Introduction Drying is an important operation in primary pharmaceutical manufacture (i.e. the synthesis of active pharmaceutical ingredients or excipients).
It is usually the last stage of manufacturing before
packaging.
Drying is defined as the removal of all or most of the liquid
associated with a wet pharmaceutical product.
A process in which the liquid is removed from a material by
application of heat & is accomplished by the transfer of liquid from a surface into an unsaturated vapour phase. NEED OF DRYING
To make products stable.
Preparation of powder and granules.
Reducing the bulk and weight.
Dried before extraction to facilitate grinding and to
avoid deterioration.
Preparation of certain products like dried Aluminum
Drying APIs is an important operation for the production
of consistent, stable, free-flowing materials for formulation, packaging, storage and transport 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 to the ‘dry’ solid state, starting with either a wet solid or a solution or suspension.
The former is usually achieved by exposing the wet solid
to moving, relatively dry air (elevated temperatures to accelerate the process are common).
The latter is possible with equipment such as the spray
dryer that is capable of producing a dry product from a solution or suspension in one operation. Most pharmaceutical materials are not completely free from moisture (i.e. they are not ‘bone dry’)
They contain some residual water, the amount of which
may vary with the temperature and humidity of the ambient air to which they are exposed.
All drying processes of relevance to pharmaceutical
manufacturing involve evaporation or sublimation of the liquid phase and the removal of the subsequent vapour. The process must provide the latent heat for these processes without a significant temperature rise.
Naturally the temperature rise will enhance the potential of
thermal degradation of the product. In the majority of cases the ‘liquid’ will be water but also more volatile organic solvents, such as isopropanol, may need to be removed in a drying process.
volatile solvents are normally recovered by condensation
rather than being vented into the atmosphere.
This is for environmental and economic, the toxicity and
flammability of organic solvents pose additional safety and process considerations. Drying of wet solids Fundamental properties and interrelationships
Moisture content of wet solids
The moisture content of a wet solid is expressed as kg of
moisture associated with 1 kg of the moisture free or ‘bone-dry’ solid.
Thus, a moisture content of 0.4 means that:
0.4 kg of water is present per kg of the ‘bone-dry’ solid that will
remain after complete drying.
It is sometimes calculated as percentage moisture content;
thus this example would be quoted as 40% moisture content. Total moisture content
It is the total amount of liquid associated with a wet solid.
Some of water can be easily removed by the simple
evaporative processes and some cannot.
The amount of easily removable water ( unbound water )
is known as the free moisture content.
The moisture content of the water that is more difficult to
remove in practice ( bound water ) is the equilibrium moisture content. Unbound water
The unbound water associated with a wet solid exists as a
liquid and it exerts its full vapour pressure. It can be removed readily by evaporation.
Unbound water (During a drying process) is readily lost
but the resulting solid will not be completely free from water molecules as it remains in contact with atmospheric air that inevitably contains dissolved water.
Resulting solid is often known as air dry
Equilibrium moisture content
The moisture content of a solid under steady-state
ambient conditions.
Its value will change with the temperature and humidity
of the air, and with the nature of the solid. Bound water.
Part of the moisture present in a wet solid may be adsorbed
on surfaces of the solid or be absorbed within its structure to such an extent that it is prevented from developing its full vapour pressure and therefore from being easily removed by evaporation.
It is more difficult to remove than unbound water.
Adsorbed water is attached to the surface of the solid as
individual water molecules which may form a mono(or bi-) layer on the solid surface.
Absorbed bound water exists as a liquid but is trapped in
capillaries within the solid by surface tension. Moisture content (MC).
The moisture content of air is expressed as kg of water
per kg of ‘bone-dry’ (water-free) dry air.
An added complication to the drying process.
Drying air also contains moisture.
Many pharmaceutical have air-conditioning systems to
reduce the humidity of the incoming process air
Removing water from air is a very expensive process
MC
The moisture content of air is altered by changes:
Temperature
The amount of moisture taken up by the air
Relative humidity (RH)
Ambient air is a simple solution of water in a mixture of
gases and as such follows the rules of most solutions – such as increased water solubility with increasing temperature, a maximum solubility at a particular temperature (saturation) and precipitation of the solute on cooling (condensation, rain!). • Lower relative humidities can be quantified in terms of percentage relative humidity
• This is approximately equal to the percentage saturation,
which is: Percentage saturation It is the more fundamental measure but the expression ‘relative humidity’ is most commonly used.
This is because the amount of water required to saturate air
is itself dependent on temperature.
In ambient air, water is in solution in the air gases and in this
case its solubility increases with increasing temperature.
If the temperature of the air is raised whilst its moisture
content remains constant, the air will theoretically be capable of taking up more moisture and therefore its relative humidity falls.
Difference between moisture content and relative humidity
of air An additional complication during a drying process Both the temperature and moisture content of the drying air (and therefore its relative humidity) could change significantly.
This arises from two separate factors:
• Uptake into the drying air of evaporated water vapour from
the drying solid. If evaporation is high and vapour removal inefficient, the drying efficiency will rapidly fall
• The cooling of the supply air (and consequently the
product) as the air transfers latent heat to the wet solid.
This phenomenon is known as evaporative cooling.
If the cooling is excessive the temperature of the air may fall to a value known as the dew point.
Here the solubility of water in the cooler air is reduced to
such a point that it is exceeded and liquid water will condense and be deposited. Thank You For Your Attention !