SIZE REDUCTION
▪ Introduction
▪ Definition
▪ Objectives
▪ Mechanism
▪ Laws governing size reduction
▪ Factors affecting size reduction
▪ Equipments
Hammer mill
Ball mill
Fluid energy mill
Edge runner mill
End runner mill
INTRODUCTION
Raw materials are generally present in large size which cannot be
used by industries ,so materials need to be converted into smaller size
particles or powders.
Definition
Process of reducing large solid masses into small unit masses.
[or]
Conversion of large sized materials into small sized particles or
powders.
THEORY
Comminution action of losing a material.(eg. mineral substance)
Diminution reduction in size.
Pulverization grinding to powder or dust.
Normally powders are polydispense it create difficulties in the production of
dosage forms.
So, uniform size particles are only used in the production it is achieved by
size separation.
OBJECTIVES
✓ Optimum particle size of the material is required.
For good suspension.
For mixing of the particles in a mixture.
For unit operation like filtration and sedimentation.
For compression of powders into tablets.
To provide excellent flow properties to powders.
Smaller the particle size ,better the absorptive properties.
✓ Optimum surface area of the material.
✓ Reduction in the bulk of the material.
MECHANISM
▪ Impact
▪ Attrition
▪ Compression
▪ Cutting
▪ Shear
▪ Impact and attrition combined method.
A) IMPACT
• High speed moving object hits a stationary material.
or
Moving particle strike against a stationary surface.
eg . Friable materials.
• IMPACT further impact
un milled particle flaws develop to cleavage of particle
with line of weakness cracks to smaller size
Eg : fluid energy mill and hammer mill
B)ATTRITION
• Breaking down of particles by rubbing action between two surfaces with
pressure and friction.
Attrition
Un milled
Particle edges break
Eg . Fluid energy mill
C) COMPRESSION
• Pressure is applied onto the material to break into small pieces.
Eg . Soft materials
pressure is
applied to the material
Eg . Roller mill
D) CUTTING
• Material is cut by means of sharp blades with their mechanical
action.
Eg. Fibrous and waxy material.
Eg . Cutter mill
E) SHEAR
• Combination of cutting and crushing.
• Equipments consists of both knife and bars.
Eg . Colloid mill
LAWS GOVERNING SIZE REDUCTION
▪ Rittinger’s theory (energy α surface area)
▪ Kicks theory (energy α size changes)
▪ Bonds theory (energy α crack length)
▪ Griffith theory (energy α crack length)
[Link] THEORY
• Energy required for size reduction of unit mass is directly proportional
to the new surface area produced.
ε = KK (Sn – Si)
where,
ε = amount of energy
KR = rittingers constant
Sn = new specific surface area
Si = initial specific surface area
KICKS THEORY
• The energy used in deforming or fracturing a set of particle of
equivalent shape is proportional to the ratio of the size changes
ε = Kk log di/dn
where,
Kk = kicks constant
di = diameter of the particle in initial
dn = diameter of new particle
BONDS THEORY
The energy required for the propagation of a crack is proportional to the new
crack length produced.
ε = 2KB (1\ 𝒅𝒏 - 1\ 𝒅𝒊 )
where,
KB = bonds work index
dn = new diameter of particle
di = initial diameter of particle
GRIFFITH THEORY
The stress applied to a particle for its size reduction is
influenced by the length of the crack and by the
application of stress at the crack apex.
Tensile strength, T=
𝑦𝑜𝑢𝑛𝑔𝑒𝑠 𝑚𝑜𝑑𝑢𝑙𝑒 (𝑦) 𝑥 𝑠𝑢𝑟𝑓𝑎𝑐𝑒 𝑒𝑛𝑒𝑟𝑔𝑦
\𝑐𝑟𝑎𝑐𝑘 𝑝𝑎𝑡ℎ 𝑟𝑒𝑞𝑢𝑖𝑟𝑒𝑑 𝑓𝑜𝑟 𝑓𝑢𝑡𝑢𝑟𝑒 (c)
𝑜𝑓 𝑜𝑏𝑗𝑒𝑐𝑡 𝑐𝑜𝑛𝑡𝑎𝑖𝑛𝑖𝑛𝑔 𝑐𝑟𝑎𝑐𝑘 (𝜀)
T = 𝑦ε\c
c = in metre
ε = joule\metre
T and Y = mega pascal.
GRAPHICAL REPRESENTSTION OF
SIZE REDUCTION
According to hookes law , this stress strain is studied.
Hookes law states The strain of the material is directly
proportional to the applied stress within the elastic limit of the material.
