Population balance based modelling of nickel laterite agglomeration behaviour

L.X. Liu
a,
, D.J. Robinson
b
, J. Addai-Mensah
c
a
School of Chemical Engineering, The University of Queensland, Brisbane, Qld, 4072, Australia
b
CSIRO Process Science and Engineering & Minerals Down Under National Research Flagship Australian Minerals Research Centre, PO Box 7229, Karawara W.A. 6152, Australia
c
Ian Wark Research Institute, ARC Special Research Centre, University of South Australia, Mawson Lakes, Adelaide SA. 5095, Australia
a b s t r a c t a r t i c l e i n f o
Available online 1 July 2011
Keywords:
Agglomeration
Nickel laterite
Coalescence kernel
Agglomerate size distribution
Agglomeration of ne mineral particles as a precursor to heap leaching is an important means of enhancing
leaching rates and metal recoveries, particularly in processing lowgrade ores. In this paper, the modelling of a
batch drum agglomeration process applied to nickel laterite using population balance model is explored. The
coalescence kernels which are linked to feed material and agglomerator operating conditions are reviewed.
The use of a physically based coalescence kernel which relates agglomerate layer thickness to binder content
and agglomerate consolidation shows great promise for the modelling of the agglomerate size distribution of
nickel laterite ore. The model parameters were then used to predict the effect of operating parameters such as
binder content on agglomerate size distribution.
2011 Elsevier B.V. All rights reserved.
1. Introduction
Agglomeration of ne mineral particles as a precursor to heap
leaching is an important means of enhancing leaching rates and metal
recoveries. It is particularly useful to capture and hold still ne
particles so that ne particle movement is limited and hence the
blockage of heap leaching is prevented. Agglomeration has the
potential to also help with the robustness of the heap, the solution
ow through materials and hence overall heap efciency. To fully
understand the underlying mechanisms and kinetics of agglomera-
tion, it is necessary to establish a useful predictive model based on
feed characteristics and agglomerator operating conditions for better
design and control of the agglomeration processes [14]. Useful rate
parameters of the agglomeration mechanisms and kinetics may be
extracted from appropriate agglomeration experiments and used for
the optimization and scale-up, and also the benchmarking of our
understanding on real ore agglomeration processes. One of the key
agglomerate quality parameters for leaching process is the agglom-
erate size distribution, as it directly affects the inter-agglomerate
space and hence the percolation rate of lixiviate and leaching
efciency during leaching process [5].
Agglomeration process can be divided into three sub-processes
wetting and nucleation, consolidation and growth by coalescence, and
attrition and breakage [6]. In addition, simultaneous drying could also
take place [7]. The formation of agglomerates initially starts with the
nucleation of primary particles by liquid binder. The nucleation
process involves the distribution of the liquid binder through the
feed powder initially, then followed by the penetration of the liquid
droplets into the powder where the binder droplets will hold the
primary particles within its surroundings to form into a nucleus. The
nuclei formed will then grow by coalescence and also undergo
consolidation during which the particles are compacted thus squeez-
ing the binder fromthe pores of the agglomerates onto the surface [8].
Boththe surface area andthickness of liquidpresent onthe surface and
within the agglomerate play a signicant role in determining the
success of a coalescence event should two particles collide with one
another [9,10]. Agglomerate breakage can also occur simultaneously
with coalescence if the agglomerates are weak or impact force in the
agglomerator is high.
Many studies on the modelling of various aspect of agglomeration
process are available in the literature [e.g., 1,8,1114]. The agglom-
eration process is often modelled using a population balance
accounting for nucleation, consolidation and coalescence, and
breakage if any. Poon et al. [8] presented a three-dimensional
population balance model on nucleation, coalescence and Ramachan-
dran et al. [15] presented a 3-D modelling of breakage and listed the
latest literature on the various models of agglomeration process. In
the minerals industry, agglomeration is often carried out in drum
agglomerators where process intensity is low and breakage is
negligible. Growth by consolidation and coalescence has been the
main focus due to the fact that it occurs in most, if not all the
agglomeration processes. Traditionally, experimental data are used to
t a certain type of coalescence kernel and the kernel is often not
related to the physical properties of the feed powders, agglomerates
and the operating conditions. Ideally, physically based coalescence
kernels should be used so that the effect of formulation and operating
conditions on agglomerate size distribution can be reected through
the population balance model.
Powder Technology 223 (2012) 9297
Corresponding author. Tel.: +61 7 33658591; fax: +61 7 33654199.
E-mail address: l.liu@uq.edu.au (L.X. Liu).
0032-5910/$ see front matter 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.powtec.2011.06.020
Contents lists available at ScienceDirect
Powder Technology
j our nal homepage: www. el sevi er. com/ l ocat e/ powt ec
The objective of the present work is to focus on agglomerate
coalescence mechanism with a physically based coalescence kernel. A
coalescence model based on agglomerate physical properties was
developed by the rst author [9,14]; however, a constant binder layer
thickness was assumed. In the present work, we intend to link the
agglomerate binder thickness to binder content in the coalescence
kernel so that the effect of binder content on agglomerate size
distribution is included in the population balance.
2. Theory on coalescence modelling
2.1. Process and particle-particle based models
Numerous studies on various agglomeration phenomena are
available in the literature. However, aggregation or coalescence has
been the main study in the past and is the main focus of the present
work. Models for coalescence (aggregation) can be broadly divided
into two categories, i.e., process based models from the basic physical
principles of agglomeration process, e.g. population balance models
(both one-dimensional and multi-dimensional) and particle-particle
based computational models such as discrete element modelling
(DEM). Comparing to population balance model on which the
majority of the models are based, DEMs have also played a small,
yet signicant part of this modeling effort thus far. Much of the DEM
work has occurred only in the past few years [16]. Many approaches
on the DEM work were well summarized by Cameron et al.[17]. One
approach used in DEMmodeling of agglomeration was taken by Gantt
and Gatzke [18]. In their work, a high shear agglomerator was
modelled using a DEM model that incorporated three key mecha-
nisms of agglomeration: coalescence, consolidation and breakage. The
rate of each mechanism is directly simulated and incorporated to
model dynamic particle size distribution (PSD). The results from their
DEMmodel were in good agreement with the results using population
balance model. However, DEM modelling on agglomeration is limited
by the computational intensity as a large number of particles are
required (for smaller particles). In addition, the DEM used a lot of
assumptions in the calculations and sometimes it is difcult to
validate these models. The use of computational modelling of
agglomeration is still at its emerging state and combination of DEM
with the process based models would give more realistic predictions
on agglomeration. Due to the limitations of DEM, the process-based
population balance model is still the mostly used modelling method
on which the present work is based.
The general form of one-dimensional population balance equation
for a well-mixed batch restricted-in-space agglomeration system for
coalescence alone [19] is:
n v; t
t
=
1
2N t

