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Chapter 20
Granulation

Dry bulky powders, semidry powders which spontaneously form variable agglomerates, and granular materials and
powders mixed with a small amount of binder solution are not a convenient feed material. These kinds of systems do
not flow well and do not fill a mold or die uniformly. For a powder system, a satisfactory semidry feed material consists
of controlled agglomerates called granules which are produced by means of granulation processes.

Granulation may be achieved directly by pressing, by extruding the material through an orifice, or by spraying a wetting
liquid or a binder solution into a stirred powder, which is called spray granulation. Granules are produced indirectly in
the process of spray drying by atomizing a slurry of the powder into a drying chamber. Modern powder pressing
operations now depend on a granule feed. Granulated material is used extensively as a feed material for calcining and
melting processes and directly as a product serving as a catalyst support. Spray drying is also used as a unit operation to
reduce the liquid content of a slurry to form a semidry material containing additives for use in extrusion.

We examine granulation processes and the characteristics of granules in this chapter.

20.1
Direct Granulation

Powder granules may be produced directly using pressing, extrusion, and spray granulation, which are sometimes
referred to as pelletizing processes. Materials prepared in this way include technical aluminas, ferrites, clays, tile bodies,
porcelain bodies, conventional refractory compositions, catalyst supports, and feed materials for glass melting and metal
refining.

Fine powders premixed with only a few percent of a wetting liquid or a binder solution may be compacted in a tableting
die or between briquetting

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rolls or belts. A mixer with a roller and a perforated bottom plate is also used to produce granulated powder. Granules
produced by compaction are commonly dense, hard, and strong if compacted above about 10 MPa. An auger extruder or
a kneader may be used to produce a granular product having a plastic consistency. Spaghetti-shaped material exiting
from an orifice plate is cut with rotary knives. In roll extrusion, moist feed is forced through perforated rolls or through
a perforated plate. Dried material is crushed to reduce the particle size.

Spray granulation is the formation of granules when a liquid or a binder solution is sprayed into a continually agitated
powder. The formation of the granules may be considered to occur in two stages:

1. Nucleation of primary agglomerates at random

2. Growth by the addition of particles or small agglomerates to the central agglomerate

When stirring the powder, particles roll and slide, and fines become airborne. A minute agglomerate called a nucleus or
seed is formed when a droplet of liquid or binder solution hits and is adsorbed on the surface of a group of particles.
Capillary forces and binder flocculation give the nuclei strength. Nuclei are more numerous when the liquid is
introduced as a fine mist and the powder is agitated vigorously. Capillary forces may cause particle sliding and
rearrangement, densification, and the migration of liquid to the surface of the agglomerate nuclei.

The growth of granules by layering occurs by the contact and adhesion of particles to the nuclei. Alternatively, the
agglomeration of young nuclei and fracture fragments can also produce a granule. These growth mechanisms are
illustrated in Fig. 20.1. The rate of each mechanism depends on the liquid feed rate, the adsorption of liquid into the
agglomerate, and the mixing action.

Fig. 20.1
Nucleation and growth of granule in spray granulation may occur by addition of
primary particles or small agglomerates.

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Rubbing between granules during tumbling may cause particle transfer at surfaces and surface smoothing. Fracture of
granules and attrition are higher when the forces during mixing are higher and the granules lack strength. The size,
shape, and surface appearance of granules formed by spray granulation are shown in Fig. 20.2.

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Fig. 20.2
Scanning electron micrograph of granules formed by
spray granulation: (a) general view and (b) shape and
surface smoothed by rubbing during tumbling.

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Fig. 20.3
Granule size development on adding a liquid with
constant mixing.

For each system, there is a critical range of liquid content for granulation. At the low end, granules are eventually
formed when the processing energy is sufficiently high. The addition of a greater amount of liquid generally increases
the mean size, the size distribution, and the porosity of the granules (see Figs. 20.3 and 20.4). The liquid requirement for
granulation is greater when the

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Fig. 20.4
Concentation of added binder solution must be controlled to obtain
maximum yield of granules within target size range.

