International Seminar on Mineral Processing Technology (MPT-2008), April 22-24, 2008

Jointly Organized by Indian Institute of Mineral Engineers & National Institute for
Interdisciplinary Science & Technology, CSIR, Trivandrum.

EFFECT OF SLURRY RHELOGY ON THE GRINDING KINETICS IN

STIRRED MEDIA MILL

Aashish Jain1, B. Venkoba Rao2, Amlan Datta1*

1- Tata Research Development and Design Centre, Tata Consultancy Services, Pune
2- Engineering and Industrial Services, Tata Consultancy Services, Pune
* Corresponding author: amlan.datta@tcs.com

ABSTRACT

In any grinding operation, specific breakage rate and breakage distribution functions are two
important parameters, which dictate the birth and death of particles in the population balance
equations. Specific breakage rate is considered to be independent of grinding environment. However, it
has been observed by many researchers that specific breakage rate depends on grinding environment
and hence on the grind time especially for ultra-fine grinding. This time-variant breakage rate is often
termed as nonlinear breakage. Experimental observations suggest that the rheological behavior of the
slurry in a fine grinding system changes as the grinding progresses. Increase in specific surface area of
particulate mass enhances the influence of inter-particle interaction to a large extent. We hypothesize
that changing slurry rheology influences non-linear grinding and hence the grinding mechanism at any
point of time. The main focus of the current exercise is to understand the effect of dynamic rheological
behavior on the nonlinear grinding kinetics as expressed in the population balance model.

INTRODUCTION

Ultra-fine particles (below 5 µm) are processed in variety of industries such mineral cement,
food, chemical and fertilizer, ceramics, paint and pigment, pharmaceutical, to name a few. Often they
offer interesting material properties in terms of surface area, optical quality, reaction kinetics, packing
characteristics. However, generating fine particle by mechanical route is an energy intensive process.
Conventional tumbling mill is not suitable since grinding media is agitated under 1G field of
acceleration. Therefore, a form of centrifugal mill is used for grinding of ultra-fine particles, where
grinding media and feed material is centrifuged in high field of acceleration. Particle grinding occurs
due to compression, shear and torsional stresses generated on the particles.
Stirred media mill is popularly used in industrial application. Here, a central shaft rotates
within a cylindrical vessel. The shaft is equipped with pins or a disc to agitate the material kept in the
vessel. Stirred media mills are available in horizontal as well as vertical configurations. Typical process
variables include stirrer design and speed, grinding media density and size, feed material properties and
distribution, physical and chemical properties of slurry. Among them the physical and chemical
properties of slurry as determined by solid content of feed slurry, pH and presence of dispersant
collectively influence the slurry rheology. With the evolution of fine particles surface properties
become very significant. The slurry rheology plays significant role in terms of grinding kinetics as well
as productivity. For example, with slight application of dispersant one can eliminate the yield stress of
high-solid slurry, which will contribute to productivity improvement.
However, the role of slurry rheology on grinding kinetics is still not very well described in
literature. Some very insightful results are presented in literature. He et al. [1] investigated the role of
various parameters on slurry rheology and subsequently on efficiency of energy utilization in stirred
media mill. Although, characterized by median size (d50) only, the authors demonstrated that evolution
particle size distribution is dependent on slurry rheology. However, Kapur et al. [2] concluded that
rheology of slurry does not have any effect on grinding kinetics. But many times contradictory
conclusions are reported in literature.

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 With this background in mind, the current research is focused on understanding the role of
complex and dynamic slurry rheology prevalent during ultra-fine grinding on the evolution of product
size distribution. Here, the product size distribution is represented by complete size distribution
spectrum up to 1 micron instead of just one characteristic size (e.g. d50). The grinding kinetics is
modeled with population balance equation incorporating nonlinear or time-dependent breakage rate [3].
Our preliminary findings with limestone material are presented in this article.

