Course Contents of Prof. Dr.

Aamir Ijazs Portion

Course Contents of Drying
Introduction
General Principles
Rate of Drying
Time of Drying
Drying Periods

Time of Drying
Constants Rate of Drying Period
First Falling Rate Period
Second Falling Rate Period

Total Time of Drying

Course Contents
CourseofContents
Prof. Dr.ofAamir
Drying
Ijaz Portion
Capillary Theory of Drying
Principal of the Theory
Drying of a Granular Material according to the capillary theory

Freeze Drying
Drying Equipment
Classification and selection of dryers
Tray or shelf dryers

Tunnel dryers
Rotary dryers
Design considerations
Drum dryers

Spray dryers

Course Contents of Prof. Dr. Aamir Ijaz Portion

The Drying of Gases

Drying

Drying

Crystallization

Course Contents of Crystallization

Importance of Crystal Size
Crystal Geometry
Crystallographic systems
Invariant crystals
Crystal size and shape factors.
Principals of crystallizations
Purity of Product
Solubility Vs. Temperature
Equilibria yields
Phase Equilibrium Diagram
Phase Equilibrium Diagram for MgSO4 - H2O
Yields
Enthalpy Balances
Super-saturation
Units of Super-saturation
Temperature difference as a potential

Course Contents of Crystallization

Nucleation
Origins of Crystals in Crystallizers
Primary Nucleation
Homogenous
Equilibrium
Heterogeneous Nucleation
Secondary Heterogeneous Nucleation
Crystal Growth
Individual and overall growth coefficients
Mass transfer coefficients
Surface-growth coefficients

Course Contents of Crystallization

The L Law of Crystal Growth
Crystallization Equipments
Variations in Crystallizers
Vacuum crystallizers
Draft-Tube-Baffle Crystallizers
Yield of Vacuum Crystallizers

Application of Principles to design

Increase the crystal size
Contact Nucleation in Crystallizers
Crystallization of ORGANIC Chemicals
Crystallizations from Melts

Text Books:
Chemical Engineering, Vol. 2, by Coulson &
Richardsons
Unit Operations of Chemical Engineering by
Warrant L. McCabe d, Julian C. Smith, Peter
Harriott
Reference Books:
Introduction to Chemical Engineering, by Walter L.
Badger & Julius T. Banchero

Difference between Drying and

Evaporation
The term drying usually infers the removal of relatively small
amounts of water from solid or nearly solid material, and the term
evaporation is usually limited to the removal of relatively large
amount of water from solutions.
In drying processes the major emphasis is usually on the solid
product. In most cases drying involves the removal of water at
temperatures below its boiling point, whereas evaporation means
the removal of water by boiling a solution.
Another distinction is that in evaporation the water is removed
from the material as practically pure water vapor, mixed with other
gases only because of unavoidable leaks. In drying, on the other
hand, water is usually removed by circulating air or some other gas
over the material in order to carry away water vapor; but in some
drying processes no carrier gas is used.

Difference between Drying and

Evaporation
Strictly speaking drying processes all cases of the removal of small
amounts of water from gases or liquids. For example, air is
sometimes dried for iron blast furnaces by passing it over
refrigerating coils which removes water as either liquid water or ice.
Organic liquids or gases are dried by passing them through a bed of
solid adsorbent, such as silica gel or activated alumina. Occasionally
they may also be dried by countercurrent contact with strong
calcium chloride brine or caustic soda. In the past batches of organic
liquids have been dried by adding calcium carbide.

Introduction to Drying Theory

The process of drying must be approached from two
points of view: first, the equilibrium relationships and,
second, the rate relationships. Thus, there is always heat
transfer to the materialin variety of ways. In addition,
there are the mechanisms by which moisture (either as
liquid or vapor) travels from the interior of the solid to the
surface, Since a wide variety of materials are encountered
in drying operations, and many of these may be complex
systems, such as soap, wood, textiles, etc., it is not
surprising that the equilibrium relationships may be more
complex than those encountered in previous operations.
And just as these equilibrium relationships are
complicated, it is also to be expected that, as the
mechanism by which water travels through the solid
varies, the form of rate equations may also vary.