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specific surface area of the powder is higher. Common liquid requirements in the range of 2036 vol% indicate that
during granulation the pores in granules are incompletely saturated. The spray geometry, mixing process, and liquid/
binder solution content must be well planned and controlled to produce the maximum yield of granules falling within a
target size range (see Fig. 20.4).

Rotating pan-type mixers, ribbon mixers, double planetary mixers, V-blenders, and continuous rotating drum and disk
pelletizers are used for directly granulating ceramic powders. Rotating drums and disks are commonly used for
producing rather coarse granules 110 mm in size as a feed for melting operations. Mixers with a more intense mixing
action produce smaller granules, but larger than the 44 µm required for flow and for pressing. A binder aids in forming
granules and increases the strength of granules of coarser powders. Increasing the temperature of the powder tends to
produce smaller granules.

Granules produced by spray granulation are more nearly spherical than granules produced by compaction and extrusion.
Capacities of industrial granulators range up to several tons per hour. Spray-granulated material is usually partially dried
to produce the powder feed for pressing operations.

20.2
Spray Drying

Cocurrent and mixed-flow spray dryers are illustrated in Fig. 20.5. Spray drying is the process of spraying a slurry into a
warm drying medium to produce nearly spherical powder granules that are relatively homogeneous. The dispersion of
small droplets of high specific surface area in the drying air provides

Fig. 20.5
Spray dryers: (left) cocurrent spray dryer with centrifugal atomizer, and
(right) mixed-flow spray dryer with a nozzle atomizer.

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a relatively high drying efficiency. Spray drying is used widely for preparing granulated pressing feed from powders of
ferrites, titanates, other electrical ceramic compositions, alumina, carbides, nitrides, and porcelain bodies. A milling
process is commonly used to disperse powder agglomerates and for mixing. The binder solution may be filtered to
remove undissolved globules. Secondary mixing during atomization further reduces the scale of inhomogeneity in the
product. When properly controlled, spray drying produces a nearly spherical, relatively dense granulated product.
Granules larger than 20 µm in size flow and compact well in pressing operations. Capacities of industrial spray dryers
range from less than 10 to several 100 kg/h.

Slurry Controls

The batch, which commonly includes recycled fines from the cyclone, is mixed to form a deflocculated, shear thinning
slurry feed. Consideration must be given to soluble inorganic impurities retained in spray drying, and the effect of the
drying on the degradation or evaporation of the organic binders and plasticizers. Aqueous systems are commonly used,
but recycled organic liquids are sometimes utilized when the chemical or thermal reactivity of the powder or binder
precludes using an aqueous system.

Slurry characterization includes the determination of the slurry density, the foam content, the percent solids, and the
viscosity behavior (Fig. 20.6). A slurry with a high solids content is desirable for technical reasons and to in-

Fig. 20.6
Viscosity behavior of alumina slurries for spray-drying is shear thinning
(determined using a concentric cylinder viscometer).

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crease the energy efficiency in drying and the product yield (see Fig. 20.7). The slurry should be relatively free of air
because air bubbles reduce the density of both the slurry and the resultant granules. The slurry density is determined by
weighing a standard volume of a slurry sample. The foam index is calculated from the theoretical density of the batch
DT and the apparent experimental slurry density DE

Often an antifoam must be added to the slurry to control the foam index below a control limit.

Weighing errors in batching may cause errors in the inorganic content of the product. The percent solids is determined
by heating a slurry sample to eliminate liquid and organic additives and comparing the experimental result with the
value for the batch. The viscosity must be determined over a wide range of shear rate to check for reproducibility and
the absence of shear thickening behavior. The shear rate during atomization may exceed 104 s-1. Wet-milled slurries
with the shear thinning viscosity behavior shown in Fig. 20.6 were satisfactory for spray drying; blunging did not
produce sufficient powder dispersion.

