Spray-Drying

Basic theory and applications

1
 Contents
Spray Drying 3

What is spray drying? 3

How does spray drying work 4
Atomization 4
Spray air contact 4
Evaporation of moisture, particle shape formation and drying 5
Particle separation 6
Particle shapes and structures 6
Optimizing the spray drying process 7
Spray gas flow (two fluid nozzle) 8
Feed concentration 8
Feed viscosity 8
Feed surface tension 8
Feed flow rate 8
Inlet temperature 9
Outlet temperature 9
Aspirator flow rate/speed 9
Residence time of the particles in the spray chamber 9
Glass transition temperature 10
Advantages and disadvantages of spray drying 10
Advantages of spray drying 10
Disadvantages of spray drying 10
Applications 10
Drying a material 10
Structural Changes 11
Encapsulation 11
Amorphous Solid dispersion 12
Selection of matrix and shell materials 13
Characteristics of matrix and shell materials 13
Frequently used matrix and shell materials in spray drying 14
Procedure to run a spray drying experiment 17
Guidelines on the choice of starting process parameters 18
Fields of application 18
Food Application 20
Chemical Application 22
Pharmaceutical Application 24
References 26

2 3
What is spray drying?
Spray drying is a widely applied method for obtaining dry
powders from aqueous or organic solutions, emulsions
and suspensions. During the process, a spray dryer at-
omizes a liquid feed into fine droplets and evaporates the
organic solvent or water by means of a hot drying gas.
It is typically used to dry a substance, to encapsulate
an ingredient within a particle or to perform a structural
change of the material.
Since the 1940s, spray drying has been a robust and
widely used manufacturing process and applications
are found in all major industries ranging from industrial
chemistry, pharmaceutical, biotechnology to food indus-
try. Dry milk powder, instant soups, instant coffee, deter-
gents and dyes are just a few examples of spray dried
products on the market.1–3
How does spray drying work
A complete spray-drying process consists of a sequence
of four steps:
X Atomization of the feed
X Spray air contact
X Solvent evaporation
X Separation of the product from the drying medium
Feed
Product
Drying gas (cold)
Drying gas (warm)
Pump (defining feedrate)
Aspirator
Heater
Figure 1: Functional principle of conventional spray dryer –
BUCHI Mini Spray Dryer B-290
4 5
Atomization
The atomization is the first process that the feed under-
goes during a spray drying process. It influences the
shape, the structure, the velocity and the size distribu-
tion of the droplets and therefore, the particle size and
nature of the final product. The dispersion of the feed into
fine droplets allows a great increase of the total surface
area of the liquid and a higher heat and mass transfer.
The large surface exposure to the solvent free gas allows
the droplets to dry very quickly, with minimal loss of heat
sensitive compounds and to finally obtain particles of the
desired morphology and physical characteristics.1,4
Figure 2: Commonly used atomizers : A Two fluid nozzle, B Rotary
atomizer, C Pressure nozzle, D Ultrasonic nozzle 3
During the atomization process, atomizers and nozzles
supply energy to the feed to form a spray of droplets.
Several atomization devices are available for research
and development depending on individual requirements.
It is however important to make sure that the device can
be used or transposed to large scale later on. Despite
the emergence of niche atomizers, the more common
remain pressure nozzles, ultrasonic nozzles, two-fluid
nozzles and rotary disk atomizers (Figure 2). Two fluid
nozzles can be used at lab scale and larger scale, where-
as rotary disk atomizers and pressure nozzles are main-
ly used at industrial scale and ultrasonic nozzles at lab
scale. Inkjet atomizers, aerosol-assisted atomizers or
electrostatic atomizers are starting to emerge and show
interesting properties. Their low throughput is however
preventing the widespread use of these nozzles. The
choice of nozzle mainly depends on the scale of the pro-
cess, the properties of the feed and the end product re-
quirements.1,4–6
Spray air contact
After atomization, the droplets come into intimate con-
tact with the heated drying medium. A rapid evaporation
of the moisture from the surface of all the droplets is hap-
pening in a uniform manner. It is critical to have a uniform
Airflow
Product
Feed
Co -Current Counter-Current Mixed Mode
Figure 3: Flow configuration of spray dryers 3
gas flow in all parts of the drying chamber.4–7
The droplet-air contact determines several important pa-
rameters such as the evaporation rate in the droplets,
the trajectory and residence time in the drying cham-
ber, the deposit on the chamber wall, the morphology
of particles, and the product quality.4–6 There are three
existent droplet-air flow patterns (Figure 3), co-current,
counter-current and the mixed-flow, which are related to
the direction of the drying gas flow with respect to the
direction of the spray.3–5,7
In the co-current flow, the spray and the drying gas enter
the drying chamber at the same point, usually the top of
the drying chamber. The spray and the drying gas meet
at its highest temperature but the droplets are kept at
a low temperature due to the high rate of evaporation.
Droplet temperature is approximately at the wet-bulb
temperature, which is the temperature at which the gas
has been cooled by the evaporation of the solvent from
the droplets. The contact between the hot gas and the
droplets is only of a few seconds during which driyng
is achieved. The evaporation of moisture is rapid, the
temperature of the gas decreases rapidly when in con-
tact with the droplets resulting to a small thermal load
on the final product, since it is in contact with the cool-
est air. Co-current flow is preferable for heat-sensitive
material.3–5,7
In the counter-current flow, the drying gas enters at the
bottom of the drying chamber, at the opposite side of the
spray. Here, the outlet product temperature is almost at
the feed air temperature. With this solution, low residual
moisture content can be achieved since the dry powder
meets the hot and dry air. The thermal impact on the
encapsulated material is higher than in co-current flow.
Furthermore, the residence time in the drying chamber is
increased due to the upward stream of air.This solution is
used for heat-resistant products.3–5,7
The mixed-flow pattern is a combination of co-current
and counter-current flow. The air enters at the top and
the spray is produced at the bottom of the drying cham-
ber. Its main drawback is the high exit temperature of the
product. It is used for drying coarse free-flowing pow-
der.3–5,7
The most common and economic drying medium is air,
however, inert gases such as nitrogen can be used to
prevent risks of explosion and to prevent oxidation of
sensitive products.3–5,7 In this case, a closed-loop sys-
tem is required to recirculate the inert gas and recover
the solvent.3–5,7
Evaporation of moisture, particle shape
formation and drying
The removal of moisture from a spray droplet is the
most critical step in particle formation and is associat-
ed with the morphology of the final product.4 The dry-
ing rate and type of particles being formed8 depend on:
X the air temperature, humidity and transport
properties
X the droplet temperature, diameter and velocity
When meeting the aerosol droplets, the gas temperature
decreases rapidly at first. The diminution in temperature
then becomes slower with an increase in drying time and
distance as the outlet temperature for the dryer is grad-
ually reached.2
Once a droplet is exposed to a hot gas, it heats up rap-
idly from its initial temperature to an equilibrium evapora-
tion temperature (Figure 4, AB) which corresponds to the
wet-bulb temperature. Moisture is removed constantly
from the surface of the droplet and drying proceeds at
a close to constant rate for as long as the droplet sur-
face remains saturated with moisture (Figure 4, BC). As
 gas temperature
F assessing those parameters is difficult due to the com-
droplet centre temperature
E gas
boiling temperature
D on the product morphology. Crust formation is reported
C to be central for particle formation during spray drying.
B wet bulb temperature
A leading to small, solid particles, the other to large, hollow
time
Figure 4: Evolution of the droplets' temperature during the spray
drying of a liquid containing suspended solids. 8
drying proceeds, moisture cannot be supplied to the sur-
face at a rate sufficient to maintain saturation and a thin
shell tends to form at the surface of the droplets. This
is described as crust formation. After crust formation,
moisture removal becomes a diffusion controlled pro-
cess and the evaporation rate depends on the diffusion
rate of vapor through the dry surface of the shell. During
this phase, the particle will begin to heat (Figure 4, CD).
If the droplet temperature reaches the moisture boiling
point, vaporization starts and the heating of the droplets
stops, since the energy is used for the vaporization pro-
cess (Figure 4, DE). Once all the remaining moisture is
removed, the temperature rises again until it reaches the
surrounding gas temperature, also called outlet tempera-
ture (Figure 4, EF).8 The highest temperature the product
will be exposed to is therefore the outlet temperature. It
is a derivative of the evaporation enthalpy of the solvent,
the concentration of the solid in the liquid and the heat
loss through the drying chamber wall.2
Particle separation
The dry products must be separated from the drying gas
and collected. The primary separation of the dried par-
ticles from the drying gas takes place at the base of the
drying chamber. The finer particles can then be recov-
ered from the drying gas by a separation device such
as cyclones, bag filters, electrostatic precipitators or wet
collectors such as scrubbers, depending on the size of
the particles carried away by the drying gas and the final
product specifications.1,3,4 The product streams are sub-
sequently mixed or segregated. Often, the grain fraction
is recovered as product while the fine material is recycled
into the process.3
6 7
gas
particles
+
particles
Figure 5: Principle of cyclone separation. The dashed arrow
represents the outer vortex while the ribbon arrow shows the
inner vortex
Cyclones are mostly utilized due to their low cost and
low maintenance requirements. As illustrated in Figure 5,
they use centrifugal force to separate the solid particles
from the carrier gas. The gas stream and the particles
enter the cyclone tangentially at the top and travel down-
wards forming an outer vortex. The increasing air veloc-
ity in the outer vortex applies a centrifugal force on the
particles and separates them from the gas stream. Once
the stream reaches the bottom of the cyclone, an inner
