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Drying: Sana I Nam Assistant Professor Faculty of Pharmaceutical Sciences, Gcuf

This document discusses drying in the pharmaceutical industry. It begins by defining drying and distinguishing it from evaporation. The key purposes of drying pharmaceutical products are preservation, improving characteristics like flow and handling properties, stability, and as the final stage of processing. Various theories of drying are described, including equilibrium relationships and rate relationships. Different types of dryers are classified, including static bed dryers and drum dryers used for dilute solutions and suspensions. Factors affecting the drying rate and important drying concepts are also outlined.

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0% found this document useful (0 votes)
94 views78 pages

Drying: Sana I Nam Assistant Professor Faculty of Pharmaceutical Sciences, Gcuf

This document discusses drying in the pharmaceutical industry. It begins by defining drying and distinguishing it from evaporation. The key purposes of drying pharmaceutical products are preservation, improving characteristics like flow and handling properties, stability, and as the final stage of processing. Various theories of drying are described, including equilibrium relationships and rate relationships. Different types of dryers are classified, including static bed dryers and drum dryers used for dilute solutions and suspensions. Factors affecting the drying rate and important drying concepts are also outlined.

Uploaded by

Rimsha Yousaf
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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You are on page 1/ 78

DRYING

SANA I NAM
ASSISTANT PROFESSOR
FACULTY OF PHARMACEUTICAL SCIENCES,GCUF
outline
what is drying?
Theories of drying
Drying of Solids
Classification of dryers
Fluidized Bed systems
Pneumatic systems
Spray dryer
Freeze drying

2
Introduction
Drying is the process of removal of small amount of liquid (water/volatile liq./moisture) by
application of heat and is accomplished by the transfer of a liquid from a surface into an
unsaturated vapour phase.
Drying and Evaporation are merely distinguishable by the relative quantity of liquid removed
from the solid.
Here are some differences between drying and evaporation
Drying --- solid quantity > liquid
Evaporation---solid quantity< liquid key point

3
4
Purpose of drying
In pharmaceutical technology, drying is carried out for one or more of the following reasons:
1. Preservation of drugs: Drying is necessary in order to avoid deterioration as it minimizes mold
& bacterial growth . A few examples are…
blood products, tissues undergo microbial growth
effervescent tablets
synthetic & semi synthetic drugs undergo chemical decomposition
2. Drying is the final stage of processing ,dried aluminium hydroxide ,spray dried lactose ,
powdered extracts
3. Improved characteristics: Drying produces materials of spherical shape, uniform size, free
flowing & enhanced solubility.
 Granules are dried to improve the flow & compression characteristics. These are essential for
production of tablets and capsules.
 Viscous & sticky materials are not free flowing, Drying modifies these characteristics

5
Purpose of drying
4- Improved handling:
Removal of moisture makes the material light in weight and reduces bulk. Thus cost of
transportation will be less & storage will be efficient.
 If moisture is present, size reduction of drugs is difficult.
5- stability:
Drying reduces the moisture content( moisture may lead to corrosion and decrease the
product or drug stability)

6
Factors affecting rate of drying
Particle size
 Nature of material
 Nature of moisture (bound/unbound)
 Surface area
 Initial and final moisture content
 Thickness of material bed
Temperature
 Amount of moisture

7
Important terms
Psychrometery
Humidity of gas
Loss on drying( LOD)
Equilibrium moisture content(EMC)

THE THEORY AND PTACTICE OF INDUSTRIAL PHARMACY BY LACCHMAN 8


Theory of drying
 In a wet solid mass water may be present in two forms;
1) Bound water: Bound water is the minimum water held by the material that exerts an
equilibrium vapour pressure less than the pure water at the same temperature.
2) Unbound water: It is the amount of water held by the material that exerts an equilibrium
vapour pressure equal to that of pure water at the same temperature.
Unbound water exists largely in the voids of solid thus in non- hygroscopic material all the
liquid is unbound water.

