Unit -3:Size Enlargement Operation

Subject: Mechanical operation

Diploma in chemical Engg.
4th sem
Munmun Laha
Lecturer in Chemical Engg.
Dr. Meghnad Saha Institute of Technology, Haldia
 Size enlargement is a process by which small particles are gathered
into larger, relatively permanent masses in which the original particles
can still be distinguished. The term encompasses a variety of unit-
operations or processing techniques dedicated to particle
agglomeration like Granulation, flocculation , extrusion, etc.
 Forces involved in size enlargement:
 Intermolecular force: These forces are due to particle-particle
adhesion.
 Electrostatic force: This force is a result of interpartcular friction or
through the generation of opposite charges.
 Liquid and solid bridges: Dispersing liquid into a powder mass will
generally result in a significant increase strength of particle-particle
agglomerates.
 Objectives of size enlargement
 Production of useful structural forms, as in pressing of intricate shapes in powder
metallurgy.
 Provision of a defined quantity for dispensing and metering, as in agricultural
chemical granules or pharmaceutical tablets.
 Elimination of dust handling hazards or losses, as in briquetting of waste fines.
 Improved product appearance, or product renewal.
 Reduced caking and lump formation, as in granulation of fertilizer.
 Improved flow properties, as in granulation of pharmaceuticals for tabletting or
ceramics for pressing.
 Increased bulk density for storage.
 Creation of non-segregating blends of powder ingredients, as in sintering of fines
for steel or agricultural chemical granules.
 Control of solubility, as in instant food products.
 Control of porosity and surface-to-volume ratio, as with catalyst supports.
 Improvement of heat transfer characteristics, as in ores or glass for furnace feed.
 Removal of particles from liquid, as with polymer additives which induce clay
flocculation.
Granulation
 Granulation is the process of forming grains or granules
from a powdery or solid substance, producing a granular
material. It is applied in several technological processes in the
chemical and pharmaceutical industries. Typically,
granulation involves agglomeration of fine particles into
larger granules, typically of size range between 0.2 and
4.0 mm depending on their subsequent use. Less commonly,
it involves shredding or grinding solid material into finer
granules or pellets.
 Granulation is carried out for following reason
 To prevent segregation of powder mix.
 To improve flow characteristics.
 For improving compression ability
Some powders are difficult to compact even if a readily compactable
adhesive is included in the mix, but granules of the same powders are
often more easily compacted. This is associated with the distribution
of the adhesive within the granule and is a function of the method
employed to produce the granule.
For example:For example, if one were to make tablets
from granulated versus powdered sugar, powdered sugar would be
difficult to compress into a tablet and granulated sugar would be easy
to compress. Powdered sugar’s small particles have poor flow and
compression characteristics. These small particles would have to be
compressed very slowly for a long period of time to make a
worthwhile tablet. Unless the powdered sugar is granulated, it could
not efficiently be made into a tablet that has good tablet
characteristics such as uniform content or consistent hardness.
 Bonding mechanisms between particles:
1. Adhesion and cohesion forces in the immobile liquid films
between individual primary powder particles.
2. Interfacial forces in mobile liquid films within the granules;
3.The formation of solid bridges after solvent evaporation;
4.Attractive forces between solid particles;
5. Mechanical interlocking.

Granulation are of two types

1. Wet granulation
2. Dry granulation
 Mechanism of wet granulation
 Nucleation: Granulation starts with particle to particle contact and
adhesion due to liquid bridges. Number of particles will join to form the
pendular state. When liquid is added to the powder causing a thin and
immobile film of liquid to form between particles. This causes an effective
decrease in inter-particulate distance and an increase in contact area
between particles. The shortening of the inter-particulate distance
increases the Van der Waals forces of attraction. More liquid is usually
added in wet granulation to form a mobile liquid film. As a result, there
are three states that can describe the distribution of liquid between
particles:
 Pendular state – usually at low moisture level, this is when the particles are
held together by lens-shaped rings of liquid, but it is mainly air between
the particles.
 Funicular state – this is an intermediary state where air starts to displace
from between particles
 Capillary state – this is when all air has been displaced from between
the particles.
In the capillary state liquid penetrates the pores of the particles and
will form a solid bridge between particles, giving the strongest form
of adhesion, when the liquid evaporates.

 Transition: Nuclei can grow in two possible ways either single

particles can be added to the nuclei by pendular bridges, or two or
more nuclei may combine. The combined nuclei will be reshaped by
the agitation of the bed.
 Ball growth: Granule growth produces large, spherical granules and
the mean particle size of the granulating system will increase with
time and agitation.
 Chopping: Bigger size are granules are chopped to smaller granules
in the process of ball growth. Chopping is repeated to achieve the
granulation end point.
 In wet granulation, granules are formed by the addition of a granulation liquid
(binding liquid) onto a powder bed which is under the influence of an impeller. The
agitation results in the aggregation of the primary powder particles to produce wet
granules. The granulation liquid contains a solvent or carrier material which must
be volatile so that it can be removed by drying, and depending on the intended
application, be non-toxic.
Typical liquids include water, ethanol and isopropanol either alone or in
combination. The liquid solution can be either aqueous based or solvent-based.
Aqueous solutions have the advantage of being safer to deal with than other
solvents.
 Water mixed into the powders can form bonds between powder particles that are
strong enough to lock them together. However, once the water dries, the powders
may fall apart. Therefore, water may not be strong enough to create and hold a
bond. In such instances, a liquid solution that includes a binder (pharmaceutical
glue) is required. Povidone, which is a polyvinyl pyrrolidone(PVP), is one of the
most commonly used pharmaceutical binders. PVP is dissolved in water or solvent
and added to the process. When PVP and a solvent/water are mixed with powders,
PVP forms a bond with the powders during the process, and the solvent/water
evaporates (dries). Once the solvent/water has been dried and the powders have
formed a more densely held masses send to milling for perfect sizing. This process
results in the formation of granules.
 Dry granulation
 Dry granulation is used to form granules without using a liquid solution because
the materials to be granulated may be sensitive to moisture and heat. Forming
granules without moisture requires compacting and densifying the powders. In
this process the primary powder particles are aggregated under high pressure. Dry
granulation has fewer process stages than wet granulation.