v
0
u; vu; t n u; t n vu; t du

1
N t

0
u; v; t n u; t n v; t du
1
where n(v,t) is the number density function, u and v are the volumes of
the coalescing agglomerates, and (v,u) is the coalescence kernel, N(t)
is the total number of particles in the system. The coalescence kernel is
the most important parameter in the population balance equation. A
brief review of the most commonly used kernels is presented in
Sections 2.2 and 2.3.
A major challenge in developing these population balances is the
identication of appropriate kernels for a particular agglomeration
process. In literature, the coalescence kernels can be broadly divided
into two categories: namely, empirical models and physically based
kernels derived fromrst principles. They are briey discussed below.
2.2. Empirical coalescence kernels
In general, the empirical models for coalescence include two parts,
namely the rate constant
0
which reects the collision frequency and
the size-dependent part f(u,v). That is:
=
0
f u; v 2
There are various forms of f (u,v) in literature [11,20]. The general
practice with empirical coalescence models is that a certain size-
dependent form of f(u,v) (e.g., f (u,v)=u+v) is chosen rst and the
kernels were then used to t the experimental data to the model so
that the rate constant
0
can be obtained [21]. Hounslow et al.[22]
proposed three types of coalescence kernels: a size-independent
kernel (SIK), Smoluchowski's shear kernel (SSK) and the equipartition
of kinetic energy kernel (EKE). Other forms of the coalescence kernel
may be found in various literatures [17,23].
However, to link the operating conditions such as binder
properties (e.g., viscosity, content) to the rate constants, experiments
need to be carried out at different operating conditions so that the rate
constants can be related to the targeted operating conditions.
2.3. Physically based coalescence kernels
The physically (or formulation) based coalescence kernel con-
siders the physical properties of two agglomerates during coales-
cence, i.e., not only the size, but also other physical properties such as
the amount of binder, the agglomerate yield stress (used to measure
the wet agglomerate strength), binder properties such as viscosity
etc.. With physically based coalescence kernels, the key concept is
when two agglomerates collide; they either form one agglomerate
(successful coalescence) or rebound (unsuccessful coalescence).
Therefore, the coalescence kernel takes the following format:
=

