Particle size reduction research

Particle size reduction definition

is a process in which the particle size of a solid is made smaller. The term size reduction is
applied to ways in which particles of solids are cut or broken into smaller pieces. Size
reduction is necessary if the starting material is too coarse, and the final product needs to be
a fine powder.

It is a unit operation in which materials are reduced to smaller pieces \coarse particles or to
still finer powder before they can be formulated into suitable dosage forms .

The importance of particle size reduction

The process of size reduction is commonly employed in pharmaceutical industries due to the
following reasons:

1- To increase the rate of solution in case of chemical substances, because reduction of the
particle size increases the surface area for the action of solvent.

To allow the rapid penetration of the solvent (menstrum ), in case of crude drugs for the - 2
.extraction of active constituents from vegetable and animal drugs

To get a uniform powder because particle size reduction helps in uniform mixing of - 3
.drugs ,required for preparing different formulations for administration

To increase the rate of absorption of a drug .The smaller the particle size , the greater is -4
.the rate of absorption

To improve the stability of certain pharmaceutical dosage form ,such as suspensions .The -5
.rate of sedimentation decreases to a large extent by reducing the particle size of drug

To help in the process of separation of solids from liquids by filtration or by sedimentation - 6

.The rate of filtration or sedimentation depends upon the particle size
OBJECTIVES OF SIZE REDUCTION

In the materials processing industry, size reduction or comminution is usually carried out in
:order to

Increase the surface area because, in most reactions involving solid particles, the rate of -
.reactions is directly proportional to the area of contact with a second phase

Break a material into very small particles in order to separate the valuable amongst the -
.two constituents

.Achieve intimate mixing -

. To dispose solid wastes easily -

- .To improve the handling characteristics

-To mix solid particle more intimate

Advantages of size reduction

Content uniformity-

Uniform flow-

Effective drying -

Increases surface area or viscosity -

- Uniform mixing and drying

-Improve rate of absorption

-Smaller the particles greater is absorption

-Improve dissolution rate

ADVANTAGES OF SIZE REDUCTION

Increase the surface area Improving dissolution rate, because in most reactions involving
solid particles, the rate of reactions is directly proportional to the area of contact with a
second phase

Content uniformity ,Uniform flow, Uniform mixing and drying ,Improve rate of absorption .
Smaller the particles greater is absorption

Improve color and/or APIs dispersion in tab. excipient

High surface area means better drying

To improve the handling characteristics

To improve mixing of solid particle together, reducing problem of uniformity of weight and
contents of tab.

Disadvantages of size reduction

- possible change in polymorphic form of the active ingredient rendering it less or totally
inactive or unstable.

- possible degradation of the drug as a result of heat build up during milling by oxidation or
adsorption of unwanted moisture due to the increased surface area.

- decrease in bulk density may cause problems in the flow ability of material .

- decrease in particle size may create static charge

- contamination

- loss of aromatic principle .

Factors affecting size reduction

Hardness: - It is a surface property of the material. - It is frequently confused with a

.property named strength

Thus, it is possible for a material to be very hard, but if it is brittle also then size reduction -
.may present no special problems

;An arbitrary scale of hardness has been devised known as Moh’s Scale -

Moh’s Scale = 1 is for graphite

Moh’s Scale < 3 is for soft material

Moh’s Scale > 7 is for hard material

Moh’s Scale = 10 is for diamond The harder the material the more difficult it is to reduce in
size

.Material structure: Some substances are homogeneous in character

Mineral substances may have lines of weakness along which the materials splits to form
.flake-like particles

Vegetable drugs have a cellular structure often leading to long fibrous particles

Abrasiveness: Abrasiveness is a property of hard materials (particularly those of mineral

.origin). It may limit the type of machinery that can be used

During the grinding of some very abrasive substances the final powder may be contaminated
.with more than 0.1 percent of metal worn from the grinding mill
Softening temperature: During size reduction process sometimes heat is generated which
may cause some substances to soften, and the temperature at which this occurs can be
.important