 Compacting the powder for dry granulation can be done either using a heavy duty
tabletting press, or the powder is squeezed between two counter-rotating rollers,
to produce a continuous sheet or ribbon of materials.

 In the case of the roller compactor, the different ingredients are first weighed and
mixed in the required proportions. The resulting mixture is conveyed to the
compaction area and compaction rollers. It is then compressed by roller
compaction (slugging) for the first time. This results in sheets of compressed
material, which are then milled into granules of exactly the agreed density, before
being lubricated and compressed into the desired final form. Roller compacted
particle are usually dense, with sharp-edged profiles. When a tablet press is used
for dry granulation, the powders may not possess enough natural flow to feed the
product uniformly into the die cavity, resulting in varying degrees of densification.
 In dry granulation there are two types of irresistible attractive physical
forces between particles that cause them to bind them together
 Electrostatic forces – there are generally weak but may cause cohesion
when the material is mixed initially.
 Vand der Waals forces – these are stronger than electrostatic forces
and they increase as the inter-particulate distances decrease during
the compression of powders.
 In dry granulation the pressure applied increases the contact area
between the adsorption layers of particles and decreases the inter-
particulate distances, thereby contributing to the final strength of the
material. The pressure applied during dry granulation may also melt
low melting-point materials where the particles touch and high
pressures are developed. When this happens the particles will bind
together and crystallization may take place when the pressure is
relieved.
 Extrusion
 Extrusion is a process used to create objects of a fixed cross-
scetional profile. A material is pushed through a die of the desired
cross-section. The two main advantages of this process over other
manufacturing processes are its ability to create very complex
cross-sections, and to work materials that are brittle, because the
material only encounters compressive and shear stresses. It also
forms parts with an excellent surface finish.
 Extrusion may be continuous (theoretically producing indefinitely
long material) or semi-continuous (producing many pieces). The
extrusion process can be done with the material hot or cold.
Commonly extruded materials include metals, polymers, ceramics,
concrete, modelling clay and foodstuffs. The products of extrusion
are generally called "extrudates".
 Process: The process begins by heating the stock material (for hot
or warm extrusion). It is then loaded into the container in the
press. A dummy block is placed behind it where the ram then
presses on the material to push it out of the die. Afterward the
extrusion is stretched in order to straighten it.
 The extrusion ratio is defined as the starting cross-sectional area
divided by the cross-sectional area of the final extrusion. One of
the main advantages of the extrusion process is that this ratio can
be very large while still producing quality parts.
 There are two types of extrusion precess
1. Hot extrusion
2. Cold extrusion
Hot extrusion: Hot extrusion is a hot working process, which
means it is done above the material's recrystallization temperature
to keep the material from hardening and to make it easier to push
the material through the die. The biggest disadvantage of this
process is its cost for machinery and its upkeep. Plastic materials
are generally extruded by hot extrusion.
Cold extrusion: Cold extrusion is done at room temperature or
near room temperature. The advantages of this over hot extrusion
are the lack of oxidation, higher strength due to cold working,
closer tolerances, better surface finish, etc. Materials that are
commonly cold extruded include: lead, tin, aluminium, copper,
steel etc.
Flocculation
Flocculation is a two-step particle aggregation process in which a
large number of small particles form a small number large flocs. In
this process colloids come come out of suspension in the form of floc
or flake, either spontaneously or due to the addition of a clarifying
agent.
Step 1: Coagulation:
Small particles usually carry negative surface charges that hinder
aggregation and settling (1a). Coagulant chemicals can adsorb to the
particles and balance the charges. The introduction of opposite
charges enables particles sticking together to form stable and well
suspended submicron flocs (1b). Rapid mixing is required for proper
dispersion of coagulant chemicals, to promote particle collisions and
submicron floc formation (1c).
 Step-2: Flocculation requires gentle mixing and the use of a high
molecular weight polymeric flocculant. The flocculant adsorbs to
the submicron flocs and facilitates bridging of gaps between flocs
(2a). Bringing particles closer together creates the effective range
for Van Der Waals attraction forces to reduce the energy barrier
for flocculation and loosely packed flocs form. Aggregation,
binding, and strengthening of flocs occurs until visibly suspended
macroflocs form (2b). At the right weight, size, and strength
sedimentation occurs. Macroflocs are very sensitive to mixing and
once torn apart by strong shear it is difficult or impossible for
them to reform.
 Flocculation happens naturally during the formation of snowflakes
or subsea sediments but it is also deliberately applied in the
biotechnology, petroleum, pulp and paper, and mining industries.
References
 Wikipedia
 Size Reduction and Size Enlargement, Richard H. Snow,
Terry Allen, Bryan J. Ennis, James D. Litster
 Particle size enlargement techniques, S.K. Savale