0
Under successful coalescence condition
0 rebound
_
3
With this type of coalescence kernels, the operating conditions are
linked to the conditions for coalescence or rebound but are not
explicitly shown in the model. A limited amount of work is reported in
literature on the physically based model, the work of Liu et al.[14]
proposed the following coalescence kernel:
=

1
for typeI or typeII coalescencewithnopermanent deformation

2
fortypeII coalescencewith permanent deformation
0 rebound or h
0
= 0
_
_
_
4
where
1
and
2
are the rate constants for type I and type II
coalescence respectively, h
0
is the binder layer thickness of the
colliding agglomerates. Type I coalescence occurs when agglomerates
coalesce by viscous dissipation in the surface layer before their surface
touch. Type II coalescence occurs when agglomerates are slowed to a
halt during rebound after their surface made contact. The successful
coalescence conditions for type I and type II coalescence are as follows
[9,14,24]:
Condition for Type I coalescence:
8 mu
0
3

D
2
ln
h
0
h
a
_ _
5
93 L.X. Liu et al. / Powder Technology 223 (2012) 9297
Condition for Type II coalescence:
Y
d
E

_ _
1=2
St
def
_ _
9=8

0:172
St
v

D
h
0
_ _
2
1
1
St
v
ln
h
0
h
a
_ _ _ _
5=4
h
2
0
h
2
a
1
_ _
+
2h
0

h
0
h
a
1
_ _
+
2h
2
0

2
ln
h
0
h
a
_ _
_ _
17:36
Y
d
E

_ _
St
def
_ _
1=4
1
1
St
v
ln
h
0
h
a
_ _ _ _
1=2
_ _
2
6
where
St
def
=
mu
2
0
2

D
3
Y
d
7
St
v
=
8 mu
0
3

D
2
8
=
8
3
_ _
1=2
St
def
_ _
1=2

D 1
1
St
v
ln
h
0
h
a
_ _ _ _
17:36
Y
d
E

_ _
St
def
_ _
1=4
1
1
St
v
ln
h
0
h
a
_ _ _ _
1=2
_ _
2
9
Where u
0
is agglomerate collision velocity, Y
d
is agglomerate yield
strength and E is agglomerate Young's modulus, is binder viscosity,
h
a
is agglomerate surface asperity and h
0
is binder layer thickness.

m
and

D are the reduced mass and diameter of the colliding
agglomerates. is the permanent deformation when two agglomer-
ates collide for type II coalescence. The detailed denition of each
parameter can be found in Liu and Litster [14].
Immanuel and Doyle III [13] extended the above coalescence
kernel by incorporating the dynamic changes in an agglomeration
process, instead of the static approach used in the work of Liu and
Litster [14]. It is probably the most advanced approach that exists
currently for meso-scale modelling of agglomeration using three-
dimensional population balance. In this work, the static approach is
going to be used due to its simplicity and fast computation time.
2.4. A modied physically based coalescence kernel
In the previous work on the use of the physically based model in
reference [14], some simplications were made to model the
agglomeration behaviour of glass beads and fertilizer. One such
assumption is that a constant binder layer thickness h
0
in Eqs. (5) and
(6) was assumed in the model. This is a very simplied assumption as
the binder layer thickness is obviously related to two key properties,
namely the binder content and agglomerate porosity . In any
agglomeration process, initially liquid binders were premixed or
sprayed onto the feed powder and the particles were held together
loosely by liquid binder. As the agglomeration process progresses,
agglomerates are consolidated with decreased porosity and binders
are squeezed onto the surface (Fig. 1) and agglomerates start to grow
quickly. Therefore, agglomerate porosity and binder content should
be included in the conditions for coalescence kernel.
If all the excess liquid binder is squeezed onto a agglomerate
surface after it reaches a critical saturation value s*, the binder
thickness h
0
can be expressed as a function of agglomerate diameter
D, binder volume fraction in the agglomerate v
b,
agglomerate porosity
and critical binder saturation s* in the pores:
h
0
=
D v
b
s