vortex is created in the reverse direction and a clean gas
exits the cyclone at the top. Particles with different size/
densities experience different forces in the cyclone. Larg-
er particles are subject to higher centrifugal forces and
thereby move closer to the wall. At the wall, the effect
of centrifugal forces becomes smaller and the particles
fall downward where they are trapped in the collector.
Fine particles move close to the center of the cyclone
in a low pressure region. Due to the slower speed, they
often move along with the upward spiral flow and escape
through the gas outlet.1,3,4,6,7
Particle shapes and structures
As illustrated in Figure 6, several types of particles can
be produced from a spray drying process. Their mor-
phology include dense, hollow, porous composite or en-
capsulated structures with spherical, wrinkled, shriveled
collapsed or cenospheres (doughnut-like) shapes.2,8
plex interaction between the variables and the unique
drying patterns of different materials subjected to the
drying process.4,9,10 Understanding the drying kinetics is
key to the comprehension of particle morphology. Fig-
Solid particles Satellites Shrivelled particle ure 7 summarizes the impact of some drying patterns
The droplets can then follow two principal pathways, one
particles.2,4,8,9
Hollow particle Cenosphere Disintegrated
As a general rule, slow drying leads to more compact
Figure 6: Common particle shapes and structures formed during particles, whereas fast drying yields the formation of hol-
a spray drying process low particles. Vehring et al. (2008) reported that several
aspects of the particle formation process are controlled
Key quality characteristics of a spray dried product such by the relationship between the surface recession and
as particle size distribution, flowability, friability, moisture the diffusion of the solutes and therefore, the Peclet
content, bulk and particle density are influenced by the number. (Eq. 1) is depicted as the main controlling pa-
particle morphology. It is therefore important to under- rameter of the droplet drying process.4,9,10
stand the parameters that influence the morphology and
how the frequently occurring morphology patterns hap- Eq. 1
pen.4 Even though literature reports that the morpholo-
gy of the particles can be altered by optimizing process where K is the evaporation rate and D is the diffusion
parameters, such as inlet and outlet temperature, flow rate.
rate of the drying gas or feed properties, quantifying and At low inlet-outlet temperature, combination, Pe is low
due to a lower evaporation rate at a higher diffusion rate.
When Pe < 1, small, solid particles with almost no void
space and a density close to that of the dry bulk material
are produced.
No particle Shattered Solid
formation Particle Particle On the other hand, when the inlet-oulet temperature
Collapse combination is high, Pe is high. When Pe > 1, the evapo-
Low solids
ration rate is high, resulting in the rapid build-up of solute
concentration, High concentration at the surface of the droplet leading to a
<1%w/w temperature
Re-Inflation
local increase in viscosity followed by a skin or shell for-
'Dry Shell' mation. The fate of the hollow particle depends on the
thickness and mechanical properties of the skin. Col-
'Wet
Shell' lapse or wrinkle can happen eventually.4,8–10
Saturated Crust Internal Bubble Uninflated
Surface Drying Formation Nucleation Shell
Initial Droplet
Optimizing the spray drying
High temperature
process
The results of the spray drying method highly depend on
material properties, equipment design and correlation of
the process parameters. Those factors have an influence
Blistered Shrivelled Inflated 'Puffed'
Particle Particle Particle on the quality of the final product in terms of morpholo-
gy, residual moisture and particle size. Optimization of
Figure 7: Different particle morphologies that can result from a
spray drying process 8
the process is usually achieved by a “trial and error” ap-
proach, however, understanding the basic guidelines of Feed viscosity Inlet temperature The most important consideration is the choice of the
spray drying can help the user with efficient use of the optimum temperature difference between the inlet and
equipment.3,4 General guidelines for optimizing the pa- The feed viscosity has a direct impact on droplet size. In The inlet temperature is understood as being the tempera- the outlet temperature. To achieve a product with a very
rameters and information related to their impact on the order to produce droplets, the atomization energy sup- ture of the heated drying gas. It is directly linked to the wet- small amount of residual moisture, the inlet temperature
products are summarized in Figure 8. plied to the nozzle needs to overcome viscous forces. bulb temperature of the surrounding hot air and is often should be set as high as possible and the temperature
The more viscosity, the more forces need to be over- associated with the dryer evaporative capacity and ther- difference must be as small as possible. Increasing the
Parameter come and the less energy is available for creating the mal efficiency. The inlet temperature is set to a value where temperature difference while holding the inlet tempera-
Aspira- Humid- Inlet Spray Feed Sample Organic droplets. This results in larger droplet and particles.4 a temperature gradient between the wet droplet surface ture constant increases the residual moisture content in
tor ity in tem- gas rate concen- solvent and the hot saturated gas leads to an evaporation of the the final product. A high outlet temperature is used to
drying perature flow tration instead
gas of water Feed surface tension solvent. A higher inlet temperature is favorable in terms achieve high moisture content to obtain agglomerated
Depen- of achieving higher throughput; however, a lower value “instant” powdered products. This is because a high out-
dence A high surface tension is difficult to atomize since it has prevents degradation or losses of active compounds.3,4 let temperature leads to rapid crust formation while the
Outlet to be overcome by the atomizer to achieve spraying. drying of the inner core is still not complete. Increasing
tempera-
ture In order to overcome the surface tension of the feed, it Outlet temperature the outlet temperature also increases particle tempera-
might therefore become necessary to prepare an emul- ture.3,4
Particle
size — — — sion with emulsifier and a homogenization step prior to The outlet temperature is determined by the heat and
Humidity
spray driying in some cases.4 mass balance in the drying cylinder and cannot be reg- Aspirator flow rate/speed
in final ulated. It is influenced by the following parameters as
product
Feed flow rate shown in Figure 9. The aspirator is associated with the supply of drying gas
Yield into the drying chamber. Altering the aspirator flow rate
The peristaltic pump feeds the spray solution to the noz- X Inlet temperature or speed enables the regulatetion of the amount of dry-
High Moderate Minor Increasing No zle. The pump rate affects the temperature difference be- X Aspirator flow rate/speed ing gas entering the drying chamber, which has a signifi-
influence influence influence parameter influence
tween the inlet and the outlet and the final particle size. X Feed flow rate cant effect on the drying performance3,4.
Invreasing variable Decreasing variable X Concentration of the material being sprayed The optimum setting must be determined experimentally.
At constant atomizing gas flow rate, an increase in the As a guideline, a higher aspirator rate leads to a higher
Figure 8: Influence of process parameters on product
characteristics.3 feed flow rate leads to an increase in droplet size, since Due to the intense heat and mass transfer in addition degree of separation in the cyclone. A lower aspirator
the nozzle has to atomize more liquid with the same to humidity loss, the particles temperature is close to rate results in a lower residual moisture content.3,4
Spray gas flow (two fluid nozzle) “energy”.4 the gas temperature at the outlet. Therefore, as a rule
of thumb, the maximal temperature experienced by the Residence time of the particles in the
The gas spray flow is the amount of compressed gas The feed flow rate also corresponds directly to the in- product is considered to be the measured outlet tem- spray chamber
needed to disperse the liquid solution, emulsion or sus- let mass. The higher the throughput, the more energy perature.
pension into a nice spray cone. In a closed mode config- is needed to evaporate the droplets into solid particles. The residence time is important with respect to the com-
uration, compressed nitrogen is used instead of air. The Thus, the outlet temperature decreases. When the pump T [°C] plete drying of the droplets and to control of the particle
gas spray flow is adjusted manually by a needle valve to rate is too high, wet and sticky particles, which adhere to temperature so that aroma loss or thermal degradation
Inlet
between 300 and 800 Nl/h. The rotameter indicates the the spray chamber wall are obtained. The optimal pump temperature of heat sensitive materials can be minimized. Fine par-
gas spray flow in a mm-height scale. rate depends also upon factors such as the viscosity of ticles containing a high amount of surface moisture will
the spray solution and tubing diameter.3 experience an easy evaporation and therefore require
As a guideline, a higher gas spray flow rate leads to small- a short residence time. Fine to semi-coarse spray that
er droplets and accordingly to smaller dried particles.3 Guidelines related to the feed pump rate are3. Gas need to be dried to a low moisture content require a
medium residence time while coarser spray that need
Aspirator rate
Feed concentration X An increase of the feed pump rate lowers the outlet Tout to achieve lower residual moisture content require a long
temperature and increases the temperature differ- residence time.4 The time required to evaporate a drop-
Product
An increase in solid concentration in the feed results in ence between the inlet and the outlet. let of pure water is reported to be of 0.03 s for a 10 μm
larger and more porous dried particles. This influence is X Reducing the pump rate, while holding the inlet Feed rate droplet and 3 s for a 100 μm droplet. These drying times
due to pure mass balance of input and output of sol- temperature and aspirator rate constant, leads to a are assumed to be considerably increased for a spray
id material. The optimal solid concentration depends drier final product. Time or Distance dired particle that forms a crust.11 The typical residence
strongly on the application.3 time for a laboratory scale spray dryer is of 0.2-0.35s.11
Figure 9: Temperature profiles of the product and gas during spray
drying in co-current mode.3