It may be noted that J=kt/l2, where k is a constant, t the time in ks and 2l is the thickness of the sheet of
material in millimeters.

Tray Dryer

They are used for lumpy or pasty in small quantity. The material is spread
uniformly over the trays and the hot air is passed parallel and over the trays. The
velocity of air varies from 1 to 10m/s and 80 to 90% of air passed is re circulated.
When drying is complete, the cabinet is opened and a new set of trays is
introduced.
In case when the material is granular, it is placed at the bottom of each tray, which
takes the form of screen. Hot air drying is passed through the permeable bed and
drying time is short due to large surface area. The drying rate is 0.2 2 kg
water/h.m2 surface and Thermal efficiency: is 20-25%.
Advantages:-

No loss of product
Low space requirement
Ease of cleaning

Disadvantages:

Long drying time

High lab our cost

They are mainly used for granular solids and may be heated directly or
indirectly. It consists of hollow inclined rotating cylinder. Feed is introduced at
the upper end and moves through the shell due to rotation, head effect and
slope of cylinder. Dried product is discharged at the lower end.
In case of direct heating hot gas is passed counter currently over the material
and in case of indirect heating, heat is transferred through the wall of the
cylinder. The drying rate is 10-50kg water/h m3 shell volume and thermal
efficiency is 50 80 %.
Advantages: Good gas contacting
Moderate drying time
High thermal efficiency
Low capital cost
Disadvantages:
Difficult scaling
Product builds up on interior walls
High structural load
Non-uniform residence time

They are used for slurries, fine suspensions and for solutions. They consist of one or more
metal rolls heated internally by steam. Material is dried outside the roll and is scrapped by
knife scrapper from slowly revolving roll. Drum pertly acts as an evaporator and partly as
dryer. They can no be used for salt solutions with limited solubility and for abrasive
material that have tendency to settle out and create high pressure blew the drum.

Pneumatic Dryers
It is used for the material which is in the state of fine division to increase surface
per unit volume. A pneumatic dryer is shown in figure. Wet material is introduced
into dryer by means of some from of mechanical feeder to give short length of
material, such as 5-10 mm. Hot gases from furnace are introduced from the bottom
which picks up the particles and carry them to column. Evaporation causes drying
of material. Hot gases are discharged out from the top and the dry product is
collected at the bottom. The contact time b/w gases and particles is small, and the
particles temperature do not exceed from the temperature of the hot gases.
Thermal and power requirements are 4.5 MJ/kg and 0.2 MJ/kg respectively

Applications of Fluidized Bed Dryers: At large scale they are used for drying of

Fertilizers

Plastic materials

Foundry sand

Inorganic salts

At small scale they are used for drying of tablet granulations are pharmaceuticals.
Dryer evaporative capacity varies from 0.2 0.3 kg/s m2 grid area. Specific air rates are
0.5 -2 kg/s m2 grid are and take total energy demand is 2.5-7.5 MJ/kg moisture
evaporated.

Freeze Dryer:In this process the material is first frozen and then dried by
sublimation in a very high vacuum, 10-40 N/m2 at a
temperature for 240 260 K. During the sublimation of ice a
dry surface layer is left. During the sublimation the
temperature is so maintained that highest vapor pressure of
water vapors is obtained without melting the material.
During this stage 95% Drying is completed and then
remaining water is removed by increasing the temperature to
ambient temperature. A typical freeze dryer is shown in fig
16.35. Heat is supplied to plates which interleave with trays
containing the product either by conduction or radiation.
Sublimed moisture condenses on refrigeration coil, located at
the far end of chamber.
Advantages:
(i) Process is carried out at low temperature
(ii) It avoids surface hardening
(iii) Useful for heat sensitive materials
Application: Used for drying of
(i)
Penicillin and other biological materials
(ii)
Foodstuffs
(iii)
Meat and vegetables.

