Agglomeration means getting smaller particles to adhere to each other to form a powder consisting of bigger conglomerates/agglomerates, which are essential for an easy reconstitution in water.

Spray Drying Agglomeration

During the spray drying process the aim is to produce particles with a big surface/mass ratio, i.e. small particles. The reconstitution in water of a powder consisting of small particles is however difficult and requires intensive mixing in order to disperse the powder, before it is totally dissolved. Bigger particles exhibit a better dispersion, but the solubility is negatively affected during the drying operation.


By agglomeration both a good dispersion and a complete solution are obtained.

In spray drying there are two ways of agglomeration: the spontaneous and the forced, both in a primary and secondary form.

TYPE DEFINITION EXAMPLES
Spontaneous primary Random, unprovoked collision of primary spray particles All atomization devices
Forced
primary Intended collision between primary spray particles from different atomization devices Collision of sprays from different nozzles
Spontaneous secondary Random, unprovoked collision of primary spray particles and fines Multi-Stage or Integrated Filter Dryers
Forced secondary Intended collision between primary spray particles and fines returned to the atomization zone Normal type when Fines Return is applied


The spontaneous primary agglomeration

is a result of a random unprovoked collision of particles in a single atomizer cloud due to particles of different diameter having different deceleration paths. It takes place in both nozzle and rotary atomizers.

The forced primary agglomeration

is a controllable means for production of an agglomerated product with certain properties, by for example collision of particles from two or more atomization clouds, typically in a multi-nozzle unit, where the sprays from the individual nozzles are forced into each other.


The spontaneous secondary agglomeration

is a result of a venturi effect at the drying air inlet to the chamber, whereby dry single particles are sucked into the wet atomizer cloud. Moist particles colliding with air-borne dry particles contained in the exhaust air on its counter-current way out of the MSD/IFD dryer.

The forced secondary agglomeration

is a controllable means for agglomeration by returning fines to the atomizer cloud, via the fines return. The spontaneous agglomeration, which will always exist, is enforced by the agglomeration applied by returning the fines to the atomizer cloud. By definition fines are the cyclone or bag filter fractions and consist of the smallest particles, which are returned to the process. The small dry particles are introduced into the dryer near the atomizing device, where they will meet and collide with atomized wet droplets thus forming agglomerates consisting of many particles stuck together having a size of 100-500 microns, depending on the parameters selected.

Due to the special air flow pattern in an MSD/IDF plant a considerable spontaneous, secondary agglomeration takes place. For production of high quality instant whole or skim milk powder this spontaneous agglomeration suffices, and the fines are just returned to the integrated fluid bed, from where they will get airborne again and reach the atomizing zone again. However, the agglomeration may be further enhanced by forced, primary agglomeration (collision of sprays overlapping each other from different nozzles in a multi-nozzle atomization unit) and/or by returning the fines to the atomization zone (forced, secondary agglomeration). Further flexibility can be gained by designing the atomization unit in a way that allows the distance between the single nozzles or between the nozzles and the fines return tube to be altere d.

Depending on the atomization device the fines return is designed in different ways:

For Rotary Atomization

The aim is to bring the fines as close as possible to the atomizer wheel. This can be done from below. via a pressure conveying system using a 3-4" dosing pipe with a fines distributor at the end inside the drying chamber. However, deposits are easily formed on this pipe, if the air disperser is not adjusted to avoid it. This adjustment is, however, not necessarily optimal from the drying point of view.

In modern dryers fines are therefore introduced from above in through the air disperser (FRAD System) via 4 fines pipes situated just above the atomizer cloud. Deflector plates at the end of each fines pipe ensure a correct introduction and distribution of the fines.


For Nozzle Atomization

The fines return is an integral part of the nozzle unit with the fines duct in the centre surrounded by nozzles at the periphery. The fines are introduced tangentially into the fines distribution duct or through a center pipe. The nozzles can be welded to the nozzle rod at a certain angle, so that by turning the nozzle rod around its axis the collision point can be altered.

Separation

is the process separating the part of fines which is entrained in the main drying air leaving the drying chamber. The efficiency of separation is determined by the air flow pattern and air velocities in the drying chamber and is therefore closely related to the chamber design and can only be marginally affected at normal running conditions, f.inst. by air disperser adjustments and variations in drying air rates.