8 9
Glass transition temperature
The glass transition temperature Tg is the temperature
above which the structure of the matrix switches from a
rigid glassy state to a rubbery state. This is associated
with product stickiness. The Tg of the feed depends on
the constituent solutes in the feed. For example, water is
known to depress Tg considerably, while high molecular
weight components such as maltodextrin can be used
to make Tg of the feed higher. In order to avoid product
stickiness and associated problems, such as caking and
lumping of the product during packaging, the outlet tem-
perature should not exeed Tg during the process.3,4
Advantages and disadvantag-
es of spray drying
Advantages of spray drying
Spray drying is a valuable technique to convert liquid
feeds into dry powder and is widely used in industries
such as the food, pharmaceuticals or materials.
It is appealing for both research work and high tonnage
production due to its rapid, continuous, reproducible,
single-step, and easily scalable process.5–7 The prod-
uct properties and quality can be effectively controlled;
spherical and relatively uniform particles can be readily
produced.6
Spray drying has many advantages. It provides the ad-
vantage of weight and volume reduction, its gentle pro-
cess can handle a broad spectrum of compounds includ-
ing heat sensitive substances such as biologic products,
pharmaceuticals or food nutrients.5–7 It also works under
inert atmospheres, needed to protect the products, or
for organic based liquids without process risks.6
When comparted to other drying techniques, such as
freeze-drying, the spray drying process is shorter and
cheaper since it does not involve deep freezing of the
samples and requires less energy consumption. Some
researchers have explored the use of spray-drying as an
alternative method to freeze-drying.7
10
Disadvantages of spray drying
Despite the many advantages, some challenges arise
when applying this technology. Due to a loss of product
on the wall of the drying chamber and into the exhaust
air, yields in laboratory scale experiments are far from op-
timal and are reported to be in the range of 20-70 %.7 At
industrial scale however, yields increase with larger scale
setups since the lost fraction is a smaller part of the pro-
duction volume.7 Insufficient forces of liquid atomization
and the ineffectiveness of the cyclone in separating fine
particles with a diameter below 2 μm, makes the produc-
tion and the recovery of sub-micron particles tedious.7
Applications
Microcapsules and microspheres can be produced from
a wide range of materials and by a large number of meth-
ods such as emulsion solvent evaporation, prilling by vi-
bration, extrusion, centrifugal extrusion, freeze-drying,
coacervation, spray-cooling, spray-chilling, spray drying
etc. Although many techniques were developed, spray
drying is one of the most common technologies to obtain
granulated substances due to its single step process, its
mild process conditions, and its scalability12,13
In general, the application for spray drying can be divid-
ed into distinct areas (Figure 11), amongst them drying,
structural change, encapsulation or amorphous solid
dispersion3,14–16
Drying a material
Simple drying of a material to a powder is still the most
common application of spray drying. Several substances
such as food, proteins or viable organisms can be spray
dried in order to reduce their moisture content. Their
availability in powder form makes them easier to handle,
facilitates storage, transport, enhances the ingredient
conservation, improves the stability of the products and
increases their shelf-life.5,17
Drying is suitable for most real or colloidal solutions, for
emulsions and dispersions, as long as the dried product
behaves like a solid. Practical application of spray drying
include drying of milk, cornstarch or dyes. The aqueous
solution of the product is dispersed into fine droplets and
the solvent evaporates immediately to form a fine amor-
phous or crystalline powder.3
Structural Changes
Structural change involves either the micronization of a
product into smaller particles or the agglomeration/gran-
ulation of small particles into larger particles.
Reducing the size of the particle allows a more consis-
tent and convenient dispersion of the particles into a
solution and will have a positive effect on the solubility or
bioavailability of the final product. Typical examples are
salts or dyes. The product is dissolved in a solvent and
the solution is then spray-dried to obtain a small, dry,
amorphous or crystalline powder.3
Free-flowing, spherical particles with uniform morphol-
ogy are highly desirable for many applications and can
be obtained by spray drying. Nanoparticles are attracting
attention in several industry applications such as ceramic
material18, atmospheric plasma spray (APS) coating19,
drug formulation20,21 or drug delivery system22. Their
small size makes them challenging to handle and can
represent a risk for the health of the personnel using such
powders19,22. Agglomerating the nanoparticles is neces-
sary to overcome the previously mentioned issue19,23. For
applications in ceramic material or drug formulation for
example, a compression of the agglomerated material
is necessary to obtain the final product. The properties
of the agglomerated material will largely determine the
compaction behavior of the powder and the uniformity of
the final product18,20.
Spray drying is an established method to produce gran-
ulated material. A suspension is created between the
nano/micro-particles and a binder solution. The suspen-
sion is then spray-dried into solid spherical particles with
precise specifications18,20,23. If the used suspension con-
sists of nanoparticles, the resulting agglomerated prod-
uct comprises nanoparticles forming a nanostructured
powder in the sub-micrometer / micrometer size range23.
Through this approach, the properties of nanoscale par-
ticles are preserved into micrometer scale particles24.
Encapsulation
Encapsulation can be defined as a process which in-
volves the complete envelopment of pre-selected mate-
rials (solid, liquid and gases) within a porous or imperme-
able matrix and/or membrane using various techniques
to give miniature sized particles ranging from a few hun-
dred nano-meters up to a several millimeters in size. In
general, particles < 1 μm in size are called nanoparticles,
1-2000 μm are termed microparticles and > 2000 μm are
referred to as macroparticles25. By spray drying, nano-
and microparticles are generated.
There are six main benefits for encapsulating a material25
which are summarized in Figure 10.
Extraction aids Improved flow or organoleptic
for recovery & properties
deliver
Encapsulated
Prediction from
material
environment for
interactions
Targeting of
compounds to
Membrane Controlled release
specific sites for delivery
Figure 10: Schematic displaying the main reasons why encapsula-
tion of a product takes place
X Protection (stabilization) of the encapsulated
material from environmental conditions or interac-
tions such as heat, moisture, oxygen, shear forces
etc. used in food-, biotechnology-, pharmaceutical-
and cosmetic industries.
X Controlled or sustained release of the encap-
sulated material. This type of encapsulation has
found a myriad of applications in industries such
as food, pharmaceuticals, agriculture, textiles and
cosmetics.
X Targeting to specific sites which enables the en-
capsulated material to be delivered directly to the
site where it is required. This has found applica-
tions in pharmaceutical, medical and biotechnology
sectors.
X To enable the encapsulated material to act as ex-
traction aides for product removal. This is a relative-
ly new application and has found applications in ag-
riculture, environmental and biotechnological fields.
X Improved flow properties of the encapsulated material,
by converting a liquid into a solid particle which
improves handling, usage and storage. Encapsulation
also prevents direct contact between the encap-
sulated material and the operator, hence, enabling
safer handling of the encapsulated toxic materials.
11
X Improved organoleptic properties which is a very
common reason for using the technology and
has being used extensively in the food industry.
Encapsulating a material can help mask its un-
pleasant taste and/or smell improve its visual ap-
pearance as well as its texture.
Typical examples for microencapsulation are flavors and
fragrances or oils. To encapsulate a liquid, an emulsion