Drying
Introduction A rigid definition of drying that shall sharply differentiate it from
evaporation is difficult to formulate. The term drying usually infers the removal of
relatively small amounts of water from solid or nearly solid material, and the term
evaporation is usually limited to the removal of relatively large amount of water
from so1utions. In drying processes the major emphasis is usually on the solid
product. In most cases drying involves the removal of water at temperatures
below its boiling point, whereas evaporation means the removal of water by
boiling a solution. Another distinction is that in evaporation the water is removed
from the material as practical1y pure water vapor, mixed with other gases only
because of unavoidable leaks. In drying, on the other hand, water is usually
removed by circulating air or some other gas over the material in order to carry
away water vapor; but in some drying processes no carrier gas is used. The above
definitions hold in many cases, but there are also notable exceptions to every one
of them. In the last analysis, the question of whether a given operation is called
evaporation or drying is largely a question of common usage. Thus the removal of
water from a solution by spraying it into a current of superheated steam fulfills
most of the definitions of evaporation; but, because this is done in an apparatus
exactly like the apparatus in which true drying operations are carried out, it is
customarily considered a drying operation..

Drying
In drying, on the other hand, water is usually removed by circulating air
or some other gas over the material in order to carry away water vapor;
but in some drying processes no carrier gas is used. The above
definitions hold in many cases, but there are also notable exceptions to
every one of them. In the last analysis, the question of whether a given
operation is called evaporation or drying is largely a question of
common usage. Thus the removal of water from a solution by spraying it
into a current of superheated steam fulfills most of the definitions of
evaporation; but, because this is done in an apparatus exactly like the
apparatus in which true drying operations are carried out, it is
customarily considered a drying operation..

A strict interpretation of the first three sentences of this chapter will

eliminate from consideration as drying processes all cases of the removal of
small amounts of water from gases or liquids. For example, air is sometimes
dried for iron blast furnaces by passing it over refrigerating coils which
remove water as either liquid water or ice. Organic liquids or gases are dried
by passing them through a bed of solid adsorbent, such as silica gel or
activated alumina. Occasionally they may also be dried by countercurrent
contact with strong calcium chloride brine or caustic soda. In the past batches
of organic liquids have been dried by adding calcium carbide. These are called
drying processes in ordinary usage but are somewhat too specialized to treat
in this book.
This chapter will first classify dryers and describe typical forms. Then the
basic course of the drying process will be discussed. The application of such
theory to the actual calculation of dryer size can be attempted only the case
of one type. Reference to any discussion of dryer design in the literature is
almost monotonous in the repeated statements that This class of dryers can
be designed only by actual tests of the material in question in a dryer of the
type involved. Finally a few general principles applicable to most dryers will
be discussed.

This process is suitable only for the drying of thin films on the surface of the
material to be dried and never for cases where the water (or solvent) to be
removed penetrates the solid. It is a very expensive dryer.
Dielectric heating is accomplished by passing the object to be dried through a
very-high-frequency (2 to 100 X 106 cycles) electrostatic field.
This generates heat uniformly throughout the object. Its only important 4 field
is in polymerizing the resin that forms the bond between layers of
plywood, which is scarcely a drying operation. It has been suggested for drying
but
is
far
too
expensive
for
any
important
applications.
Vaporization from ice has been applied in special cases. The vapor pressure of
water from pure ice is 4.6 mm. Consequently, if a substance containing water is
exposed to a vacuum of less than this amount, it will freeze and water will
sublime
from
solid
ice.
If
substances
are
in
solution,
- the pressure at which vaporization takes place will be lower. The method is
slow and expensive and calls for very large equipment. Its usefulness is
practically confined to the drying of biological products that must not be
exposed to elevated temperatures or oxidation. It has been suggested for fruit
juices.

