Summary

The experiment was sorted on the basis of the operation of the spray dryer, the continuous
transformation of feed from a fluid state into dried particulate form by spraying the feed into a
hot drying medium. It is the preferred method of drying heat-sensitive materials. In the
experiment, a pilot plant consisted of mixed flow spray dryer and two fluid atomizer was used.
With the help of atomizer, the liquid milk solution as feed was atomized into fine droplets. It
involved bringing together a highly dispersed liquid and a sufficient volume of hot air by counter
current flow to produce evaporation and drying of liquid droplets as a result of heat and mass
transfer. The hot air along with moisture and the atomized particle flowed concurrently to the
cyclone separator. The separation was occurred mainly in the Cyclone separator by centripetal
force. The air supplied the heat for evaporation and conveyed the dried product to the collector,
and the air was then exhausted with the moisture. The quantity of recovered milk powder was
compared with the input. For that calculation, a known amount of milk powder was taken
initially and after spray drying operations, the amount of solid milk powder was weighed again.
From the data, the percentage recovery and the drying rate were measured. It was seen that the
percentage recovery and drying rate were found different in three different groups. The
percentage recoveries of milk powder were 45.8%, 15.6% and 20% and the drying rate were
29.87 g/min, 35.15 g/min and 26.39 g/min respectively.

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Table of Contents

Declaration...................................................................................................................................................i
Acknowledgement.......................................................................................................................................ii
Summary....................................................................................................................................................iii
Table of Contents........................................................................................................................................iv
List of Figures..............................................................................................................................................v
List of Tables.............................................................................................................................................vii
List of Symbols.........................................................................................................................................viii
1. Introduction.................................................................................................................................1
2. Theory.........................................................................................................................................3
2.1 Atomization.......................................................................................................................................5
2.2 Classification of Spray Dryers.........................................................................................................10
2.3 Design data required for spray dryer................................................................................................12
2.4 Operating Variable..........................................................................................................................14
2.5 Operation and Maintenance.............................................................................................................14
2.6 Maintenance....................................................................................................................................16
2.7 Application and Uses of Spray Dryer..............................................................................................17
3. Materials and Methods...............................................................................................................20
3.1 Experimental Setup..........................................................................................................................20
3.2 Procedure.........................................................................................................................................22
4. Result and Discussions..............................................................................................................23
5. Conclusion.................................................................................................................................28
6. Reference......................................................................................................................................29
7. Appendices................................................................................................................................30
7.1 Appendix A: Sample Calculation....................................................................................................30
7.2 Appendix B: Process Block Diagram (PBD)...................................................................................31
7.3 Appendix C: Process Flow Diagram (PFD).....................................................................................32
7.4 Appendix D: Advantages & Disadvantages of Spray dryer.............................................................33
7.5 Appendix E: Evaporation of Moisture.............................................................................................34
8. Marking scheme............................................................................................................................36

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List of Figures

Figure 1: Co-current Flow Dryer...................................................................................................10

Figure 2: Counter current Flow Dryer...........................................................................................10
Figure 3: Mixed Flow Dryer..........................................................................................................11
Figure 4: Schematic diagram for spray drying..............................................................................20
Figure 5: Cyclone Separator used in laboratory............................................................................21
Figure 6: Process Block Diagram (PBD) for the entire spray drying system...............................31
Figure 7: Process Flow Diagram (PFD) for the entire spray drying system................................32
Figure 8: Temperature history during spray drying of a liquid droplet ........................................34

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List of Tables

Table 1: Data for temperature of air..............................................................................................23

Table 2: Data for temperature of air..............................................................................................24
Table 3: Data for temperature of air..............................................................................................25
Table 4: Data for percentage of powder milk recovery & drying rate..........................................26

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List of Symbols

Symbol Significant Unit

Total time required for drying min

t

Weight of powder milk g

mp

Weight of the water g

mw

Weight of the empty beaker g

m1

Weight of the empty beaker g

m2 with recovered milk

Weight of the liquid milk g

M

R Drying rate g/min

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1. Introduction

Spray drying is a process which is perpetually evolving and emerging across years in terms of its
design, operation and widely varied applications. This process outweighs other liquid drying
techniques in terms of its ability to handle feedstock of varying nature and transform it into free
flowing powders of unique characteristics. Spray drying is a well-known method of particle
production which consists on the transformation of a fluid material into dried particles, taking
advantage of a gaseous hot drying medium. Its first observation was dated 1860 and a primitive
spray dryer device was patented by Samuel Percy in United States in 1872. The development of
spray drying equipment and techniques evolved over a period of several decades from the 1870s
through the early 1900s. Spray drying came of age during World War II, with the sudden need to
reduce the transport weight of foods and other materials. This technique enables the
transformation of feed from a fluid state into dried particulate form by spraying the feed into a
hot drying medium. It is a continuous particle processing drying operation. The feed can be a
solution, suspension, dispersion or emulsion. The dried product can be in the form of powders,
granules or agglomerates depending upon the physical and chemical properties of the feed, the
dryer design and final powder properties desired (Michael, 1993). [1]

The typical spray dryer consists of a spray drying chamber, where the spray is dried, and
succeeding separation equipment such as one or more cyclone separators. When it comes to the
atomization device it varies between applications. Spray-drying mechanism is based on moisture
elimination using for that a heated atmosphere to which the feed product is subjected. The
process may be described by five major phases. A nozzle is usually used to make the droplets as
small as possible, maximizing heat transfer and the rate of water vaporization. Droplet sizes can
range from 20 to 180 μm depending on the nozzle. There are two main types of nozzles: high
pressure single fluid nozzle (50 to 300 bars) and two-fluid nozzles: one fluid is the liquid to dry
and the second is compressed gas (generally air at 1 to 7 bars). It is a unique drying process since
it involves both particle formation and drying. The characteristics of the spray dried powder can
be controlled and the powder properties can be maintained constant throughout the continuous
operation. [2]

