Granulation

Fine particles are

difficult to handle
and to process
Granulation-converts
fine particles to
granular materials
with controlled
physical properties
Why granule?

Reason

Typical Application

To produce useful structural forms

Powder metallurgy

To provide a defined quantity for dispensing Agricultural

chemical
and metering
Pharmaceutical tablets
To estimate dust handling hazards or losses Briquetting of waste fines
To improve product appearance

Food products

To reduce caking and lump formation

Fertilizer

granules,

To improve flow properties for further Pharmaceuticals, ceramics

processing
To increase bulk density for storage
detergents
To control dispersion and solubility

Instant food product

To control porosity and surface to volume

ratio
To improve permeability for further
processing
To create non-segregating blends of powder
ingredients

Catalyst supports
Ore smelting
Ore
smelting,
agricultural
chemicals,pharmaceuticals

Size enlargement - granulation, compression

Granulation - uses a liquid
blender
to
form
interparticle bonds and
agitates the powder-liquid
mass to promote liquid
dispersion and granular
growth. Fluidized beds
tumbling drums and pans
Mixer granulators

Compression- use pressure

to promote interparticle
bonds. These processes
are often performed dry.
Powder flow is enhanced
by adding water
Roll pressing, extrusion
(wet or dry) tableting
and briquetting

granulation
Granulation used to produce
granules
with
defined
properties to meet specific end
use requirement.
Main
primary properties are granule
size distribution and porosity

Case study:
Herbicide and pesticide
powders must be dispersed in
water by the farmer before
spraying onto crops. Small
particle size is needed so that
particles do not setle out in
the tank. However fine
powders are hard to disperse
in the water. They are dusty,
cake in the bag and can be
inhaled by the farmer.

Water dispersible granules

It is critical in processing to
To achieve the desired
control the granule
properties, clays and
surfactants are added to porosity. If the porosity is
too low, the granule will
the formulation to help
not disperse in water;
granules disperse once
they are wet. Additional too high, and granules
binders may be added to attrit to produce dust
during handling
give the granules dry
strength during
transportation.

Particle and granule morphology

Good particle design means
understanding particleparticle and particle fluid
interaction and using this
knowledge to properly
design processes and
product

It is the properties of the

particle that dictate these
interaction.
The discrete nature of a
particulate system means
that it is heterogeneous.
Two particles in the same
system do not have the
same properties- hence
need to measure property
distributions and sampling
is a major issue

Particle and granule morphology

The properties of particulate

system cannot be tabulated like
the thermodynamics
properties of fluid. The
properties of the system
depend not only on the
chemical composition but also
on the particle morphology.
You cannot look up surface
area of sand in the handbook
of chemistry and physics but
you have to measure it

The properties are not always

easy to define.example is
particle size - volume diameter,
surface diameter, stokes or drag
diameter,specific surface
diameter , particle sieve
diameter,projected area
diameter,ferets diameter,
martins diameter, scattering
diameter
Historically, many particle
properties have been difficult
and time consuming to measure

GRANULE PROPERTIES
Morphology
dependent
properties : bulk
density, flowability,
reactivity,
permeability,
dispersibility
and
dissolution

PERFORMANCE AREA

RELEVANT PROPERTIES

MEASUREMENT
TECHNIQUE

Strength,attrition
resistance

Fracture toughness
Hardness
Porosity
Internal angle of friction
Wall angle of friction
Unconfined yield stress
Bulk density
Size distribution
Size distribution

Uniaxial compression
Indentation,notched bar
Mercury porosimetry
Shear cell

Bulk solids flow

Packaging and storage

Segregation
Dispersion
dissolution

Caking

and Contact angle

Porosity
Pore size distribution
Dissolution rate
Moisture content
Hydroscopy tendency
Phase transition