is created between the liquid immiscible product and a
solution containing the carrier substance and the filmog-
en. This emulsion is then spray-dried, leading to a solid
matrix around dispersed droplets of the liquid, forming
an immiscible product.3
The process to encapsulate a solid is analogous to the
process above. A dispersion is created between the
solid product and a solution containing the carrier and
the filmogen. The dispersion is spray dried to lead to an
agglomeration or coating of the suspended particles.3
Small droplets of the product are stored in the carrier
substance and embedded in the filmogen.
Amorphous Solid dispersion
Amorphous solid dispersion is principally used in the
pharmaceutical industry to increase the dissolution rate
of a particular drug and thereby improve its bioavailability.
Many new drugs have low solubility in aqueous media.
In the amorphous state, the drug molecules can interact
with solvents molecules through intermolecular interac-
tion thereby improving drug solubility. The excess ther-
modynamic properties of the amorphous form, however,
also results in a tendency to crystallize with non-negli-
gible adverse consequences on drug solubility. When
incorporated into an amorphous polymeric carrier, the
drug amorphous state is stabilized and the dissolution
rate and bioavailability are improved.
In order to form a solid dispersion, the drug and the car-
rier(s) are dissolved in a solvent in which they are all sol-
uble. The solution is then spray dried so that the drug is
incorporated in amorphous polymeric carriers14–16.
12
Drying Amorphous solid dispension Selection of matrix and shell
materials
A
Carriers and wall materials are amongst the most im-
portant components of the spray drying process. Their
choice affects feed properties, such as emulsion stabil-
ity and powder properties, such as flowability, mechan-
B
D E F ical stability and shelf life of the product.14,26 Criteria for
A B C selecting the right matrix should be based on physi-
A: Liquid product B: Droplets C: Solid particles co-chemical properties, such as chemical composition,
C solubility, molecular weight, glass/melting transition tem-
peratures, crystallinity, viscosity, diffusibility, film forming
A: Polymer D: Solution of drug and polymer in solvent B and emulsifying properties.13,14,26 A wide variety of natural
B: Drug E: Droplets
C: Solvent F: Molecular mixture of API and polymer(s) and synthetic polymers is available depending on the
core material and the characteristicts desired in the final
Micronization Agglomeration & Granulation product.13
Characteristics of matrix and shell
materials
A A
Solubility
Since a spray dryer often deals with aqueous feed
preparation, the polymer should be soluble in water.13,14,26
C D E C D E Nowaday however, many molecules are insoluble in wa-
ter. In this context, the polymer should be soluble in a
solvent that is compatible with the molecule being en-
capsulated.16
B B
A: Solid product D: Droplets A: Solid products D: Droplet Emulsification property
B: Solvent E: Solid particles B: Binder dissolved in solvent E: Agglomerate of solid particles The emulsification property can be defined as the abil-
C: Solution of the solid product C: Suspension of solid particles
dissolved in the solvent in binder solution
ity to form a stable emulsion. It defines the maximum
amount of core that can be detained in the wall material
Encapsulation of liquids Encapsulation of solids and determines the encapsulation efficiency and struc-
tural stability together with droplet size. For hydrophobic
Liquid Solid cores, such as essential oils or lipids, the wall material
A A acts as stabilizer for the core.26
Film forming ability
Film formation can be defined as the ability to form a
thin and dense membrane around the atomized droplets
C D E C D E
while moisture is being removed at a rapid rate. The fast-
er the wall dries out to form a dense membrane around
the core, the better is the protection of the sensitive and
B B volatile coumpounds. The hardening of the wall materi-
al during spray drying forms a protective barrier against
A: Liquid product C: Emulsion A: Solid products D: Droplet
B: Solution of carrier D: Droplets B: Solution of carrier and filmogen E: Solid particles oxygen diffusion around the core and maintains low core
and filmogen E: Solid particles C: Dispersion temperatures despite high drying temperatures.13,26
Figure 11: Applications of spray drying
13
Viscosity
In order to facilitate atomization and to protect the ac-
tive component by early crust formation, it is important
that the wall material exhibits a low viscosity even at high
concentrations.13,26
Glass transition temperature
The glass transition is a phenomenon observed when an
amorphous system is changed to a rubbery, viscoelastic
material during heating. The temperature at which this
transition from glassy to rubbery happens is called glass
transition temperature (Tg).26
Below the glass transition temperature, the glassy state
is less vulnerable to recrystallization than the supercooled
liquid state above the glass transition temperature.16
The diffusion of the core material through the wall mate-
rial depends on whether the material remains in amor-
phous glassy state during the spray drying process. If the
particles remain below the glass transition temperature,
the polymer remains amorphous and the diffusion of the
core through the wall material is limited. On the other
hand, when the glass transition temperature is over-
reached, the wall material becomes rubbery and fast dif-
fusion of the core molecules occurs.26
In order to achieve a good stability of the powder, it is im-
Frequently used matrix and shell exhibit low viscosities at high solids content and have
materials in spray drying a good water solubility. They, however, lack interfacial
properties required for a high encapsulation efficiency
Several matrices are available for spray drying, each of and are therefore often associated with other materials
them having different properties and release character- such as proteins or gums.13,14,26,27
istics. The selection of an appropriate material is there-
fore an important step in a successful process. In the Cellulose derivatives
following sections, commonly used polymers will be dis- Natural celluloses are unbranched polysaccharides
cussed. where the monomer glucose units are connected by 1,4
glycosidic β-linkage. Pharmaceutical cellulosic excipients
Carbohydrates are typically semi-synthetic derivates of natural cellulose.
Carbohydrate polymers are some of the mostly used Their solubility mainly depends on the degree of substitu-
polymers in spray drying. They can be classified in five tion (3 hydroxyl groups per glucan unit), molecular weight
subcategories (Figure 12): starch derivatives, cellulose and uniformity of the substitution. HPMC (hypromellose)
derivatives, plant exudates and extracts, marine extracts, is the most extensively employed cellulosic derivative. It
microbial and animal polysaccharides.13,27 works as a stabilizer for the preparation of amorphous
solid dispersion of poorly water-soluble drugs. HPMC
Plant Marine Microbial/Animal is a physicochemically diverse family of polymers, with
properties ranging from very high to low viscosity, solu-
Polysaccharides · Alignate,... · Chitosan
bility and surface activity. This variety arises due to a mix
· Xanthan
Starch derivatives
· Maltodextrine, of different grades with varying degree of methyl and/or
modified starch
hydroxypropyl substitutions of the hydroxyl groups of the
Cellulose derivatives
· HPMC... cellulose monomer.14,16
Plant extrudates
Gums
Gums are mainly used for their film forming and emulsion
stabilization properties. Acacia gum, also called gum
Arabic, is widely used due to its high solubility and low
viscosity in aqueous systems. It is also reported to have
excellent emulsification properties attributed to the pres-
ence of a protein fraction in its composition. Gum Arabic
can play a dual role as both a surfactant and a drying
matrix in the spray srying process. Acacia gum is known
to protect lipids from lipoxygenase and free radicals and
is stable over a wide range of pH. 13,14,26,27
The natural origin of this polymer however makes it prone
to variability in supply and quality.13,14,26,27
Pectin
Pectin is a natural water-soluble polysaccharide obtained
from the cell wall of plants. It shows good emulsifying
properties due to the presence of protein residues and
a high content of acetyl groups within the polymer com-
position.13,28

