Drying

Shadeed Gad, B.Sc. (Pharm.), M.Sc., PhD., M.P.S.E.

Drying

Introduction Purpose Moisture content of a material Equilibrium moisture content Bounded moisture Free moisture

Introduction

Drying means reduction in moisture content to acceptable final value. It is the last operation in a manufacturing process, and is carried out immediately prior to packaging or dispatch. Adjustment and control of moisture levels by drying is important in the manufacture and development of pharmaceutical products. Also drying may be carried out to: (A) Improve handling characteristics, as in bulk powder filling and other operations involving powder flow. (B) Stabilized moisture -sensitive materials, such as aspirin and ascorbic.

The equilibrium moisture content (EMC)

If a material is exposed to air at certain temperature and humidity, the material will either lose or gain water until an equilibrium condition is established (EMC). A non-porous insoluble solid, such as talc, zinc oxide, or sand, will have an EMC approaching zero for all humidity values and temperatures, but many organic materials, such as wood, textiles, and leather, show variation of EMC

The moisture may be present n the following two forms:

(a) Bound moisture: water may be retained in small capillaries, adsorbed on surfaces, or in solution in cell walls. (b) Free moisture: This is the water that is in excess of the EMC.

Notes

In drying practice, two different kinds of solids are found: porous or non- porous. Between these two extremes, many solids are intermediate. The bed of solids to be dried may by static or moving. The rate of drying will consequently vary and will depend upon both the type of solid and the condition of the bed.

Porous particles

Non porous particles

Rate of drying

1- rate of drying in static beds

a) static beds of non porous solids

AB, Constant rate Period rate governed by diffusion from the surface through the stationary air film in contact with it., so it is affected by the particle size of the solids. During this period, liquid must be transported to the surface at a rate sufficient-to maintain saturation. point B is the "Critical Moisture Content", (CMC), and a linear fall in the drying rate, occurs with further drying. BC First falling Rate Period". At and below the CMC, the movement of moisture from the interior is no longer sufficient to saturate the surface. As drying proceeds, moisture reaches the surface at a decreasing rate and the mechanism which controls its transfer will influence the rate of drying.

For any material, the critical moisture content, CMC, decreases as the particle size decreases. CD "Second Falling Rate Period" is controlled by vapour diffusion a factor which will be largely independent of the conditions outside the bed but affected by the particle size due to the latter's influence on the dimensions of pores and channels. During this period, the surface temperature approaches the temperature of the drying air.

If the soluble matter forms a skin or gel on drying rather than a crystalline deposit, a different curve is obtained. The constant rate period is followed by a continuous fall in the drying rate in which no differentiation of first and second falling rate periods can be made. During this period, drying is controlled by diffusion through the skin which is continually increasing in thickness. Soap and gelatine are materials which behave in this way.

b) static bed of porous solids

2- rate of drying in moving beds

drying rates is 10-20 times greater as fresh solids are continually exposed to the hot surface. The heat treatment received by the solid will be more uniform. it is possible to project air upwards through the bed at a velocity high enough to fluidize the particles. Or , the material may be mechanically subdivided and introduced into the drying stream. Both methods give high drying rates due to high interfacial constant between the drying surfaces and the air stream. Fluidized-bed dryers and spray dryers, respectively, use these principles.

Equipments

Equipment
Batch Dryer
Tray Or Shelf Dryer
Turbo Shelf Dryer

Continuous Dryer

Vacuum Tray Dryer Tumbling Dryer

Drum Dryer Spray Dryer

Flash Dryer (Pneumatic Dryer)

Freeze Dryer
Batch And Continuous Dryer Fluidized Bed Dryer

Rotary Dryer

Infra Red Dryer

a) Batch dryers

1- Tray or shelf dryer

2- Vacuum tray dryer

3- Tumbling dryer 4- Freeze dryer

Tray or shelf dryer

Tray or shelf dryer

used for granular materials. They operate by passing hot air over the surface of the solid which is spread over trays arranged in racks inside a chamber, most commonly rectangular in shape, whose walls contain suitable heat-insulating materials. Such hot-air ovens are probably the simplest and cheapest dryers. On small unites air is heated electrically, larger units may use steam-heated.

The advantages of the hot air oven are its low initial cost. With the exception of dusty solids, materials of almost any other physical form may be dried. However, the disadvantages are: A large floor space is required for the oven and for trayloading facilities. Labour costs for loading and unloading the oven are high. Long drying times, (24 hours), are necessary. Solvents can only difficultly be recovered from the drying air. Unless carefully designed, variable temperature from location to location (7 C) may occur.

Note

If the material is of suitable granular form, drying times may be reduced to an hour or less by passing the air downwards through the material laid on mesh trays. The oven in this form is called a Batch Through Circulation Dryer.

Vacuum Oven

Vacuum tray dryers, is bigger than laboratory vacuum oven, offer an alternative method for drying small quantities of material at a reduced temperature. But it is expensive due to the use of vacuum pump. So they only used when a definite advantage over the hot-air oven is secured, such as low temperature drying of thermolabile materials, The recovery of solvents from the bed, or The exclusion of air or oxygen during drying.

The system consists of a condenser, receiver, and dry vacuum pump. The condenser is used as moist air is highly destructive to vacuum pumps. The receiver used to drain condensed moisture without need to shut off then re-operate the vacuum pump.