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Spray dryer has wide range of non- pharmaceutical and pharmaceutical applications. Nowadays,
application of spray dryers in different industries is growing more than ever. Generally it is used
for preparation of tableting constituents, vaccines, vitamins, blood products, enzymes, hormones,
algae, yeast extracts. Spray drying plants are tailor made to suit product to be dried and its
properties desired. One of the recent advancements of this technology is the reparation and
processing of medicinal and food microcapsules with the aid of spray dryers. Despite of some
discrepancies, the product quality, various usage and potential of this technique and also addition
of the more advanced equipment to pave the way toward reproducible and scalable processes that
are critical to the bench-to-bedside translation of innovative products have made spray dryer
more efficient and exacting.

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2. Theory

Spray drying is an industrial process for dehydration of a liquid feed containing dissolved or
dispersed solids, by transforming that liquid into a spray of small droplets and exposing these
droplets to a flow of hot air.

A conventional spray dryer mainly involves with few steps. At first, the feed is pumped from the
product feed tank to the atomizing device which is located in the air disperser in the top of the
drying chamber. The drying air is drawn from the atmosphere via a filter by a supply fan and
is passed through the air heater to the air disperser. The atomized droplets meet the hot air
and the evaporation takes place cooling the air at the same time. After the drying of the spray in
the chamber, the majority of the dried product falls to the bottom of the chamber and enters a
pneumatic conveying and cooling system. The fines, which are the particles with a small
diameter, will remain entrained in the air, and it is therefore necessary to pass the air through
cyclones for separation of fines. The fines leave the cyclone at the bottom via a locking device
and enter the pneumatic system, too. The air passes from the cyclone to the atmosphere via the
exhaust fan. The two fractions of powder are collected in the pneumatic system for
conveying and cooling and are passed through a cyclone for separation, after which they
are bagged off. The instrumentation comprises indication of the temperature of the inlet and
outlet air, as well as automatic control of the inlet temperature by altering the steam pressure,
amount of oil or gas to the air heater, and automatic control of the outlet temperature by altering
the amount of feed pumped to the atomizing device. [2]

Essential parts of spray dryers include heating, atomizing, drying tower and recovery systems.
Design method and operation conditions at different drying stages along with the physical and
chemical properties of the food material determine properties of the final dried product. The
other adjacent facilities such as fans and cooling systems are used to enhance the system
efficiency.

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Heating System

Inlet air heating system is designed by two direct and indirect methods. In the direct method, air
is directly in contact with a heating source such as a flame. However, in the indirect method, air
is indirectly heated by a heat exchanger [3]. Airflow rate and temperature as well as air thermo
physical properties are the most important design parameters in the indirect method.

Drying Chamber

Spray drying operation is carried out in the drying tower chamber. In these systems, moisture is
removed from a food material through spraying it as tiny droplets into hot air in the drying
chamber. When the droplets are moved by hot air circulation, their moisture is evaporated and is
exited from the drying chamber along with the air. The major part of the drying process happens
at the constant rate period and the mass transfer on the droplet surface is regarded as the drying
limiting factor. When the moisture is reached the critical moisture content, the structure of the
dried food particles determines drying rate in the falling rate period. During this stage, moisture
diffusion from the particles is the limiting factor of drying rate. It should be noted that size and
dimensions of drying chamber depend on the feed rate and type of the food material, the
atomizer type, the distribution type of feed and inlet hot air

Air Distribution

The air distribution is one of the most vital points in a spray dryer. There are various systems
depending on the plant design and the type of product to be produced. Dryer design falls into
three categories:

 Co-current flow: In a co-current dryer, the spray is directed into the hot air entering the
dryer and both pass through the chamber in the same direction.
 Counter-current flow: In this dryer design, the spray and the air are introduced at opposite
ends of the dryer, with the atomizer positioned at the top and the air entering at the bottom.
 Mixed flow: Dryers of this type combine both concurrent and counter current flow. In a
mixed flow dryer, the air enters at the top and the atomizer is located at the bottom.

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2.1 Atomization

The atomizing device, which forms the spray, is the ´heart´ of the spray drying process. Atomizer
is an equipment that breaks bulk liquid into small droplets, forming a spray [4]. Prime functions
of atomization are:

 A high surface to mass ratio resulting in high evaporation rates

 Production of particles of the desired shape, size and density

The aim of atomizing the concentrate is to provide a very large surface, from which the
evaporation can take place. The smaller droplets, the bigger surface, the easier evaporation, and a
better thermal efficiency of the dryer are obtained. The ideal from a drying point of view would
be a spray of drops of same size, which would mean that the drying time for all particles would
be the same for obtaining equal moisture content. In order to produce top-quality products in the
most economical manner, it is crucial to select the right atomizer. Three basic types of atomizers
are used commercially:

 Rotary atomizer
 Pressure nozzle
 Two-fluid nozzle

Ultrasonic energy & vibrations have also been studied, but as yet have found few commercial
applications. These different kinds of atomizers are used in different cases considering their
advantages and disadvantages.

Rotary Atomizers: (atomization by centrifugal energy)

Rotary atomizer uses the energy of a high speed-rotating wheel to divide bulk liquid into
droplets. Feedstock is introduced at the center of the wheel, flows over the surface to the
periphery and disintegrates into droplets when it leaves the wheel.

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Advantages:

 Great flexibility & ease of operation.

 Low pressure feed system.
 No blockage problems.
 Handling of abrasive feeds.
 Ease of droplet size control through wheel speed adjustment.