portant that the wall material exhibits a high Tg.16,26 Gen-

· Gum arabic
· Gum karaya Microencapsulation - Main Matrix and Shell Materials
· Pectin
erally, Tg of a polymer material depends on its molecular
Poly sacharides (and derivates): Microbial- or animal polysacharides:
weight and chain lengths. Tg increases with an increase
∙ Starch and ∙ Chitosan
in molecular weight and chain length.26 Figure 12: Carbohydrate matrix material and their sources27
∙ modified Starch ∙ Xanthan
The process yields also depend on Tg since the spray dry- ∙ Amylose ∙ Alginate Carrier
er should be operated with an outlet temperature below Maltodextrin and modified starches ∙ Amylopectin
Film forming
Acids: Emulsifier
Tg so that the wall material does not become sticky.3,4,26 Starch in its native state is insoluble in cold water and ∙ Dextrins Barrier to oxygen and water
needs to be modified chemically, biochemically and phys- ∙ Maltodextrins ∙ Tartaric acis Encapsulant
Degree of crystallinity ically to accommodate specific purposes. Many deriva- ∙ Polydextrose ∙ Malonic acis Water soluble
∙ Cyclodextrin Organic solvent soluble
If we assume that a sample can be subdivided into a tives of starch available on the market are cross-linked, Lipids
∙ Cellulose and Antioxidant
crystalline and an amourphous phase, the degree of oxidized, acetylated or partially hydrolyzed to provide a ∙ modified Cellulose ∙ Fatty acids
crystallinity is defined as the fraction of polymer that ex- large array of functional properties. Maltodextrins are the ∙ Mannitol ∙ Fatty alcohols
ists in a relatively ordered crystalline state. most common example of this class and are manufac- ∙ Trehalose ∙ Waxes
An increased degree of crystallinity leads to a reduced tured by hydrolysis of starch. The degree of hydrolysis is ∙ Phospholipids
Plant exudates and extracts:
rate of hydration and the release of the core is then de- assigned as a dextrose equivalent value (DE). The higher Synthetic (mainly for pharma)
∙ Gum Arabic
layed due to the poymer rigidity. The barrier and dissolu- this value is, the shorter is the glucose chain and the
∙ Gum Karaya ∙ Lutrol E127 (Poloxamer)
tion properties of the wall material are also influenced by higher are the sweetness and the solubility. Maltodextrins ∙ Pectins ∙ Eudragit (various)
the crystallinity, a higher degree of crystallinity favorises moreover have the ability to rapidly form a dense skin ∙ Etc. ∙ Polylactic acid (PLA),
barrier properties whereas a lower crystallinity leads to a around the core while drying, thereby increasing core ∙ poly(lactic-coglycolic acid) (PLGA)
Proteins: ∙ Kollidon (Polyvinylpyrrolidone PVP)
quicker dissolution.26 retention. They provide a good oxidative stability to the
The degree of crystallinity is therefore an important prop- core and their simple two-dimentional glucose structure ∙ Casein and
whey proteins
erty in terms of mechanical strength, permeability or dif- makes them easy to digest.
∙ Gelatin
fusibility and dissolution. Modified starches, corn syrup solids or maltodextrins ∙ Gluten