YOUNGES MODULE = Slope of the linearity ,which means the nature
of the solid (stiff or solid)
ELASTIC DEFORMATION = The material within the hookes region
which means does not exceed the elastic limit.
YIELD VALUE = Elastic limit of the particle.
IRREVERSIBLE DEFORMATION = Once the stress applied to the
particle curve exceeds the yield point and fracture of the particle
takes place.
MERITS
➢ UNIFORM MIXING
By decreasing the particle size uniform particle size can be
achieved it helps in the formulation of low dose drugs.
➢ FLOW CHARACTERISTICS OF PARTICLE
By decreasing the particle size the uniformity can be
achieved it helps in the flow characteristics of tablet and
capsule manufacture.
➢ EXTRACTION OF DRUGS
By decreasing the particle size the surface area is increased
so the extraction is also increased.
➢DRYING PROCESS
with optimum size particles drying can be easily achieved.
➢ PHYSICAL STABILITY
By reducing the particle size the physical stability of emulsion
and suspension can be increased.
➢ DISSOLUTION RATE
By reducing the particle size the surface area is increased ,so
the dissolution rate is also increased.
➢ ABSORPTION RATE
By reducing the particle size absorption can be increased.
DEMERITS
➢ DEGRADATION OF DRUGS
If the particle size is reduced the surface area is increased so it
causes increased degradation.
eg. Thermolabile drugs susceptible to heat during size reduction.
➢ INEFFECTIVE MIXING
Very small size particles forms lumps due to increased adhesive
forces so ineffective mixing occurs.
➢ CONTAMINATION
Contamination may happen due to milling apparatus.
APPLICATIONS
a) Size reduction is used in the extraction process of insulin
from pancreas.
b) It is employed in the preparation of medicinal plant
products as it fastens the drying process of medicinal
products.
c) It is employed in the manufacturing of sulphonamides and
calomel dosage forms as it enhances their respective
antibacterial and antiseptic properties.
d) It is also employed in the preparation of gum acacia of
higher grades.
e) It finds use in the preparation of chlorampenicol as fine
particles of the drugs show enhanced rate of absorption.
f) It is employed in the manufacturing of griseofulvin , since
finely powdered griseofulvin is more effective than the coarse
dosage form.
g) It is employed as a quality control check in the
manufacturing of pharmaceuticals as it serves as a key
factor to achieve the desired particle size.
f) Suspensions and emulsion have slow rate of settling and
creaming.
FACTORS INFLUENCING SIZE
REDUCTION
1) Hardness
2) Toughness
3) Stickiness
4) Material structure
5) Moisture content
6) Softening temperature
7) Physiological effect
8) Feed size
9) Bulk density
1) HARDNESS
• Very hard material can be size reduced.
• Hardness of the material affects the process of size reduction.
• Mohrs scale is an arbitrary scale used to measure hardness.
• A scale is numbered from 1 to10 for mineral substances from graphite
to diamond.
• The soft material are numbered from 1 to 3(eg. graphite).
• Hard materials are numbered above 7 ( eg. Diamond)
• Intermediate materials are numbered between 3 and 7 (limestone).
2) TOUGHNESS
A soft material which is tough is difficult to be size reduced.
Eg . Vegetable drugs which are fibrous in nature like barks, roods and
twigs.
3)STICKINESS
Material which are sticky in nature ,stick to the grinding surfaces.
Inert substances like kaolin is added to prevent it.
4)MATERIAL STRUCTURE
Many of the substances have characteristic structures.
Eg . Mineral substances - have lines of weakness.
Vegetable drugs - have cellular structure
5) MOISTURE CONTENT
If material undergoes dry grinding – material concentration should
be less than 5%.
If material undergoes wet grinding – material concentration should
not be more than 50%.
6) SOFTENING TEMPERATURE
Waxy substances like stearic acid or drug containing oils or fats,
become softening during the size reduction process, if heat is
generated . This can be avoided by cooling the mill.
7) PHYSIOLOGICAL EFFECT
Very potent substances are size reduced in enclosed mills.
Eg . Hormonal drugs.
8) FEED SIZE
Small feed size is generally introduced in size reduction
apparatus to produce fine grinding.
9) BULK DENSITY
Bulk density increases ,efficiency of mill is also increased.
