SIZE ENLARGEMENT /

AGGLOMERATION
Ukuran Pembesaran / Pengelompokan
Pendahuluan
• menggabungkan partikel kecil menjadi
massa tetap yang besar di mana unit
utama awal masih dapat diidentifikasikan

• Sasaran :
– Meningkatkan penanganan dan daya alir
– Mengurangi debu atau kehilangan bahan
– Memproduksi bentuk struktural yang berguna
– meningkatkan penampilan……
Pendahuluan

• Dikenal di berbagai nama

– Granulation (granulasi)
– Tableting (pembentukan tablet)
– Briquettingpembuatan briket)
– Pelletizing (pembentukan pelet)
– Encapsulation (enkapsulasi)
– Agglomeration (Pengelompokan)
Agglomeration (Pengelompokan)
• Proses di mana partikel bergabung atau
mengikat satu dengan yang lain, dengan cara
acak, berakhir dengan agregat struktur berpori
jauh lebih besar dalam ukuran dari bahan
awalnya.
• Aglomerasi diterapkan pada proses dimana
tujuan utamanya adalah untuk mengontrol
porositas dan densitas material dalam rangka
mempengaruhi sifat seperti dispersi dan
kelarutan (instantizing).
Instantizing Process
• Untuk menggambarkan penyebaran dan
melarutkan sifat serbuk/bubuk.
• Beberapa contoh serbuk instan: susu, kopi,
makanan bayi, sup, saus, minuman ringan,
campuran gula, vitamin dan bubuk obat.
• Proses instantizing membuat bubuk makanan
dengan atribut "instan" sehingga mereka dapat
dilarutkan atau didispersikan dalam air lebih
mudah daripada ketika mereka dalam bentuk
bubuk asli mereka.
• Dua proses instantizing utama: aglomerasi dan
metode non aglomerasi
Instantizing Process
• Agglomeration method :
• straight-through (jalur langsung) agglomeration
• (spray drying and agglomeration),
• rewetting agglomeration,
• spray-bed dryer agglomeration and
• penekanan agglomeration.
• Non agglomeration method :
• freeze drying,
• osmotic drying and
• drum drying, menambahkan aditif seperti lesitin
(dalam susu kering), menghapus komponen tertentu
seperti lemak (susu rendah lemak kering), dan
menerapkan perlakuan termal untuk bahan amorf
Instant Properties
• (Wettability)
Kemampuan basah : penembusan cairan/air ke dalam
sistem gumpalan berpori karena aksi kapiler atau
kemampuan menggumpal untuk ditembus oleh cairan
• Sinkability:
Tenggelamnya gumpalan di bawah permukaan cairan.
• Dispersibility:
penyebaran gumpalan dengan sedikit pengadukan
• Solubility (Kelarutan/ daya larut):
pelarutan gumpalan larut dalam cairan
Wettability
• Pertama langkah pelarutan
• Kapasitas partikel yang menyerap air pada
permukaannya, sehingga memulai pengenceran.
• Tergantung pada ukuran partikel dan sifat materi.
• partikel kecil memiliki nilai besar area spesifik dan tidak
dapat dibasahi secara individual.
• Meningkatkan ukuran partikel dan / atau aglomerasi
partikel dapat mengurangi timbulnya penggumpalan.
• Kehadiran lemak bebas di permukaan mengurangi
keterbasahan.
• Penambahan zat aktif permukaan seperti lesitin kadang-
kadang dapat meningkatkan wettability dalam bubuk
kering lemak mengandung
Sinkability
• Second dissolution step.
• Depend on particle size and density.
• It is not critical if the wetting takes place easily.
• The ability of particle to sink quickly into the water.
• Larger and Denser particle usually sink faster than finer
and lighter ones.
• Particle with a lot of included air may be relatively large
in size but exhibit poor sinkability because of their low
density
Dispersability and Solubility
• Dispersability describes the ease with which the powder
may be distributed as single particle over the surface
and throughout the bulk of the reconstituting water.
• Solubility refers to the rate and extent to which the
components of the powder particles dissolve in the
water.
• Dispersability is reduced by clump formation and is
improved when the sinkability is high, whereas solubility
depends mainly on the chemical composition of the
powder and its physical state.
Instant Property Evaluation
• A standard procedure to measure the instant properties
must define the specific solvent temperature, the liquid
surface area, amount of material to dissolve, the method
of depositing a certain amount of material onto the liquid
surface, unassisted or predetermined mixing steps and
timing procedure.
• Many objective method to determine the instant properties
are available and satisfactory methods have been
developed especially for the most important instant
properties such as wettability and dispersability.
Measuring Wettability