Atomization

Slurry screened to remove coarse particles is commonly atomized using either a nozzle or a rotary atomizer. In a
pressure nozzle, slurry accelerating through small channels achieves turbulence and breaks up into droplets. Pressure
noz-

Fig. 20.7
Output of powder granules from a spray drying
as a function of powder content in feed slurry.
Dryer evaporative capacity of water is 100 kg/h
and a yield of 100% is assumed.
[From S. J. Lukasiewicz, J. Am. Ceram. Soc.,
72(4) 618 (1989).]

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zles are relatively inexpensive but are subject to blocked flow, and the high operational pressures, ranging up to 10
MPa, increase abrasion rates. In a two-fluid nozzle (Fig. 20.8), a high-velocity gas is mixed with the slurry to produce
turbulence and droplets. Operating pressures may be reduced to less than 1 MPa. Centrifugal energy from a disk or
wheel rotating at several thousand revolutions per minute produces droplets in a rotary atomizer. The larger flow
channels and lower operating pressure increase the feed rate capacity and the reliability. Spray dryers using radial
atomization are relatively large in diameter because of the larger radial/axial flow pattern of the spray.

Parameters that control the droplet size in the spray are listed in Table 20.1. Characteristics of spray-dried alumina
granules listed in Table 20.2 are indicative of these trends. Granules ranging up to about 400 µm may be produced using
pressure nozzles, and sizes up to about 150 µm using a rotary atomizer. Relative to a pressure nozzle, a two-fluid nozzle
usually produces a larger fraction of sizes, < 40 µm.

AtomizationDrying Air Configuration

Drying involves simultaneous heat and mass transfer. The airflow pattern influences the droplet drying time, residence
time in dryer, residual liquid content, and wall deposits. Heat is transferred by convection from the air to the droplet.
Heat absorbed evaporates the liquid and the vapor is transported by convection into the drying air. A cocurrent dryer
design positions the atomizer and drying-air inlet at the top of the dryer to provide cocurrent flow (see Fig. 20.5).
Atomized slurry is of maximum liquid content when it encounters the laminar flow of hot incoming air. Using this
design, the maximum product temperature is relatively low and the evaporation time is relatively short. However, the
product exits with moist air, and the exit temperature must be relatively high to obtain a dry product. Using a
countercurrent design, slurry and drying air inlets are at opposite ends of the drying chamber. Droplets encountering the
incoming hot air have already been partially dried, and the product heating is greater. The mixed flow design (Fig.
20.5), which increases the residence time of the spray and provides a means for reducing the size of the chamber needed
for drying, is a convenient compromise and is characteristic of many small industrial and laboratory dryers.

Fig. 20.8
Two-fluid nozzle with
external mixing for
atomizing a slurry.

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Table 20.1 Parameters Influencing Droplet Size

Atomization Size Proportional To
Pressure nozzle Surface tension (viscosity)/pressure
Pneumatic (2-fluid) Surface tension (viscosity)/mass(air/slurry)
Centrifugal Surface tension (viscosity) (slurry feed rate)/(speed × diameter) of wheel

Drying Droplets to Form Granules

The rate of drying varies directly with the rates of heat and mass transfer and depends on the temperature and humidity of the air, the transport
properties of the air near the droplet, and transport properties within the drying droplet. Considerable evaporation must occur during the first
few milliseconds of drying to prevent the formation of agglomerated granules and a coating of sticky agglomerates on the wall of the dryer.
The velocity of the droplets from the atomizer is considerably higher than the velocity of the drying air. Incoming air keeps the humidity low
and carries moisture away. Filtered drying air is commonly heated using natural gas or electrically to a temperature in the range of 250600°C.
The inlet air temperature depends directly on the dryer design, the product residence time, and the thermal limitations of the product. The
product temperature is normally lower than the outlet air temperature and is usually maintained below 100°C when using organic binders and
additives.