Disadvantages:

 Produce large quantities of fine particles, which can result in pollution control problems.
 High capital cost.
 Very expensive to maintain.
 Cannot be used in horizontal dryers.
 Difficult to use with highly viscous materials.

Pressure Nozzles: (atomization by pressure energy)

Pressure nozzle is the most commonly used atomizer for spray drying. Nozzles generally
produce coarse, free flowing powders than rotary atomizers. Pressure nozzles used in spray
drying are called “vortex” nozzles because they contain features that cause the liquid passing
through them to rotate. The rotating fluid allows the nozzle to convert the potential energy of
liquid under pressure into kinetic energy at the orifice by forming a thin, high-speed film at the
exit of the nozzle. As the unstable film leaves the nozzle, it disintegrates, forming first ligaments
and then droplets. Pressure nozzles can be used over a large range of flow rates, and can be
combined in multiple-nozzle installations to give them a great amount of flow rate and particle
size flexibility. The range of operating pressure range for pressure nozzles used in spray drying is
from about 17.4 bar to about 690 bar. [Barbosa Canovas and Vega-Mercado, 1996; Tratnig et al.,
2009; Lee et al., 2010]

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Advantages:

 Pressure nozzles result in particles with less occluded air when compared to twin fluid
atomizers.
 Consequently, the powdered product is of higher density, with good flow characteristics.
 Depending on the specifications of the end product, it is also capable of producing particles
with relatively greater size.

Disadvantages:

 At high feed rates, sprays are generally less homogeneous and coarser than rotary
atomizers.

Two-fluid or Pneumatic Nozzles: (atomization by kinetic energy)

Liquid feedstock and compressed air are combined in a two-fluid nozzle. The design utilizes the
energy of compressed gas to atomize the liquid. Two advantages of the two-fluid nozzle are its
ability to produce very fine particles and to atomize highly viscous feeds. However, two-fluid
nozzles are expensive to operate because of the high cost of compressed air. Two fluid nozzles
are often used in laboratory and pilot plant spray dry applications because of their ability to
produce a wide range of flow rates and droplet sizes. The range of operating pressure range for
pressure nozzles used in spray drying is from about 17.4 bar to about 690 bar. [4]

Advantages:

 Twin fluid nozzles are capable of handling highly viscous feed.

 These atomizers also produce much finer and more homogeneous spray when compared to
pressure nozzles.
 These nozzles exert better control over the droplet size.

Disadvantages:

 The requirement of compressed air adds to the cost of operation.

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 Twin fluid nozzles result in high occluded air content within the particles, resulting in low
density.
 Twin fluid nozzles exhibit a higher tendency to clog, especially when the liquid feed is of
mucilaginous or fibrous nature.
 A further disadvantage of this type of liquid‐gas nozzle is the “downstream turbulence”
which causes the fine particles to be carried away to the atmosphere by the large gas flows
used.

Ultrasonic Atomization:

Recently ultrasonic energy has been used in place of pressure or centrifugal force to form
droplets. In this method, a liquid is placed on a rapidly vibrating surface at ultrasonic
frequencies. At sufficiently high amplitude, the liquid spreads, becomes unstable and collapses,
resulting in the formation of very fine droplets. These devices are excellent for droplets below 50
microns. Their use is expected to grow over the next few years. [5]

Powder Separation

In almost every case, spray-drying chambers have cone bottoms to facilitate the collection of the
dried powder. When the coarse powder is to be collected, they are usually discharged directly
from the bottom of the cone through a suitable airlock, such as a rotary valve. The gas stream,
now cool and containing all the evaporate moisture, is drawn from the center of the cone above
the cone bottom and discharge through a side outlet. In effect, the chamber bottom is acting as a
cyclone separator. Because of the relatively low efficiently of collection, some fines are always
carried with the gas stream. This must be separated in high-efficiency cyclones, followed by a
wet scrubber or in a fabric filter (bag collector). Fines are collected in the dry state (bag
collector) are often added to the larger powder stream or recycled.

Cyclone Separator

A cyclone separator, often integrated with a spray dryer, is a stationary mechanical device that
utilizes centrifugal force to separate the solid particles from a carrier gas. It consists of an upper
cylindrical part, referred to as the barrel, and a lower conical part, referred to as the cone. The
gas stream, loaded with solid particles, leaving the spray dryer enters tangentially at the top of

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the barrel and travels downward into the cone, forming an outer vortex. The increasing air
velocity in the outer vortex exerts a centrifugal force on the particles, separating them from the
gas stream. When the gas stream reaches the bottom of the cone, an inner vortex is created, thus
reversing its direction and exiting out at the top as clean gas. The particulates fall into the
collection chamber attached to the bottom of the cyclone. [5]

Bag filter

The bag filter comprises a metallic housing designed for continuous operation and automatic
cleaning. The particle‐laden air enters under suction or pressure through the collector in the
center or bottom part of the bag filter. The air, with particles, travels through the filter bag, which
retains the product particles on its surface. The clean air passes out through bags and plenum to
the outlet of bag filter. Accumulation of dust on bags causes an increase in the differential
pressure across the filter bags. Compressed air is pulsed by a timer‐actuated series of normally
closed pulse valves at preset intervals, causing the valves to open. The compressed air is stored
in a reservoir located beside the higher filter chamber. Above each row of bags there is a tube
with holes that are aligned with the central air passage gap, located on top of the bags, through
which compressed air is injected to invert the gas flow momentarily. This causes the particulate
material accumulated outside the bags to be removed. [5]

Electrostatic precipitator

Electrostatic precipitation is a method of particle collection in spray drying that uses electrostatic
force. An electrostatic precipitator (ESP) comprises of discharge wires and collecting plates. A
high voltage is applied to the discharge wires to form an electrical field between the wires and
the collecting plates. This high voltage ionizes the air around the discharge wires to supply ions.
As the drying air that contains the product particles flows between the collecting plates and the
discharge wires, the particles in the gas are charged by the ions. The Coulomb force caused by
the electric field causes the charged particles to be collected on the collecting plates and the air is
purified. [5]

The selection of particle separation equipment is governed by various factors such as collection
efficiency, suitability for product handling, operational features, and cost and space requirement.