_ _
6
; v
b
s

0; v
b
< s

_
10
As agglomerate porosity decreases with agglomeration time due to
consolidation, the model will incorporate the agglomerate porosity
through the following equation [23]:

min

min
= e
kt
11
where is the agglomerate porosity,
min
is the minimum porosity
reached by the agglomerates and k is the consolidation rate constant
and t is the agglomeration time.
The binder volume fraction in agglomerates v
b
can be related to the
binder mass content w (mass binder per mass solid) through the
following relationship:
v
b
= s =
w
s
1 + s
b
1

b
12
where s
b
is the solubility of the ore in binder solution (g/g of solution),
s is binder saturation,
s
and
b
are the densities of the solid and
binder respectively.
Substituting Eqs. (11) and (12) into Eq. (10) we have the
relationship between the binder layer thickness h
0
and binder content
w:
h
0
=
D
w 1 + s
b

s

b
1 s

_ _
6
; when
w
s
1 + s
b
1

0; when
w
s
1 + s
b
1

< s

_
13
and:
=
min
+
0

min
e
kt
14
When two agglomerates collide, the average binder layer
thickness of two agglomerates with diameters D
1
and D
2
can be used.
Eq. (13) illustrates that binder layer thickness h
0
increases with
decreasing agglomerate porosity, which indicates that h
0
increases
with agglomeration time, as agglomerate porosity decreases with
agglomeration time. The critical saturation value s* is reached when
the agglomeration proceeds to a critical time t*, which is formulation
dependent. For formulations with viscous binder (less deformable
systems), the t* is much higher, whereas for less viscous and
deformable systems, the t* value might be very short (closer to
zero). In addition, the binder layer thickness is also proportional to the
agglomerate diameter. With the newly developed model for agglom-
erate binder layer thickness h
0
(Eq. (13)), the coalescence conditions
for type I and type II coalescence (Eqs. (5) and (6)) can be calculated
and the rate constant for any two colliding agglomerates with certain
sizes can then be set.
Fig. 1. Illustration of agglomerate consolidation process with liquid binders squeezed
onto agglomerate surface (Sanders et al. [1]).
94 L.X. Liu et al. / Powder Technology 223 (2012) 9297
3. Model validation with nickel laterite ore
Agglomeration experiments with nickel laterite ore and sulphuric
solution (44% of H
2
SO
4
by weight in water) as a binder were carried
out in a laboratory drum agglomerator. The nickel laterite powder
with a particle size below2 mmwas used as primary particles. It has a
median particle size of 119 m and 90% of the mass is less than
553 m. The experiments were carried out in a lab-scale stainless steel
drum agglomerator with internal diameter of 300 mm and length of
200 mm. Initially, the experimental conditions used for agglomeration
is a load of 1.5 kg of nickel laterite powder with binder content of 20%
by weight and no comprehensive design of experiments was carried
out. This is because strong nickel laterite agglomerates that are
suitable for heap leaching can be obtained under such conditions. As
the operating conditions such as binder type and content are
restricted to the industry requirements of producing strong agglom-
erates with a size range of 540 mm, the range of conditions that can
be used is rather limited. However, experiments with a wider range of
conditions are planned for future work.
Before the agglomeration experiments, 1.5 kg of nickel laterite was
thoroughly mixed with 20% (by weight) of sulphuric solution and was
then placed in the drum at a rotational speed of 60 rpm. Due to the
fact that the binder solution is quite viscous, regular scraping of the
materials from the drum wall is required. Small samples were taken
out at different times and their size distributions were measured by
sieving using sieve size in the range of 250 m to 40 mm. When the
samples were taken out from the agglomerator, efforts were made to
take a representative sample by scooping the samples from the
bottomof the agglomerate heap to the top. Three repeats were carried
out for the agglomeration experiments and the experimental error on