The agglomerated powder leaves the chamber at the base or from the integrated fluid bed and enters the Vibro-Fluidizer. During the passage down the wall of the chamber cone some stabilization of the already induced agglomeration takes place. In the static fluid bed and/or the Vibro-Fluidizer the powder is met by a warm airstream evaporating the excess moisture content, as was the case i n the two-stage drying process.

Attrition
is defined as the partial break down of agglomerates in fluid beds or powder conveying systems resulting in creation of either fines and smaller agglomerates (abrasion) or of a number of smaller sized particles (fragmentation). This often overlooked phenomenon is the result of mechanical motion between the agglomerate and another body which may be the walls of the fluid bed or another particle. The most likely cause of attrition in fluid beds is particle/particle interaction, as interparticle impact velocities can be very high, caused by high air jet velocities out of the holes in the perforated plate that forms the bottom of the fluid bed. Factors affecting the extent of attrition is the jet velocity, determined by the pressure difference across the perforated plate, the fluidization velocity and the actual design of the perforated plate.

Classification

is defined as the separation of fines in fluid beds. The efficiency of classification is mainly determined by the fluidization air velocity, but also fluid bed design features are of importance in securing that separated fines are kept airborne and entrained in the exhaust fluid bed air.

After the final drying the powder enters the cooling section where the powder is cooled by means of air at ambient temperature followed by cooled, dehumidified air. The powder is finally passed over a sifter where any oversize particles are removed. It is also possible to install a sifter with two nets thus removing any remaining particles/agglomerates of small diameter. Together with the fines, this fraction may be returned to the atomizing device thus producing a powder with a well defined agglomerate size distribution. The f ines removal in the fluid beds is, however, regarded as sufficient from a product point of view, and plants with above mentioned sifter are only used when particular product specifications have to be met. 

Agglomerate structure and powder properties

Depending on the design and adjustment of the fines return system - particularly the location of the introduction of the fines in relation to the atomization device - different agglomerate structures result, which influences certain powder properties, such as bulk density, mechanical stability, dispersibility and slowly dispersible particles.

The relation between agglomerate structure and certain powder properties is illustrated in Fig. 90a.

AGGLOMERATE STRUCTURE:
Onion ---> Raspberry ---> Compact grape ---> Loose grape

PARTICLE MOISTURE CONTENT AT COLLISION:
High -----------------------------------------> Low

MECHANICAL STABILITY:
High-----------------------------------------> Low

BULK DENSITY (no attrition):
High-----------------------------------------> Low

BULK DENSITY (after attrition):
High----------------> Low------------------> High

SLOWLY DISPERSIBLE PARTICLES:
Many-----------------------------------------> Few
DISPERSIBILITY (after attrition):
Poor ----------------> Good----------------> Poor

Fig. 90a Agglomerate structure/powder properties relationship

If the fines are introduced close to the atomizing devise the moisture content of the primary spray particles is high and thereby their plasticity and stickiness, and the fines particles may penetrate primary particles or be completely covered by concentrate . Such agglomerates have been termed 'onion'-structured. When collision takes place at a progressively longer distance, away from the atomizing device, less compact agglomerate structures are obtained. Such structures have been termed 'raspberry'- and 'grape'-structures in decreasing order of compactness.

'Onion'-structured agglomerates are characterized by a high mechanical stability and a high bulk density, but they will often appear as slowly dispersible particles after reconstitution. They may a l so be collected during the different dispersibility tests in use and jeopardize the general quality evaluation of the product.

With progressively looser agglomerate structures the bulk density and mechanical stability decrease gradually, and the overall instant properties improve. However, if a 'loose grape'-structure is eventually obtained, the mechanical stability may be so low that the powder becomes very susceptible to attrition resulting in deteriorated instant properties. A 'compact grape'-structure is regarded as the ideal compromise where the powder has simultaneously good instant properties and sufficient mechanical strength to enable necessary transport and packaging.