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2.2 Classification of Spray Dryers

Structural design of spray dryers are based on the flow type, the stage number, position and the
cycle type. Based on the flow type, spray dryers are classified into three types of dryer. [2]

The Co-current flow Dryers: Here the air and the product flow are in the same direction which
is appropriate for heat-sensitive foodstuffs such as dairy products. This is because the hottest air
is contacted with the droplets at their maximum moisture content.

Figure 1: Co-current Flow Dryer

The Countercurrent flow Dryers: The product and the air are introduced at opposite ends of
the dryer with the atomizer positioned at the top and the air entering from the bottom. Therefore,
the most dried particles are brought into contact with the hottest air. The counter-current dryers
offer more rapid evaporation and higher energy efficiency in comparison with the co-current
designs. Soaps and detergents are commonly processed in the counter-current dryers.

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 Figure 2: Counter current Flow Dryer
The Mixed flow Dryers: This type of dryers is the combination of the co-current and counter
current flows. A mixed flow dryer exposes the driest particles to the hottest air, so this design is
not used with heat-sensitive products.

Figure 3: Mixed Flow Dryer

Based on the stage number, spray dryers can be classified into two types of dryer.

Single stage Dryer: In a single stage dryer, the moisture is reduced to the target (typically 2-5%
by weight) in one pass through the dryer. The single stage dryer is used in the majority of
designs.

Multi Stage Dryer: In a multi stage dryer, the moisture content of the product leaving the
chamber is about 5-10%. To further reduce the moisture content, other dryers such as fluidized
bed dryers are used. Design of the multi stage dryers allows the use of lower temperatures in the
dryers, making the dryers a good choice for products that are particularly heat sensitive. In
general, multi stage dryers show high heat efficiency and besides preserving the taste and flavor
of the products, they are used for processing viscous and high-fat foodstuffs.

Based on the position of spray dryer, it can be divided into two types.

Vertical Dryer: The chamber of a vertical dryer has the form of a tall cylinder with a cone-
shaped bottom. Inlets for the drying air may be located at the top, bottom or side of the chamber.

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Vertical spray dryers are usually large and the residence time of sprayed particles is relatively
long, allowing the use of higher flow nozzles such as the TD, which produce relatively large
particles.

Horizontal Dryer: The chamber of a horizontal dryer has the form of a rectangular box with
either a flat or a “V” shaped bottom. Box dryers are usually small and the particle residence time
relatively short, requiring the use of low flow nozzles, which produce relatively small particles.

Based on the cycle type, spray dryers can be divided into three types.

Open Cycle Dryer: In an open cycle dryer, drying air is drawn from the atmosphere, heated,
conveyed through the chamber and then exhausted to the atmosphere. This is by far the most
commonly used design.

Closed Cycle Dryer: A closed cycle dryer recycles the drying gas, which may be air or more
commonly, an inert gas such as nitrogen. Closed cycle units are the dryers of choice when,
Feedstock consists of solids mixed with flammable organic solvents, complete recovery of
solvent is required, the products are toxic, explosion risks must be eliminated and finally the
powder will degrade by oxidation during drying.

Semi-closed Cycle Dryer: This dryer design is a cross between open and closed cycle dryers. A
direct-fired heater is used and the air entering the system is limited to that required for
combustion. An amount of air equal to the combustion air is bled from the system at the other
end of the process. The gas is recycled through the dryer. The recycled gas has very low oxygen
content, making it suitable for materials that cannot be exposed to oxygen, due to explosive
hazard or product degradation.

Nano Spray Dryer: Nano spray dryers refer to using spray drying to create particles in the
nanometer range. To emphasize the small particle sizes possible with this new technology, it has
been described as Nano spray drying. Particles can be produced in the range of 300 nm to 5 µm
with a narrow size distribution. High yields, up to 90%, can be produced and the minimal sample
amount is 1 mL. The spray drying process is scalable and the small scale spray dryer are
available in many flexible configurations enabling process simulation of larger industrial size
dryers.

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2.3 Design data required for spray dryer

The variables which influences the design of a spray dryer are in general as follows -

 Atomizer selection
 The size and installment of the drying chamber
 Method of air introduction and the air disperse
 Separation auxiliaries

The selection of the variable are determined by the physical characteristics of the desired
products, such as-

 The required particle size, as directed by the powder specification.

 The particle form of the final spray dried powder
 The maximum temperature to which dried particles can be subjected
 The amount of products that is needed to produce

The selection of the atomizer for a given spray drying operation depends upon the nature of the
feed and the particle size distribution required in the final dried product. The choice of the
atomizer influences the design of the entire spray chamber. Nozzles spray axially in the spray
chamber and require a vertically long, relatively thin tower. So here the spray tower must have a
large diameter but can be shorter. The cone-angle at the bottom of the tower is usually 60-70
degrees and thus most of the tower height where a disk atomizer is used will be occupied by this
cone.

The design of the drying chamber is dependent on the consideration of direction and degree of
atomization, air flow pattern, desired products characteristics and the reaction time for drying, air
flow rates and discharge requirements. The basic design will be determined by the direction to
which the atomized droplet will take an injection from the atomizer.