Penetration Speed Test

Measured the time required until the entire bed submerged

An effective method to determine the optimum agglomerate size
for wetting if there are different sized fraction of an experimental
batch of agglomerates to be evaluated
Measuring Wettability

Dynamic Wetting Testing

Measuring Wettability

• The force measured by the weighing cell is proportional

to the liquid the liquid volume absorbed due to capillary
pressure and its plotted against time.
• The penetration behaviour of the agglomerates can be
completely described by the force-time plot until all the
thhe material in the cell is wetted
Measuring Dispersibility

• Sample powder is dispersed consist of

dispersing material and residual material
• Dispersing material consist of soluble and
suspended material
• Residual material consist of non wetted
material and deposited or floating material
at the surface
Measuring Dispersibility
Measuring Dispersibility

D = Dispersability value
Cd = mass concentration of the dispersed proportion
Cr = mass concentration of the residual material
Cd and Cr is measured gravimetrically
Measuring Dispersibility
• A rapid photometric method
• In this method, the sample is dispersed and divided into
dispersed and residual portion that are then
homogenized and filled into corresponding funnel
separately. Each portion is in turn pumped continuously
through a cuvette to measure the light transmission value

Td is the transmission value for the dispersed portion

Tr is transmission value for the residual portion
IDF Standard Method

• It is spcifically designed to determine the dispersibilty of

instant dried milk and is also a rapid routine method to
determine wettability (wetting time).
• A certain amount of dried milk powder (26 g for instant
dried skim milk and 34 g for instant dried whole milk),
held in a glass tube with a glass plate on the top of a
beaker, is scattered on the water surface by withdrawing
the glass plate underneath the glass tubing. The water in
the beaker weigh about 250 g and its temp is adjusted to
around 25 oC. After a defined procedure for stirring,
sampliing and solid content measuring, the dispersebility
D is calculated as
IDF Standard Method

Cs is the total solid content of the liquid in % (m/m)

W is the water content of the pre treated test sample in %
(m/m)
IDF Standard Method

• For measuring the wettability is almost the same as that

for the dispersibility measurement, except that the
following stirring, sampling and solid content measuring
steps are omitted.
• Measure the time required for all the sample particle to
sink below the water surface or remain on the surface
but have a typical wet appearance is recorded.
Agglomeration

• Mechanisms of Particle Bonding

– Solid Bridges
– Immobile or freely movable liquid bridges.
– Attraction forces between solid particles
– Form-closed bonds or interlocking bonds
• More than one apply to any particular
system for agglomerate stability
Mechanism of Particle Bonding

• May be developed by diffusion of molecules from one

particle to another through partial melting at points of
contact where high pressure develop especially at
elevated temperature.
• Can also be built up by chemical reaction, crystallization
of dissolved substances, hardening of binders and
solidification of melted components.
• The force depend on the diameter of the contact area
and the strength of the bridge material.
Mechanism of Particle Bonding
• arises either from the surface tension of the liquid/air
system (as in the case of a liquid droplet) or from
capillary pressure.
• The immobile film of highly viscous bonding media can
form exceptionally strong bonds, the strength of which
can exceed that produced by mobile liquid layers.
• Attraction forces between solid particles is due to Van
der Waals and electrostatic forces (particle
composition).
Mechanism of Particle Bonding

• Form-closed bonds or interlocking bonds is the smallest

bond than other.
• Fibers, little platelets or bulky particle can interlock or
fold around each other resulting in “form-closed” bonds.
• In general, the particle bonding is the function of
coordination number (k) and the porosity or void volume
(ε)
Mechanism of Particle Bonding
Mechanism of Particle Bonding
Mechanism of Particle Bonding
Agglomeration
• Agglomeration Methods
– Tumbling of powder (Rewetting
agglomeration)
– Pressure agglomeration
– Specific Agglomeration methods
• Straight-through agglomeration
• Spray-Bed Dryer agglomeration
• Atomizer wheel
• Freeze drier
Tumbling of Powder
(Rewetting Agglomeration)
• The overall growth process is complex and involves both
disintegration of weaker bonds and re-agglomeration by
abrasion transfer and coalescence of larger units.
• The most important and effective separation force
counteracting the bonding mechanism is the weight of
the solid particle.
• For particle below 10 µm, natural attraction force such as
molecular, magnetic and electrostatic, become
significantly larger than the separation process (natural
agglomeration).
• The mechanism of tumble/growth agglomeration is
similar to natural agglomeration.
Tumbling of Powder
(Rewetting Agglomeration)
Tumbling of Powder
(Rewetting Agglomeration)

• Need addition of binders.