the cumulative mass fraction (95% condence level) was calculated
and presented in Fig. 2. Regular scraping of the sticky mixtures from
the agglomerator wall caused poorer reproducibility of the agglom-
erate size distributions at the same agglomeration time, a phenom-
enon that occurs more often with a viscous binder.
The population balance model (Eq. (1)) together with the
modied coalescence kernel was solved using Hounslow's method
of discretization [25]. The numerical package used for solving the
population balance model was the MATLAB function ode15s,
which is an ODE solver for solving stiff equations within the
Optimization toolbox. It is a variable order, multi-step solver
based on the numerical differentiation formulas. The parameters
were estimated through the minimization of the objective function J
between the measured cumulative mass fraction Cum
i
(t
j
) and the
predicted cumulative mass fraction Cum
i
t
j
_ _
at different agglomera-
tion times:
J =
n
j
j =1
Cum
i
t
j
_ _
Cum
i
t
j
_ _ _ _
2
15
Where i refers to agglomerate size interval and j refers to the
different times at which agglomerate size distributions are measured.
In this work, the relative error tolerance from the ODE solver is set at
10
4
and the two rate constants were then obtained. Numerous works
have been reported on the effective parameter estimation within a
multi-dimensional population balance model (e.g., [26,27]) and it is
beyond the scope of this work.
The model input parameters are listed in Table 1 and they can be
broadly divided into three categories, namely (1) fundamental
material properties which are mostly measured (2) agglomerate
property and process parameters which were either measured or
inferred from literature. Specically, the agglomerate initial and nal
porosity were based on the measured porosity of the agglomerates.
The consolidation constant was inferred from the data of Iveson [23]
and the yield stress was calculated from the dynamic strength model
reported earlier [28]. The average agglomerate collision velocity was
assumed to be one hundredth of the maximum tangential velocity.
This is similar to the assumption of agglomerate velocity used in the
work of Poon et al.[4] in which the average collision velocity is
0.0
0.2
0.4
0.6
0.8
1.0
0 10 20 30 40
C
u
m
u
l
a
t
i
v
e

m
a
s
s

f
r
a
c
t
i
o
n

u
n
d
e
r
Granule size, mm
1 min
8 min
14 min
8mins-model
14mins model
Fig. 2. Fittings between model and experimental agglomerate size distribution of nickel
laterite ore at 44% sulphuric solution (w/w), 20% binder content.
Table 1
Model input parameters.
Fundamental material
properties
Binder viscosity 0.00273 Pa.s
Particle density (
s
) 2290 kg/m
3
Binder density 1370 kg/m
3
Binder content w (mass binder per
mass solid)
0.25
Radius of the primary particle size
r
p
0.059* 10
3
m
Measured solubility of minerals in
binder
0.06 g/g
Agglomerate properties and
process parameters
Agglomerate yield strength (Y
d
) 13 kPa
Agglomerate initial porosity 0.55
Final agglomerate porosity 0.37
Y
d
/E 0.008
Agglomerate consolidation
constant k
0.28 min
1
Collision velocity of the
agglomerates
0.0094 m/s
Agglomerate surface asperity h
a
0.25 r
p
Critical binder saturation in
agglomerate pores s*
0.38
0
0.2
0.4
0.6
0.8
1
0 10 20 30 40
C
u
m
u
l
a
t
i
v
e

m
a
s
s

f
r
a
c
t
i
o
n

u
n
d
e
r
Granule size, mm
w=18%
w=20%
w=22.5%
Binder content
Fig. 3. Predicted nickel laterite agglomerate size distributions with different binder
contents at agglomeration time of 14 min.
95 L.X. Liu et al. / Powder Technology 223 (2012) 9297
0.005 m/s for the same sized drum with a rotational speed of 25 rpm.
The chosen Y
d
/E value of 0.008 is closer to the lower range of 0.01
0.05 suggested by other workers [29]. The agglomerate surface
asperity h
a
is assumed to be 0.25 times of the mean primary particle
radius r
p
. The critical binder saturation value in agglomerate pores is
an adjustable input parameter so that the calculated and the
experimentally obtained agglomerate size distributions are matching
each other by visual observations. All these parameters are less-
sensitive parameters in comparison to the coalescence rate constants