A vacuum tray dryer generally consists of a rectangular iron shell, which contains a number of hollow shelves. Heat is usually supplied by passing steam, or hot water, through these hollow shelves, upon which the material may be placed in suitable trays. The steam or hot water in the shelves heats the material spread in the trays to a temperature such that water will evaporate under the reduced pressure existing in the dryer. This water is condensed in the condenser placed between the dryer and the vacuum pump. With these types of dryer, drying times are long and usually of the order of 12 to 48 hours.

Tumbling dryer

Tumbling dryer

tumbler dryer has double cone shape. operating under vacuum low temperature, solvent recovery, and increased drying rates Optimum conditions are established by changing the vacuum, the temperature, and, if the material passes through a sticky stage, the speed of rotation. With correct operation, a uniform powder should be obtained as distinct from the cakes produced when static beds are dried.

Notes

waxy solids, cannot be dried by this method because the tumbling action causes the material to aggregate into balls. It was found that drying, periods of 2 to 3.5 hours in tumbling dryers replaced timed of 18 hours in hot-air ovens.

(4) Freeze Dryers:

Freeze drying is a vacuum drying in which the solid is frozen and drying takes place by subliming the solidified ice-phase. Low temperatures and high vacuum are used and establishing and maintaining these conditions, together with the low drying rates obtained, create a most expensive method of drying which is only used when other methods are inadequate. So it is used when high rates of decomposition occur during normal drying. The substances which can be dried at higher temperatures but are thereby changed in some way.

Freeze Dryers (examples)

Fruit juices may lose flavour and odour by other drying methods pertinacious materials are denatured by the concentration and higher temperature blood plasma and some antibiotics are important largescale application of freeze drying. On a smaller scale, it is extensively used for the dehydration of bacteria, vaccines, blood fractions and tissues.

Freeze drying is theoretically a simple technique. Pure ice exhibits an equilibrium vapour pressure of 4.6 mm. Hg at 0C. and 0.1 mm. Hg at -40C. The vapour pressure of ice containing dissolved substances will, of course be lower. If however the pressure above the frozen solutions less than its equilibrium vapour pressure, the ice will sublime, eventually leaving the solute as a sponge-like residue equal in apparent volume to the original solid and, therefore, of low bulk density. The latter is readily dissolved when water is added, and freeze drying has been called for this reason" lyophilic drying" or" lyophilization". No concentration, in the sense of the sense of the word, occurs and structural change in, for example, protein solutions, are minimized.

SEM micrograph of SFD dried PVP 360k system

SEM micrograph of SFD PVP 40k /AC (90:10) system

Tray Freeze Dryer

b) Continuous dryers

Turbo shelf dryer Used for sticky materials It consists of rotating trays arranged in a vertical stack. Heated air is circulated over the trays by turbo-type fans mounted in the centre of the stack. Wet mass fed through the roof of the dryer is leveled by a wiper. After about seven-eighth of a revolution, the material being dried is pushed on the tray below, where it is again spread and levelled. The same procedure continues throughout the heights of the dryer until the dried material is discharged at the bottom.

Turbo-shelf Dryer

b) Continuous dryers (cont.)

2- Drum dryer

a- single drum dip feed b- single drum pan feed c- single drum splash feed d- double drum dip feed e- double drum top feed f- single drum vacuum dryer g- double drum vacuum dryer

If a solution is run on to a steam heated drum which is slowly rotating, drying will take place. The dip-feed system is used where the liquid can be picked up form a shallow pan. The agitator prevents settling of any particles, and the spreader which is sometimes used, helps to produce a uniform coating on the drum. The knife, which is employed for removing the dried material, function in a similar manner to the doctor blade on the rotary filter; if the material is dried to give a free flowing powder this will come away from the rum quite easily.

Double -drum may be dip feed and top feed. Top feed gives a larger capacity, as a thicker coating is obtained. It is important to arrange for uniform feed to a top feed machine, and this may be affected by using a perforated pipe for solutions and a travelling though for suspensions.

Vacuum drum dryers

used when it is desired to keep low temperature. The dried material is collected in screw conveyors and carried to receivers. It is usual to have two receivers so that one can be tilled while the other is emptied and operation, thus, will not be interrupted.

Double drum vacuum dryer

Vacuum Drum-dryer

b) Continuous dryers (cont.)

3-

Spray dryer a- Swenson spray dryer b- Instant spray dryer

Spray dryers

they handle only fluid materials such as solutions, suspension, and thin pastes. The fluid is dispersed as fine droplets into a moving stream of hot gas where they evaporate rapidly before reaching the wall of the drying chamber. The product dries into a fine powder, which is carried by the gas current into a collection system.

Standard Spray-dryer

Start

The advantages of spray dryers are

very short drying time (2 to 20 seconds) which permits drying of highly heat sensitive materials. The production solids of hollow spherical particles, with desired consistency, bulk density, appearance. Spray dryers yielding form a solution, slurry, or thin paste, in a single step a dry product that is ready for the package. A spray dryer may combine the functions of an evaporator, a crystallizer, a dryer, a size-reduction unit, and a classifier.

c) Batch and continuous dryer

1- Fluidized bed dryer If a gas is allowed to flow upward at a velocity greater than the setting velocity of the particles. The resultant mixture of solids and gas behaves like a liquid and the solids are said to be" fluidized". The fluidization technique is very efficient for the drying granular solids, because each particle is completely surrounded by the drying gas. In addition, the intense mixing between the solids and gas results in uniform conditions of temperature, composition, and particle size distribution throughout the bed.

Fluidized-bed Dryer