The evaporation rate initially increases as the droplet is heated. Volume shrinkage occurs as liquid is lost and the PF of the particles increases.
Evaporation reduces the air temperature. The drying rate remains high as long as the temperature of the drying air is maintained and the
surface is saturated with liquid. At some point the rate of flow of liquid to the surface becomes rate controlling. Slow capillary flow and fast
evaporation (i.e., a relatively high inlet air temperature and a relatively low humidity) may form a dried surface layer almost instantaneously.
Capillary flow is reduced by parameters which

Table 20.2 Characteristics of Spray-Dried Alumina Granulesa

Slurry Granule Sizec (µm) Granule Density Filld Density
(%) (%)
Solids Binder 90% < 50% < 10% <
(vol%) (wt%)b
1.0 54 30
35 172 92 40
0.5 55 32
35 144 74 27
0.5 58 34
50 202 118 54
0.5 57 34
52 216 113 41
aTwo-fluid nozzle, utility dryer.
bFully hydrolyzed polyvinyl alcohol; powder basis.
cSieving data.
dBulk density after pouring into graduated cylinder.

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lessen the permeability, such as binder molecules, binder migration forming a surface skin, and the migration of fine
particles or precipitated salts into pores near the surface. Rapid heating may cause liquid to evaporate within the droplet,
forming a vapor bubble which may expand the agglomerate. The granule is nearly in equilibrium with the warm, moist
air leaving the dryer, and the outlet air temperature is controlled to maintain a product with a constant moisture content.

The majority of the spray-dried product is discharged through a rotary valve into interchangeable containers attached at
the base. Product fines entrained in the exhaust air are separated using a cyclone or bag filters. Product fines may be
used in some pressing operations but are commonly recycled into the feed slurry. Periodic cleaning of the dryer using a
liquid spray is required to remove the granulate crust. Cleaning is facilitated when the dried binder system is readily
redissolved. Abnormally large granules and flakes of granulate crust from the wall of the dryer are undesirable and are
commonly removed by screening.

Granule Character

Instability causes the high-velocity slurry stream to break up into droplets, as shown in Fig. 20.9. Flow required to
produce a spherical shape is motivated by surface tension and resisted by the viscosity. Colliding droplets may coalesce
into a larger droplet which, if viscous, will be less nearly spherical in shape or form a granule that is a cluster of smaller
agglomerates that are partially merged. Air bubbles present in the feed slurry or occluded during atomization

Fig. 20.9
High-speed photograph of droplet forming from ''slurry comet" during
spray drying.
(Photo courtesy of Niro Atomizer Inc., Columbia, MD.)

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Fig. 20.10
Scanning electron micrographs of spray dried granules: (a)
smooth, round, dense granules of alumina and (b) granules
of zinc oxide having a "donut" shape.

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using a two-fluid nozzle may persist as relatively large pores in the ultimate granule.

Granules with a large crater or a donut shape are often observed in industrial spray-dried material (Fig. 20.10), regardless of the atomization
method used. The tendency for these shapes is higher when the inlet temperature is relatively high, the binder content is relatively high, and
the solids loading in the slurry is relatively low. Rapid surface drying and the formation of surface material of low permeability produce a
greater initial heating rate. Momentary internal evaporation may form a vapor bubble. When the bubble breaks through the last formed,
binder-deficient surface regions and the agglomerate is viscous, surface tension induced flow causes a dimpled or donut shape to be formed.
Granules containing an abnormally large internal pore may be produced when the migration of finer particles, salts, or binder during drying
produces a surface layer of higher PF that shrinks relatively less on drying.

Characteristics of granules prepared by spray drying and spray granulation are listed in Tables 20.2 and 20.3. The PF of 0.550.58 for the
particles in spray-dried alumina granules is a few percent lower than the PFmax for this powder. Relative to the spray-granulated product, the
spray-dried granules are somewhat finer, of comparable bulk density, and slightly faster in flow rate owing to their more nearly spherical
shape. The ratio of tap density to fill density is an index of hindered packing during gravity settling after pouring and is slightly higher for the
less spherical spray-dried granules. The higher fill density for the whiteware composition reflects the higher granule density achieved for the
more densely packing AFDZ particle size distribution.

