CHAPTER 10 / PARTICLE SIZE REDUCTION  easily reduced by lowering temperature

below the glass transition point

 Aid efficient processing of solid particles by  stearic acid - waxy
facilitating powder mixing or the production of  gums - sticky
suspensions  moisture content of the feed material influences the
 comminution process of size reduction
Other special functions: • below 5% for dry grinding
 Exposing cells in plant tissue prior to extraction of the • greater then 50% requires wet grinding
active principles
 Reducing the bulk volume of a material to improve ❖ Energy Requirements of Size Reduction Process
transportation efficiency  2% of the total energy is used in comminution
  Only a very small amount of energy put into a
✓ Influence of Material Properties on Size Reduction comminution operation affects size reduction
❖ Crack Propagation and Toughness  Remainder is lost by:
 Propagated through regions of material that possess 1. Elastic deformation
the most flaws or discontinuities, and are related to 2. Plastic deformation without fracture
the strain energy in specific regions 3. Deformation initiate cracks that cause
 Theory of crack propagation – Griffith fracture
 Stress in the material is concentrated at the tip of a 4. Deformation of metal machine parts
rack 5. Interparticulate friction
 Rapid propagation that excess energy from strain 6. Particle-machine wall friction
relaxation dissipates and concentrates at other 7. Heat
discontinuities = cascade effect 8. Sound
 Not all materials are brittle and resist fracture 9. Vibration
therefore they undergo plastic flow and allows strain  Theories relating Energy input to the degree of size of
relaxation reduction produced:
 Ease of comminution depends on the brittleness or a) RITTINGER
plasticity of the material because of their relationship  Energy is proportional to the new surface
with crack initiation and crack propagation area
b) KICK
❖ Surface Hardness  Energy is proportional to the change in size
 Hardness of a material can be described by its c) BOND
position in a scale devised by a german mineralogist  Energy used to crack is proportional to the
MOHS new crack length
 Mohs Scale of Hardness d) WALKER
• Diamond >7 – hard that it can scratch  Link theories of Rittinger and Kick and in
anything below it some, Bond
• Talc <3 – soft enough to be scratched by
anything above it ✓ Influence of Size Reduction on Size Distribution
 More quantitative measurement of surface hardness 1) Uneven Milling
was devised by BRINELL  Broken down and particles in different size ranges
• harder materials are more difficult to undergo breakage
comminute and can lead to abrasive wear of 2) Particle Agglomeration
metal mill parts, which can result to product  Causes size enlargement
contamination  Interactive cohesive forces dominate comminution
• Rubber stresses over increasing surface areas
 has large elastic component are
extremely soft yet difficult to reduce ✓ Size Reduction Methods
 capable of absorbing large amounts of ❖ Cutting Methods
energy through plastic and elastic o Size Reduction Range
deformation without crack initiation  100-100,000 um
o Principles of operation
CASTILLO 3I PH
  CUTTER MILL
 consists of series of knives attached to a
horizontal rotor that act against a series of
stationary knives attached to the mill casing
 during milling, size reduction occurs by
fracture of particles between the 2 sets of
knives, which have a clearance of a few mm
 screen is fitted in the base of the mill casing
and acts to retain material in the mill until
sufficient degree of size reduction has been
affected
 High shear rates are useful in producing coarse
degree of size reduction of dried granulations
prior to tableting
 Useful in producing a coarse degree of size
reduction of dried granulations prior to
tableting and fibrous crude drugs such as
roots, peels or barks prior to extraction
 Two cylindrical rolls horizontally and rotated
about their long axes
❖ Impact Methods
o Size Reduction Range
 Vibration mills: 50-8000 um
 Hammer mills: 1-1000 um
o Principles of operation
 HAMMER MILL
 Consists of four or more hammers hinged on a
central shaft enclosed within a rigid metal case
 Produce powders with narrow size
distributions
 Hammers may be: square-faced, tapered to a
cutting edge or have a stepped form

