Drying

Drying Vs evaporation
Non-thermal way of drying: expression, extraction, absorption, dessication
Importance of drying: In pharmaceutical technology, drying is carried out for one or more
of the following reasons:
1. To avoid or eliminate moisture which may lead to corrosion and decrease the product or
drug stability.
2. To improve or keep the good properties of a material, e.g. Flowability, compressibility.
3. To reduce the cost of transportation of large volume materials (liquids).
4. To make the material easy or more suitable for handling.
5. Preservation.
6. The final step in Evaporation, Filtration, Crystallization.
• Drying is a complex operation involving transient transfer of heat and mass along with
several rate processes, such as physical or chemical transformations, which, in turn, may
cause changes in product quality.
• Physical changes that may occur include: shrinkage, puffing, crystallization, glass
transitions.
• In some cases, desirable or undesirable chemical or biochemical reactions may occur
leading to changes in color, texture, odor or other properties of the solid product. In the
manufacture of catalysts, for example, drying conditions can yield significant differences
in the activity of the catalyst by changing the internal surface area.
• Drying occurs by effecting vaporization of the liquid by supplying heat to the wet
feedstock. Heat may be supplied by convection (almost 85%, direct dryers), by
conduction (contact or indirect dryers), radiation or volumetrically by placing the wet
material in a microwave or radio frequency electromagnetic field.
• All modes except the dielectric (microwave and radio frequency) supply heat at the
boundaries of the drying object so that the heat must diffuse into the solid primarily by
conduction. The liquid must travel to the boundary of the material before it is transported
away by the carrier gas (or by application of vacuum for non-convective dryers).
• Transport of moisture within the solid may occur by any one or more of the following
mechanisms of mass transfer:
Liquid diffusion, if the wet solid is at a temperature below the boiling point of the liquid
Vapor diffusion, if the liquid vaporizes within material
Knudsen diffusion, if drying takes place at very low temperatures and pressures, e.g., in
freeze drying
Hydrostatic pressure differences, when internal vaporization rates exceed the rate of vapor
transport through the solid to the surroundings.
Combinations of the above mechanisms.
Note that since the physical structure of the drying solid is subject to change during drying,
the mechanisms of moisture transfer may also change with elapsed time of drying.
Psychrometry: The determination of the vapor concentration and carrying capacity of the
gas is termed psychrometry.
Absolute humidity: weight of water vapor per unit weight of dry air.
Saturation humidity: is the absolute humidity at which partial pressure of water vapor in the
air is equal to the partial pressure of free water at the same temperature.
Dew point: Temperature at which a given unsaturated air-vapor mixture becomes saturated.
Below dew point, the water vapor condenses to produce a two phase system of saturated air
and droplets of free water.
Relative Humidity: Ratio of partial pressure of water vapor in air to the vapor pressure of
the free water at the same temperature.
Percent humidity or percent absolute humidity: the ratio of absolute humidity to saturation
humidity at the same temperature. For point A 78/161= 48%
Wet bulb temperature, Twb : It defined as the equilibrium temperature reached by an
evaporating surface when the rate of heat transferred to the surface is equal to the rate of
heat lost by evaporation. Liquid temperature attained when large amounts of air-vapor
mixture is contacted with the surface. In purely convective drying, drying surface reaches
Twb during the constant rate period. It can be measured by means of a thermometer whose
bulb is covered by a wick saturated with water.
Dry bulb temperature, Tdb :The actual temp. of the air as measured by thermometer is called
the dry bulb temperature.
The psychrometric chart is entered at the wet bulb temp and the coordinate is followed
vertically upward until it intersects the saturation or 100% relative humidity curve. Then the
constant wet bulb temp line is followed until it intersects the dry bulb temp coordinate.
From the absolute humidity, the relative humidity can be calculated.
• Wet bulb temp is approx. the same as the adiabatic saturation temp. Tas i.e. the temp that
would be attained if the air were saturated with water vapor in an adiabatic process. This
the case when drying is carried out by dry air only.