Resistance to fluid flow

Permeability
Size distribution

Appearance

Shape
colour

Sessile
washburn,flotation

Drying
Differential scanning
Calorimetry
Dilatometry
Permeameter

Image analysis

drop,

Properties of Granulation product

inhalation and explosion risks
Improved flow and handling which facilitates controlled
metering
Increased bulk density
Reduced pressure loss for fluid flow through a packed bed
useful in blast furnaces and leach heaps
Controlled dissolution rates
Co-mixing of particles segregate during handling
Maintain a high proportion of the surface area of the
original particles useful application involving catalyst or
processes required rapid dissolution
reduced dustiness which minimese losses

Granulation and tabletting

Oral solid dosage forms (i.e. tablets) are the preferred delivery route for many
drugs.The final properties of the tablet and their dissolution characteristics are
influenced by
the process parameters of the tablet press - impeller speed, granulation
time,amount of binder liquid and its rate of addition
the choice of ingredients and
by the various preparatory processes such as granulation.
Most common type wet granulation
liquid binder is distributed over the bed to initiate granule formation. Result
granule-consists of the primary particles arranged as a three dimensional porous
structure

Wet granulation is often required as a pre-processing step to tabletting as not all

drugs are suitable for dry agglomeration or direct compression due to poor
compactability, bad flow or segregation.

Granulation and tabletting

Impeller speed controls granule size and granulation rate .
Granulation time is the length of mixing time after the binding
liquid has been added.
Control of this parameter is essential for successful granulation.
Longer granulation times lead to higher densification of the
granules .
Feeding rate and quantity of granulating liquid determines particle
size of the granulate and also influences granule density .

Liquid addition is critical as the process of agglomeration proceeds

within a narrow range of liquid content . The granulation process is
susceptible to over wetting which leads to uncontrollable
agglomerate growth.

Granulation Rate Processes

Formation or agglomerates is controlled by three rate processes.

Wetting and nucleation where the liquid binder is brought into

contact with a dry powder bed and is distributed through the bed to
give a distribution of nuclei granules

Consolidation and coalescence- where collisions between two

granules, granules and feed powders, or a granule and the equipment
lead to granule compaction and growth

Attrition and breakage- where wet and dried granules break due to
impact, wear or compaction in granulator or during subsequent
product handling

Granulation Rate Processes

The first stage distribution of the liquid binder
through the feed powder
Two extreme cases:
1)

The liquid drop size is large compared to unit

particle size

2)

The particle size is large compared to the drop size

When the drop size is larger than the particle size,

wetting the powder with the liquid gives a
distribution of seed granules or nuclei

Four stages of nucleation process

Droplets are formed at the spray nozzle at
some size distribution and frequency
Binder droplets impact on the powder
surface. Drops may coalesce at the powder
bed surface and increase the effective drop
size
The drops spread across the bed surface
and penetrates into the bed by capillary
action to give a loosely packed nuclei
granule
Shear forces within the bed may break up
large wet clumps and nucleate into smaller
entities
These processes combine to define the nuclei
size distribution produced as the powder
passes through the spray zone of the
granulator

Drop size smaller than particle

When the drop size is small
compared to the unit particle
size, the liquid will coat the
particles. The coating is produced
by collision between the drop
and the particle followed by
spreading of the liquid over the
particle surface. If the particle is
porous, then liquid will also suck
into the pores by capillary action.
The wetting dynamics control the
distribution of coating material
which has a strong influence on
the latter stages of growth

Distribution of liquid binder through the feed

powder
The initial wetting and liquid distribution to produce nuclei or coat particles is
important because
Poor wetting leads to very broad nuclei size distributions - a mixture of
overwet and ungranulated material
Often the granulation retains a memory of the nucleation stage with broad
nuclei size distributions leading to broad granule size distributions
Preferential distribution of liquid between individual ingredients can cause
component segregation with granule size
Wetting phenomena also influence downstream granule processes such as
drying and redispersion in fluids.
Both the rate and extent of wetting are important for understanding
nucleation and binder distribution

Powder surface properties

When a drop of liquid sits on
a solid surface, there are
three surface (intefacial)
energies to consider
Solid liquid interfacial
energy,sl
Liquid vapour interfacial
energy, lv
Solid-vapour interfacial
energy sv