o Alternative Techniques
 VIBRATION MILL
 Filled to approximately 80% total volume with
porcelain or steel balls
 The whole body of the mill is vibrated, and size
❖ Compression Methods reduction occurs by repeated impaction
o Size Reduction Range
 End-runner mills: 50-10,000 um
 Roller mills: 1000- more than 100,000 um
o Principles of operation
 Small laboratory scale: mortar and pestle
 Mechanized forms: end-runner mills and edge-runner
mills---both now rarely used
 EDGE RUNNER MILL
 A weighted pestle is turned by the friction of
material passing beneath it as the mortar
rotates under power
❖ Attrition Methods
 Pestle equivalent mounted horizontally and o Size Reduction Range
rotating against a bed of powder, so that size
 Attrition methods: 1-200 um
reduction occurs by attrition as well as
o Principles of operation
compression—rarely used in pharmaceutical
 ROLLER MILLS
production
 are used to produce size reduction of solid in
o Alternative Techniques
suspensions, pastes or ointments
 ROLLER MILLS
 Two or three porcelain or metal rolls are
 one roller is driven directly
horizontally mounted with a 20um gap
 the other is rotated by friction

CASTILLO 3I PH
  Rollers rotate at different speeds so that the  Turbulence: ensures particle-particle
material is sheared as it passes through the gap collisions are high
 Transferred from a faster to slower roll using  A particle size classifier is incorporated
scraper
❖ Combined Impact and Attrition Methods
o Size Reduction Range
 Fluid energy mills: 1-50,000 um
 Pin mills: 10-10,000 um
 Ball mills: 1-200 um
o Principles of operation
 BALL MILL
 Hollow cylinder rotated on its horizontal
longitudinal axis
 Usually contain balls with many different
diameters owing to self-attrition—this helps to
improve the product as the large balls tend to
break down the coarse feed materials and the
smaller balls help form the fine product by
reducing void spaces between balls  PIN MILLS
 The balls occupy 30-50% of the total volume  Two discs with closely spaced pins rotate
 Too much feed produces a cushioning effect against one another at high speeds
 Too little causes loss of efficiency and abrasive  Impaction between pins as the particle
wear of the mill parts travels outwards causes particle size
 Speed rotation: greatest importance in the reduction
operation  It is influenced by centrifugal force
 Low angular velocity
 the balls move with the drum until the force
due to gravity exceeds
 Size reduction is minimal because there is
relative movement of balls.
 High angular velocity
 the balls are thrown out on the mill wall by
centrifugal force
 no size reduction occurs
 Usually 0.5 rev/sec.

o Alternative Techniques
 FLUID ENERGY MILLING
 Jet mill
 Hollow 20-200 um toroid
 Fluid is injected as a high-pressure jet
through nozzles at the bottom of the loop
 High kinetic energy causes the particles to
impact with other particles
CASTILLO 3I PH
 ✓ Selection on Particle Size Reduction Method
Mohs Hardness Tough Sticky Abrasive Friable
FINE <50um
1-3 (soft) Ball, vibration (under liquid nitrogen) Ball, vibration Ball, vibration, pin,
fluid energy
3-5 (intermediate) Ball, vibration Ball, vibration, fluid
energy
5-10 (hard) Ball, vibration Ball, vibration,
fluid energy
COARSE 50-1000um
1-3 (soft) Ball, vibration, pin, roller, hammer, Ball, pin Ball, roller, pin,
cutter (all under liquid nitrogen) hammer, vibration
3-5 (intermediate) Ball, roller, pin, hammer, vibration, Ball, roller, pin,
cutter vibration, hammer
5-10 (hard) Ball, vibration Ball, vibration,
roller
VERY COARSE >1000um
1-3 (soft) Cutter, edge runner Roller, edge Roller, edge cutter,
runner, hammer hammer
3-5 (intermediate) Edge runner, roller, hammer Roller, hammer
5-10 (hard) Roller Roller

CASTILLO 3I PH