• Humidity measurement: Gravimetric analysis by absorbing material, sling psychrometer,
with dew point, mechanical hygrometer
Drying: Heat and mass transfer
The rate of evaporation of liquid film on material is related to the rate of heat transfer by the eq.
dW/dθ = q/λ
Where dW/dθ is the rate of evaporation, q is the overall rate of heat transfer[BTU per hour and λ is
the latent heat of vaporization of water (BTU per pound)].
Since this is related with humidity gradient
dW/dθ = k’A(Hs-Hg)
Where A is the area in feet, Hs is the absolute humidity at the evaporating surface and Hg is the
absolute humidity in the passing air stream.
k’ = cGn
Where c proportionality constant, G rate of flow of air (pounds of dry air/ hour in square feet) and n
is fractional exponent usually about 0.8.
If q is expressed as the sum of the rates of heat transfer by convection, radiation and conduction,
then rate of heat transfer
dW/dθ = (qc + qr + qk)/λ = k’A(Hs-Hg)
• The rate of convection can be increased by increasing the air flow rate and by raising the inlet air
temperature. The radiation heat can be speeded up by introducing a high temperature radiating
heat source into the drying chamber. The conduction heat can be stepped up by reducing the
thickness of the material being dried and by allowing it to come in contact with raised
temperature.
• Increasing the air velocity also speeds up the rate by increasing the coefficient of mass transfer,
k’.
• Dehumidifying the inlet air increases the humidity differential, thereby increasing the rate of
drying.
• What is the effect of heating the air in a drier to 150°F if the outside air is 81°F with 50% relative
humidity?
• Note: These discussion holds till the film of moisture on the material is there to dry. Once the
becomes partially or completely dry, heat and mass transfer equations more complex.
Drying of solids:
• Loss on drying: The moisture in a solid can be expressed on a wet-weight or dry- weight
basis. On a wet weight basis, the water content of a material is calculated as a percentage
of the weight of the wet solid, whereas on the dry weight basis, the water is expressed as a
percentage of the weight of the dry solid. With the help of moisture balance.

• Moisture content: Another measurement of the moisture in a wet solid is that calculated
on a dry weight basis. This is referred to as moisture content or MC.

• Suppose 5gm of moist solid is dried to 3 gm. Calculate %LOD and %MC.
• The MC % is more realistic than LOD.
Behaviour of solids
• Sample drying on balance
• Rate of drying vs drying time
• Drying rate with moisture content: The
difference in moisture content between any
two measurements divided by the time period
between measurements represents the rate of
drying for this time period. This value is
plotted against the midpoint of the time period
for a drying rate vs time curve or against the
midpoint of the moisture content values for a
drying rate vs moisture content curve.
Classification of solids based on drying
behaviour: (a) Granular or crystalline solids (b)
amorphous solids
• The water in crystalline solids is held in shallow and open surface pores, hence they are
easy to dry. Eg Calcium sulfide, zinc oxide
• The amorphous, fibrous or gelatinous solids have moisture as integral part of the
molecular structure as well as being physically entrapped in fine capillaries and small
interior pores. Eg starch, casein, yeast
• Equilibrium moisture content: The moisture content of a material that is in equilibrium
with an atmosphere of a given relativity is called the EMC of the material at this
humidity. The vapor pressure of water in the surrounding air is equal to the water vapor of
the material.
• Equilibrium relative humidity: The relative humidity surrounding a material at which the
material neither gains nor loses moisture is called the ERH.
• water activity aw: Ratio of vapor pressure (p) exerted by water in solid to that of pure
water (pw) at the same temperature. Pure water is assigned as aw =1.
Classification of dryers
Heat transfer is important in demonstrating gross differences in dryer design, operation and energy
requirements.
Solid handling is suited when handling of solid is more important given the nature of the material to
be dried. 1. static bed dryer 2. Moving bed dryer 3. Fluidized bed dryers 4. Pneumatic bed dryers
Static bed Dryers:
Tray/truck/ Shelf/Cabinet/compartment dryers:
• It is the simplest form of dryer, in this arrangement of heater at the bottom in cabinet e.g.
laboratory oven.
• In that the best type of tray dryer is directed circulation form, in which air is heated & is directed
across the material in a controlled flow.
