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The effect of granulation conditions on bulk density of a product

Article · January 2004

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Physicochemical Problems of Mineral Processing, 38 (2004) 177-186
Fizykochemiczne Problemy Mineralurgii, 38 (2004) 177-186

Tadeusz GLUBA, Andrzej OBRANIAK, Estera GAWOT-MŁYNARCZYK∗

THE EFFECT OF GRANULATION CONDITIONS

ON BULK DENSITY OF A PRODUCT

Received April 15, 2004; reviewed; accepted June 8, 2004

Changes in bulk density of a bed during wet granulation of silica flour in a batch drum granulator
were studied. Three size fractions of the flour were used in the studies. They differed in the particle
size composition and mean particle dimension. Variable parameters were the wetting conditions
(droplet diameter, degree of bed saturation) and particle size composition of the raw material. The bed
of loose material was wetted while tumbling, at a constant volumetric flow rate, using a system of two
pneumatic spray nozzles. In each trial at determined time intervals feed samples were taken from the
drum to specify the particle composition and bulk density of granulated material at a given stage of
the process. The effect of droplet diameter, mean size of raw material particles and the saturation of
granulated bed on changes in the bulk density of a product was estimated. A correlation equation
describing the effect of tested parameters on bulk density changes was proposed.

Key words: drum granulation, bulk density

INTRODUCTION

One of significant parameters that describe properties of granular materials is their

bulk density. For granulated materials this parameter is of special importance. By
selecting proper conditions of granulation process a product of possibly high density
can be obtained, which has an influence on a better utilisation of storage area and
means of transport. Bulk density of a granulated product depends both on raw material
properties (density, particle size composition), concentration of particles in the formed
granules (granule porosity), and on the obtained particle size distribution on which the
volume of intraparticle space depends Gluba and Grabowski (2001), Podczeck and
Lee-Amies (1996)]. In the process of granulation bulk density of the processed bed
undergoes systematic changes that are related both to the mechanisms of formation

∗
Technical University of Lodz, Faculty of Process and Environmental Engineering
Stefanowskiego 12/16, 90-924 Lodz, Poland, [email protected]
178 The effect of granulation conditions on bulk density of a product

and growth of agglomerates, their concentration, and also the mechanisms of

destruction. Problems related to the effect of granulation conditions on bulk density of
a product are not frequently discussed in literature. Obraniak (2002) presented changes
in bulk density of granulated material produced from foundry bentonite in reference to
process and equipment parameters and wetting time. He obtained a linear relation of
bulk density changes with the time of granulation. Zuurman et al. (1995) conducted
studies on the effect of a binding agent on bulk density and compactibility of granules
of two types of lactose, using two different wet granulation techniques. They found
that efficiency of the binder increased with a decrease of bulk density of the
granulated bed. Yu et al. (1995) studied the effect of moisture content on coal
agglomeration and bulk density. They observed among the others that the density of
agglomerates increased with an increase of moisture content to a certain maximum,
and next it started falling down, while bulk density of the bed decreased with an
increase of moisture content to some minimum and then it started growing.
So far, the bulk density of a granulated bed has been investigated for selected
groups of materials, which made it impossible to propose general relations.
Additionally, there are no studies in which the effect of other parameters (beside
moisture content) that characterise bed wetting is taken into account.

AIM OF STUDIES

The aim of studies was to assess the effect of bed wetting conditions and particle
size of raw material on changes in the bulk density of feed during wet drum
granulation.