14 15
Chitosan
Chitosan is a polyaminosaccharide normally obtained by
alkaline deacetylation of chitin, one of the components
found in crustacean shells, invertebrates skeletal or fungi
and insect wall constituents. Chitosan is generally ob-
tained from the process waste of the shellfish industries.
Chitosan is a linear non-toxic, bioabsorbable polymer
with good film-forming properties. It is soluble in acidic
to neutral media and behaves as a linear polyelectrolyte
at acidic pH. It is however insoluble in aqueous medium.
Below pH 6.5, chitosan carries highly positive charge
density.
Chitosan is ideal for gradual release applications of vari-
ous compounds, it can adhere to the gastric mucosa and
is non-toxic, biodegradable and biocompatible. Since the
permeability of chitosan increases with a decrease in pH,
it has limited applications when the components need to
resist the acidic conditions of the stomach if release in
the intestines is required. Chemical modification of the
chitosan molecule to incorporate hydrophilic groups in
the structure can overcome the insolubility issue of chi-
tosan in water.26
Poly(lactic acid) polymers
In the past decades, biopolymers based on lactic acid
and glycolic acid and their copolymers have attracted
much interest as carriers in the preparation of different
medical devices and drug delivery systems due to their
excellent biocompatibility, biodegradability and non-tox-
icity in humans. 29
Poly(lactic acid) PLA is a relatively hydrophobic materi-
al belonging to the aliphatic polyesters commonly made
from α -hydroxy acids.30 It is a high-strength, high-modu-
lus polymer prepared from renewable resources and de-
gradable without any catalyst, by a simple hydrolysis of
the ester bond.30,31 PLA contains an asymmetric α-carbon
and therefore, possess two enantiomeric forms (D and L)
poly-D-lactic acid (PDLA) and poly L-lactic acid (PLLA)
and a racemic form.32 PLGA, poly D,L-lactic-co-glycolic
acid, is created when the D- and L- lactic acid forms are
in equal ratio.30,31 The molar ratios of lactic to glycolic ac-
ids in PLGA polymers is critical in determining the in vivo
degradation rates.32 PLGA polymers are commercially
available and approved by the US Food and Drug Ad-
ministration (US FDA) for human use at various molecular
weights and lactic/glycolide ratios. They are commonly
used for controlled release of various molecules and sev-
eral products can be found on the market.33
16
Proteins
Whey protein
Whey proteins are a by-product of cheese production.
They exhibit good film and gel-forming properties and
are efficient emulisfiers. They are reported to efficiently
entrap volatile and non-valatile molecules in their matrix
and to have inherent antioxidant activity.26 To avoid unde-
sirable effect such as flocculation due to the unfolding of
the protein structure, it is important to pay attention to the
pH of the system. This aspect needs to be taken into ac-
count when the process involves major changes in pH.26
Gelatin
Gelatin is a low price, non-toxic, biodegradable by-
product of animal products processing. It is a combina-
tion of peptide and proteins obtained by the hydrolysis
of collagen. Reports show that compared to commonly
used matrices such as maltodextrin or mannitol, gelatin
has all the properties of an effective entrapping agent. It
has a good water-solubility and wall-forming ability, high
emulsifying and stabilizing abilities due to the proteins
present in its compostion and forms a fine an dense net-
work upon drying.13,26
Lipids
Lipids have very poor powder flowability due to their
sticky and tacky nature and low melting point. Usually,
they are used in combination with a hydrophobic glidant,
such as Aerosil 200, that can also affect release proper-
ties. A good balance between flowability and release can
then be created.16
Vinyl polymers
Vinyl polymers are commonly used as carriers in spray
dryed formulation. They consist of a vinyl backbone and
various types of substutions. The chemistry of the side
chains produces vinyl polymers with different proper-
ties.16 Polyvinylpyrolidone (PVP) are commonly known
by their trademarked name Kollidon. They are made of
N-vinylpyrrolidone monomer units and are often used as
carriers. They are stable and soluble in a variety of sol-
vents such as water, alcohols, chlorinated hydrocarbon
(DCM), esters/ethers, which makes them easy to spray
dry along with molecules of varied solubility profiles.
PVP are available with several viscosities. The suffix “K”
in PVP is obtained by measuring the polymer viscosity
in a water solution. K12 to K30 are the most commonly
used types of PVP.14,16
(Meth)acrylate polymers 9. The outlet temperature can be regarded as the up-
Poly(meth)acrylate are commonly available with the tra- per thermal load on the product. Make sure that the
dename Eudragit. They are synthetic polymers with vary- product is not damaged by an excessively high out-
ing ratios of two to three methacrylate monomers, such let temperature.
as methacrylic acid, methacrylic acid esters or dimethyl- 10. As soon as the desired operating conditions are
aminoethyl methacrylate. These polymers are suitable found and are stable, the feed tube is changed from
matrix or coating agents for targeted release, since they the pure solvent to the prepared feed solution. The
show a high pH dependence in their aqueous solubil- spray drying process starts.
ity influenced by the ratio of monomers. The solublity 11. After the solution is completely spray dried, switch
of poly(meth)acrylate in a large range of solvents also back to the pure solvent and continue spraying for
makes them easy to spray dry along with molecules of a short time to remove product deposits in the hos-
various solubility profiles.16 es and the nozzle. Occasionally take the feed tube
out of the solvent reservoir and allow some air to
  be sucked through. This will help ensure an efficient
Procedure to run a spray dry- cleaning process.
ing experiment 12. Pump the feed tubing empty, turn off the peristaltic
pump and lower the pump bed.
To carry out a spray drying trial with the Mini Spray Dryer 13. Turn off the the heater. The system can now be al-
B-290, the following procedure is suggested.3 lowed to cool down.
14. As soon as the temperature in the instrument falls
1. Switch on the instrument. The instrument carries out below 90 °C, the aspirator can be turned off and the
an automatic self check and then switches automat- product collection vessel with the product can be
ically to the operating mode. removed.
2. Adjust the spray gas flow to about 40 mm with the
rotary valve.
3. Pre-select the desired inlet temperature with the
push-button.
4. Turn on the aspirator. For standard applications, the
aspirator rate should be 100 % to maximize the sep-
aration rate within the cyclone. If a small powder hu-
midity is required, the aspirator rate can be decreased.
5. Turn on the heater and wait until the system has
reached steady conditions.
6. Switch on the peristaltic pump. Use pure solvent,
e.g. distilled water in case of aqueous solutions, at
the beginning of a trial.
7. Check if the spray cone is symmetrical and located
in the axis of the spray cylinder. If this is not the case,
the nozzle may be dirty or defective.
8. Adjust the outlet temperature by adjusting the flow
rate of the pure solvent. The feed pump rate can be
adjusted by means of the push-buttons for the per-
istaltic pump control. The pump rate strongly influ-
ences the outlet temperature, since the water draws
energy from the gas by evaporation. Thus, the outlet
temperature can be set to the desired value by vary-
ing the quantity of liquid via the pump rate setting of
the peristaltic pump.
17
 
Guidelines on the choice of X A high aspirator rate yields a higher degree of sep-
starting process parameters2–4 aration in the cyclone.

X To achieve a product with low residual moisture and
high thermal efficiency, the inlet temperature should
be set as high as possible.
X To achieve a final product with low residual
moisture, the inlet temperature has to be set as
high as possible and the difference in temperatures
betwen the inlet and the outlet temperature has to
be as small as possible.
X The choice of the inlet temperature should take into
consideration the heat sensitivity of the compo-
nents of the feed.
X A lower aspirator rate leads to lower residual
moisture content.
X The outlet temperature should be below the glass
transition temperature (Tg) of the product in order to
prevent product collapse and stickiness in the col-
lection vessel.
X Adding high molecular weight components, such
as maltodextrin in the feed material can increase
the Tg of the feed material.
Fields of application

X Increasing the feed flow rate reduces the outlet
temperature and increases the difference between
the inlet and the outlet temperatures. This results
in a product with higher residual moisture content.
X The higher the feed flow rate, the larger the size of
the particles in the final product.
Over the past years, spray drying has gained importance
as a method to produce dry powder, due to its continu-
ous, gentle, single step, scalable process. It is success-
fully used in, food- ,chemical- and pharmaceutical-in-
dustries (Figure 13) for production and research24.