9
Theory of drying

10
Theory of drying
 Theory of drying can be discussed under two headings
◦ Equilibrium relationships
◦ Rate relationships
 Equilibrium relationships:
 Air of constant humidity and temperature is passed over wet material after…. long exposure
equilibrium is reached.
Equilibrium moisture content (EMC): It is amount of water which exerts vapour pressure
equal to the vapour pressure of atmosphere surrounding it.
Based on the conditions of temperature and humidity solid will either lose or absorb the
moisture

11
Theory of drying

Moisture in solid>EMC=desorption (lose water)


Moisture in solid<EMC=sorption (gain water)

12
Theory of drying
Free moisture content (FMC):
It is the amount of water that is free to evaporate from solid
FMC =Total water content – EMC

13
Theory of drying ( drying of solids)
Rate relationships:
Rate relationship is observed by considering a simple model which mimic the conditions of a
dryer.
 In this model wet slab of solid is considered and hot humid air is passed over it. The change
in weight is determined by weighing the slab at different time interval and following
calculations are made

14
Theory of drying ( drying of solids)

15
Theory of drying ( drying of solids)
From the data obtained by the above experiment graph is plotted by taking MC on x-axis and
drying rate on y-axis
the curve obtained is known as drying rate curve

Fig: period of drying

16
Theory of drying ( drying of solids)

17
Theory of drying ( drying of solids)

18
Theory of drying ( drying of solids)

19
Theory of drying ( drying of solids)

20
Theory of drying ( drying of solids)
When drying rate is equal to zero, starting at point E, the equilibrium moisture period begins
& solid is in equilibrium with its surroundings
After that continuing drying is a waste of time and energy
The curves may have different shapes for different levels of moisture ( can be observed
differently in amorphous and crystalline solids)
Classification of solids based on drying
1. Granular or crystalline type solids
2. Amorphous ,fibrous and gelatinous type solids
Amorphous more difficult to dry than granular or crystalline type solids & often requires use of
lower temperatures, reduced pressure and increased air flow

21
Theory of drying
Drying process involves both heat transfer and mass transfer operations.
 It can be understood more easily if attention is focused on the film of liquid at the surface of
material being dried
 The rate of evaporation of this film is related to the heat transfer by following equation;
dW/dθ=q/λ --------(1)
Where,
dW/dθ= rate of evaporation of water per hour
q= overall rate of heat transfer
λ= latent heat of vaporization of water

22
Theory of drying
The rate of diffusion of moisture into air stream is expressed by rate equation similar to
heat transfer where driving force is humidity difference.
The rate equation is given as;
dW/dθ= k'A(Hs-Hg) ----- (2)
Where,
k´= coefficient of mass transfer (it is not constant, but varies with velocity of passing air
stream)
A = area of evaporating surface
Hs = absolute humidity at evaporating surface
Hg = absolute humidity in passing air stream

23
Theory of drying
The coefficient of mass transfer k' is not constant the relationship is in the form:
k'=cGn ----- (3)
Where,
c= proportionality constant
G= rate of flow of air
n= fractional exponent, usually about (0.8)2

24
Theory of drying
After an initial adjustment period the rate of evaporation is equal to the rate of diffusion of
water and the rate of heat transfer so,

dW/dθ=q/λ= k'A(Hs-Hg) ----- (4)

If the overall rate of heat transfer is expressed as the sum of heat transfer by conduction,
convection and radiation eq. 4 is expanded to;
dW/dθ=(qk+qc+qr)/λ = k'A(Hs-Hg) ----- (5)
where,
qk, qc & qr are the rates of heat transfer by conduction , convection & radiation respectively

25
Theory of drying
The rate of drying may be accelerated by increasing any of the individual term in eq.(5)
The rate of conduction heat transfer ,qk, can be raised by reducing the thickness of drying
material.
The rate of convection heat transfer ,qc, can be increased by increasing the air flow rate and
by enhancing the temp. of inlet air.
The rate of radiation heat transfer ,qr , can be stepped up by introducing a high temp
radiating heat source into drying chamber.
coefficient of mass transfer, k´ , can be speeded by increasing the velocity of air.
 humidity difference ,(Hs-Hg), can be enhanced by dehumidifying the internal air.

26
Theory of drying

27
Classification of dryers

28
Classification of dryers

29
1- static- bed dryers

30
Dryers for dilute solution, suspension and
slurries
1- Drum dryer /Roller dryer/Film dryer
(static bed dryer --- continuous type)
Principle:
 heated hollow cylindrical drum is rotate on longitudinal axis, which is dipped into the
solution to make it dry.