1
and
2
.
With the above input parameters for the coalescence conditions
and the initial size distribution at 1 min, the population balance model
was solved using the experimental data at 8 min and 14 min to obtain
the coalescence rate constants. The rate constants obtained are

1
=30.5 min
1
,
2
=0.98 min
1
respectively. The higher value of
1
shows that the majority of successful coalescence is due to the liquid
binder on agglomerate surfaces. Fig. 2 shows the comparisons of the
modelled agglomerate size distribution and the experimental results.
As can be seen from Fig. 2, quite good matching between the model
calculations and experimental results is obtained.
As the ultimate objective of any modelling work is process
optimization, let us have a look on how the model can be used for
predictive purpose. As binder content was directly linked into the
conditions for coalescence, we can use the model to predict how
changes in binder content affects agglomerate size distribution. Fig. 3
shows the predicted agglomerate size distribution at 14 min with two
binder contents. The agglomerate size distribution at the tted
conditions (w=20%) is also shown. Fig. 4 shows how the median
agglomerate size at different binder contents changes with time. As
shown in Figs. 3 and 4, the agglomerate size increases signicantly
with the increase of binder content. Likewise, the agglomeration time
required to achieve the desired agglomerate size is much shorter at
higher binder content. The benet of modeling work is clearly shown
in this example.
To validate if the model predictions are accurate, the agglomerate
size distributions at different agglomeration times with 22.5% of
H
2
SO
4
solution as a binder are shown in Fig. 5. The experimental data
at 8 min of agglomeration is also shown in Fig. 5. In considering the
fact that this set of the experimental data was not used in obtaining
the tting parameters, the model and experimental results agree quite
well.
4. Conclusion
A physically based coalescence model that relates binder, particle
and agglomerate physical properties is developed. The model in-
corporates agglomerate consolidation and relates binder layer
thickness directly to binder content in the agglomerates. The benet
of this type of mechanistic kernels is that it provides some physical
insight into the agglomeration mechanism, instead of pure data
tting. The validation of the model was initially carried out with nickel
laterite ore and the comparisons between the model and batch
agglomeration experiments showed close correspondence in terms of
agglomerate size distribution. The model developed can demonstrate
how binder content affects agglomerate size distribution. The
predictive capability of the model is clearly shown by the good
agreement between the model predictions and experimental agglom-
erate size distribution at a different binder content. Further
experimental work with different types of nickel laterite ore,
sulphuric solutions with different acid concentrations and water are
underway so that model validation can be carried out with a wide
range of experimental results.
Acknowledgements
Financial support provided under CSIRO Minerals Down Under
Cluster project funding is gratefully acknowledged as is assistance of
Artem Borysenko and Ataollah Nosrati.
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0
5
10
15
20
25
30
35
0 5 10 15
M
e
d
i
a
n

g
r
a
n
u
l
e

s
i
z
e

D
5
0

(
m
m
)
Granulation time (mins)
w=18%
w=20%
w=22.5%
Binder content
Fig. 4. Predicted nickel laterite agglomerate median size at different binder (44% H
2
SO
4
solution) contents.
0
0.2
0.4
0.6
0.8
1
0 10 20 30 40 50
C
u
m
u
l
a
t
i
v
e

m
a
s
s

f
r
a
c
t
i
o
n

u
n
d
e
r
Granule size, mm
4 mins
8 mins
11 mins
14 mins
8 mins-exp.
Fig. 5. Predicted agglomerate median size for nickel laterite ore with 22.5% (w/w) of
44% H
2
SO
4
solution and comparisons with experimental data.
96 L.X. Liu et al. / Powder Technology 223 (2012) 9297
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