra
©Dr. Avinash Chandra
Time of drying
©Dr. Avinash Chandra
©Dr. Avinash Chandra
©Dr. Avinash Chandra
©Dr. Avinash Chandra
©Dr. Avinash Chandra
©Dr. Avinash Chandra
©Dr. Avinash Chandra
©Dr. Avinash Chandra
Classification of dryers
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.
Spray Dryer
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.....
©Dr. Avinash Chandra
©Dr. Avinash Chandra
• 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.
• 6- Labour costs are low, the process yielding a dry, free-flowing powder
from a dilute solution, in a single operation with no handling.
Freeze Drying
• Thus a liquid –to-vapour transition takes place, but here three states of
matter involved: liquid to solid, then solid to vapour
©Dr. Avinash Chandra
• This will only happen if the pressure is prevented from rising above the
triple point pressure .
Freeze Dryer
©Dr. Avinash Chandra
• 1-The depression of the freezing point caused by the presence of dissolved solutes
means that the solution must be cooled below the normal freezing temperature for pure
water (-10-30).
• 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.
©Dr. Avinash Chandra
• 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.
©Dr. Avinash Chandra
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.
©Dr. Avinash Chandra
• 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.
©Dr. Avinash Chandra
• 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
©Dr. Avinash Chandra
• 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.
©Dr. Avinash Chandra
Constant-rate period: It is found that the evaporation rate from the drying
bed is similar to that of
the solvent alone from a free
liquid surface under the same
conditions, indicating that the
evaporation takes place from
the wet surface of the solid, and
that the surface remains wet in
this period as a result of the liquid
being replaced from below as
fast as it is vaporized
Controlling factors in this
period are the rate at which
heat can be transferred and
the rate of removal of the vapour.
©Dr. Avinash Chandra
• 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........
©Dr. Avinash Chandra
©Dr. Avinash Chandra
©Dr. Avinash Chandra
- 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.
©Dr. Avinash Chandra
• 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.
©Dr. Avinash Chandra
• 2- Fine particles may become entrained in the fluidizing air and must
be collected by bag filters, leading to segregation and loss of fines.
• 3-The vigorous movement of particles in hot dry air can lead to the
generation of static electricity charges. The danger is increased if the
fluidized material contains a volatile solvent such as isopropanol.
Adequate electrical earthing is essential.
©Dr. Avinash Chandra
• 3- Radiation:
• The transfer of heat by radiant energy in the form of electromagnetic
waves, which travel in straight lines at the speed of light, is referred
to as radiation heat transfer. As a body is heated, it emits radiant
energy, e.g. sun and infrared heat lamps. When this radiation strikes
another body, portions may be reflected
©Dr. Avinash Chandra
Vacuum oven
• 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.
©Dr. Avinash Chandra
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.