31
Drum dryer /Roller dryer/Film dryer
Construction:
It consist of horizontally mounted hollow steel
drum of 0.75 to 1.5m diameter and 2m to 4m
length which is heated internally by steam &
rotated on its longitudinal axis.
Below the drum feed pan is placed in such a
way that the drum dips partially into the feed.
One side of the drum has spreader and on
other side knife is placed. The solution is carried
as a film on the surface of the dryer and dried to
form a layer. Dried material is removed from
the surface of drum with the help of a doctor
knife, in the form of flakes.
Storage bin is placed to collect the material

32
Drum dryer /Roller dryer/Film dryer

33
Drum dryer /Roller dryer/Film dryer
Drying process in drum dryer completes in less than one cycle so the time of contact of
material with drum is only 6 to 15 seconds
Advantages:
Quick method
Compact size
Suitable to heat sensitive substances
uses:
the products dried are milk products, starch products, iron salts, suspension of kaolin ,
suspension of zinc oxide, malt extracts and pigments.
Calcium panthothenate, streptomycin sulfate

34
Dryers for dilute solution, suspension and
slurries
2- spray dryer
( pneumatic dryer ----- continuous type)

35
Tray and Truck dryer
(static bed dryer --- batch type)
Most commonly used in pharmaceutical industry
Hot air oven
Principle:
In tray dryer hot air is continuously passed over wet mass. Heat transfer takes place
by forced convection.
 Construction:
It consist of rectangular chamber whose wall is insulated. Trays are placed in the
chamber according to need.
 trays have solid ,perforated or wire mesh bottom( added advantage of controlled
circulation)------line with paper----- as disposable tray

36
Tray and Truck dryer
Number of tray varies according to size of dryer
Large dryers can hold as many as 20 trays

37
Tray and Truck dryer

38
Tray and Truck dryer

39
Tray and Truck dryer
Working:
Wet solid is loaded into trays.
Trays are placed in the chamber.
 Fresh air is introduced through inlet which
passes through the heaters and heated up.
 The hot air is circulated by means of fans at 2
to 5 meter per second.
The water is picked up by air and moist air is
removed from outlet.
During the cycle of drying only 10 to 20 % of
fresh air is introduced and 80 to 90% air is
circulated back

40
Tray and Truck dryer

41
2- Moving bed dryers
Systems in which drying particles are partially separated so that they flow over each other
 motion may be induced by mechanical method
More rapid heat transfer and mas transfer that static bed

42
Turbo-Tray Dryers

43
Turbo-Tray Dryers

44
Turbo-Tray Dryers
https://youtu.be/-XpohB2hUoM

Turbo-tray dryer (1, shelves; 2, blades; 3,


heater; 4, fan rotors; 5, shelf and fan drive).

45
Pan dryers ( batch –type)

46
Pan dryers

https://youtu.be/vCIPGKmFSR0

47
Pan dryers

48
3- Fluidized bed dryers
 systems in which the solid particles are suspended in an upward moving gas stream
particles are lifted and fall back in a random manner so that the resultant mixture of gas and
solid behaves like a boiling liquid
Excellent gas solid contact
Better heat and mass transfer than static and moving bed dryer
Designed both in batch and continuous type
most widely used technique for drying pharmaceutical powders and granulation

49
Fluidized bed dryer
Principle of Fluidization:
 The principle of operation of fluidized systems are based on the fact that if a gas is allowed
to flow through a bed of particulate solids at velocity greater than the settling velocity of the
particles and less than the terminal velocity for pneumatic conveying , the solids get partially
suspended in the stream of upward moving gas.
The gas stream ( air / inert gas) negates the gravitational pull due to weight of particles to
enable the suspended state of the solid.
The resultant mixture of solids and gas behaves like a liquid and thus solids are called
Fluidized.

50
Fluidized bed dryer
Construction:
Fluidized bed dryer is available in two forms;
1. Vertical FBD
2. Horizontal FBD
Vertical FBD
 The dryer is made up of Stainless steel or plastic.
 A detachable perforated bowl is placed at the bottom of the dryer which is used for charging and
discharging of material.
 A fan is mounted in the upper part for circulating hot air.
Fresh air inlet, pre-filter and heat exchanger are connected serially to the required temperature.
 Bag filters are placed over bowl for recovery of fines

51
Vertical FBD
https://youtu.be/dwHFKyf_ZLc
https://youtu.be/vz4audqdx5o

52
Vertical FBD
Working:
The wet granules to be dried are placed in detachable bowl and bowl is placed into the dryer.
Fresh air is allowed to pass through pre-filter which subsequently gets heated by passing
through heat exchanger.
Hot air is passed through the perforated bottom of the container containing granules to be
dried and fan is allowed to rotate.
The granules rise in the container because of high velocity gas and later fall back in random
motion
The hot gas surrounds every granule to completely dry them.