The other design variables are the drying rate, the time exposure if the droplets to the drying
atmosphere, thermal efficiency, method of separation etc. The drying rate depends upon the
temperature, humidity and flow conditions of the drying gas, the size of droplets produced by the

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atomizer and the properties of the materials being dried. The time exposure depends on the drop
size, particle shape and density and gas flow rate and velocity.

Thermal efficiency can be increased by increasing the inlet temperature. Heat recovery is now
also of much greater interest to the chemical industry. When product properties allow the product
to be contacted with high temperature air for a short period of time, semi-closed cycle systems if
the partial recycle type are an attractive possibility for recovering some of the waste heat from
the exhaust air normally vented to atmosphere. [6]

2.4 Operating Variable

 Inlet temperature of air: Higher the temperature of inlet air, faster is the moisture
evaporation but the powder is subjected to higher temperature, which may distort the
chemical or physical properties of heat sensitive product.
 Outlet temperature of air: It governs the sizing of powder recovery equipment, higher is the
outlet air temperature, larger will be the size of powder recovery equipment. Outlet air
temperatures control final moisture content of powder.
 Viscosity: High viscosity hinders correct drop formation. As the viscosity is lowered, less
energy or pressure is required to form a particular spray pattern.
 Solid content: care must be taken with high solid loadings to maintain proper atomization to
ensure correct droplet formation.
 Surface tension: Addition of a small amount of surfactant can significantly lower the surface
tension. This can result in a wider spray pattern, smaller droplet size, and higher drop
velocity.
 Feed temperature: As the temperature of a solution to be sprayed is increased, the solution
may easily dry as it brings more energy to the system.
 Volatility of solvent: A high volatility is desirable in any drying process. Unfortunately,
choices are limited today. In many cases, these restrict the solvent choice to water.
 Nozzle material: The most pharmaceutical applications use stainless steel inserts. However,
tungsten carbide nozzles are often available and have excellent resistance to abrasion and
good corrosion resistance for most feedstock.

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2.5 Operation and Maintenance

Operation (Prior to Start Up)

1. The liquid distributor and the atomizer wheel must be correctly mounted, having the specified
distance between them. The vanned wheel freely rotates should be checked.

2. All duct connections should be checked for tightness. All gaskets must be correctly mounted.

No false air must be sucked into the drier system due to air leakage around the duct connections.

3. It should be checked that the glass jar under the cyclone is securely fastened. The glass jar
must be clean and dry. It is recommended to preheat (warm) the glass jar to prevent
condensation occurring in the jar during the early stages of the drying.

4. It must be checked that the silencer is mounted on rotary atomizer.

Dryer Control

The drying operation is controlled by maintenance of the required outlet air temperature
at a constant inlet temperature. For a given feed liquid of constant physical properties, the
outlet air temperature is related directly to the moisture content of the dried powder.
Increase in outlet temperature reduces the moisture content, decreasing the temperature
increases the moisture content. Once the outlet temperature range to obtain dried product from
the drying chamber has been established, the outlet temperature can be precisely adjusted to
obtain the required moisture content. During the drier operation it is most important to
keep the outlet air temperature constant so as to maintain the moisture content level.

This is carried out by regulating the rate of feed. Usually the outlet air temperature does not
change, once the feed rate has been adjusted. Alterations of the viscosity and the solids content
of the product will influence the outlet air temperature.

If the feed rate is too large, it is likely that the powder, already in the chamber, will
absorb moisture and stick to the chamber wall. Any adjustments must take place very
slowly, with intervals of sufficient length to enable the resulting effects to be registered on the
thermometer.

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The powder is collected in the glass jar mounted under the cyclone. It is important that the glass
jar is exchanged before it becomes completely full as this will result in product losses from the
cyclone.

Products that are difficult to dry must be atomized at the highest possible speed of the vaned
wheel. A low speed will give a coarser droplet size but may result in wet wall deposits. A high
speed gives fine droplets which are retained in the chamber air flow thus dried before reaching
the chamber wall.

Dryer Shut Down

Before the unit is shut down a changeover of feed from product to distilled water must take
place. The amount of water fed to the atomizer must be regulated so that the outlet air
temperature does not decrease. This is most important as the powder in the drying chamber will
absorb excess moisture.

The unit is to run 10 - 15 minutes with water in order to flush clean the atomizer wheel and the
feed pipe. The air heater is then switched off. After that the water supply is turned off.
Approximately 3 minutes later the atomizer is stopped.

When the outlet air temperature is 50ºC the chamber is opened by means of the pneumatic
lifting device. If powder is retained in the chamber, it can be swept down. Finally the operation
is switched off by cutting power supply. If it is necessary to stop the spray drier suddenly, it is
most important that the feed rate is stopped immediately. [6]

2.6 Maintenance

The success of uniform drying in spray dryer depends on the care and maintenance of different
parts of it. The main points to be considered for proper care and maintenance are as follows:

 Atomizer is a heart of spray drying plant, the nozzles of pressure atomizer should be cleaned
regularly.

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 The drive mechanism of disc type of atomizer should be properly lubricated.
 The filter pads for inlet air for conveying the powder should be cleaned at regular time
intervals.
 The rotary valve for discharge of powder should be checked properly and it should not get
blocked.
 Powder deposits on hot surfaces should be avoided to avoid fire explosion.
 Magnetic hammers or vacuum should be used to avoid powder deposition on inner wall of
spray drying chamber.
 Thermostats should be placed in the air inlet and outlet duct that sounds alarm and cuts off
the air heating system if the air inlet and/or outlet temperature exceeds a certain
predetermined value.
 A fire extinguishing system should be provided consisting of sprinklers in the
chamber ceiling.
 The dryer can be equipped with fire detectors to prevent fire.
 The spray dryer should be provided with powder recovery systems from outlet air like bag
filter, cyclone separator, wet scrubbers etc.
 The spray dryer should be provided with heat recovery systems.
 All cyclone separators and bag filters should be cleaned properly at regular time
intervals.
 Other parts of the spray dryers should be followed with preventive maintenance.