EXPERIMENTAL

Limestone powder (97% CaCO3) provided by ACC Cements, Thane (Mumbai) was used for
grinding experiments in this study. The powder has a density of 2700 kg/m3. The size distribution of
the material was measured by sieve analysis. The median size (d50) of the feed is 62 µm and 80%
passing size is 178 µm.
The stirred media mill has a grinding chamber volume of 3 liter. 3.1 mm diameter mild steel
grinding media with density of 7800 kg/m3 was used in this study. Media occupied 70 % of the mill
volume. Limestone–water slurry was prepared at pre-determined solid concentrations. The stirrer speed
was maintained at 250 rpm.
A rotational viscometer with concentric cylinder geometry (Brookfield DV-III, Brookfield
Engineering Laboratories, Inc., USA) is used to determine the rheological properties of the slurry. The
inner cylinder (spindle number SC4-27) rotates at different speeds covering shear-rate range of 0.03 to
85 s-1. Each slurry sample is first pre-sheared for 3 min at the highest shear rate (corresponding to the
250 rpm), then the measurement started from this highest shear rate. About 20 ml of slurry sample is
required for each measurement. The mean values of shear stress, shear rate and viscosity are reported
after three measurements.
The particle size distribution was measured using a particle size analyzer LA-920 (Horiba
Instruments Inc., USA) based on light diffraction. This instrument can be used for the measurement of
particle size range of 0.02-2000 µm accurately.

MATHEMATICAL MODEL

The model is adapted from asymptotic self-similarity solution to population balance equation [4]. The
final form of the solution expressed in terms of cumulative distribution is given by

⎛ b ⎛ x ⎞ a ⎛ Γ ((b + 1) / a ) ⎞ a ⎞
γ ⎜ , ⎜⎜ ⎟ ⎜ ⎟ ⎟
⎜ a ⎝ u1 (t ) ⎟⎠ ⎜⎝ Γ (b / a ) ⎟⎠ ⎟
F ( x, t ) = ⎝ ⎠ (1)
Γ(b / a )

Where K1 and K0 are constants, u1(t) is the characteristic size of the distribution at grind time t, which
denotes the first moment of the mass-diameter density function (i.e. mean of the distribution). u1(t) is
given by following expression

1 (2)
u1 (t ) = 1 /( a − c )
⎛ ⎛ c ⎞⎛ Γ(b / a ) ⎞ a
⎞
⎜ A⎜1 − ⎟⎜ ⎟ t⎟
⎜ ⎝ a ⎠⎜⎝ Γ((b + 1) / a ) ⎟⎠ ⎟
⎝ ⎠

Hence, the whole distribution is described by four breakage parameters A, a, b and c, which are
described below. Please note that the time dependency of breakage rate as given in Eq. (3). The
nonlinearity is included through the parameter c.

b
k ( x, t ) = Ax a u1 (t ) − c ⎛x⎞ ⎛x⎞
and B⎜ ⎟ = ⎜ ⎟ (3)
⎝v⎠ ⎝v⎠

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 Details of the model development can be found elsewhere [3].

RESULTS AND DISCUSSIONS

The rheological analyses during grinding experiments are shown in Figure 1 and 2. In Figure
1, flow curve for grinding with 40% solid is presented. With progress of grinding the slurry becomes
more difficult to shear. It developed a distinct yield point which also increases with grinding.

100 1200
30 % wt

Apparent Viscosity (cp)

1000
Shear stress (N/m )

40 % wt
2

800

10 600

400

5 mins 200
20 mins
40 mins
0
1
0 10 20 30 40 50
0 10 20 30 40 50 60 70 80 90
Shear rate (1/sec) Grinding time (mins)

Fig 1. Flow curve at different grinding times for Fig 2. Apparent viscosity at 51s-1 at different
40% solid grinding times.