EXPERIMENTAL SET-UP AND METHODOLOGY

Granulation was carried out batch-wise in a horizontal drum of diameter D=0.5 m

and length L=0.4 m. The drum was driven by an electric motor through a toothed gear
and belt transmission. In the entire series of investigations a constant rotational speed
of the granulator n=20 rpm was applied and a constant volumetric degree of drum
filling with the raw material k=0.1, determined in reference to the bulk density of
loosely packed material was used. A tested material consisted of three size fractions of
silica flour from Strzebłowska Mine of Mineral Raw Materials at Sobótka. Particular
fractions denoted by the symbols MK 0,056, MK 0,075 and MK 0,10 differed in the
maximum particle size and range of particle size composition. For each raw material
the basic physical properties were determined. The particle size distribution was
estimated by means of a laser particle analyser ANALYSETTE 22, and on this basis
the mean particle size dz was determined. Raw material density ρs and bulk densities
in the material loosely packed ρbl and concentrated to the minimum volume ρbc were
also determined. Fine-grained material placed in the drum was wetted while tumbling
by means of two pneumatic spray nozzles introduced axially into the drum. Constant
 T. Gluba, A. Obraniak, E. Gawot-Młynarczyk 179

flow rate of the wetting liquid (distilled water) through the nozzles, equal to
Qw=12 · 10-3 m3/h was applied. Changes in the wetting liquid dispersion (droplet size)
were obtained by changing the rate of air flow through the nozzles in the range
Qp=1 to 3 m3/h. Droplet size distribution in the dispersed stream at specified
parameters of nozzle operation, characterised by the dispersion degree q= Qw/Qp, was
measured by a DANTEC laser analyser. On the basis of these distributions, the mean
droplet diameters dk obtained at given parameters of nozzle operation were calculated.
The operating parameters of the nozzle used in the investigations are given in Table 1.
Each time, a determined volume of the binding liquid was supplied to the bed. The
volume was determined for a specified value of feed saturation degree S, taken as a
ratio of the volume of the added liquid to the volume of intraparticle space in the
loosely packed material in the drum. Granulation was studied at three degrees of
saturation S = 0.32, 0.34 and 0.36. After wetting the process of granulation was
continued until the moment when water pressed from the granules onto their surface
caused intensive sticking to the drum walls hampering in this way a further process. In
determined moments samples were taken from the drum and on their basis properties
of the formed granulated product were specified. The first sample was taken
immediately after the wetting had been finished (tg=0), and the last one after
completing the process. The particle size composition was determined on the basis of
screen analysis and bulk density was calculated on the basis of the mass and volume
of a sample placed in a measuring cylinder (after subtracting the mass of water
contained in it).

Table 1. Operating parameters of spray nozzles

Qw Qp q dk
3
[m /h] [m3/h] [-] [µm]
0.012 1.0 0.0120 235.70
0.012 1.5 0.0080 211.90
0.012 2.0 0.0060 194.11
0.012 2.5 0.0048 154.16
0.012 3.0 0.0040 143.90

RESULTS AND DISCUSSION

On the basis of analysis of samples taken immediately after finishing the wetting it
was found that the bed contained both non-granulated raw material and a specified
percent of nuclei and still weak granules. Mutual quantitative proportions between the
finest fraction (of dimensions < 1 mm), containing non-granulated material and nuclei
of granules and bigger agglomerates appeared to be dependent on the bed wetting
conditions and also on particle size of the raw material. Percentage of the smallest size
fraction in the bed was in the range from 40 to 60%. Structure of the bed formed after
180 The effect of granulation conditions on bulk density of a product

wetting had an immediate influence on its bulk density. The effect of particle size of
the raw material and wetting parameters on the bulk density of the bed (after wetting)
was described by the power function of several variables. As a result of regression,
equation (1) with the correlation coefficient R = 0.93 was obtained:

ρ bn = A ⋅ d k0,32 ⋅ d z0,37 ⋅ S −1,8 (1)

where A is constant.