2.7 Application and Uses of Spray Dryer

Encapsulation

The application of the spray drying encapsulation technique is to prepare ‘dehydrated’ powders
of substances which do not have any water to dehydrate. For example, instant drink mixes are
spray dries of the various chemicals which make up the beverage. The technique was once used
to remove water from food products; for instance, in the preparation of dehydrated milk. Because
the milk was not being encapsulated and because spray drying causes thermal degradation, milk

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dehydration and similar processes have been replaced by other dehydration techniques.
Skim milk powders are still widely produced using spray drying technology around the
world, typically at high solids concentration for maximum drying efficiency. [2]

Pharmaceutical Industry

Spray drying is an interesting manufacturing technique for the pharmaceutical industry since it
uses a one-step process for formation and drying of powders. Using this technique the
number of unit operations is reduced, improving production efficiency and reducing costs,
especially since spray drying is a technique which can be easily automated and equipped for in
line product analysis. In addition, spray drying can be considered a continuous process, thus
reducing time-to-market because of scale-up benefits and better quality. Spray drying has a wide
range of applications in the pharmaceutical and biotech industry. It is a convenient method to
produce excipients. Spray drying is applied to improve the compact ability of drugs and
to perform microencapsulation, granulation and complex formation. In addition, spray
drying is successfully used for the modification of biopharmaceutical properties and the
formulation of dry powder aerosols and heat sensitive materials.

Food Industry

Many food ingredients, such as enzymes and probiotics, are spray dried to provide a longer shelf
life. Spray drying process has been used for decades to encapsulate food ingredients such as
flavors, lipids, and carotenoids. During this drying process, the evaporation of solvent, that is
most often water, is rapid and the entrapment of the interest compound occurs quasi-
instantaneously. This required property imposes a strict screening of the encapsulating materials
to be used in addition to an optimization of the operating conditions. Likewise, if the
encapsulated compound is of hydrophobic nature, the stability of the feed emulsion before drying
should also be considered. Thus, spray-drying microencapsulation process must rather be
considered as an art than a science because of the many factors to optimize and the
complexity of the heat and mass transfer phenomena that take place during the microcapsule
formation. The application of the spray drying encapsulation technique is to prepare
"dehydrated" powders of substances which do not have any water to dehydrate. For example,
instant drink mixes are spray dries of the various chemicals which make up the beverage.

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Production of coffee, tea, eggs, cereal, spices, flavorings, starch and starch derivatives,
vitamins, enzymes, stevia, colorings, etc. also require spray drying process.

Aerosol Formulation

Salbutamol sulphate particles, for use in dry powder aerosol formulation, were prepared by spray
drying, using a Mini spray dryer. Spray freeze-dried liposomal ciprofloxacin powder for inhaled
aerosol drug delivery had been prepared with a two-fluid nozzle.

Chemical Industry

The chemical industry uses drying in sectors ranging from agricultural products and fine
chemicals through plastics and paints. Methods vary with material and application.
Polycarbonate and polyvinyl products and many other organic and inorganic chemicals,
ceramics, agricultural products, dyestuffs, mineral and ore products, cellulose etc. require
spray drying process.

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3. Materials and Methods

3.1 Experimental Setup

Figure 4: Schematic diagram for spray drying.

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The experimental setup for study of spray dryer used for the experiment performed has been
given in Figure. Spray dryer used for the experiment was large cylindrical chambers with a cone
bottom. Small nozzles were located in the chamber walls through which the feed material was
atomized to a fine droplet. Air entered into the chamber through three holes and milk solution
through one hole. There was a two fluid atomizer in the chamber. For hot air supply, air was
driven through the heater and the dryer by low-pressure, high-capacity blowers. A compressor
(20 psig) was used. Drying chambers were equipped with service doors, inspection windows,
light sources, air sweep doors. When the drying part was done, the dried powder was separated
from the gas by cyclone separator. This device had a cylindrical upper part, the barrel, and a
conical part on its bottom, the cone (Figure). The streamline of air containing the dried particles
coming from the drying chamber was supplied into the cyclone at its top tangentially. Through
vortex separation, the air and moisture were expelled from the cyclone at its top, whereas the
particles settled into a collection bottle placed on its bottom. During the experiment, inlet and
outlet temperature of the air was measured by thermometer.

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 Figure 5: Cyclone Separator used in laboratory

3.2 Procedure

At first some milk powder was taken in a beaker and weighed. Then it was mixed with water
thoroughly to make a solution. The spray dryer was started by turning on the hot air blower. The
pressure of the compressed air supplied to the atomizer was adjusted to 20 psig. Inlet and exit air
temperature were measured by thermometer. The milk solution was poured in a milk container at
the top of the drying chamber and it entered into the spray dryer. Inside the chamber, the milk
solution was atomized into a spray of fine droplets with the help of atomizer and compressed air
inlet. The hot air from air blower came to contact with the liquid milk droplets by counter-
current flow and exchanged heat between each other. Then the solid powder and gas mixture
flowed co-currently to the cyclone separator. Thus the whole process was called mixed flow
spray drying. In the cyclone separator, the mixture was rotated vigorously. Since the milk
powder has higher size and density, it got separated from the gas. The residual air and moisture
flew through exhausted outlet pipe and dried milk powder was collected in a bottle. The outlet
temperature reading was taken. Then the dried milk powder was weighed and percentage
recovery was calculated. Dividing the weight of water by total time required, the drying rate can
be estimated.

