PARTICLE SIZE REDUCTION

By: [Link] Rawal

 Advantages of size reduction
[Link] uniformity– Ease of Mixing: Mixing turn out to be effective only when the ingredients are small and of uniform
size. As the particle is of small size, the no of particles per unit dose is large. And greater the no. of particles, mixing
becomes more efficient. This criterion is particularly more important for the formulations that contain low dose drugs.
[Link] flow– If the size of particle is optimum, the flow of powder into dies during the compression of tablets is
effective.
[Link] extraction of drugs– Penetration of solvent into tissue or cells of organic origin becomes rapid when the
particle size is smaller.
[Link] drying– If the size of granules is small, then the drying of granular mass becomes rapid.
[Link] physical stability– In suspensions and emulsions, the rate of sedimentation decreases if the particles are
of small and uniform size.
[Link] rate of dissolution– When the surface area is larger, than the dissolution of a substance increases. Thus
size reduction facilitates in increasing the surface area.
[Link] absorption rate– Smaller the particle, the faster is the absorption is the absorption because the dissolution
is also enhanced.
[Link] irritation: Grittiness or coarse particles in ointments
9. Enhanced physical appeal and appearance: especially in creams, ointments, pastes.
10. Dosage form requirements: DPI-particle size <60 mm required for efficient lung deposition.
Factors affecting size reduction:
Material properties:
1. Hardness: Surface property of the material, devised by the Moh’s scale (1-10). Material of
hardness is 1-3 for talc and waxes, 4-7 for bauxite, limestone. 8-10 for quartz, diamond.
2. Toughness: Soft but tough is difficult to reduce than hard but brittle.
3. Abrasiveness: property of hard materials. 0.1% contamination may occur due to wear from the
mills
4. Stickiness: Property to stick may block the screen and adhere to grinding surfaces, obstructing
milling.
5. Slipperiness: may resist milling due to lubrication action.
6. Softening temperature: Heat generation during milling may be an issue for waxy substances.
7. Moisture content: Moisture content affects hardness, toughness, viscosity affects milling
efficiency. <5% moisture is adequate for dry milling and > 50 % for wet milling.
8. Crystallinity: Crystalline property breaks across CLEAVAGE PLANES
9. Fines to coarse particle ratios
[Link] energies of solids
Factors affecting size reduction:

Machine properties:
1. Inefficient Feed control
2. Insufficient capacity of discharge conveyor
3. Power consumption
4. Selection of appropriate crushing chamber.
 Mechanism of Particle fracture and size reduction

9
 Mechanism of Particle fracture and size reduction
 Particles, be it amorphous or crystalline, will have flaws to a definite degree.
 These constitute weak parts in the particles.
 When ,sufficient stresses such as impact, shear and compression are applied, the
weak flaws develop into cracks, which eventually lead to cleavage (Figure 6- 1 a).
 Thus, smaller particles are obtained with additional surface area .
 When stress in the form of attrition is applied, the particle surfaces chip and
produce small particles (Figure 6-1 b ).

10
The Mechanism of Size Reduction
In the grinding process, materials are reduced in size by fracturing them.
In the process, the material is stressed by the action of mechanical
moving parts in the grinding machine and initially the stress is absorbed
internally by the material as strain
energy.

Stress>> Strain>>> Fracture in lines of Weakness >>>Released Heat

When the local strain energy exceeds a critical level , which is a function
of the material, fracture occurs along lines of weakness and the stored
energy is released. Some of the energy is taken up in the creation of new
surface, but the greater part of it is dissipated as heat.
Loss of energy
-ln Figure, the initial- linear·
portion is defined by Hooke's
law. It states that stress is
proportional to strain.
-The slope of linear portion
represents -Young's modulus.
-It expresses the stiffness or
softness in mega pascals.
- If the force of impact (stress)
doesn’t exceed the elastic limit
(region of Hooke's law), the
material is reversibly deformed.
20
 Theories of Size reduction

21
22
23
 Energy for Size reduction:

24
27
28
• Some other laws:
• Holmes law
• Harris law
• Developed on a stress-
strain diag. for cubes
under compression.
Hence is more used for
mechanisms that ‘re
explained by
compression.
• Assumes that material
has flaws distributed
throughout the internal
structure.

• Limitations: The Kick’s

theory applies only
under the condition that
all energy is transferred
to surface free energy,
which is ideally
unpractical.
Applicable to the brittle materials
undergoing fine milling.

Limitations: The Rittinger’s theory

ignores particle deformation
before particle fracture.

OR
K= [Link]
W= 10 Wi (1/√dn-1/ √ di)

Wi
 Limitations of energy laws:

1. Does not exactly express the performance of any grinding or crushing process.
2. Information related to optimum operating condition and size of powder put through mill
cannot be utilized.

