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Microgranulation of Fine Powders by A Novel Rotating Fluidized Bed Granulator

This document describes a study that used a novel rotating fluidized bed system to microgranulate fine cornstarch powder. The system consisted of a rotating horizontal porous air distributor inside a plenum chamber. Experiments measured the minimum fluidization velocity and pressure drop of cornstarch powder under various rotation conditions. The system was then used to wet granulate the cornstarch by spraying a binder solution while rotating. Tests showed that microgranulation improved the flowability of the cornstarch by producing spherical granules with a narrow size distribution and without much size enlargement. Operating parameters like rotation speed and airflow rate affected the properties of the resulting granules.

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0% found this document useful (0 votes)
25 views6 pages

Microgranulation of Fine Powders by A Novel Rotating Fluidized Bed Granulator

This document describes a study that used a novel rotating fluidized bed system to microgranulate fine cornstarch powder. The system consisted of a rotating horizontal porous air distributor inside a plenum chamber. Experiments measured the minimum fluidization velocity and pressure drop of cornstarch powder under various rotation conditions. The system was then used to wet granulate the cornstarch by spraying a binder solution while rotating. Tests showed that microgranulation improved the flowability of the cornstarch by producing spherical granules with a narrow size distribution and without much size enlargement. Operating parameters like rotation speed and airflow rate affected the properties of the resulting granules.

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Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Powder Technology 131 (2003) 250 255

www.elsevier.com/locate/powtec

Microgranulation of fine powders by a novel rotating fluidized


bed granulator
Satoru Watano a,*, Yasushi Imada a, Kenji Hamada b, Yoshihiro Wakamatsu b,
Yoshiaki Tanabe b, Rajesh N. Dave c, Robert Pfeffer c
a

Department of Chemical Engineering, Osaka Prefecture University, 1-1 Gakuen-cho, Sakai, Osaka 599-8531, Japan
b
Nara Machinery Co., Ltd., 2-5-7, Jonan-Jima, Ohta, Tokyo 143-0002, Japan
c
New Jersey Institute of Technology, Newark, NJ 07102-1982, USA
Received 8 July 2002; received in revised form 24 December 2002; accepted 9 January 2003

Abstract
A novel rotating fluidized bed system has been developed for fluidizing, granulating and coating cohesive fine powders to tailor their
properties and functionalities. The system basically consists of a plenum chamber and a horizontal porous cylindrical air distributor, which
rotates around its axis of symmetry inside the chamber. The pressure drop and minimum fluidization velocity of cohesive fine cornstarch
powder (mass median diameter of 15 Am, Geldart Group C powder) were measured under various rotating conditions and the fluidization
behavior was studied. The system was then used for wet granulation of the cornstarch powder and the effects of operating parameters on the
granule properties such as granule size, size distribution, density and flowability were investigated. The experimental results indicated that
the flowability of cohesive fine cornstarch was dramatically improved by the microgranulation resulting in spherical granules with a narrow
size distribution while inhibiting the size enlargement.
D 2003 Elsevier Science B.V. All rights reserved.
Keywords: Granulation; Cohesive fine powder; Flowability; Rotating fluidized bed

1. Introduction
Fine powders have become of major interest lately. Many
industrial sectors such as pharmaceutical, agriculture, foods,
chemicals, ceramics and electronics are expected to find
applications and take advantage of the new functionalities
and many desirable properties attributed to ultrafine powders.
Fluidization is one of the major techniques for fine
powder handling and its applications has been extended to
a wide variety of processes such as cracking of hydrocarbons, combustion of solid fuels/wastes and roasting of
ores by chemical processing and filtration, drying, wet
granulation and coating by physical processing. This is
because fluidization exhibits excellent advantages of high
heat and mass-transfer rates, temperature homogeneity and
high flowability of particulate materials. However, as
pointed out by Geldart [1] in his classification map, powders
in Group C (fine size and low density) fluidize poorly,

* Corresponding author. Tel.: +81-722-58-3323; fax: +81-722-54-9911.


E-mail address: [email protected] (S. Watano).

exhibiting channeling, lifting as a plug and forming rat holes


when aerated. Therefore, the development of reliable techniques to improve the fluidization of cohesive fine powders
is required.
So far, several mechanisms such as vibration [2],
mechanical agitation [3], sound [4] and magnetic force [5]
have been used to improve the flowability of cohesive
powders. The application of these methods will help in
the handling of fine powders and fluidization can often be
obtained. However, unit operations before or after fluidized
bed processing such as conveying, weighing, packing and
tabletting still present problems originating from the cohesive properties of fine powders, which remain the same
regardless of any external forces applied. Therefore, an
improvement in the flowability of fine powders is needed
before they are further processed since their poor flowability
is due to their small size.
In this study, a novel rotating fluidized bed has been
developed for improving the flowability of cohesive fine
powders. Microgranulation, where the flowability of cohesive fine powders is improved, while inhibiting size enlargement as much as possible, has been conducted. The physical

0032-5910/03/$ - see front matter D 2003 Elsevier Science B.V. All rights reserved.
doi:10.1016/S0032-5910(03)00007-X

S. Watano et al. / Powder Technology 131 (2003) 250255

251

properties of the granules were evaluated experimentally


and the performance of the system was investigated.