dk=194.1, S=0.32
1,3
dk=143.9, S=0.36
1,2
1,1 bentonite, dk=3mm

1 dolomite, dk=143.9,
ρ b [kg/dm ]
3

S=0.36
0,9
0,8
0,7
0,6 Linear relation typical for silica
0,5 flour granulation

0,4
0 5 10 tg [min] 15 20

Fig. 1. Examples of changes in the bulk density of the bed during granulation

At the further stage of the process (granulation) systematic changes in the

granulated bed properties took place leading to changes in bulk density of the bed. An
example of changes in bulk density of the granulated bed of silica flour compared to
the results obtained for other materials (dolomite and foundry bentonite) [Gluba
(2003), Obraniak (2002)] is shown in Fig. 1. For most trials with silica flour a linear
increase of bulk density with granulation time was obtained. In certain process
conditions when a longer time of granulation was required, changes of bulk density in
time departed from linearity (e.g. for dk=0.1439). Analogous relations were obtained
during dolomite granulation in similar wetting conditions. The required granulation
time for this material was usually longer than for silica flour, which had an effect on
the character of changes in bulk density (the presence of an extremum). A different
character had the changes observed during bentonite agglomeration. In this case the
process mechanism was different; in the whole granulation period wetting liquid in the
 T. Gluba, A. Obraniak, E. Gawot-Młynarczyk 181

form of droplets with uniform size (about 3 mm) was supplied to the bed at low
wetting intensity.
The differences observed in particular cases are a consequence of the dominance of
various mechanisms of formation and growth of agglomerates at different stages of the
process. To explain this problem some theoretical analysis should be made.
Bulk density of the feed during granulation can be determined on the basis of its
mass m and volume V using the formula:

m
ρb = (2)
V

The mass of processed feed m is a sum of solid mass ms and the mass of supplied
wetting liquid mw, while the volume of the bed consists of the volume of material
particles Vs, binding liquid volume Vw and air volume Vp, hence:

ms + mw
ρb = (3)
Vs + Vw + V p

The mass of raw material particles ms is constant during the process, but the
proportions between the mass of particles that form agglomerates and the mass of still
non-granulated powder are changing continuously. A total volume of all particles in
the bed Vs has also a constant value. The volume of air contained in the bed prior to
wetting can be determined on the basis of the bulk density of a given raw material ρbs
and specific density ρs. Changes in this volume during the process are very complex
and difficult to describe because of a simultaneous interaction of many mechanisms
that determine the formation, growth and also destruction of agglomerates.
From the practical point of view important is the bulk density of a dried product. In
this case, when air of the same volume replaced the evaporated liquid, bulk density
can be defined by the equation:

ms ms
ρb = = (4)
Vs + Vw + V p m m
s
+ w + Vp
ρs ρw

Substituting the relation for bed moisture content into equation (4)

mw
w= (5)
ms
form (6) is obtained:
182 The effect of granulation conditions on bulk density of a product

1
ρb = (6)
1 w Vp
+ +
ρs ρw ms

Due to constant value of the final bed moisture content w (in a given trial) and raw
material mass ms and taking into account that specific powder density ρs and water
density ρw do not change during the process, the above relation shows that changes in
bulk density of the granulated bed ρb at the stage of granulation depend only on
changes in the volume of air contained in the bed Vp.
To determine monotonicity of the above relation, the differential should be
calculated:

dρ b −1 1 dV p
= 2
⋅ ⋅ (7)
dt ⎛ 1 w V p ⎞ ms dt
⎜⎜ + + ⎟⎟
⎝ ρ s ρ w ms ⎠

In order to set up the sign of this relation the differential dVp/dt should be analysed.
The air in the granulated bed can be contained in the formed granules (V1),
between these granules (V2) and between particles of still non-granulated raw material
(V3).
Hence:

dV p dV1 dV2 dV3

= + + (8)
dt dt dt dt

Owing to the fact that the percentage of non-granulated particles decreases with the
process, the value of V3 decreases which brings about a negative value of derivative of
this component after the granulation. Along with the granulation time the formed
agglomerates are concentrated which results in a systematic decrease of pore size
inside the granules leading to negative dV1/dt. Changes in the volume V2 are a result
of changes in granule compactibility in the bed which depends on its homogeneity.
Results of investigations on drum granulation obtained in this study as well as those
presented by other authors [Gluba and Heim (2000)] show that with the granulation
time grows monodispersity of the processed bed (Fig. 2) which causes that spaces
between the formed granules increase. This is confirmed by the presented relation of
changes in bed homogeneity coefficient s/d with the granulation time (where s –
standard deviation, and d – mean particle size). It can be observed that despite
decreasing values of the coefficient s/d (the bed homogeneity increase) bulk density
determined for both dry and wet product increases.
 T. Gluba, A. Obraniak, E. Gawot-Młynarczyk 183