• In modern tray dryers, a uniform temperature & air flow is maintained by the use of a well cabinet
with strategically placed fans & heating coil.
• In that heater is fixed in a such way that the air is reheated before passing over each shelf.
• When the air passes over each shelf a certain amount of heat is given up to provide latent
heat of vaporization
Truck Dryer are with wheels.
Tunnel and conveyer dryer: It is the same like tray dryer but only modification in which
oven is replaced by a tunnel. In which, receive the damp material at one end & discharge the
dried product at the other end. In that conveyor belt system can also be used to pass the
material through the tunnel.
Application: • For drying of sticky material & granular mass. • Drying of crude drugs,
chemicals, powders, tablet granules etc
Advantages : Easy to operate. batch process for different product, can useful for drying of
verity of material. Tunnel dryer are semi-continuous and conveyer dryer is continuous type.
Disadvantages: Require labor, cost increasing, time consuming.
 Truck dryer
Tray dryer

Conveyor dryer Turbo tray dryer Pan dryer

Turbo tray dryers: A continuous shelf, moving bed dryer.
• Having series of rotating annular trays arranged in a vertical stack.
• Drying rates are better than tunnel dryer.
https://www.youtube.com/watch?v=-XpohB2hUoM
Pan dryer: batch type, under pressure or vacuum, heat is supplied by steam or air, pan with rotating
plows. https://www.youtube.com/watch?v=vCIPGKmFSR0
Fluidized bed system: It is a best dryer because, in that rapid drying occurs. If a gas is allowed to
flow upward through a bed of solid particles at a velocity greater than the velocity of the particles,
the particles are partially suspended in the gas stream. The resultant mixture behaves like a liquid,
so solids is said to be fluidised.
This has advantage over conventional tray drying for tablet granulations as they have the proper
particle size. The particles should not be wet as they can stick together and should not be friable as
to produce excessive amount of fine particles through attrition.
https://www.youtube.com/watch?v=dwHFKyf_ZLc
It have two types: Vertical & Horizontal fluidised bed dryer.
In that fan is mounted in the upper part of the dryer. Air is heated by heaters & passed through the
wet material contained in a drying chamber. This chamber is fitted with a wire mesh support at the
bottom. The air flow rate is adjusted by re-circulation control. Fabric filter bags are provided to
prevent the passage of fine particles. It is used for batch type dryer & the drying chamber is removed
from the unit for charging.
Advantages : Fast process, available in different capacity, easy handling, reduce labor cost, high
thermal efficiency, suitable for applying high temp, suitable for thermo-labile substances.
Disadvantages: Develops electric charges. attrition may occur
https://www.youtube.com/watch?v=LCz7dP6QMj8
Pneumatic dryer
Spray dryer: These dryers are for fluid materials like solutions, slurries and thin pastes.
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 diffusion of the liquid from the core to the shell is slower than
transfer of heat to the core, leading the droplet to swell. The shell becomes thinner,
allowing faster diffusion. If the shell is nonelastic or impermeable, it ruptures, producing
either fragments or bud like forms on the original surface.
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.
Spray dryer can be operated efficiently at various feed rates. Useful for thermo-labile,
hygroscopic material.
https://www.youtube.com/watch?v=ZKCk7K4Ew7c
Spray dryer
Spray dryer atomizers are of three types pneumatic atomizers (fluid or gas atomizing), pressure and
spinning disc atomizers.
The spary drying process is better because it can (i) dry heat sensitive material (ii) change the physical
form of materials for use in tablet and capsule manufacture and (iii) encapsulate both solid and liquid
particles.
Solid particles by spray drying of suspension of the material in solution of coating agent. The coating
provides taste and odor masking, improvement in stability, enteric coating and sustained release. Oily
liq. can be encapsulated by emulsification in water with the aid of a gum such as acacia, or starch and
subsequent spray drying. As the water evaporates the oil is entrapped in a shell of the gum.
Spray Congealing or chilling: This consist suspending particles in molten coating material and
pumping the slurry in the atmosphere of cold air. The slurry droplets congeal on coming into contact
with the air. This requires much higher ratio of coating agent then does spray drying as only coating
material constitute the liq phase.