Waxy substances, such as stearic acid, or drugs containing oils or fats are examples that may
.be affected

Some methods can be used to overcome this like cooling the mill, either by a water jacket or
.by passing a stream of air through the equipment

Moisture content: It is found that materials do not flow well if they contain between about 5
and 50 per cent of moisture. Under these conditions the material tends to cake together in
the form of balls. In general, grinding can be carried out satisfactorily outside these limits.
Crushing strength: The power required for crushing is almost directly proportional to the
.crushing strength of the material

Friability: The friability of the material is its tendency to fracture during normal handling. In
general, a crystalline material will break along well-defined planes and the power required
for crushing will increase as the particle size is reduced.

Stickiness: A sticky material will tend to clog the grinding equipment and it should therefore
be ground in a plant that can be cleaned easily.

Soapiness: In general, this is a measure of the coefficient of friction of the surface of the
material. If the coefficient of friction is low, the crushing may be more difficult.

Explosive: Such materials must be ground wet or in the presence of an inert atmosphere.
Materials yielding dusts that are harmful to the health: Such material must be ground under
conditions where the dust is not allowed to escape.

Mechanism of size reduction

1- Impact —particle concussion by a single rigid force (hammer).

2- Compression—particle disintegration by two rigid forces (nutcracker).

3- Shear —produced when the particle is compressed between the edges of two hard
surfaces moving tangentially.

4- Attrition —arising from particles scraping against one another or against a rigid surface (a
file)
When impact force are apply?

Gravity impact

1. In gravity impact ,the free falling material is momentarily stopped by the stationary
object.

2. Example – coal dropped onto a hard steel surface

Dynamic impact

1. Most often used when it is necessary to separate two material which have relatively
different friability

2. The more friable material is broken first

3. Less friable material remains without broken

4. Example – material dropping in front of a moving hammer

A cubical particle are needed or material too hard.

When compression forces needed?

- If material is hard

- If material is abrasive

- If the material is not stick

- When material will break cubically

-Where the finished product is to be relatively coarse in size.

Size reduction theories

The energy requirement for particle size reduction is a function of input and output of
particle size, hardness, strength and other properties of solids.

Various theories for energy requirement are:

- Rittinger’s theory

- Kick’s theory

- Bond’s theory.

Integrating equation (1),

E= C ln(di/dn) …. (2)

(di/dn) = reduction ratio.

If n=1.0 equation (2) becomes Kick’s theory.

If n=1.5 equation (2) becomes Bond’s theory.

If n=2.0 equation (2) becomes Rittinger’s theory.

According to this theory energy E required for size reduction of unit mass is directly
proportional to the new surface area produced.

E=KR (Sn – Si) . …. (3)

Where

Si = initial surface area

Sn = new specific surface area

KR = Rittinger’s constant.

E= amount of energy.

Applications:

Applicable to brittle materials undergoing fine milling.

This theory ignore deformation before fracture.

Bond’s work index is the work required to reduce unit weight from a theoretical infinite size
to 80% passing 100µm. This theory is useful for rough mill sizing. The work index is useful for
comparing efficiency of milling operations.

For compression of large particles kick’s theory is useful.

Rittinger’s theory:- (n=2.0) Energy α new surface area formed.

Bond’s theory:- (n=1.5) Energy used in crack propagation α Crack length produced.

Kick’s theory:- (n=1.0) Energy α Ratio of change in size.

classification of size reduction equipment

1- cutting methods

2-compression methods

3-impact methods

4- attrition methods

5-combined impact and attrition methods.

size reduction equipment

1- cutting methods

The material is cut by sharp blade .

1. Size reduction range 100-100000 µm

2. Cutter mill consists of a series of a knives attached to a horizontal rotor which act against a
series of knives mounted on stationary mill

3. Size reduction by fracture of particles between the two sets of knives

4. A screen is fitted to collect the derived size of powder Eg ., fibrous crude drugs , roots,
peels, barks, prior to extraction.

1- cutter mill

Consist of a series of knives attached to a horizontal rotor which act against a series of
stationary knives attached to the mill casing .