54
Vertical FBD
The air leaves the dryer by passing through bag filter.
 The entrained particle remain adhere to the inside surface of bags.
 Periodically the bags are shaken to remove the particles.
 The material is collected after some time so as to reach the ambient temperature.
Drying is achieved at constant rate.
The residence time for drying is about 40 min.

55
Horizontal FBD
Continuous Type Horizontal Vibrating Conveyor Fluid Bed Dryer
Construction
 width---------12 -57 inch
Length--------- 10- 50 feet
Bed depth----- 3 inch
Dryer capacity --- limited to retention time by conveying speed
Pharma . Operation capacity range is 1-2 tons/hr.

56
Horizontal FBD
Working:
Heated air is introduced into a chamber below the vibrating conveying deck and passes up
through the perforated or louvered conveying surfaces ---through fluidized bed of solids ----
into an exhaust hood
Fluidized bed of uniform density and thickness is maintained in any given drying zone by the
vibrations
Dryer is divide into several different zones with independent control of airflow & temp.
( max. drying rate in each stage)

57
Horizontal FBD
Residence time in any drying zone is dependent on
1. Length of the zone
2. The frequency and the amplitude of the vibration
3. Use of dams
These unit supplies 60-80 % heat necessary for drying
https://youtu.be/3r4yj0QEGUI

58
Horizontal FBD

59
Fluidized bed dryer
ADVANTAGES:
 It requires less time to complete drying i.e.,20 to 40 mins . It is 15 times faster than tray dryer
 It needs less labour cost.
thermal efficiency is 2 to 6 times than tray dryer.
Available in different sizes ( 5 kg to 200kg.)
 Hot spots are not observed in the dryer, because of its excellent mixing and drying capacities.
 It facilitates the drying of thermo labile substances, since the contact time is short.
The free movement of individual particles eliminates the risk of soluble material migrating as may
occur in static bed.
 mixing efficiency is high so can be used for mixing

60
Fluidized bed dryer
Disadvantages:
 Some organic material may develop electrostatic charge so requires efficient earthing of
dryer
Due to attrition fines are observed in large quantity

61
Fluidized bed dryer
Uses:
1. For drying granules.
2. It can be used for drying, mixing and granulation process. ( FB granulator)
oDry ingredients are placed in chamber and fluidized while the granulating liquid is sprayed
into the bed causing the particles to agglomerates into granules. After the granulating cycle
drying is carried out by fluidizing hot air.
3.It is modified for coating
oFluidized bed coaters are used widely for coating of powders, granules, tablets, pellets, beads
held in suspension by column of air.

62
Fluidized bed dryer
oThe three types (Top spray, Bottom spray, Tangential spray) are mainly used for aqueous or
organic solvent-based polymer film coatings.
oTop-spray fluidized bed coating is used for taste masking, enteric release and barrier films on
particles/tablets.
oBottom spray coating is used for sustained release and enteric release .
oTangential spray coating is used for SR and enteric coating products.

63
4-Pneumatic dryers
 systems in which drying particles are entrained and conveyed in a high velocity gas stream
Further improve on fluidized bed with no channeling or short circuiting of gas flow through
a bed of particles
Each particle is completely surrounded by an envelope of drying gas
Extremely rapid heat and mass transfer
 short drying times

64
Spray dryer
Solutions, slurries and thin pastes of drugs can be spray dried by contact with hot air
Unique as involves both particle formation and drying
Principle:
 In spray dryer the fluid to be dried is atomized into fine droplets which are thrown radially
into moving stream of hot gas.
The temperature of the droplets is immediately increased and fine droplets get dried
instantly in the form of spherical particles.

65
Spray dryer
Construction:
1. Feed delivery system
2. Atomizer
3. Heated air supply ( inlet air filter, Supply Fan, air heater)
4. Drying chamber ( made of stainless steel with a conical bottom)
5. Solid gas separator
6. Product collection system( cyclone separator, filter bag ,scrubber)

66
Spray dryer

67
Types of spray dryers
The different spray drying systems are
1. open cycle
2. closed cycle
3. semi closed cycle
Open cycle systems :
The majority of the industrial spray dryers handle aqueous feeds and use this system.
Air for drying is drawn from atmosphere and the exhaust drying air is discharged to
atmosphere Before discharging , the exhaust air is cleaned using combinations of bag filters,
and scrubbers.