Table 20.3 Characteristics of Granulated Whiteware Bodiesa

Parameter Wall Tile Spray Drying Hotel China Spray Drying Hotel China Spray Granulation
Moisture Adsorption (wt%)
33% RH 2.7 3.5 2.4
92% RH 4.8 4.9 3.5
Granule size (µm)b
90% < 300 446 992
50% < 151 148 403
10% < 55 99 122
Flow time (s)c
33% RH 7 10
92% RH 8 12
Fill density (%)
38 40 41
Tapped density/fill density
1.15 1.13 1.20
aGranules larger than 1000 µm removed.
bSieving data.
cFunnel test.

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Summary

Granulated powders are commonly used for pressing, calcining, and melting operations. Compaction and extrusion
processes produce a relatively large granulated product. Spray granulation is used to produce granules that are
satisfactory for use as a pressing powder for traditional ceramics and refractories and some fine-grained technical
ceramics. Spray-drying is used to produce granules that are more homogeneous. Controls for spray-drying include
slurry formulation and control, atomization, the droplet-drying air configuration, and the drying conditions. Spray-
drying must be properly controlled to avoid the formation of granules with irregular shapes and large internal pores.
Spray-drying is relatively efficient because the product is well dispersed in the drying medium and has a high specific
surface area.

Suggested Reading

1. F. V. Shaw, "Spray Drying: A Traditional Process for Advanced Applications," Am. Ceram. Soc. Bull., 69(9),
14841489 (1990).

2. S. L. Lukasiewicz, "Spray-Drying Ceramic Powders," J. Am. Ceram. Soc., 72(4), 617624 (1989).

3. H. B. Ries, "Methods of Preparing Bodies for the Preparation of Oxidic and Non-Oxidic Ceramics," Keram. Z., 35(2),
6771 (1983).

4. P. J. Sherrington and R. Oliver, Granulation, Heyden and Sons. London, 1981.

5. K. Masters, Spray Drying, Wiley-Interscience, New York, 1979.

6. W. H. Engelleitner, "Pelletizing as Applied to the Ceramic Field," Am. Ceram. Soc. Bull., 54(2), 206207 (1975).

7. D. A. Lee, "Comparison of Centrifugal and Nozzle Atomization in Spray Dryers," Am. Ceram. Soc. Bull., 53(3),
232233 (1974).

8. R. H. Perry and C. H. Chilton, Chemical Engineers' Handbook, McGraw-Hill, New York, 1973.

Problems

20.1 Sketch the change in the physical character of the granules in Fig. 20.4 on increasing the content of binder solution
from 11.5 to 14%.

20.2 The size data in Table 20.2 are log normal. Estimate and compare the parameters and g for the powders.

20.3 Alumina slurries of 60, 70, and 80 wt% solids are spray dried. Calculate and contrast the relative mass of liquid
removed per mass of product formed. Assume 0.4 wt% moisture in product.

20.4 Assuming that the evaporation rate (mass water/time) is a constant value during the drying of the granules in
Problem 20.3, calculate and compare

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the relative product formation rates when the residual moisture content in the product is 0.4 wt%.

20.5 A slurry for spray drying contains 40 vol% zirconia powder (Dp = 6.0 Mg/m3) and 60 vol% water. The measured
density of the prepared slurry is 2.60 Mg/m3. Calculate the foam index.

20.6 Assuming that in spray granulation the liquid requirement is directly proportional to the specific surface area of the
powders used, calculate the ratio of liquid required for two powders having specific surface areas of 1.2 and 12 m2/g.
What is the ratio for a powder containing 2/3 of the coarser powder and 1/3 of the finer powder (relative to the coarser
powder)?

20.7 Alumina granules with a solids fraction of 0.48 are produced on spray drying an aqueous slurry containing 80 wt%
alumina. Did the droplets shrink in size during drying?