X With a two fluid nozzle, a higher spray gas flow

tends to result in smaller particles.

Food Chemical Pharmaceutical

applications applications applications

Milk powder, eggs, coffee Cosmetics Pulmonary delivery,

granulation, encapsulation

Infant food Detergents, soaps,...

Biopharmaceutical
Pesticids, herbicids,
products such as enzymes,
Animal feed fungicides, insecticids,
hormones, amino acids,
fertilizers,... peptides and protein

Encapsulation of flavors Pigments, paints and dyes

Encapsulation of flavors, Antibiotics, vaccines,

Ceramic materials and vitamins, yeast,..
bioactive compounds,
material sciences
neutraceuticals

Figure 13 : Applications of spray drying

18 19
Food applications

In food technology, products such as coffee, dried eggs, products with good solubility properties, keeps flavor
powdered milk, animal feeds, cake mixes, infant formu- loss to a minimum, allows processing of heat sensitive
las, starch derivatives, nutritional oils or yeasts are usu- foods with high retention of their nutritive content, and
ally manufactured by spray drying. Spray drying yields has an economic potential for scale up6,24,34.

Table 1 shows examples of common applications in the food industry and gives their starting process parameters.

Sample Nozzle Sample Solvent Carrier Filmogen Inlet Outlet Aspirator Gas spray flow Feed rate Yield
concentration temperature temperature speed

Two-fluid - Water - - 150 °C 100 °C 38m3/h 650 L/h n.a n.a

Coffee
Ultrasonic
- Water - - 150 °C n.a 20m3/h max 3.6m L/min n.a
60kHz, 0.8W

Beer Water
Two-fluid Original - - 180°C 108°C 100% 550 L/h n.a 80%
(Alcohol 5%)

Baby food Two fluid 40% Water - - 160 °C 95 °C n.a n.a n.a n.a

Milk (whole) Whole milk

Two-fluid Water - - 130 °C 90 °C 34m3/h 600 L/h n.a 60-80%
concentrated to 50%

Milk (semi-skimmed) 180 °C

Two-fluid 10% Water - - 100 °C 38m3/h 700 L/h n.a 60-80%
Nozzle needs to be cooled

Milk (skimmed) Two-fluid 10% Water - - 130 °C 75 °C 27m3/h 630 L/h n.a 74%

Egg yolk 66% (80g egg yolk

Two-fluid Water - - 100°C 54°C 38m3/h 600 L/h n.a 10%
40g water)

Whey Two-fluid 6-45% Water - - 180°C 80°C n.a n.a n.a n.a

Casein Two fluid 6% Water - - 150 °C 90 °C 38m3/h 600 L/h n.a 60%

Lactose Two-fluid 30% Water - - 160 °C 105 °C 38m3/h 400 L/h n.a 60%

Starch Two-fluid 30% Water - - 100 °C 65 °C 38m3/h 600 L/h n.a 50%

Citric acid Gelatin

Two-fluid 15% Water - 150°C 95°C 38m3/h 650L/h n.a 80%
Concentration n.a

Plant extract None or

Two-fluid - Water/Ethanol 1:1 - 120 °C 70 °C 38m3/h 600 L/h n.a 60%
Maltodextrin 10%

Fruit concentrate Maltodextrin

Two-fluid 30% Water - 150°C 90°C 38m3/h 700 L/h n.a 65%
Maltodextrin : fruit 8:2

Juice Maltodextrin
Two-fluid - Water - 150-175°C 95-115°C 38m3/h 600 L/min n.a 60%
5% or more

Flavour Two-fluid 25-80% Water Maltodextrin Arabic gum 120-160°C 75-95°C 38m3/h 600 L/h n.a 60-70%

Arabic gum
Two-fluid 25-80% Water Maltodextrin 130 °C 90 °C 38m3/h 650 L/h 6 mL/min 60%
5% w/V
Oil
Three-fluid Maltodextrin 20% w/w Shell : 4.5mL/min
5% w/V Water 150 °C n.a 38m3/h 1750 L/h n.a
nozzle 10% w/V Maltodextrin/Arabic Gum 2:1 Core : 0.2mL/min

6% w/w 1010cfu/g Gelatin / Arabic gum /

Bifidobacteria Two-fluid Water Gelatin / Arabic gum / starch 100 °C 50-60 °C 38m3/h n.a n.a 82%
dry weight starch

Yeast Two-fluid 11% Water - - 210 °C 120 °C 38m3/h 550 L/h n.a 77%

X More information about the encapsulation of bioactive oils X BUCHI, application note 218/2016, Spray drying skim X BUCHI, Application note 302/2017, Protection of
can be found in the following application notes: milk, concentrated milk and full cream milk bioactive oils using encapsulation

20 21
Chemical applications

In the chemical industry, products such as cosmet- persion into paint. Additionally,, granulation via spray in order to obtain free-flowing powders. These powders X Coatings in turbine engines, automotive parts, pho-
ics, detergents, pesticides, herbicides, pigments and drying can improve flow and distribution of molecules are then further processed to batteries, bioceramics, tocatalytic and biological implants (titania, alumina,
dyes or ceramic materials are commonly obtained by and particles in the final product. In material science, or used for advanced materials research purposes24. zirconia, yttria coatings)
spray-drying. Reducing the size of particles found in spray drying is mainly applied to granulate nanoparti- Spray dryed nanomaterials (nanoparticles, nanosus- X Advanced Ceramics of metal carbides, nitrides or
dyes enables a more consistent and convenient dis- cles into sub-micrometer- to micrometer size particles pensions) are often used as:∙ borides (eg. new super conducting ceramics)
X Toners and Magnetic Tapes (eg. ferrites)
Table 2 shows examples of common applications in the chemical industry and gives their starting process parameters.

Sample Nozzle Sample Solvent Carrier Filmongen Inlet Outlet Aspirator Gas spray flow Feed rate Yield
concentration temperature temperatue speed
Acrylamid Two-fluid 50 % Water - - 125 °C 70 °C n.a n.a n.a n.a
Aluminium oxide Two fluid 67% Water - PVA 180 °C 120 °C 38m3/h 630 L/h n.a 76%
Ammonium chloride Two-fluid 20% Water - - 120 °C 57 °C 38m3/h 650 L/h n.a 73%
Ammonium nitrate Two-fluid 20% Water - - 180 °C 100 °C n.a n.a n.a n.a
Calcium carbonate Two-fluid 50% Water - - 180 °C 100 °C 38m /h3
800 L/h n.a 73%
Chinese / Egypt blue Two-fluid 30% Water Silicium oxide - 180 °C 120 °C 38m3/h 700 L/h n.a 70%
Diamond powder Two-fluid 10-45% Water - - 200 °C 125 °C 38m /h3
650 L/h n.a 60-99%
Dye Two-fluid 45% Water - - 120 °C 100 °C 38m3/h 650 L/h n.a 86%
Essential Oil Two-fluid 20-30% total solid Water Maltodextrin Arabic gum 120-150 °C 70-100 °C 38m /h3
500-700 L/h n.a 60-80%
Foam bath Two-fluid 20% Water Sodium chloride - 150 °C 100 °C 38m3/h 650 L/h n.a 60-80%
Glass powder Two-fluid 50% Water - - 140 °C 90 °C 38m3/h 600 L/h n.a 65%