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4. Result and Discussions

The data of temperature of air collected during experiment through thermometer were listed at
Table 01, Table 02 and Table 03. Also Table 04 represents calculated data for percentage of
powder milk recovery and drying rate of three groups.
Group A1 (2)
Working pressure, P = 20 psig

Total time required for drying, t = 31.80 min

Weight of milk powder, mp = 50 g

Weight of water, mw = 950 g

Weight of liquid milk, M = 1000 g

Weight of empty beaker, m1= 561.50 g

Weight of beaker with recovered milk m2 = 584.40 g

Table 1: Data for temperature of air

Air Temperature Initial Temperature (℃) Final Temperature (℃)

Inside the chamber 150 150

Outlet 77 64

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Group A1 (3)

Working pressure, P = 20 psig

Total time required for drying, t = 27.30 min

Weight of milk powder, mp = 50 g

Weight of water, mw = 950 g

Weight of the liquid milk, M = 1000 g

Weight of empty beaker, m1= 561.50 g

Weight of beaker with recovered milk m2 = 569.30 g

Table 2: Data for temperature of air.

Air Temperature Initial Temperature (℃) Final Temperature (℃)

Inside the chamber 150 150

Outlet 76 63

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Group A1 (4)

Working pressure, P = 20 psig

Total time required for drying, t = 36 min

Weight of milk powder, mp = 50 g

Weight of water, mw = 950 g

Weight of the liquid milk, M = 1000 g

Weight of empty beaker, m1= 561.50 g

Weight of beaker with recovered milk m2 = 571.50 g

Table 3: Data for temperature of air

Air Temperature Initial Temperature (℃) Final Temperature (℃)

Inside the chamber 150 150

Outlet 79.8 72

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Table 4: Data for percentage of powder milk recovery & drying rate.

Group number Percentage of powder milk Drying Rate of water, (g/min)

recovered, %

A1 (2) 45.80 29.87

A1 (3) 15.60 35.15

A1 (4) 20 26.39

From Table 04, it can be seen that the percentage of powder milk recovered were quite low.
Though same amount of milk powder was taken for three groups, drying rate and percentage of
recovery were different. This could happen for different time duration or temperature. Also there
had some technical restrictions and discrepancies, for these the recovery couldn’t gain
satisfactory result. Some of the discrepancies are described below:

At the very beginning of the experiment, the liquid milk solution supply was high and so a
considerate amount of milk solution was stuck on the chamber wall and accumulated there. This
loss contributed to the less percentage of recovery. The pressure of the compressed air supplied
to the atomizer was adjusted to 20 psig. But it was hard to maintain the pressure constant
throughout the whole experiment that could result in medium coarseness but a poor homogeneity
of droplets. Whereas atomizer was used to have large surface area of droplets. Because the very
large surface area of the spray droplets causes evaporation of the water to take place very
quickly, converting the droplets into dry powder particles. Here two fluid nozzles was used
which had some limitation such as it introduced extra cold air into the spray chamber in the
atomization and reduced the temperature gradient that exists between the finely divided droplet
and the surrounding drying medium. This impaired the effectiveness of heat transfer between the
droplet and hot drying medium. A further problem of the nozzle was the downstream turbulence

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which caused the fine particles to be carried away to the atmosphere by the large gas flows used.
This overspray phenomenon tended to contaminate the atmosphere which was in close proximity
to the nozzle, and demands expensive cleanup and tedious maintenance procedures [7]. The
spray drying chamber had a conical bottom to facilitate the easy collection of the dried powder
but this bending caused some loss of the dried powder milk. As a drying collector cyclone
separator had been used. If the droplets were so fine, then it would require less weight and then it
couldn’t be separated by cyclone separator. Some of fine particles departed with exhausted air.
The ambient condition had also impact on these. Dryer capacity was limited by the total moisture
in the air leaving the spray-drying chamber. Evaporation is defined as the difference between
inlet and outlet temperature. The larger the difference, the greater the capacity of the spray dryer.
The outlet temperature was a manifestation of the relative humidity in the outlet air. If the outlet
temperature was too low, the product particles in the drying chamber would not become dry
enough in the time allowed, enabling sticky particles to cause blocking or plugging. If the outlet
temperature is too high, excess capacity remains unutilized. The easiest way to minimize the loss
is to recycle the leaving stream. In order to optimize the efficiency of spray dryer, the maximum
allowable dissolved solid mass flow rate should be used and the inner surface of spray dryer
should be smoothen so that no milk particle can stick to its wall. Spray drying energy
efficiency can be improved by widening the gap between inlet and outlet temperatures and
adding heat recovery equipment. Inlet temperature can be limited for process reasons when the
difference in temperatures have been optimized and the maximum outlet humidity has been
reached. This means evaporating as much water as possible and operating just above the
product’s sticky point [7]. Optimum mixing between the liquid spray and the hot air entering
the milk spray drying chamber can be achieved by using the widest possible spray angle
together with multiple nozzles. To increase the percentage recovery of solid particles vibrator
attached with cyclone separator can be used or bag filter, wet scrubber, electrostatic precipitator
can be used.

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5. Conclusion

The experiment was sorted to deliver the knowledge about spray dryer. Different techniques,
mechanism, working principle, operating variables of spray drying and types of material
handle in spray dryer had been known through this experiment. It also gave idea about
advantage and disadvantage of spray dryer over other types of dryers. Spray-drying is a rapid,
continuous, cost-effective, reproducible and scalable process for the production of dry powders
from a fluid material by atomization through an atomizer into a hot drying gas medium. It is
congenial to dry materials that are sensitive to heat or oxidation without degrading them,
even when high temperature air is employed. The advantages and drawbacks of spray dryer of
each parameter should be weighed in order to produce products with desirable characteristics.
From the result, it can be concluded that the percentage of recovery of milk powder was not so
high due to some technical restriction and some discrepancies. Thus this whole experiment had
provided with great deal of engineering knowledge regarding spray drying process.