Methods of characterizing powder surface properties

Washburn test measures the
penetration profile of a liquid in a
powder bed as a function of time.
First, the penetration profile for a
liquid that perfectly wets the
powder (zero contact angle) is
measured to determine the
effective capillary radius, R. Then,
the contact angle of any other fluid
can be measured from the
penetration profile for that liquid
through a similarly prepared
powder bed

Penetration of liquid into a powder bed

Washburn test

The equilibrium height of rise =balance

between capillary and gravity forces
acting on the liquid in the capillary:

When the fluid first starts to rise up the

capillary, it will be resisted by viscous
losses. From Hagen-Poiselle equation,
the viscous pressure drop at some height
h is:

this P drop is equal to the available capillary

P difference:

Penetration of liquid into a powder bed

If gravity is ignored (h<<he)
then P drop is equal to the
available capillary pressure
difference

Substitute into equation 2 and

integrate which give the
height of liquid in the
capillary as a function of
time:

The contact angle

can be calculated
from the slope of a
plot of h2 vs t
provided R, and
lv are known

Wetting and nucleation regime for granulation

Identification of conditions to
ensure good nucleation
Nucleation Process can be break
down into three regimes:
Droplet controlled-most
favourable
-Each
individual
drop
wets
completely and quickly into the
powder bed to form a single
nuclei granule. The nuclei size
distribution
is
essentially
controlled by the drop size
distribution

Two conditions are required to

achieve drop controlled
nucleation
Drop penetrate into the bed
quickly and do not roll on the bed
surface and contact other drops
Drops overall on the powder
surface is minimal
Drop penetration rate is set by
wetting thermodynamics and
kinetics-primarily influence by
formulation properties
Drop overlap-related to flux of
drops hitting the powder surface
and is set by operating
parameters

Drop controlled nucleation regime

-occur at low penetration time
At high spray flux, 1, there will
and low dimensionless spray flux,
significant overlap of drops hitting
the powder bed. Nuclei granules
formed will be much larger and their
size will no longer be a simple
Where Q=solution flow rate, vs =
function of the original drop size. At a
powder velocity in the spray
given spray flux value, the fraction of
zone, dd=average drop diameter
the powder surface that is wetted by
and ws = width of the spray. The
spray drops as it passes beneath the
dimensionless spray flux is a
spray zone (
) is given by
measure of the density of drops
falling on the powder surface. At
low spray flux (
<<1),drop
and the fraction of nuclei
formed by
footprints will not overlap and
n drops,
each drop will form a separate
nucleus granule

Wetting and nucleation regime for granulation

Shear controlled
Liquid pooling or caking
occurs where the spray
meets the bed. Binder
distribution occurs only
by breakage of lumps or
granules due to shear
forces within the powder
bed and the nuclei size
distribution is
independent of the drop
size distribution

Intermediate:
Some agglomeration does
occur in or near the
spray zone without
complete caking or
pooling
Refer page 345 for
Nucleation regime map

Wetting and nucleation regime for nucleation

Wetting thermodynamics,
wetting kinetics and ratio
of powder to liquid fluxes
in the spray zone
influence the nucleation
regime. It is much easier
to control the size and
size distribution of drops
from a spray nozzle than
it is to mechanically
disperse the liquid
through the bed.

Drop penetration into

powder beds
Theoretical prediction of drop
penetration time
Consider a drop hitting the
loosely packed,moving
powder bed surface in a
tumbling or mixer
granulator.
How long will this drop take to
penetrate into the powder
bed and what is the effect
of formulation properties
on penetration time?

Drop penetration into powder beds

The porous powder bed
consists of a series of
capillary pores. For a drop
to penetrate the pores, the
contact angle between the
liquid and the powder must
be less than 90 (wetting
thermodynamics). If this is
so, drop penetration is
driven by capillary suction
and the rate at which liquid
penetrates the pore is given
by the washburn equation

Consider a drop of volume Vd

hitting the powder surface.
The drop will have a circular
footprint on

The rate at which the liquid

flows from the drop is (1)

Drop penetration into powder beds

Where is the powder
voidage. The average
velocity in the pore, is
given by the differential
form of the washburn
equation (2):

Combining equation 1
and 2 and integrate
gives the penetration
time i.e the time for the
total volume of drop to
penetrate the bed

Conclusion
Improved wetting is
desirable. It gives a
narrower granule size
distribution and
improved product
quality through better
control over the
granulation process.