33
SUMMARY
 Example 1 : Sugar is ground from crystals of which it is acceptable that 80% pass a 500
μm sieve (Standard Sieve No.35), down to a size in which it is acceptable that 80%
passes a 88 μm (Standard Sieve No. 170) sieve. Calculate the work (energy consumed
W) if Wi is 1.272 with Bond’s equation.

Wi= 10 Wi (1/√dn-1/ √ di)

35
Size Reduction Mechanisms
 Size Reduction Equipments

A. Crushers (coarse and fine) Coarse mine material is crushed

1. Jaw crushers into lumps of 250 to 150 mm. Again
2. Gyratory crushers these lumps are broken into
3. Crushing rolls particle of 6 mm in size.

B. Grinders (intermediate and fine) Grinders reduce crushed feed to

1. Hammer mills, Impactors powder. The product from an
2. Attrition mills intermediate grinder might pass a
3. Tumbling mills 40-mesh screen and product from
a. Rod mills fine grinders pass a 200-mesh screen
b. Ball mills with a 74 m opening.
C. Ultrafine grinders
1. Fluid-energy mills Feed < 6 mm
2. In. Classified H.M Product: 1- 50 m
3. Agitated Mills
D. Cutting machines
Give particles of definite size and
1. Knife cutters, slitters shape, 2 to 10 mm in length
 MILLS AND THEIR APPLICATIONS
MILL ACTION PRODUCT SIZE USE FOR NOT USED FOR
Fibrous
CUTTER MILL CUTTING 20 to 80 mesh Crude(animal and Friable materials
vegetable drug)

Roller Mill COMPRESSION 20 to 200 mesh soft material Abrasive material

Hammer Mill Impact 4 to 325 mesh almost all drugs Abrasive material

soft and sticky

Disintegrator Impact 20 to 80 mesh almost all drugs
materials.
Attrition and
Ball Mill 20 to 200 mesh Brittle drugs soft materials
impact
Moderately hard
Attrition and soft and sticky
Fluid Energy Mill 1 to 30 microns and friable
impact materials
materials
Crushing and
Edge Runner Mill 20 to 80 mesh almost all drugs sticky materials
shearing
 Crushers

 Slow-speed machines

 coarse reduction

 large quantities of solids.

 The main types are

 jaw crushers
 gyratory crushers
 smooth-roll crushers
 Toothed-roll crushers

 The first three operate by compression and toothed-roll crushers

tear the feed apart as well as crush it.
 Jaw Crushers

 Two jaw - V opening

 One – Fixed jaw – anvil jaw

 Other – moving jaw – swinging jaw

 Angle b/w jaws 20o – 30o

 Jaws are flat or slightly bulged

crushed at upper portion & then dropped and recrushed at

narrow end
 250 – 400 times per min
Feed size = 1.8 m and product size = 250 mm
Capacity = 1200 ton/hr
Jaw Crushers
 Gyratory Crushers

 Jaw crusher with circular jaws

 Conical crushing head

 Funnel shaped casing open at the top

 Crushing head is carried on heavy shaft

 solid broken and re-broken again & again

 125-425 gyrations per min

 motion – Slow

 Product – continuous

 Capacity – 4500 ton / hr

 Relatively less power as well as maintenance required

Gyratory Crushers
 Crushing Rolls

 Heavy rolls rotating at slow speeds

 two heavy smooth faced metal rolls

 turning on parallel horizontal axis

 compression b/w rolls and then drop out

 turn to each other with same speed

 50 – 300 rpm

 narrow faces as compared to diameter

 feed 12 – 75 mm

 product 12 – 1 mm

 R.R < 5
 Crushing Rolls

49
Toothed Roll crusher

 Roll faces – corrugations , breaker bar, teeth

 may be One roll or Two rolls
 One roll working again a stationary curved breaker plate
 Disintegrators – two corrugated rolls – different speeds
 Small high speed rolls with transverse breaker bars on
its face turning toward a large slow speed smooth rolls
versatile but cannot handle very hard material
 Compression + Impact + Shear
Feed < 500 mm
 Capacity upto 500 tons/hr
 Toothed Roll crusher

51
Principle
Principle
 Grinders
 The term grinder describes a variety of size-reduction machines
for intermediate and fine duties.

 The product from a crusher is often fed to a grinder, in which it

is reduced to powder.