The agglomeration is improved by:

  • High solids content in the concentrate
  • Bigger quantity of fines returned to the atomizing device
  • Fines introduction closer to the atomizing device
  • Shorter distance from nozzle to fluidized layer in a static fluid bed
  • Higher moisture content from the primary drying stage
  • Bigger primary particles
  • Lower pasteurization temperature of the milk prior to the evaporation

When leaving the sifter the powder should not be exposed to strong mechanical conveying, neither by means of air nor by fast moving mechanical screws. However, today's lenient vacuum-low speed air systems are used without too much damage to the agglomerates. The best thing, however, is to install the plant so high that filling into bags or tote-bins is possible by gravity.

 

Rewet Agglomeration

Since many powders may become instant by the mere agglomeration, many processes have been developed during the past years to agglomerate ordinary powders consisting of single spray particles usually produced in plants with pneumatic conveying system, as described on page 115 and 139.

The historic development started with the pioneering research of Mr. David D. Peebles in the beginning of the fifties, and instantized non-fat dry milk was marketed from 1954. Soon it replaced the regular spray dried products on the retail market. Peebles' instantizer is shown in Fig. 91.


Fig. 91  The Peebles Rewet Instantizer

Another example of a rewet agglomeration plant is shown in Fig. 92, which illustrates the principle of a method developed by Nestlé for agglomerating milk powders, chocolate-flavoured beverages and soups. When agglomerating skim milk powders the tank (1) would contain a 10% solution of skim milk solids in water cooled to about 6ºC. The liquid is sprayed at a pressure of 20 bar by means of the pump (2) and nozzle (3), which is designed to give a flat jet with a high velocity of up to 8 m/sec. Skim milk powder, which is fed by means of a vibrator/screw conveyor (4), is dispersed over the jet where the single powder particles become rewetted to a moisture sufficiently high (10-15%) to make them sticky on the surface, so that any collision between particles will result in an agglomeration in the chamber (5). The powder is finally dried at 90ºC to 3% moisture (6) and bagged off.


Fig. 92  Rewet agglomeration plant (Nestlé)

The main features of the rewet agglomeration process are:

  • Wetting of the surface of the particles
  • Agglomeration
  • Redrying
  • Cooling
  • Sizing

Wetting

Wetting of the surface of the particles is done with humid air, steam, atomized water either pure or containing milk solids, sugar or other soluble components. The water may further contain additives such as vitamins (water soluble), minerals, colour and surface-active agents. The atomization of the moistening agent can be carried out by means of nozzles or a rotary atomizer. If a rotary atomizer with two feed pipes is used, it is possible to use a combination of steam and water or use two moistening agents, which cannot be mixed for various reasons.

If the product is insoluble, an adhesive can be dissolved in the moistening agent. When doing so products otherwise impossible to agglomerate can be agglomerated with a good result.

Agglomeration

Agglomeration, whereby the moist sticky particles collide due to the turbulence and adhere to each other forming agglomerates, is essential for the rewet process.

As powders with different compositions do not behave in the same way during the rewetting and agglomeration process, different equipment is needed to obtain an optimal agglomeration.

In principle there are two ways of performing the agglomeration:

  • Droplet agglomeration
  • Surface agglomeration

Droplet Agglomeration

In the droplet agglomeration process the powder particles are wetted with droplets of liquid atomized by means of a nozzle or a rotary atomizer while suspended in air, as described in Fig. 93. The powder may either be introduced around the rotary atomizer or the nozzle by means of gravity or pressure air conveying, or from below by means of pressure conveying.


Fig. 93  Feed system for a rewet plant (wetting by means of warm water atomized by an atomizer)

The actual agglomeration takes place by collision of the single particles wetted and sticky on the surface, and when they reach the agglomeration chamber wall they will roll down whereby the compactness of the agglomerates is obtained.

Droplet agglomeration can also be performed by spraying the wetting agent through a number of nozzles positioned right above the fluidized powder layer in a Vibro-Fluidizer. To obtain stable agglomerates the powder should contain sufficient binding material, like carbohydrates.

Some powders (containing a high content of fat and sugar) become so sticky when wetted, that heavy deposits in the conical part of the agglomeration chamber develop. A mechanically revolving scraper or similar is therefore necessary in order to get the powder out of the chamber. Another and technically better solution is to let the conical part of the agglomeration chamber rotate slowly and have a stationary scraping device such as a knife scraping off the powder. The rotating cone is mainly used when the powder contains cereals and starch, such as baby foods.