10-19. Introduction to drying theory. The process of drying must be

approached (as in other operations discussed in this book) from two points
of view: first, the equilibrium relationships and, second, the rate
relationships. Operations already discussed are of some help. Thus, there is
always heat transfer to the materialin variety of ways, but all
understandable from previous sections. The vaporization of water from a
surface into a stream of air was discussed in Chap. 8. In addition to these
there are the mechanisms by which moisture (either as liquid or vapor)
travels from the interior of the solid to the surface, Since a wide variety of
materials are encountered in drying operations, and many of these may be
complex systems, such as soap, wood, textiles, etc., it is not surprising that
the equilibrium relationships may be more complex than those encountered
in previous operations. And just as these equilibrium relationships are
complicated, it is also to be expected that, as the mechanism by which water
travels through the solid varies, the form of rate equations may also vary.
A review of drying apparatus in the previous pages shows that, while some
dryers (vacuum drum dryers, for instance) dry with the material in contact
with water vapor alone, the majority of methods use air as a carrier of the
water vapor. The following discussion will be confined to these last methods.

10-20. Equilibrium moisture content. Suppose that a wet solid is brought

into contact with a stream of air, of constant temperature and humidity, in
such amounts that the properties of the air stream remain constant, and
that the exposure is sufficiently long for equilibrium to be reached. In such a
case the solid will reach definite moisture content
Moisture content may be expressed either on the wet basis, i.e., pounds of
moisture per pound of solid plus moisture, or on the dry basis, i.e., pounds
of moisture per pound of moisture-free solid. The dry basis is more
convenient from the standpoint of ricii1ation (see a similar choice for
humidity, Sec. 8-10) and will be used throughout the remainder of this
chapter that will be unchanged by further exposure to this same air. This is
known as the equilibrium moisture content of the material under the
specified conditions. For many materials the equilibrium moisture content
depends on the direction in which equilibrium is approached. A different
value is obtained according to whether a wet sample is allowed to dry
(desorption) or whether a dry sample is allowed to adsorb moisture
(sorption). For drying calculations only the desorption value should be used.

If the material contains more moisture than the equilibrium value, it will dry
until its moisture content reaches the equilibrium value on the desorption curve.
On the other hand, if the material is dryer than the equilibrium value and is
brought into contact with air of the stated temperature and humidity, it will
adsorb water until it reaches the equilibrium point on the sorption curve. For air
of zero humidity, the equilibrium moisture content of all materials is zero.
For any given percentage humidity, the equilibrium moisture content varies
greatly with the type of material. For example, a nonporous insoluble solid will
have an equilibrium moisture content of practically zero, as far as the buld of the
solid is concerned, for any humidity and temperature. On the other hand,
certain organic materials of fibrous or colloidal.
Some typical equilibrium moisture curvesare given in Fig. 10-15. These are
merely sample curves and must not be considered to hold for all varieties of the
substance described. So, for instance, curve 7 is not general for all samples of
leaf tobacco, but holds only for the particular sample tested. Relative humidity is
used as the abscissa for Fig. 10-15, since this is the customary form in which
equilibrium-moisture-content curves are given. The relative humidity (see
footnote, Sec. 8-10) defined as the ratio of the partial pressure of water vapor in
the gas phase to the vapor pressure of liquid water at the same temperature,
and is usually expressed as a percentage.

The equilibrium moisture content of a solid decreases with an increase in

the air temperature. Figure 10-16 shows the effect of temperature on the
equilibrium moisture content of raw cotton,2 Temperatures are in degrees
Fahrenheit.
1.
International Critical Tables, vol. 2, pp. 322-325.
2.
The curves presented for raw cotton are based on the
experimental data reported by J. G. Wiegerink, J. Research Nat. Bur.
Standards,
24:
645664
(1940),
as
recalculated
by R.K Toner, C. F. Bowen, and J. C. Whitwell, Textile Research J., 17:7 7-18
(1947).
will have an equilibrium moisture content of practically zero, as far as the
bulk of the solid is concerned, for any humidity and temperature. On the
other hand, certain organic materials of fibrous or colloidal structure such
as wood, paper, textiles, soap, and leather have equilibrium moisture
contents that vary regularly and through wide ranges as the humidity and
temperature of the air with which