The rate of wetting

increased by:
Reduce viscosity
Increase surface tension
Minimizing contact angle
Increasing the size of
pores within the powder
Viscosity is determined by
the binder concentration
and the operating
temperature

Granule Consolidation
Consolidation used to
describe the increase in
granule density caused by
closer packing of primary
particles as liquid is
squeezed out as a result
of collisions.
Only occur whilst the
binder is still liquid
Determines the porosity
and density of the final
granule

Factors:
Particle size
Particle size distribution
Binder viscosity
Granule saturation
(fraction of pore space
filled with liquid) is
influenced by granule
porosity and liquid level

Granule Consolidation

Saturation increases as the porosity increases

Saturation exceeds 100%, further consolidation
pushes liquid to the granule surface,making the
surface wet

Growth
Stokes number is the
parameter which
determines whether
coalescence will occur or
not
A measure of the ratio of
collisional kinetic energy
to energy dissipated
through viscous
dissipation

For coalescence to occur,

The stoke number must
be less than a critical
value Stk*

Growth
Three regime of granule
growth for batch system
with relatively low
agitation intensity
Non inertial
Inertial
Coating regimes

Non inertial
-Stokes number is less than
Stk* for all granules and
primary particles and all
collisions result in
coalescence.
Growth rate is independent of
liquid viscosity, granule or
primary particle size and
kinetic energy of collision.
The rate of wetting of the
particles control the rate of
growth

Growth
Inertial regime
As granule grow, some collision
will occur for which the stokes
number exceeds the critical
value.
Growth rate is dependent of
liquid viscosity, granule or
primary particle size and
kinetic energy of collision.
The proportion of collisions for
which the stokes number
exceeds the critical value
increases and the proportion
of successful collisions
decreases

Coating regimes
Stokes number for the powder
mass in the granulator is
comparable with the critical
value, granule growth is
balanced by breakage and
growth continues by coating
of primary particles onto
existing granules.

TWO TYPES OF GROWTH BEHAVIOUR

STEADY STATE
Granule size increases is roughly
proportional to granulation
time- a plot of granule size
versus time is linear
INDUCTION GROWTH
Occurs when there is a long
period during which no
incresae in size occurs. The
granules form and
consolidate,but do not grow
further until the granule
porosity is reduce enough to
squeeze liquid to the surface.

Figure 13.5

This excess free liquid on the

granules causes sudden
coalescence of many granules
and a rapid increase in granule
size.

Granule growth regime map

Deformation during granule
collisions can be characterize by a
stokes deformation number,Stdef
relating the kinetic energy of
collision to the energy dissipated
during granule deformation.
All types of granule growth can be
described using the saturation
and deformation,Stdef and the
granule growth regime map.
At very low liquid contents, the
product is similar to a dry
powder. At slightly higher granule
saturation,granule nuclei will
form but there is insufficient
moisture for these nuclei to grow
any further.

For systems with high liquid

content, the behaviour
depends on the granule
stength and Stdec. A weak
system will form a slurry, an
intermediate strength system
will display steady growth and
a strong system (low St def)
wil exhibit inductive time
behaviour. At extremely high
liquid saturation, rapid growth
occurs when the granule grow
in size extremely quickly and
any induction time is reduced
to zero

Granulation equipment
Tumbling granulator
Particles are set in
motion by the
tumbling action
caused by the
balance between
gravity and
centrifugal forces.
These granulators
have the following
characteristics:

Product granule size is in the range 220mm. Not suitable for producing very small
granules
-good for producing high density `balls or
pellets. It is more difficult to produce high
porosity agglomerates
Can also be used for coating relatively large
(group D) particles
Discs and drums generally operate
continuously and can be up to 4 m in
diameter. They are capable of very large
throughputs ( up to 100 tonne/hr) and are
therefore extensively used in mineral
processing and fertilizer granulation

Disc Granulator

Wetting fluids which promote

growth are generally applied by
a series of single-fluid spray
nozzles distributed across the
face of the bed. Solids feed and
spray nozzle locations have a
pronounced
effect
on
granulation performance and
granule structure. Variations of
the simple pan shape include (1)
an outer reroll ring which allows
granules to be simultaneously
coated or densified without
further growth, (2) multistepped
sidewalls, and (3) a pan in the
form of a truncated cone.