Advantages: Very rapid & continue process, low labor cost, gives product of uniform sphere form &
fine droplet, suitable for sterile products
Disadvantages: very bulky & expensive. huge equipment (not easy to operate), low thermal efficiency.
Flash dryer: The moistened solid mass is suspended in finely divided state in a high velocity, high
temp. air stream. The dispersed particles can may be carried in the air stream to an impact mill, or
pneumatic flow itself may reduce the particle size of friable material. The resultant attrition
exposes new surfaces for more drying. The dried solid is collected by cyclone separator. Referred
as Flash because of extremely short drying time.
Freeze dryer or Lyophilization: It is also called as sublimation drying process, In that process
water is sublimed & removed from the product after it is frozen at the reduced pressure. Material is
frozen in a container connected to a high vacuum system. Vapor pressure of material is reduced
below the vapor pressure at which it is dried i.e below the triple point. Under these conditions, heat
transferred is used as latent heat of sublimation to the product by means of radiant heat. Ice
sublimes to vapors. Water vapors are removed by condensation.
Chamber for vacuum drying: having shelves for keeping the material. Vacuum source: vacuum
pump is connected to the chamber. A heat source: heat is provided by conduction or radiation or
both. A vapour removal system: the condenser consists of large cooled surface by solid carbon
dioxide mixed with acetone or ethanol.
Pre-treatment : first solution is concentrated under normal vacuum dryer before introducing in the
chamber. Pre-freezing : ampoules, vials & bottles having aq. solution is packed & frozen in cold
shelves at a temperature below -50°C. Primary drying: The material is spread.
Temperature & pressure are kept below the triple point of water. Heat is supplied. Ice sublimes
into vapours. Vapours are removed from the chamber. 98-99% moisture removes during primary
drying.
Secondary drying : remaining moisture is removed by vacuum drying at 50-60°C. Secondary
drying takes about 10-20 hrs. Packing : biological products are dried packed in aseptic condition
immediately after drying.
Use: thermolabile subst, microbiological cultures, biological products.
Microwave drying: In conventional heating the caloric transmits from the surface to the interior
while the moisture is transferred opposite way from the inner to the SURFACE WHERE it is
suppose to evaporate. Using deep affecting microwaves heats the inner pushing the moisture to the
lower pressure space that is on the cool surface since the surrounding air is not affected by
microwaves. This mechanism of water pump considerably accelerate and improves removing the
moisture.
High energy efficiency: Water as extremely polar material absorbs efficiently the
microwave energy converting it almost entirely to heat. In physical principle the comparable
efficiency can be hardly achieved by any other method although using the conventional heat
can be caused by other factors then the efficiency.
Uniform and steady of the whole volume heating: From the components of the material
usually the water molecules are most affected and on the contrary dry parts of the material
is often MW transparent. This effect can be used for equalizing of the moisture level among
the various parts of the material – in case of non uniform moisture spreading at the
beginning of the process.

Fast moisture transfer: Conventional drying of the solid state material often creates very dry
layer on the surface crust breaking the capillary transfer of the moisture from the core. The
dry crust can also insulate thermally the core of the material. Using the microwaves on the
contrary avoids creating the crust since the moisture pushed from the core preserves the
humid surface and supports the capillary.
For many cases the rapid drying is far less important than the necessary condition of achieving it at
relatively low temperatures (avoiding harm of the product).
Drying foods conventionally often degrades their thermosensible components (such as vitamins,
essences…) – as well as deteriorates their organoleptic properties
For chemicals there is often necessary to take n to account parameters of flammability, explosiveness,
or many undesirable changes. The process has to run keeping the under critical temperatures in the
whole volume (such as flammable temperature, boiling temperature, sintering etc. Moreover certain
dissolvents can be dried out at relatively low temperatures preventing the fire danger
Glues and paints can be dried out without harming the base material. Conventional methods often
warm the material surface up to 180 °C while microwaves keep it down on 100°C or below. Moreover
fast MW treating enables to avoid overdrying of surface layer and material damage.