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6. Reference

[1] Foust, A.S., L.A. Wenzel, C.W. Clump, L. Maus, and Andersen, L.B. (1980). Principles of
Unit Operations, 2nd edition, New York: John Wiley & Sons.

[2] https://www.google.com/search?rlz=spray+drying , (Accessed 2019.07.20, 12.08 am)

[3]https://www.gea.com/en/expert-knowledge/milk-powder-manufacture/fundamentals-spray-
drying.jsp , (Accessed 2019.07.20, 12.08 am)

[4] http://www.bete.com/pdfs/BETE_SprayDryManual.pdf accessed on November 11, 2008

[5] Cal K, Sollohub K. Spray drying technique. I: Hardware and process parameters. Journal of
Pharmaceutical Sciences.

[6] http://www.bestdryermachine.com/spray-dryer-working-principle, (Accessed 2019.07.21,

10.17 pm

[7] https://www.powderbulksolids.com/article/spray-dryer-optimization, (Accessed 2019.07.20,

12.80 pm)

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7. Appendices

7.1 Appendix A: Sample Calculation

Weight of liquid milk, M = Weight of milk powder (mp ) + Weight of water (mw )

= (50 + 950) g

= 1000 g

Weight of recovered milk mr = m2- m1

= (584.40- 561.50) g

= 22.9 g

weight of the recovered milk , mr

Percentage of powder milk recovered = × 100%
weight of the milk powder ,mp

22.9
= × 100%
50

= 45.80%

weight of the water , mw

Drying rate, R =
total time ,t

950 g
=
31.8 min

= 29.87 g/min

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7.2 Appendix B: Process Block Diagram (PBD)

Figure 6: Process Block Diagram (PBD) for the entire spray drying system.

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7.3 Appendix C: Process Flow Diagram (PFD)

Figure 7: Process Flow Diagram (PFD) for the entire spray drying system.

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7.4 Appendix D: Advantages & Disadvantages of Spray dryer

Advantages:

 Product quality and properties can be effectively controlled and maintained through the entire
drying operation.
 Thermo labile products/pharmaceutical can be dried at atmospheric pressure and low
temperature.
 Spray dryer permits high- tonnage production in continuous operation adaptable to
conventional PLC control (Programmable Logic Controller) and it is relatively simple to
operate.
 Feedstock in solution, slurry, emulsion, paste and melt form can be dried if pump-able.
 Corrosion problem is minimal and the selection of materials of construction of spray dryer is
simplified since the dried material comes in contact with the equipment surfaces in an
anhydrous condition.
 Spray dryer produces dry powder particle of controllable particle size, shape, form, moisture
content and other specific properties irrespective of dryer capacity and heat sensitivity.
 Spray dryer handles a wide range of production rate and provides extensive flexibility in its
design that is product specification are readily met through the selection of appropriate spray
dryer design and its operation from a wide range of available design.
 It is an energy-intensive equipment because;
i. Specific heat of evaporation can be supplied in a short time.
ii. The temperature difference across the drying chamber is relatively small and
iii. An appreciable amount of heat is lost with exhaust air

Disadvantage:

 Spray dryer is bulky and also expensive to install.

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 It is difficult to clean after use.
 It has a low thermal efficiency that is a lot of heat is wasted during operation.
 Solid materials cannot be dried using spray dryers.
 Product degradation or fire hazard may result from product deposit on the drying chamber.

7.5 Appendix E: Evaporation of Moisture

The most critical step in particle formation, this process step is associated with the morphology
of the final product. Evaporation of moisture during spray drying can be visualized as two stages:

 Constant rate period

 Falling rate period

Initially, when the droplet is exposed to hot gas, rapid evaporation takes place. During this
exposure, the droplet is heated from its initial temperature to the temperature of equilibrium
evaporation temperature During this period, the removal of moisture follows the constant rate
period of the drying rate curve as the moisture is removed constantly from the surface of the
droplet keeping it sufficiently cool. The droplet surface remains saturated with moisture at
this stage and its temperature is constant at the wet‐bulb temperature. Wet‐bulb temperature is
the temperature that the drying gas reaches when it is saturated with vapor from the liquid. Also,
the droplet shrinks due to the evaporation of the aqueous phase.

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Figure 8: Temperature history during spray drying of a liquid droplet (Handscomb et al.,
2009.Reproduced with permission of Elsevier).

As the moisture removal from the droplet proceeds, the solute dissolved in the liquid reaches a
concentration beyond its saturation concentration and tend to form a thin shell at the droplet
surface described as “crust formation”. After the crust formation, the moisture removal turns
into a diffusion‐controlled process, and the evaporation rate is dependent upon the rate of
water vapor diffusion through the dried surface shell. This constitutes the falling rate period.
During the falling rate period, although the particle will begin to heat, it is almost at the coolest
part of the dryer, where the drying gas is at or near the outlet temperature of the dryer.
Consequently, the particles are never heated above the outlet temperature of the dryer, despite
the fact that the inlet temperature may be considerably higher.

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 8. Marking scheme

Formal report on ‘STUDY OF SPRAY DRYER’

Name: Synthia Rashid

Student No.: 1602009
Marks Allocated Marks

Summary (10%)

Introduction (5%)

Theory (10%)

Method of Experiment (20%)

Results & Discussion (40%)

Conclusion (5%)

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Appendix (10%)

Total (100%)

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