The droplet agglomeration process is especially used for powders containing fat such as whole milk powder and powders with a high content of sugar such as cocoa-milk-sugar mixtures. If cold-water instant whole milk powder is produced, a lecithin dosing equipment is installed between two Vibro-Fluidizers (see page 235). However, it should be mentioned that the final product quality will never be as good as that produced on a drying plant equipped with fines return, fluid beds and lecithin dosing equipment.

Surface Agglomeration

 In the surface agglomeration either steam or warm moist air with a high relative humidity is used as the moistening agent. The surface of the individual dry particles is wetted due to condensation of the water vapour on the colder particles, whereby the stickiness required for the agglomeration is created. The subsequent agglomeration will take place, if the particles are exposed to sufficient mechanical impact. The impact can for example be accomplished in a vortex tube into which the moistening medium is introduced tangentially and the powder to be agglomerated along the centre axis. It is very important that the humid air/steam used for the rewetting does not contain any droplets of water, as that, in combi-nation with the intensive mechanical impact, will result in overwetted agglomerates being too compact for a quick rate of rehydration.

The warm humid air is usually made by spraying steam into warm air at a given temperature to obtain a relative humidity of 100%. Any water droplets are re-moved in a demister, after which the air is heated further to give the desired relative humidity. By changing the air temperature prior to the steam injection and the subsequent air temperature, it is possible to obtain air with a given temperature and relative humidity. See Fig. 94.


Fig. 94  Feed system for a rewet plant. Wetting by means of warm moist air

The surface agglomeration is mainly used for skim milk powder when large agglomerates are aimed at. The final product properties depend to a great extent on the raw material used for the rewetting, and below is shown a specification for a recommendable basis powder:

Bulk density, tapped 1250x: 0.80 g/cm3
WPNI: 2-3 mg/g powder *)
Insolubility index: < 0.1 ml
Particle density: 1.35 g/cm3
Mean particle size: approx. 50 μm
Amount above 100 μm: max. 25%

*) corresponding to a pasteurization temperature of 
≈90ºC prior to evaporation.

The surface agglomeration can also be used for whole milk powder, but the agglomerates get too compact for obtaining a powder with good rehydrating properties.

Redrying

As the basis powder used for agglomeration is remoistened to obtain the desired surface characteristic for an optimal stickiness, this additional moisture has to be evaporated again in order to reach the specified moisture content.

The agglomerates may break down again, if they are exposed to extensive mechanical handling, such as in a pneumatic conveying system. It is therefore necessary to perform the drying in a Vibro-Fluidizer as mentioned on page 119. However, as the rewetted powder is to be compared to a layer of wet snow when entering the Vibro-Fluidizer, a relatively high air velocity is required to fluidize the powder. Otherwise, lumps will be formed, and the drying efficiency of the Vibro-Fluidizer will decrease.

Cooling

Like the redrying the cooling is performed best in a Vibro-Fluidizer.

Sizing

Usually, there is a well defined requirement to the agglomerate size distribution of the final powder. It is therefore necessary to sift the powder. This is done in a sieve with two different net sizes placed above each other. Thus it is possible to remove any agglomerates/lumps considered to be too big in the final product. This oversize fraction may be milled and returned to the process. Powder passing through the upper net may be further fractionated on the lower net into a main fraction and a fines fraction consisting of single particles and agglomerates being too small. This fines fraction is together with the cyclone fraction from the Vibro-Fluidizer recycled back to the process.

The actual powder feeding system consists of a silo and a screw conveyor with variable speed. The powder is by means of a rotary blow-through valve fed into a high-pressure air line conveying the powder to the agglomerating module.

It is usually a requirement to most rewet installations that they are product flexible. Therefore, both droplet and surface agglomeration methods are often installed in the same plant. The rotating cone may also easily be incorporated in the plant thus giving the possibility of agglomerating any milk based product. Lecithination may naturally also be applied to this process, if cold water fat-containing products are aimed at. In Fig. 95 a flow sheet of a rewet plant NIRO design is shown, with the possibility of all above mentioned agglomeration systems.


Fig. 95  Niro multi-purpose rewet agglomeration plant

 

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