Summing up the above considerations, the character of the effect of particular

volume components can be presented in the form of inequality:

dV2 dV1 dV3

> 0, <0, <0 (9)
dt dt dt
Taking the above into account, it can be stated that during the process of wet
tumbling granulation changes in the bulk density may be both increasing and
decreasing – depending which of the mentioned derivatives has a decisive influence in
a given stage of granulation. So, it can be concluded that the character of changes
depends both on the loose material properties and process parameters. To explain the
impact of particular parameters applied in the investigations the obtained results
should be analysed thoroughly.

dg s/dg
16 1,8
wet. dry. 1,6
14

s/dg [-], ρb [kg/dm3]

12 1,4
1,2
10
dg [mm]

1
8
0,8
6
0,6
4 0,4
2 0,2
MK 0,056; S=0,320; dk=211,9
0 0
0 1 2 4 6 7
tg [min]

Fig. 2. Comparison of changes in bulk density of wet and dry granular material, variability coefficient
and mean granule diameter during granulation

When considering changes of the bulk density as a function of granulation time

(Fig. 3), for materials of different particle size composition, at constant saturation and
the same droplet size it was found that for the materials with bigger particles, the bulk
density is higher. This character of the obtained relations is related both to the
compactibility of the particles in the formed granules, to the packing of the granules in
the bed, and to the mean distance between the particles of non-granulated raw
material. Fine-grained materials used in the study were characterised by a growing
range of particle size composition with an increase of the mean particle size (a
simultaneous growth of dz and s/dz). For these materials, with an increase of the mean
184 The effect of granulation conditions on bulk density of a product

particle size, it is possible to reach denser packing of particles in the granules, which is
followed by a general increase of the bed bulk density. The study has shown that
during the process of granulation there is a systematic unification of the particle size
composition (a decrease of variability coefficient s/dg) which in turn has an effect on
the compactibility of granules in the bed. It was observed that with an increase of the
mean size of raw material particle the bed in the same process conditions becomes less
homogeneous (s/dg increases). This means that the bed obtained from the material of
bigger particles is characterised by a denser packing of granules, which influences its
bulk density increase.
Results of the studies revealed also a significant effect of dispersion of the wetting
liquid stream (droplet size) on the process of granulation and consequently on the bulk
density of the processed bed. A comparison of changes in the bulk density of feed
during the process of granulation for different mean size of droplets is shown in Fig. 4.
It follows that the feed bulk density increases with an increase of wetting liquid
droplets [Gluba (2002)]. Bigger droplets enable formation of stronger liquid bridges
which as a result leads to bigger condensation of particles in the granules.
Additionally, the bed wetted with bigger droplets is characterised by higher
polydispersity. These two factors have an influence on the increase of bulk density of
the bed with an increase of droplet size during wetting.

1
0,95 dk=194,1µm
0,9
ρb [kg/dm ]
3

0,85
0,8
0,75 MK 0,056
0,7 MK 0,075

0,65
0,6
0 1 2 tg [min] 3 4 5

Fig. 3. Comparison of bulk density changes during granulation for the same droplet size and two types
of raw material (S = 0.320)

On the stage of granulation, after wetting, continuous transformations induced by

the mechanisms of formation, growth and destruction of agglomerates take place in
the bed. A result of these transformations is an increase of the size of granules,
 T. Gluba, A. Obraniak, E. Gawot-Młynarczyk 185

condensation of their inner structure and change in the particle size composition.
These transformations being a determined function of granulation time lead also to
specific changes in the bed bulk density. The change in bulk density of the bed in time
is a combination of these transformations of the bed properties dependent on the
properties of raw materials and process parameters.