Indigo Two-fluid 30% Water Sodium sulphate - 150 °C 90 °C 38m3/h 600 L/h n.a 85%
Lead oxide Two-fluid n.a Water - - 150 °C 90 °C 38m /h3
500 L/h n.a 60-80%
Metal oxide Two-flluid 10-60% Water - PVA 130-200 °C 80-100 °C 38m3/h 600-750 L/h n.a 50-80%
Polyacrylamide Two-fluid 9% Water - - 204 °C 111 °C 38m /h3
600 L/h n.a 45%
Polyacrylate Two-fluid 10% Aceton - - 65 °C 49 °C 38m3/h 600 L/h n.a 26%
Polyacrylic acid Two-fluid 20% Water - - 150 °C 80 °C 38m /h3
750 L/h n.a 33%
Polycarbonate Two-fluid 10% DCM - - 180 °C 130 °C 38m3/h 750 L/h Gas: N2 n.a. 80%
PVC Latex Two-fluid 32% Water - - 160 °C 90 °C 38m3/h 630 L/h n.a 71%
Rubber latex Two-fluid 20% Water - - 120 °C 70 °C 38m /h3
500 L/h n.a 60%
Silicon (metallic) Two-fluid 50% Isoporopanol - - 168 °C 110 °C 38m3/h 600 L/h Gas: N2 n.a. 68%
Silicon carbide (SiC) Two-fluid 40% Isopropanol - - 145 °C 90 °C 38m /h3
600 L/h n.a 75%
Sodium Aluminium-
Two-fluid 20% Water - - 125 °C 70 °C 38m3/h 600 L/h n.a 60-80%
silicate
Sodium Citrate Two-fluid 20% Water - - 160 °C 90 °C 38m3/h 630 L/h n.a 60%
Sodium dihydrogen- Two-fluid 40% Water - - 180 °C 107 °C 38m3/h 650 L/h n.a 85%
phosphate
Sodium sulphite Two-fluid 24% Water - - 180 °C 90 °C 38m3/h 800 L/h n.a 87%
Low viscosity
Strontium titanate Two-fluid 30% Water - 160 °C 79 °C 38m3/h 660 L/h 12mL/min 68%
Na-Alginate 0.35%
Tantalum Two-fluid 50% Water/Ethanol 1:1 - - 170 °C 100 °C 38m3/h 400 L/h n.a 60%
Titanium carbide Two-fluid 40% Water - PVA 150°C 81°C 38m3/h 350 L/h n.a 60%
Titanium dioxide Two-fluid 4% Water - - 212 °C 103 °C 38m3/h 700 L/h n.a 70%
Zeolite Two-fluid 10% water - - 180 °C 120 °C 38m /h3
630 L/h n.a 60%
Zirconium hydroxide Two-fluid 50% Water - - 180 °C 110 °C 38m3/h 600 L/h n.a 60%
Zirconium oxide Two-fluid 50% Water - - 180 °C 100 °C 38m /h3
600 L/h n.a 98%
Zirconium oxide:
Two-fluid 30-60% Water - - 175 °C 130 °C 38m3/h 700 L/h n.a 77%
yttrium oxide 9:10

More information about the use of spray drying in flavors and fra- X BUCHI, Application note 248/2017, Micro-encapsulation of X BUCHI, Application note 250/2017, Spray drying strontium titanate X BUCHI, Application note 293/2018, Graphene-based compos-
grance or advanced material applications can be found in the fol- Flavors and Fragrances by Spray Drying X BUCHI, Application note 289/2017, Spray drying cemented ites for lithium batteries by spray drying
lowing documents: X BUCHI, Best@Buchi 69/2015, Spray drying of advanced material tungsten carbide

22 23
Pharmaceutical applications

In pharmaceutical industries, applications include the properties for controlled drug release35, or to improve
spray drying of excipients, of pure drugs or the encap- the dissolution of low water soluble drugs such as car-
sulation of drugs. Spray drying is widely used to man- bamazepine, ibuprofen or ketoprofen.
ufacture products with defined physical and chemical

Table 3 shows examples of common applications in the pharmaceutical industry and gives their starting process parameters.

Sample Nozzle Sample Solvent Carrier Filmongen Inlet Outlet Aspirator Gas spray flow Feed rate Yield
concentration temperature temperatue speed
Albumin Two-fluid 5% Water - - 110 °C 60 °C 38m3/h 650 L/h n.a 60%

Amino acids Two-fluid 3% 7N NH4OH - - 196 °C 93 °C 38m /h

3
650 L/h n.a 69%

Algae Two-fluid 9-17% Water - - 120-220 °C 62-130 °C 38m3/h 670 L/h 8 mL/min 71-98%

Antibody (anti-IgE Ab) Two-fluid 80:20 anti-IgE Water Lactose and mannitol 90-140 °C 50-55 °C 38m3/h 900-1050 L/h 5-15 mL/min 50-90%
Ab :mannitol
Bacillus subtilis spores Two-fluid 3% Water Milk powder - 100 °C 73 °C 38m3/h 650 L/h n.a 80%

Blood plasma Two-fluid 5% Water - - 180 °C 100 °C 38m /h

3
600 L/h n.a. 75%

Budenoside Two-fluid 10% Water Mannitol - 130 °C 93 °C 38m3/h 700 L/h n.a 62%

Carotenoid Two-fluid 25% Water Gelatine - 170 °C 100 °C 38m3/h 630 L/h n.a 60%
Gelatine: Carotenoide
6:4
Diclofenac Two-fluid 1mg/mL Water 55% Aerosil 200 in suspension 140 °C 90 °C 38m3/h - n.a 60-70%
Eudragit S90
Enzyme/coenzyme Two-fluid 12% Water - - 80 °C 55 °C 38m3/h 630 L/h n.a 60%

Gelatin Two-fluid 13% Water - - 160 °C 110 °C 38m /h

3
630 L/h n.a 60%

Inuline Two-fluid 25% Water - - 170 °C 90 °C 38m /h

3
650 L/h n.a
53%

Lactose Two-fluid 30% Water - - 160 °C 105 °C 38m3/h 400 L/h n.a 60%

Mannitol Two-fluid 10% Water - - 150 °C 90 °C 38m3/h 700 L/h n.a 67%

Pollen Two-fluid - Water/Ethanol 1:3 Maltodextrin Arabic gum 190 °C 100 °C 38m3/h 700 L/h n.a 60-80%
750 L/h
Polycarbonate Two-fluid 10% DCM - - 180 °C 130 °C 38m3/h n.a 80%
Gas : N2
Polymethylacrylates Two-fluid 5% Methanol - - 99 °C 60 °C 38m3/h 800 L/h n.a 48%
Eudragit
Streptococcus Two-fluid 40% Water Low fat milk powder, Gelatin low 90 °C 70 °C 38m3/h 800 L/h n.a 45%
glucose viscosity
Vaccine mixture Two-fluid - Water - - 190 °C 140 °C 38m3/h 600 L/h n.a 60-80%

Warfarin Two-fluid 20% Water - - 150 °C 95 °C 38m /h

3
650 L/h n.a 60%

More information about the use of spray drying in the pharma and X BUCHI, Application note 245/2016, Spray drying of microalgae X BUCHI, Best@Buchi 57/2010, Laboratory scale spray drying of X BUCHI, Best@Buchi 59/2010, Laboratory scale spray drying of
biotech industries can be found in the following documents: X BUCHI, Application note 291/2017, Micro-encapsulation of lactose: A review inhalable drugs: A review
nucleic acids by spray drying

24 25
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