BULK DENSITY = weight of dry powder
------------------------------
bulk volume
•
CLASSIFICATION OF MILLING EUIPMENTS
Intermediate and fine Ultra fine grinders Crushers Cutting machine
grinders
-- Tumbling mill -- Fluid energy mill --Edge runner -- Rotary knife
-- Hammer mill -- Colloid mill mill cutter or
-- Pin mill or centrifugal -- End runner Rotary cutter
impact mill mill mill
-- Roller mill
[Link] MILL
PRINCIPLE
Works on the principle of impact
that is material is stationary and
hits a moving object at high
speed.
CONSTRUCTION
▪ Hammer are made by hardened steel, Stainless steel (S.S)
▪ Hammers may have 2 shapes
a) bar
b) Stirrup
▪ Hammers may be rigid/ swing type.
▪ Hammers are fixed to a shaft.
▪ Hammers are enclosed by a drum.
▪ At bottom of drum, screens will be placed.
WORKING
▪ Feed placed into the hopper.
▪ Hammers are allowed to rotate at 8000 to 15000 Rpm.
▪ Rotating hammers beat the material to yield smaller particles.
▪ Then these particles pass through the sieve.
▪ The screens are interchangeable , so that any grade of fineness
can be achieved.
USES
▪ Fine to moderate grinding of powders may be obtained depending
on the speed of hammer.
▪ Particle size may vary from 10 to 400mm.
▪ Used to mill dry materials, herbal medicines , etc.
ADVANTAGES
▪ Easy to setup, dismantle and clean –up.
▪ Occupies less space.
▪ It is versatile i.e speed and screen can be changed rapidly.
▪ As it is generated in closed environment, dust can be reduced.
DISADVANTAGES
▪ Screen may get clogged.
▪ Product degradation is possible due to heat buildup during milling.
▪ Cannot be used to mill sticky, fibrous and hard materials.
[Link] MILL/ TUMBLING MILL / PEBBLE MILL
PRINCIPLES:
Works based on the principle
of impact ( High speed moving
object hits stationary material) and
attrition ( Breaking down of particle
by rubbing action between two
surfaces.
With centrifugal force particles remain
At top without falling.
NOTE
Usefull for wet grinding.
• a) low speed with sliding.
• b High speed with centrifuging.
• c) correct speed with cascading.
CONSTRUCTIONS
▪ Large mill is about 3m in diameter, 4.5m in length.
▪ Diameter of balls in 25-125mm.
▪ Hollow cylinder.
▪ Rotates on its longitudinal axis.
▪ Length of cylinder is greater than its diameter.
▪ Cylinder is made of a metal and usually lined with chrome.
▪ Cylinder contains balls that occupy 30 to 50% of mill volume.
▪ Ball size depends on size of feed and diameter of the mill.
▪ Balls are made of steel, Iron or stoneware.
WORKING
▪ Material is put into cylinder and allowed to rotate.
▪ The speed of rotation is very important.
▪ At low speed, balls roll over each other and SR will not occur at optimum
level.
▪ At high speed the balls will stick to the walls of the cylinder and no SR will
occur.
▪ At optimum speed the balls will just taken upto the top and they will fallen
down.
USES
▪ Ball mill at low speeds is used for milling dyes, pigments and
insecticides.
▪ Used to grind brittle drugs to fine powder.
▪ Stainless steel balls are preferred in the production of ophthalmic
and parenteral product
ADVANTAGES
▪ It can produce very fine powder.
▪ Suitable for milling toxic materials.
▪ Suitable for both wet and dry grinding process.
▪ Balls can be various shapes and sizes.
▪ Installation, generation and labour costs are high.
DISADVANTAGES
▪ Very noising machine.
▪ Contamination of products may occur as a result of wear and tear
from the balls.
▪ Slow process.
▪ Soft, sticky, fibrous materials cannot be milled by ball mill.
[Link] ENERGY MILL / MICRONIZER / ULTRA
FINE GRINDERS
PRINCIPLE
Works based on the principle
of impact ( High speed moving
object hits stationary material) and
attrition ( Breaking down of particle
by rubbing action between two
surfaces.
*Milling take place because
of high velocity collisions between
the suspended particles.
CONSTRUCTION
▪ Consist of an elliptical pipe height of 1.23 – 2.4m diameter, ranges from 20 to
200m.
▪ Made of Stainless steel or tough ceramics.
▪ Grinding nozzles (2 to 6 ) placed tangentially to the initial flow path of a powder.
▪ Outlet with classifier is fitted to allow escape of air.
WORKING
▪ Powder is introduced through inlet.
▪ The air enters through grinding nozzles, transports the powder in elliptical track of
the mill.
▪ In the turbulent steam of air, the suspended particles collide with each other
and break.