20.8 Spray-dried granules of alumina and barium titanate powders have a granule density DG = 55%. Contrast this
density to the powder bulk density for each given in Tables 5.3 and 5.4.

Examples

Example 20.1 Granules for pressing tile are prepared by spray granulation at 14 wt% water; these are dried to 10 wt%
water for the pressing feed. Prepared by spray drying, the starting slurry contains 60 vol% water and the spray-dried
product has 10 wt% water. Contrast the weight of water removed per weight of product for the two processes. The
density of the powder is 2.60 Mg/m3.

Solution. For spray granulation, the as-formed granules contain 86 g of powder and 14 g of water. The product contains
90 g of powder and 10 g of water. Relative to 100 g of powder, the corresponding liquid contents are 16.3 g asformed
and 11.1 g after drying. The relative weight loss is

W/Wproduct = (16.3 g 11.1 g) 100/(100 g + 11.1 g) = 4.7%

For the spray drying, the weight percent water in the slurry is

Water (wt%) = 0.60 (1 g/cm3) 100/[0.60 (1 g/cm3) + 0.40 (2.60 g/cm3)]

Waterslurry = 36.6 wt%

On drying, for a basis of 100 g of powder,

W/Wproduct = (57.7 g 11.1 g) 100/(100 g + 11.1 g)

W/Wproduct = 42%

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Considerably less water is removed by drying in the spray granulation process and this component of the processing
cost is lower. However, granules made by spray granulation are commonly less homogeneous.

Example 20.2 When preparing a slurry for spray drying, an antifoam must often be added to reduce the foam content of
the slurry. Otherwise, the granule density and the fill density may be unacceptably low. How is the foam content
determined?

Solution. The foam content can be determined by comparing the measured slurry density with the calculated slurry
density. For example, consider a slurry which consists of 100 g of alumina powder, 60 g of water + deflocculant, and 1
g of polyvinyl alcohol. The experimental density DE of the slurry determined by measuring the mass and volume VE of
a sample from the bulk of the mixed slurry is 1.58 g/cm3. The volume calculated VT assuming no foam is

VT = Wi/Di

VT = 100 g/(3.98 g/cm3) + 60 g/(1.00 g/cm3) + 1 g/(1.26 g/cm3)

VT = 85.9 cm3 for a 161-g batch, and the calculated density DT is

DT = 161 g/85.9 cm3 = 1.87 g/cm3

The foam index FI is calculated as

FI (%) = (VE VT) 100/VE = (DT DE) 100/DT

FI (%) = (1.87 g/cm3 1.58 g/cm3)/1.87 g/cm3 = 16%

100 mL of slurry will contain 16 mL of occluded air which may cause an increased porosity in the atomized droplets
and the granules.

Example 20.3 Table 20.2 indicates that increasing the binder concentration and the solids content of the slurries altered
the sizes and the density of the spray-dried granules. What caused these results?

Solution. Increasing the binder content will increase the viscosity of the slurry and the droplet size on spraying;
increasing the powder content in the slurry will have a similar effect. The consequence is larger granules and clearly the
solids content had the bigger effect. The granule density will depend on steric hindrance of particle motions during
drying and the reduced Kp for fluid transport produced by the binder. Increasing the solids content of the slurry and
reducing the binder content contributed a higher packing density in the droplet and granule.

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Example 20.4 Compare a granule density of 58% and a fill density of 34% with the bulk density of 1.8 Mg/m3 for the
capacitor grade barium titanate powder in Table 5.4. The density of barium titanate is 6.0 Mg/m3.

Solution. The bulk density Dbulk of the powder is

Dbulk = (1.8 Mg/m3) 100/6.0 Mg/m3 = 30%

The granule density of 58% is nearly twice the density of the dry powder. However, the interstices within the granules
and larger interstices between the granules cause the fill density of the granules to be only slightly higher (34%). But the
higher density and larger size of the granules endows the granules with much better flowability.

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