BTE3481 (Separation Processes 1)
Lecture Outline
1. Drying principles:
a. Water in solids & gases;
b. Heat & mass transfer.
2. Dryers description & operations:
a. Vacuum-shelf dryer;
b. Rotary dryer;
c. Spray dryer;
d. Freeze dryer.
Recall: Overview of bioseparations
1. Drying Principles
What is drying?
The process of removing all or most of liquids by supplying latent heat to
cause thermal vaporization, i.e. a liquid is converted into a vapour.
Reasons for drying?
1. To prevent degradation of product due to chemical (e.g. deamidation or
hydrolysis) and/or physical (e.g. aggregation or flocculation) reactions
during storage;
2. Help in the preservation of products by preventing fungal or bacterial
growth (their enzymes may lead to product degradation).usually under
10% wt, microb will not grow;
3. Convenience in the final use of the product - it is often desirable that
pharmaceutical drugs be in tablet form;
4. More economical and convenient to store them in dry form rather than
frozen;
5. To reduce bulk & weight, therefore reducing the cost of transportation;
Typical pharmaceutical manufacturing process:
Drug
synthesis
Crystallization
Excipients
Milling
Granulation
Lubrication
Tabletting/
Encapsulation
Filtration
Packaging/
Storage/
Transport
Drying
Drying
Suspension
Spray
dryer
Wet solid
- removal of bound water.
Evaporative
dryer
- will not remove all moisture because
the solid equilibrates with the moisture
present in the air.
How water is held within biological solids?
Water contained
within solids
Unbound
water
-
Also called free water;
Mainly held in the voids of the solid;
Exerts its full vapor pressure;
Easily be removed by evaporation.
Magnified cross-section of a wet solid
Bound
water
- Water that is adsorbed on surfaces
of the solid (to form a mono- or bilayer) or trapped in capillaries within
solid structure;
- Cannot exert its full vapor pressure;
- Not easily lost by evaporation.
Relative humidity (RH) of air
The percentage RH is defined as:
Amount of water vapor in
air at a given temperature
x 100
Maximum amount of water vapor the
air could hold at the same temperature
100% RH means that at a given temperature, air has taken up water vapor until
it is saturated.
Moisture content of a wet solid can be expressed as g of water presents in 100
g of water-free or dry solid.
Similarly, moisture content of air can be expressed as g of water presents per
100 g of dry air.
The equilibrium moisture content of a solid exposed to moist air varies with the
RH, as exemplified by the equilibrium-moisture curves below:
The curves give valuable information about the water capacity of solids:
Water remained in solid at 100% RH = bound water
Unbound water = Water contained in wet crystal bound water
Example 1:
The wet antibiotic cefazolin sodium crystals contain 30 g of water per 100 g of
dry antibiotic. Determine the percentages of bound and unbound water in the
wet crystals.
Solution:
The equilibrium-moisture curve for the
antibiotic can be extrapolated to give a
water content of the solid at 100% RH:
Since water remained in solid at
100% RH = bound water;
Bound water for the antibiotic crystals
= 23 g/100 g dry solid
% bound water =
23 g/100g
x 100%
30 g/100g
23
= 76.7%
% unbound water = (100.0 76.7)%
= 23.3%
The properties of air (dry and moist) are provided by the humidity or
psychrometric chart:
Relative
humidity (%)
Dry bulb
temperature
Moisture content of air
(g/kg dry air)
Example 2:
Air at 1 atm and 25C with a relative humidity of 50% is to be heated to 50C
and then to be used in drying wet crystals of the antibiotic cefazolin sodium.
Determine the moisture content of the crystals after drying.
Solution:
In order to use the equilibrium-moisture
curve for the antibiotic to find the water
content of the crystals after drying (at
50C), requires the RH value at the
same temperature. This can be found
using the humidity chart:
Move from a point at a temp of 25C &
50% RH to a point at a temp of 50C,
keeping the moisture content constant.
By interpolation, the RH of the air is
read to be 13%.
25
Solution (continued):
From the equilibrium-moisture curve for the
antibiotic, the moisture content of the
antibiotic after drying (i.e. at 13% RH) = 8 g water/100g dry solids
13
Exercise 1:
Wet insulin crystals containing 32 g water per 100 g of dry insulin
need to be dried in air to a moisture level of 5 g water per 100 g of
dry insulin. Determine:
1. The percentage of bound and unbound water in the wet crystals
before drying;
2. The humidity of the air to accomplish the drying;
3. For drying with air at 20C, what should be the moisture content
of the air (g moisture/g dry air)?
Water content (g/100 g dry solid)
40
40
30
30
20
20
10
10
5
0
20 26
40
60
Relative humidity (%)
80
100
29
4
20