10-21. Bound, unbound, and frees water. If the equilibrium curves of Fig. 10-15
are continued to their intersection with the axis for 100 per cent humidity, the
moisture content so defined is the least moisture that this material can contain
and still exert a vapor pressure as high as that exerted by ordinary liquid water
at the same temperature.2 If such a material contains more water than that
indicated by this intersection, it can still exert only the vapor pressure of water
at the given temperature. This makes possible a distinction between two types
of water held in a given substance. The water up to the lowest concentration
that is in equilibrium with saturated air (given by the intersection of the curves
of Fig. 10-15 with the line for 100 per cent humidity) is called bound water,
because it exerts vapor pressure les than that of liquid water at the same
temperature. Substances containing bound water are called hygroscopic
substances.
Bound water may exist under several conditions. Liquid water in very fine
capillaries will exert an abnormally low vapor pressure because of high concave
curvature of the surface; moisture in cell or fiber walls may suffer a vapor
pressure lowering because of solids dissolved in it; water in natural organic
structures is in physical and chemical combination, the nature and strength of
which vary greatly with the nature and moisture content of the solid. Unbound
water, on the other hand, exerts its full vapor pressure.

Free moisture content is the moisture in a sample above the equilibrium

moisture content. Since the equilibrium moisture is the limit to which the
material can he dried under a specific set of conditions, it is the moisture above
this point that can be removed by the drying processnot the Eotal moisture
content. So, for instance, a sample of wool for which curve 2 of Fig. 10-15 is valid
has an equilibrium moisture content of 12.5 per cent in contact with air of 50 per
cent relative humidity and 25C. if a given sample of wool contains 20 per cent
moisture, all this 20 per cent is not removable by drying in a current of air at 25C
and 50 per cent humidity. Only 20 12.5 or 7.5 per cent is so removable, and
this is the free moisture of this sample for these conditions.
10-22. Rate-of-drying curves. The experimental data obtained in an
investigation of the effect of external conditions on the drying of a solid by air
are usually the moisture content of the solid as a function of time under constant
drying conditions. The term constant drying conditions means that the air
velocity, temperature, humidity, and pressure are maintained constant and that
the outlet air conditions are substantially the same as those at the inlet.
Differentiation of the data either graphically or numerically gives the drying rate,
which may be plotted vs. either free moisture content or Lime. A plot of the
drying rate per unit area of drying surface vs. free moisture content is the form
most often used. Figure 10-17 illustrates such a curve for the drying of sand. r1he
sand was held McCrvacly and McCabe, Trun.s. A in. 1nt, Citem. Enjrs., 29: 131
160 (1933).

In a tray whose bottom and sides were insulated, and heated air at constant
humidity was blown over the surface of the tray. The time required for a
predetermined loss in weight was read, and this was repeated for successive
changes in weight. The temperature near the surface of the solid, as measured
by a thermocouple, is also shown.
The drying-rate curve (Fig. 10-17) may be divided into a constant-rate period,
such as the portion AB, and the falling-rate period BD.* The free moisture
content 1 at point B is called the critical moisture content. The moisture
content plotted here is the average moisture content of the solid, since at any
time during the drying operation the actual local moisture content is not
uniform throughout the solid but varies with position. The drying periods
described do not occur in all cases. If the desired moisture content is larger
than the critical moisture content, only he constant-rate period will occur. In
other cases, for example the drying of soap, the initial moisture content is
lower than the equilibrium moisture content and the entire drying operation
takes place in the falling period.

Figure 10-17 is only one of the types of drying-rate curves that may be
obtained and represents the case of a granular solid composed of nonporous
particles. Figure 10-18 shows other typical drying-rate curves that may be
obtained. These curves are for the air drying of slabs, with the air flowing
past both surfaces of the slab. The form of the drying-rate curve depends on
the structure and composition of the solid and on the mechanism by which
moisture moves within the solid.
* In most cases there is an unsteady-state period that precedes the constantrate pe nod. During this period conditions in the solid are changing from the
values at which the solid was introduced into the dryer to those
corresponding to the constant-rate period. This unsteady-state period has
not been shown in Fig. 10-17. Usually, the unsteady-state period is only a
small fraction of the constant-rate period.