68
Types of spray dryers
Closed cycle spray dryers
used to handle flammable solvents, highly toxic products and oxygen sensitive products to avoid
atmospheric pollution and/or to establish complete recovery of the evaporated solvent.
is based upon recycling and reusing the gaseous drying medium, which usually is an inert gas such
as nitrogen.
Drying chambers are incorporated with a cyclone/bag filter and solvent vapour condenser
Semi-closed cycle spray dryers
classified into
either the partial recycle mode (recycling of up to 60% of the exhaust air as inlet air to the dryer,
for effective heat utilization)
 or the self-inertising mode

69
70
Spray dryer
Spray drying consists of 4 process stages.
1-First stage
The liquid feed introduced into drying chamber through the atomizer either by gravity or using
suitable pump.
The atomization stage must create a spray that when in contact with the drying medium creates
optimal conditions for evaporation leading to a dry wall operation and discharging a dried product
of the required properties from the drying chamber
The are 3 basic designs of atomizers, defined by the source of energy utilized in the droplet
formation process:
1. rotating wheel or spinning disc atomizers(centrifugal energy )
2. pneumatic atomizers (kinetic energy )
3. pressure atomizers (pressure energy )

72
Spray dryer
1-spinning disc atomizer

The liquid is fed to the center of a rapidly rotating disc(3000 to 50,000 rpm) where the
centrifugal force breaks the fluid up into droplets
Wide utilization in pharmaceuticals as can handle all types of liquid feed ( high viscous liquids
& slurries that would clog other atomizer)
2- Pneumatic atomizers
 the liquid feed is broken up into droplets by a high velocity jet of air or other gas
Used to produce small particles & for spraying more viscous liquids than can be handled by
pressure nozzles

73
Spray dryer
2- Pressure atomizers
Liquid feed is delivered under high pressure ( up to 7000 pounds / sq. inch) and is broken up
on coming into contact with air or by impact on another fixed plate or jet.

Atomizers are selected according the droplet sizes to be produced in order to meet the
powder Specifications
Atomization device ------------------------ Median Droplet Size (μm)
spinning disc atomizers------------------- 10 – 200
Pneumatic nozzle --------------------------- 5 – 100
Pressure nozzle ------------------------------ 30 – 350

74
Spray dryer
2-second stage
 involves the spray-air contact, mixing and droplet/particle flow
 the three basic flow design are
1. Co-current flow
2. Countercurrent flow
3. mixed flow

75
Spray dryer

76
Spray dryer
3- Third stage
combines drying and particle formation
Evaporation of the solvent takes place immediately after contact between spray droplets and the
drying air. Diffusion of solvent from within the droplet maintains saturated surface conditions,
resulting in a constant drying rate.
4- fourth stage
Particles are dried and fine one are collected in a cyclone separator. ( primary collector)-----
cyclone product
Product(coarser in size) that reaches the wall of chamber is removed from the bottom of the
chamber ---chamber product
Final dried product is a mixture of both chamber and cyclone product
 All these processes are completed in few seconds.

77
Spray dryer
Process parameter such as inlet and outlet temp. of the drying medium and the atomization
pressure influence the physicochemical properties of produced powders.
The characteristics of the spray dried powder can be controlled, and the powder properties
can be maintained constant throughout the continuous operation.

78
Spray dryer
 Advantages
1. The dried powder will have a uniform particle size and shape.
2. Because of good flow properties, the spray-dried powder can be easily compressed into the
form of tablets.
3. It is useful in the coating and encapsulation of both solids and liquids.
4. Labor cost is low since the material is dried in a single operation with no handling.
Disadvantages
1. Solid materials cannot be dried.
2. The equipment is very costly and bulky.
3. Since the equipment is bulky, cleaning is time consuming.
4. There is a lot of heat wasted.

79
Spray dryer
Application
1. for the drying of liquid materials like emulsion, suspension, solution, slurries, thin pastes,
etc.
2. to dry materials that are sensitive to heat or oxidation
3. The liquid feed is dispersed into droplets, which are dried in seconds because of their high
surface area and intimate contact with the drying gas.
4. The product is kept cool by the vaporization of the enveloping liquid, and the dried product
is kept from overheating by rapid removal from the drying zone.
5. The improvement in flow and reduction of air entrapment make the spray-dried material
suitable for use in the manufacturing of tablets and capsules.

80

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