 The types of commercial grinders are hammer mill, impactors,

attrition mills and tumbling mills.
 Hammer Mills

 High speed rotor

 Cylindrical casing
 Horizontal shaft
 Swing hammers attached with rotor
 Hammers – impact + rubbing
 Discharge opening – Screen
 Feed (top) – Break(casing) – Product (bottom)
 4 – 8 hammers on single shaft
 Intermediate – 25 mm to 20 mesh size
 Fine - < 200 mesh at 0.1 to 15 ton/hr
 Versatile
 Capacity & Power req. – feed nature
 Reduce 60 – 240 kg per kWh
Principle:
 Construction & Working
 A hammer mill is essentially a hardened/stainless
steel drum containing a vertical or horizontal
rotating shaft or drum on which hammers are
mounted.
 The hammers swings on the ends or fixed to the
central rotor.
 The rotor is rotates at a high speed inside the drum
while material is fed into a feed hopper.
 The material is put into the hopper which is
connected with the drum.
 The material is powdered to the desired size due to
fast rotation of hammers and is collected under the
screen.
These are mainly operated at 2500 rpm or 1000 to 2500 rpm for the reduction
of the large sized particles. High speed rotor uses 8000-15000 rpm speed.

Output particle size : 10-400 um.

Factors affecting fineness:
The particle size of the material to be reduced can be easily controlled by changing the
speed of the rotor, feed rate, numbers and hammer type, clearance between hammers
and grinding plates, shape and size of the screen.
 Working:
• Hammers are allowed to be in continuous motion.
• The feed material is placed in hopper , ahioch flows vertically down and then
horizontally, while the hammers are in continuous motion.
• These roatating hammers beat the material to yield smaller particles.
• The particles then pass through the screen.
• Due to tangential exit, the size of particles is considerably smaller than the screen
aperture.

59 Commercial Hammer mill: [Link]

 ADVANTAGES OF HAMMER MILL
 Easy to setup, install, dismantle and clean-up.
 Occupies less space
 Versatile: can handle various feedstocks.
 It is rapid in action and operates in a cloased setup. Dust can be
prevented and explosion hazards too.
 They are easy to install and operate, the operation is continuous.
 There is little contamination of the product with metal abraded
from the mill as no surface move against each other.
 DISADVANTAGES

 Heat buildup during milling is more, therefore, product

degradation is possible.
 Hammer mills cannot be employed to mill sticky, fibrous
and hard materials.
 The screens may get clogged.
 Wearing of mill and screen is more with abrasive
materials.
 Impactor

 Heavy duty hammer mill except screen

 Impact alone
 Primary reduction machine
 Capacity = 600 TPH
 Nearly equi-dimensional particle
63
 Tumbling Mills

 Cylindrical shell
 Slowly turning about its horizontal axis
 Half filled by solid grinding medium
 Grinding medium
 metal rods in Rod mill
 balls of metal, rubber or wood in Ball mill
 pebble, porcelain or zircon spheres in pebble mill

 Operation - Continuous or Batch

 Impact + attrition
 Product - fines
 BALL MILL
 These are also knows as tumbling mills.

 Principle: The ball mill works on the principle of impact between

the rapidly moving balls and the powder material, both enclosed
in a hollow cylinder.
 Working: At low speeds, the ball roll over each other and attrition
(rubbing action) will be the predominate mode of action. Thus, in
the ball mill, impact or attrition or both are responsible for the
size reduction.

Ball Mill in working: [Link]

 The cylinder contains balls that can occupy
30-50% of the mill volume.
 Weight of the ball and size of balls depends
on feed size and diameter of the mill
 Balls/ grinding medium may be made up of
steel/iron/zirconium/ceramic material
 Drug + Balls should not occupy more than
60 % of the mill volume.
ADVANTAGES:
 It can produce very fine powder.
 Ball mill is used for both wet and dry grinding
processes.
 Toxic substances can be ground, as the cylinder is closed
system.
 Rod or bars can also be used as grinding media.
 (example: Sticky material are size reduced) In ball mill,
 installation, operation and labour costs are low.
Sterility can be maintained
DISADVANTAGES:
The ball mill is a very noisy machine.

Ball mill is a slow process.

Soft, fibrous material cannot be milled by ball

mill.
Wearing from the grinding media may cause
contamination
 Rod Mills

 Rolling compression + attrition

 Several sizes of rods – 25 to 125 mm in diameter
 intermediate grinders
 20 mm feed to 10 mesh product

Ball Mill or Pebble Mills

 Impact + Compression
 ball 25 to 125 mm
 Pebble 50 to 175 mm
Uses:
• Fine grinding for up to 100-5 micron product size.
• Preferred for harder and abrasive materials.
• SS. Balls when used, the mill can be used for ophthalmic
product formulation
• Also can be used for pesticides, dyes and pigments.
Continuous ball mill: [Link]
 Ultrafine Grinders

 All particles passing a standard 325-mesh (44 μm)

 high speed hammer mill with internal classification
 Fluid energy or jet mills
 Agitated mill (wet)
 Colloid Mills
 Fluid Energy Mills

 Particles suspended in high velocity gas stream (fluidization)

 Elliptical or circular path
 inter - particle interaction + striking + rubbing
 Coarse particles remain in circulation
 Working
 product – 0.5 to 10 μm
Feed – 1 ton/hr - non sticky
 1 – 4 kg of steam or 6 – 9 kg of air
per kg of product
Principle