• Type of tumble/growth agglomeration : inclined disc,
rotating drum, any kind of powder mixer and fluidized
beds.
• Fluidized bed provide good random of mixing of the
powder, along with stable and uniform temperature
profile.
• Post treatment used : drying and heating, cooling,
screening, adjustment of product characteristic by
crushing, rescreening, conditioning and recirculation of
undersize material
Tumbling of Powder
(Rewetting Agglomeration)
Tumbling of Powder
(Rewetting Agglomeration)

• Agglomeration is initiated by rewetting the powder with a

liquid binder (example: water) that may be atomized pure
liquids or solutions, steam or combination of both.
• For example: granulated enzyme products can be
manufactured by mixing the enzyme solution with a
suitable filler to form a dough which is then pressed into
fine granules. The granules are then sprayed with a
suitable binder and further dried in a fluidized bed dryer.
Tumbling of Powder
(Rewetting Agglomeration)
Pressure Agglomeration

• Pressure forces act on a confined mass of particulate

solid which is then shaped and densified.
• Pressure agglomeration is carried out in two stages:
– A force rearrangement of particles due to applied pressure.
– A steep pressure rise during which brittle particles break and
malleable particle deform plastically.
• Two limiting factors that may limits the speed of
compaction and the capacity of the equipment that can
cause cracking and weakening of agglomerated
product).
– Compressed air in the pores
– Elastic springback
Pressure Agglomeration
Pressure Agglomeration

• These two factors can be reduced if the maximum

pressure is maintained for some time (dwell time) prior to
release.
• Pressure agglomeration can be performed employing a
low, medium or high pressure mode.
• The result differentiating in the porositiy.
• Low and medium pressure agglomeration is achieved in
extruders, including the screen extruder, the screw
extruder and the intermeshing gears extruder.
• High pressure agglomeration is performed in process
such as the punch and die press, the compacting roller
press and the briquetting roller press
Pressure Agglomeration
Pressure Agglomeration
Straight-through Agglomeration

• Spray-Bed Dryer Agglomeration

• Atomizer wheel
• Freeze drying
Straight-through Agglomeration

• Liquid concentrate is used.

• When powder are produced by spray drying, the
agglomeration process can be accomplished in a
fluidized bed connected directly to the spray dryer,
where the operating condition can be controlled so that
the partially dried particles formed in the upper part of
the dryer are still sticky.
• Sometimes, steam or atomized water can be injected
into the fluidized bed to assist in the agglomeration
process.
• Final drying and cooling are also accomplished in the
bed, and the agglomerated product is removed for
storage and packaging.
Straight-through Agglomeration

• Applied in coffee, baby foods, skim and whole milk, non-

caking whey, milk replacer and ice cream mix.
• In instant whole milk production, the straight-through
process is followed by lecithin addition, improving
wettability and dispersibility.
Straight-through Agglomeration
 BINDERS
• Binders are adhesive that provide the cohesiveness
essential for the bonding of solid particles.
• The binder may be dissolved in the granulating solvent,
which is then added to the powder, or mixed dry with the
powder and the granulating solvent (generally water).
• Selection of the quantity of binder required in a particular
system can be studied in optimization studies, using
parameters such as granule friability, hardness or
disintegration time.
• Binders differ in their bonding efficiency
• Factors affecting efficiency of binders: concentration,
viscosity, mechanical properties of the binder,
interparticulate interaction between binder the substrate
and binder distribution
BINDERS
Selection Criteria

• Feed Characteristic
• Agglomerated Powder Properties
• Alternative methods
Feed Characteristic

• Parameters :Particle size and distribution.

• Larger particles need more binders
• In general, it is difficult to agglomerate narrow particle-
size distributions or mono-sized particles.
• Other parameters : mechanical properties, chemical
properties such as particle density, brittleness, elasticity,
plasticity, wettability and abrasivity.
Agglomerated Powder Properties

• The purpose of agglomeration: granular, free flowing

characteristic or dust-free features can be done almost
all method of agglomeration.
• Spherical products are desirable (difficult obtained by
high pressure agglomeration).
Alternative Method

• Agglomeration process can be carried out in batch or

continuous.
• Batch modes are generally low in capacity, but are
characterized by a better control than that exercised in a
continuous process.
• Most large volume applications operate in a continuous
form, but may be accompanied by significant variation in
quality
• In growth agglomeration, uncontrolled buildup must be
removed, whereas in pressure agglomeration, worn
parts must be replaced
Alternative Method

• Most of the growth methods are wet process using

binding liquids for forming agglomerates
• High pressure method operated as dry process.
• Cost, availability etc.
Alternative Method
Design Aspect Of Agglomeration Process
Design Aspect Of Agglomeration Process
Design Aspect Of Agglomeration Process
Design Aspect Of Agglomeration Process
Design Aspect Of Agglomeration Process
Agglomerating Skim Milk Powder
Agglomerating Skim Milk Powder
Agglomerating Skim Milk Powder