Chemical Engineering Journal 145 (2009) 505–513
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Chemical Engineering Journal
journal homepage: www.elsevier.com/locate/cej
Exploring the regime map for high-shear mixer granulation
Wei-Da Tu
a
, Andy Ingram
b
, Jonathan Seville
c
, Shu-San Hsiau
a,∗
a
Department of Mechanical Engineering, National Central University, Taiwan 32001, R.O.C
b
Centre for Formulation Engineering, Department of Chemical Engineering, University of Birmingham,
Birmingham B15 2TT, UK
c
School of Engineering, University of Warwick, Coventry CV4 7AL, UK
article info
Article history:
Received 21 March 2008
Received in revised form
11 September 2008
Accepted 23 September 2008
Keywords:
Granule size distribution
GSD
High-shear mixer
Growth behaviour
Regime map
Sieving
Agglomeration
abstract
The aim of this study was to investigate the applicability of the regime map approach proposed by Lit-
ster/Iveson and co-workers [S.M. Iveson, J.D. Litster, Growth regime map for liquid-bound granules, AIChE
Journal 44 (1998) 1510–1518; S.M. Iveson, P.A.L. Wauters, S. Forrest, J.D. Litster, G.M.H. Meesters, B. Scarlett,
Growth regime map for liquid-bound granules: further development and experimental validation, Powder
Technology 117 (2001) 83–97] over the whole parameter range, for a given material and agglomeration
method. Agglomeration behaviour in a high-shear mixer granulator was investigated and categorised
using the evolution of granule size distribution (GSD). MCC 102 (Microcrystalline cellulose, Avicel 102)
and aqueous PEG 6k (Polyethylene Glycol 6000) were employed as solid and liquid materials. Different
operating conditions were applied by changing impeller speeds and L/S (liquid-to-solid) ratios (weight
of liquid/weight of solid). 12 representative settings were selected and typical agglomeration behaviours
were identified, forming a regime map for the system. The effect of impeller speed was found to depend
on the L/S ratio, very little effect being seen at low L/S ratio (L/S = 85/150), but much more effect at higher
binder ratios. In general, the effect of L/S ratio is of paramount importance in these systems and usually
determines the growth behaviour.
© 2008 Elsevier B.V. All rights reserved.
1. Introduction
Wet agglomeration is a widely applied process in which fine par-
ticles are combined to form larger, more easily handled, granules
by mixing with a suitable binder. It is a fundamental technique for
many industries, particularly pharmaceutical materials handling,
mining processes and advanced materials processing, because it
can greatly influence the granule properties. For example, in catal-
ysis/absorbents industry, high-shear granulation is used to modify
the properties of products (strength, attrition resistance, porosity,
and surface area) and thereby to control the efficiency of a chemical
reaction [3]. In the pharmaceutical industry, Lee and his co-workers
[4,5] have also revealed correlations between drug dissolution rate
and the properties of granules (Carr’s index, mixing index, surface
area, and particle size distribution) in wet granulation. There are,
however, many operating variables and these interact with each
other, leading to complex behaviour and it is often a challenge to
manufacture products consistently to specification [3,6,7]. There-
fore a better understanding of granulation mechanisms is required
∗
Corresponding author. Tel.: +886 3 426 7341; fax: +886 3 425 4501.
E-mail address: sshsiau@cc.ncu.edu.tw (S.-S. Hsiau).
for predicting growth behaviour, as well as to achieve optimal con-
trol.
Since 1998, work has been directed to produce regime maps
that describe and enable prediction of granule growth in equipment
such as rotating drums and high-shear mixers [1,2,8]. These maps
show how growth behaviour (changing rate of growth with time)
is determined by the work done to deform the granules relative to
their deformability (characterized by a Stokes deformation number
(St
def
)) and the maximum saturation states of granules (character-
ized by the maximum pore saturation (S
max
)). The map from Litster
et al. [1,2,8], shown in Fig. 1, identifies four classes of agglomeration
growth behaviour: nucleation, steady growth, induction and rapid
growth. Nucleation occurs when the binder is brought into contact
with a powder bed and granule nuclei are formed, but there is not
enough binder to promote further growth. With more binder addi-
tion, granules will start to grow and the rate of growth will depend
on the deformability of the granules and/or the rate of work done.
At the start of granulation, binder tends to get trapped in pockets
within granules. The key to growth is redistribution of binder to the
surface so that granules can stick together. If the granules are weak
or deformable then the process of redistribution is rapid and gran-
ules tend to grow immediately and at a steady rate (steady growth).
With stronger granules, or less powerful agglomeration processes,
1385-8947/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.cej.2008.09.033