▪ Thus Impact and attrition generates in Size reduction.
▪ The coarser particle undergo re-circulation in the chamber.
▪ These re – circulated particles collide again with each other.
▪ The powder remains in the mill until its size is reduced sufficiently.
▪ Upto 6000 kg of feed can be milled per hour.
USES:
• Used to reduce the particle size of most of the drugs like, antibiotics
and vitamins.
• It is used in case where high purity is required.
ADVANTAGES:
• No moving parts, hence heat is not produced during
milling.
• Contamination is not possible.
• Very fine size of particles can be obtained by using this
mill.
DISADVANTAGES:
• Not suitable for soft, tacky and fibrous materials.
• Expensive.
[Link] RUNNER MILL / ROLLER MILL
PRINCIPLE
• Size reduction is done by crushing
(compression) and shearing due
to heavy weight of stones.
• Shearing force is also involved
during the movement of the
stones.
CONSTRUCTIONS
▪ 2 Heavy rollers weighs several tons.
▪ Rollers moves on a bed which is made up of stone\granite.
▪ Rollers are mounted on a horizontal shaft and move around the bed.
WORKING
▪ The material to be grind is placed on bed
▪ Stones travel on their axis.
▪ The outer part of the wheel has to travel a greater distance then the
inner, so that SR is achieved by shearing .
▪ A scrapper is used to bring the feed in the path of the stones.
▪ Powder is collected and passed through a sieve.
USES
▪ Used for size reduction of drugs to a fine powder.
ADVANTAGES
▪ It does not require attention during geration.
DISADVANTAGES
▪ Occupies more space.
▪ Contamination is possible.
▪ Not used for sticky materials.
▪ Energy consumption is quite high.
▪ Time consuming.
5. END RUNNER MILL ( MORTAR AND PESTLE TYPE)
PRINCIPLE:
The material is getting crushed
and shearing stress due to weight
of heavy pestle and shearing
force which get applied during
the movement of these stones.
CONSTRUCTIONS
• Mechanical mortar and pestle.
• Mortar is shallow and the bottom of pestle is flat rather than round.
• Shallow mortar is made up of bed of stones.
• Pestle is dumb-bell shaped has a flat bottom and cylindrical and it
carries a hinged arm.
• Inside the shallow mortar, a scrapper is arranged which brings the feed
material towards the grinding surface.
WORKING
• Material to be grind is placed in mortar.
• Scraper puts the materials in path of pestle.
• The mortar revolves at high speed.
• The pestle is placed in mortar.
• The rotating mortar causes the pestle to revolve.
• During this process size reduction is achieved by shearing as well as
crushing.
• Material is collected and passed through a sieve to get the powder of
desired size.
USES
• Used for fine grinding.
• Used for grinding of brittle drugs.
ADVANTAGES
• It is a laboratory scale mill.
DISADVANTAGES
• It is not suitable for drugs , which are in unbroken or slightly broken
conditions.
[Link] MILL
Colloid mill is specifically used for
preparing biphasic liquid dosage forms.
It is a Rotor – stator type.
NOTE
It should be sterile
PRINCIPLE
High velocity fluid shear due to which the
suspended particles or liquid droplets
are milled which gives uniform and
stable suspension or emulsion.
CONSTRUCTION
• Cone shaped rotor (rotated)
• Stator (stationary) both are enclosed in a vessel.
• Space between rotor and stator can be adjusted upto 25 micron depends on
particle size required.
• Diameter of rotor is 6-15 inches.
• Capacity of small size mill is 30-50gdl/hr, capacity of large size mill is 1000/hr.
• Rotor is made up of invar
• Feed inlet at top, outlet present at bottom.
TYPES
1. Orifice device.
2. Hammer mill
3. Smooth surface disk
4. Rough surface disk
WORKING
• Pre-milled feed is added via hopper.
• Motor is switched on.
• Rotor is operated at 3600 rpm.
• Allow feed to enter between rotor and stator.
• Due to high velocity fluid shear is generated with 1m or less in size from discharge.
NOTE
By circulating cold water to decrease generated heat during the process such as 40
degree C to 20 degree C.
DEMERITS
• Air gets trapped.
• Heat generated.
• Not suitable for dry milling.
• High energy consumption.
MERITS
▪ Size of 1m or less can be achieved.
▪ Mill can be sterilized.
▪ Easy cleaning.
APPLICATIONS
▪ Syrups , paints, milk, purees are processed.
▪ Ointments, Suspensions are processed.
▪ Fibrous materials can also be processed.
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