The apparent viscosity, measured at 51 s-1, is shown in Figure 2. As expected, with evolution of finer
particle size distribution, the apparent viscosity of the slurry increases. However, it appears that for
40% slurry, the apparent viscosity abruptly goes up between 20 min and 40 min of grinding. On the
contrary, for 30% solid the increase in apparent viscosity is reasonably gradual.
100
Cumulative wt% finer

5 mins-40% wt
10
20 mins-40% wt
40 mins-40% wt
5mins-30% wt
20mins-30% wt
40mins-30% wt

1
1 10 100
Particle size (microns)
Fig. 3. Evolution of particle size distribution with
respect to solid content.

The progression of grinding with respect to time and solid content is shown in Figure 3. Initially the
product fineness is nearly comparable for both cases. However, with increasing time the speed of fines
generation is more in case of 40% solid. In particular, after 40 minutes, significantly more fines are
generated for experiment with 40% solid. Perhaps, this is the reason behind sudden jump in apparent
viscosity after 40 minutes of grinding (refer Fig. 2).
Attempt was also made to model these grinding experiments with population balance equation
using nonlinear breakage rate. The results are shown in Figure 4 for 30% solid. In general model

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 predictions are in good agreement with experimental data except in the initial grinding times. It is to be
noted that this model was developed using the asymptotic self-similarity nature of product size
distribution [4]. Therefore, in the initial period, the model is not able to fit the experimental data.
Similar trend is also evident for experiments with 40% solid.

100

Cumulative wt% Finer

2 min
10
5 min
10 min
15 min
30 min

1
1 10 100
Particle size (micron)
Fig. 4 Model validation with grinding experiment with 30%
solid. Simulated data – solid line, symbols – experimental
data.

In the grinding model (Eqs. 1 and 2), the parameter c basically denotes the nonlinearity of the
breakage rate. Note (+ ve) sign of c indicates acceleration of breakage rate, whereas (- ve) sign means
deceleration of breakage. In case of 30% solid c is (+ 0.1699), while for 40% solid it is (- 0.1912). This
is counterintuitive considering Figure 3 demonstrates that generation of fine particles is faster for 40%
solid. Schonert [5] showed from particle breakage experiments that breakage probability of a coarse
particle reduces when it is surrounded by fine particles. Perhaps, this is the reason behind deceleration
of breakage rate for 40% solid. But, energy transfer is far more efficient for higher solid content [1]
which causes faster fine particle generation for 40% solid. Furthermore, in an earlier exercise [3], it
was demonstrated using data of Kapur et al. [2] that depending upon the rhelogical condition, the sign
of c can change.
This is a preliminary exercise, further research is required to understand the acceleration and
deceleration of grinding and capture that in a modeling framework. Nonetheless, it is evident from the
current exercise and also from published literature that rheology plays a significant role in ultra-fine
grinding and its effect is quite complex. Also, the slurry characteristic is very much dependent on the
other grinding parameters.

CONCLUSIONS

Dynamic rheological behavior of slurry and its effect on particle size evolution is investigated.
The grinding experiment shows that speed of fines production increases with solid content. The
grinding data was simulated with nonlinear population balance model. The simulation results indicate
deceleration of breakage rate at 40% solids content and acceleration at 30% solids content. These two
results are contrary to each other. Further research is in progress to elucidate nonlinearity of breakage
during fine particle grinding as affected by properties of slurry.

REFERENCES

1. M. He, Y. Wang, E. Forssberg, Powder Technology, 2006, Vol. 161, pp. 10-21.
2. P. C. Kapur, T. W. Healy, P. J. Scales, D. V. Boger, D. Wilson, Int. J. Miner. Process, 1996,
Vol. 47, pp. 141–152.
3. B. V. Rao, A. Datta, Powder Technology, 2006, Vol. 169, pp. 41-48.
4. P. C. Kapur, Chem. Eng. Sci., 1972, Vol. 27, pp. 425–431.
5. K. Schonert, Int. J. Miner. Process, 1996, Vol. 44-45, pp. 1-16.

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