Granulation equipment
The required disc-rotation speed
is given in terms of the critical
speed, i.e., the speed at which
a single particle is held
stationary on the rim of the
disc due to centripetal forces.
The critical speed is Nc= (g sin
f/ 2p2D) ^0.5.Where g is the
gravitational acceleration, f is
the angle of the disc to the
horizontal, and D is the disc
diameter. The typical
operating range for discs is 50
to 75 percent of critical speed,
with angles f of 4555.

This range ensures a good

tumbling action. If the speed is
too low, sliding will occur. If the
speed is too high, particles will
be thrown off the disc or
openings develop in the bed,
allowing spray blow through and
uneven buildup on the disc
bottom.
Proper
speed
is
influenced by flow properties of
the feed materials in addition to
granulation performance.

Granulation equipment
Discs range in size from
laboratory models 30 cm in
diameter up to production
units of 10 meters in diameter
with throughputs of 100
ton/hr. When scaling up from
laboratory or pilot tests it is
usual to keep the Same disc
angle and fraction of critical
speed. Power consumption
and
throughput
are
approximately proportional to
the square of disc diameter,
and disc height is typically 1020 percent of diameter

It should be emphasized
that these relationships
are best used as a guide
and in combination with
actual experimental data
on the system in question
in order to indicate the
approximate effect of
scale-up. A key feature of
disc operation is the
inherent size.

Granulation equipment
Fluidized
Granulators
(fluidized beds and
spouted beds)
Application:
fertilizers,
industrial
chemicals,
agricultural chemicals,
pharmaceutical
granulation, and a
range
of
coating
processes.

Fluidized bed granulator

Advantages
High volumetric intensity
Simultaneous
granulation
and
drying removes the need for
additional dryer
Mechanically simple
Can easily produce small (minus
1mm) porous granule from
powder feeds
Can produce high strength layered
granules with a very tight size
distribution from liquid feeds
Very good heat and mass transfer
rates
Robust and sensitive with regard to
the impact of operating variables
on product quality

Disadvantages
Defluidization due to
quenching (excessive
growth) if the operating
variables are not controlled
well
High operating costs for air
handling
Attrition rates may be high
and dust recovery
equipment is essential
Poor operation with fine,
cohesive powders

Mixer Granulators

Use a mechanical impeller to cause powder motion,

while the granulator as a whole is usually fixed in
space.Liquid binder is sprayed onto the moving
powder bed

Mixer granulator s
Advantages
Can process cohesive
powders and spread
viscous binders
Will generally produce a
product
Only process to make
small (less than 1 mm)
dense granules

Disadvantages

High capital, maintenance

and operating costs
Granules are less
spherical than tumbling
granulators
Most complex of
granulators
Difficult to scale and
maintain product
attributes

Mixer granulator s
High Shear mixers
Impeller/chopper
rotate at moderate
to
high
speed
generating
high
shear rates and
impact velocities in
some region of the
mixer

Batch high shear

granulators
Vertical shaft
:Fielder,Diosna,Gral
Horizontal shaft: Lodige
Eccentric shaft: Eirich
Impeller rotates at speeds
of between 60 and 800
rpm
Capacity: 10 L to 1200L
Typical batch time: 5 min

Mixer granulator s
F

Fielder

Lodige

Granulator
Method

Product Granule

Tumbling
0.5-2.0
(disc,drum)
Mixer(continuous 0.1-2
and batch high
shear)
Fluidized beds,
0.1-2
(bubbling, spouted
beds)

Granule density

Scale/Throughput

Moderate

0.5-800 t/h

Low < 200

kg/batch

< 50 t/h or
cohesive

High

<500 kg/batch