During milling , size reduction occurs by fracture of particles between the two sets of knives .

A screen is fitted in the base of the mill casing and acts to retain material in the mill until a
sufficient degree of size reduction has been affected.

The high shear rates present in cutter mills are useful in producing a coarse degree of size
reduction of dried granulations prior to tableting an of fibrous crude drugs such as roots,
peels or barks prior to extraction .

2- rotatory knife cutter

Eight rotating knives operate with two stationary knives . all knives are adjustable to
accommodate a specific product .

Industrial construction is provided for continuous operation. Machines case is built with 1\2
inch plate steel.

Main bearings are 2 7\16 type E double row roller .

Rotor shaft is also 2 7\26 and is built with cold rolled steel .

Width of cutter at point material enters is 24 inches

Size of cutters screen 24 7\8 by 35 1\2 . with 2600 of screen surface .

Complete V-belt drive and motor base is provided as standard equipment .

2- compression methods

small scale batches were carried out on a using a mortar and pestle

– End runner mill

– Edge runner mill

– Roller mill

1. End runner mill the weighed pestle is turned by friction of material passing beneath it as
the mortar rotates .
2. Edge runner mill pestle equivalently mounted horizontally and rotating against abed of
powder by attrition as well as compression.

Roller mill two cylindrical rolls is driven directly while second is rotated by friction as .3
material is drawn Eg., Ointment

Principal : Material is crushed by the application of stress (attrition). Stress is applied by

rotating heavy 2-5 wheels or rollers . The rollers rotates at different speeds so that the
material is sheared and compressed as it passes through the gap between the rollers and is
.transferred from the slower to faster roll, from which it is removed by means of a scraper

Uses: for crushing seeds before extraction of fixed oil. Also used to crush soft tissue to help
in penetration of solvents. ts, two rollers rotate at different speed and direction.
3- impact methods

HAMMWE MILLS

Principal: Material is impact between rapidly moving hammers on a rotor ( up to rpm)& the
powder material which fed from top or center. The material discharged through the
perforated screen covering the discharge opening which retain coarse material for further
.grinding

Uses: it is used to mill dry materials, wet filter press cakes, ointments, slurries etc. Brittle
material is best fractured by impact from blunt hammers; fibrous material is best reduced in
size by cutting edges.

Advantages of Hammer mill

.It is rapid in action, and is capable of grinding many different types of materials .

They are easy to install and operate .2

There is little contamination of the product with metal abraded from the mill as no .3
.surface move against each other

The particle size of the material to be reduced can be easily controlled by changing the .4
.speed of the rotor, hammer type, shape and size of the screen

.small space requirements.5

.easy to clean.6

Disadvantages

1.Heat buildup during milling is more, therefore, product degradation is possible.

2. Hammer mills cannot be employed to mill sticky, fibrous and hard materials.

3. The screens may get clogged.

4. Wearing of mill and screen is more with abrasive materials.

Two types of hammer mill:

Ball mill or Pebble mill or Tumbling mill

Principal: Material is impact between rapidly moving (steel or pebble)balls & the powder
material, both enclosed in hollow cylinder. At low speed, the balls roll over each other &
attrition (rubbing action) will be predominant. In ball mill, impact or attrition or both
.responsible for size reduction

Uses: Ball mill at low speed is used for milling dyes, pigments & insecticides. Stainless steel
balls are preferred in the production of ophthalmic & parental products.