950

900

850
ρn [kg/m ]
3

800 dk=235.7
dk=194.1
750
dk=154.1
700 dk=143.9

650
MK 0.075 S=0.32
600
0 1 2 3 4 5 6
tg [min]

Fig.4. Comparison of bulk density changes during granulation for different droplet sizes

The effect of tested parameters on the increment of the bed bulk density at the
stage of granulation is described by the power relation:

ρ b − ρ bn = B ⋅ d k0,3 ⋅ d z3,5 ⋅ t (10)

where B is constant.
The above relation was obtained at the correlation coefficient R = 0.96.

CONCLUSIONS

1. During wet drum granulation of silica flour, bulk density of the processed bed
increases linearly in time;
2. The value of bulk density after wetting depends on the conditions of bed wetting
(dimensions of the wetting liquid droplets and bed saturation) and on the size of
raw material particles;
3. An increase of bulk density of the bed during granulation depends on the size of
raw material particles and wetting liquid droplets;
4. The effect of tested parameters on the increase of bulk density of the bed during
the process can be described by the power equation.
 186 The effect of granulation conditions on bulk density of a product

ACKNOWLEDGEMENT

The study was carried out within the research project no. 4 T09C 023 22 sponsored by KBN in the years
2002-2005.

REFERENCES

GLUBA T. (2003), The effect of wetting droplet size on the growth of agglomerates during wet drum
granulation, Powder Technology 130, 219-224
GLUBA T (2002), The effect of bed wetting conditions on the quality of a product obtained during drum
granulation, 15th International Congress CHISA
GLUBA T., GRABOWSKI R. (2001), The effect of wetting conditions on granule porosity, Prace
Naukowe Instytutu Górnictwa Politechniki Wrocławskiej 95, Konferencje 31, 15-24
GLUBA T., HEIM A. (2000), Wzrost aglomeratów w procesie mokrej granulacji bębnowej surowca
mineralnego o różnym składzie ziarnowym, Inż. Chem. i Proc., 21, 329-344
OBRANIAK A. (2002), Dynamika złoża ziarnistego w poziomych bębnach obrotowych, Praca doktorska,
Wydział Inżynierii Proc. i Ochrony Środowiska PŁ
PODCZECK F., LEE-AMIES G. (1996), The bulk volume changes of powders by granulation and
compression with respect to capsule filling, International Journal of Pharmaceutics, 142, 97-102
YU A.B., STANDISH N., LU L. (1995), Coal agglomeration and its effect on bulk density, Powder
Technology, 82, 177-189
ZUURMAN K., BOLHUIS G.K., VROMANS H. (1995), Effect of binder on the relationship between
bulk density and compactibility of lactose granulations, International Journal of Pharmaceutics, 119,
65-69

Gluba T., Obraniak A., Gawot-Młynarczyk E., Wpływ warunków granulacji na gęstość nasypową
produktu, Physicochemical Problems of Mineral Processing, 38, (2004) 177-186 (w jęz. ang.).

Przeprowadzono badania zmian gęstości nasypowej podczas procesu granulacji mączki kwarcowej w
granulatorach bębnowych. W badaniach parametrami zmiennymi były: parametry nawilżania tzn.:
średnica kropli, współczynnik saturacji oraz skład ziarnowy surowca. Złoże materiału sypkiego
nawilżano kroplowo w czasie jego ruchu przesypowego, przy stałym objętościowym natężeniu dopływu
cieczy, za pomocą zestawu dwóch dysz pneumatycznych zapewniającego równomierne podawanie cieczy
zwilżającej. Podczas każdej próby mierzono w stałych odstępach czasowych skład ziarnowy i gęstość
nasypową granulatu na danym etapie procesu. Przeprowadzono ocenę wpływu średnicy kropel, średniego
wymiaru surowca oraz saturacji granulowanego złoża ziarnistego na zmianę gęstości nasypowej
produktu. Zaproponowano równanie korelacyjne opisujące wpływ w/w parametrów na zmianę gęstości
nasypowej.

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