:Advantages of ball mill

It can produce very fine powder. 2.Ball mill is used for both wet and dry grinding .1
processes.3. Toxic substances can be ground, as the cylinder is closed system. 4.Rod or bars
can also be used as grinding media. (example: Sticky material)5. In the ball mill, installation,
.operation and labor costs are low

Disadvantages of ball mill:1.The ball mill is a very noisy machine.2. Ball mill is a slow
process.3. Soft, tacky, fibrous material cannot be milled by ball mill.4. difficult to clean and
.needs high energy
FLUID ENERGY MILL (MICRONIZER)

Principle: Fluid energy mill operates on the principle of impact and attrition. In this
equipment , the feedstock is suspended within a high velocity air stream . Milling takes place
.because of high velocity collisions between the suspended particles

Fluid energy mill It consists of a loop of a pipe, which has a diameter of 20 to 200 mm,
depending on the overall height of the loop which may be up to about 2 meters, a fluid,
usually air, is injected at high pressure through nozzles at the bottom of the loop, giving rise
to a high velocity circulation in a very turbulent condition, Solids are introduced into the
stream and, as a result of the high degree of turbulence, impact and attritional forces occur
between the particles. A classifier is incorporated in the system, so that particles are
retained until sufficiently fine. The feed to the mill needs to be pre-treated to reduce the
particles size to the order of 100 mesh, enabling the process to yield a product as small as 5
micrometers or less.

Uses: It is used for to reduce the particle size of antibiotics & vitamins. Moderately hard
.materials can be processed for size reduction. Ultra fine grinding can be achieved

Advantages: 1.Up to 6000 kg of feed is milled per hour. 2. Feed particles of size 12 mm are
easily size reduced. 3. Since there is no wear of the mill, contamination is not possible.4.
heat-labile material can be milled because of the cooling effect of air and heat exchange bet.
Particles and air. 5. air can be replaced with inert gas to decrease the oxidation to
.susceptible materials

Disadvantages: 1.Fluid energy mill is not suitable for milling of soft, tacky and fibrous
material. 2.The equipment is expensive, because it needs additional accessories particularly
fluid energy source and dust collection equipment.
COLLOID MILL

Principal: Colloidal mill consists of two steel discs having distance (clearance) between them.
When the material is passed through these discs, they get sheared. Thus coarse particles are
.broken down in small particles due to shear

Uses: Colloidal mill is used for preparing colloidal dispersion, suspension, emulsion &
ointments. Fibrous material can be milled using rough surface rotor & stator.

PIN MILL

Pin Mills are type of Disc Grinders.

Also known as Centrifugal Impact Mills (CIM)

Pin mills are a type of high-speed-impact mills consisting of a feed inlet, a set of two disks
with concentric rings of pins and a product outlet.

Particle size of as low as 2 µm can be achieved with the use of finest quality Pin Mills.

Pin mills are capable of very fine grinding without the need for screens and provide a
uniform product size.

PRINCIPLE

Pin mill employs shearing and impact forces to produce fine particles

The grinding action within the Pin Mill is achieved by impacting the product particles with a
series of hardened steel pins.
 The product enters through the eye of the machine and then passes through rows of pins
rotating at high speed between stationary pins.

The product particles are shattered into fragments as they progress towards the outlet,
progressive becoming smaller in size as they approach the periphery(this is because the
distance between the pins decreases as we move radially outwards)

Pin Mill consists of two round disks parallel to each other.

Material is fed continuously in the gap between the rotating disks.

Depending on the type of the machine, one or both disks can rotate. In cases where both
disks rotate, the second disk rotates in counter direction.

Feeding of the product is usually done by means of a chute, shifting the product in the hole
center of one of the two disks.

To reduce the temperature increase, air is blasted during grinding or in construction to

avoid oxidation, cooled inert gas is used; Blast of inert gas helps prevent accumulation of
particles in between the pins and on the disks.

APPLICATIONS Spices Foodstuff Biotech & Pharma Chemical Germ Salt Spaghetti Pill Ore Iron
oxide Curry Rice Red bean Collagen Rosin Talcum powder Clove Oats Black bean Chitosan
Sulfur Washing powder Garlic MSG Green bean Medicine Shellac Chemical materials Fagara
Sugar Pearl barley Agar ager Ceramic Calcium carbonate Crocus Xylitol Banana chip
Monascus Dyestuff Mustard Barley Healthy food Antibiotics Pigment Starch Dry vegetable
Yeast powder Gypsum Wheat Glutinous rice Chinese herbs Feldspar Soybean Polysaccharide
Pesticides.