2. Experimental
2.1. Equipment
A schematic diagram of the experimental apparatus is
shown in Fig. 1. The rotating fluidized bed composes of a
plenum chamber and a porous cylindrical air distributor
(ID 400  D 100 mm) made of stainless sintered mesh
with 20 Am openings. The horizontal cylinder (air distributor) rotates around its axis of symmetry inside the
plenum chamber. There is a stationary cylindrical metal
filter (ID 140  D 100 mm, 10 Am openings) inside the
air distributor to retain elutriated fine powder. A binary
spray nozzle mounted on the metal filter sprays binder
mist (mist size is around 7 10 Am) into the powder bed.
A pulse air-jet nozzle is also placed inside the metal filter,
which cleans up the surface of the metal filter in order to
prevent clogging. An air knocker is installed outside the
plenum chamber to prevent powder adhesion onto the air
distributor mesh and front cover. Pressure taps are
mounted on the inlet and exhaust air pipes and on the
metal filter, so that the manometer (1) measures the
pressure drop across the powder bed and air distributor,
while manometer (2) measures pressure drop across the
metal filter. In this study, the pressure drop across the
powder bed, DP, is defined by Eq. (1)
DP P1  P2

where P1 is the pressure drop across the powder bed and


air distributor measured during the experiments and P2 is

Fig. 1. Schematic diagram of a novel rotating fluidized bed.

Fig. 2. Powder fluidization mechanisms.

the pressure drop across the air distributor measured


during idling without powder, respectively.
Fig. 2 illustrates the powder flow mechanism in the
rotating fluidized bed. In a conventional fluidized bed,
the air distributor is mounted horizontally and powder
samples are introduced onto the distributor. Powders are
lifted up by a vertical airflow (drag force and buoyancy
against the gravity force). In a rotating fluidized bed,
powder samples are introduced inside the air distributor
and are forced to the wall by a centrifugal force due to
the rotation of the distributor. Air flows radially inward
through the air distributor and the forces on the powder
are balanced by the airflow (drag force and buoyancy)
and the centrifugal force. Unlike conventional fluidized
beds, a rotating fluidized bed can impart a high centrifugal force, which enables fine particles to behave as
Geldart Group A powder [6]. The centrifugal force can
be made much larger when compared to other mechanical forces given by vibration [2], mechanical agitation
[3], sound [4] and magnetic force [5]. This implies that
the rotating fluidized bed can uniformly fluidize much
finer powders than conventional fluidized beds even
when equipped with these mechanical devices. Theoretically, if the distributor rotates at a high enough speed
and the airflow increases correspondingly to keep a
uniform fluidization, the adhesion force between powders
can be neglected as compared to the centrifugal and drag
forces.
It is noteworthy that the energy consumption of a
rotating fluidized bed is not very large because the
rotating fluidized bed can operate near the minimum
fluidization velocity (usually less than 3 times the minimum fluidization velocity), whereas a conventional fluidized bed always operates at a velocity more than 5 10
times the minimum fluidization velocity, especially in wet
granulation and coating, to avoid blocking. Also, the
contact efficiency between the particles and air is very
good, so that the operating time can be shortened. In
addition, due to an air sealing between the inner metal
filter and the rotating air distributor, mechanical abrasion
is negligible.

252

S. Watano et al. / Powder Technology 131 (2003) 250255

Table 1
Operating conditions
Rotational speed
Airflow rate
Air temperature
Spray air pressure
Binder feed rate
a

5.57 rps (25G)a


0.596 m/s (u/umf = 3.0)
333 K
0.3 MPa
10 g/min

1G = 9.8 m/s2 (gravity acceleration).

adhered to the surface of the funnel sleeve pipe and also


formed bridges inside the funnel, so that powders could
not be discharged smoothly [7] and instead were discharged in a pulsatory manner. This caused poor reproducibility of the measured angle of repose. Therefore, we
decided to use the discharge test instead of using the
angle of repose method to determine flowability.

2.2. Powder sample

3. Results and discussions

Cornstarch with a mass median diameter of 15 Am was


used in this work. This powder belongs to Geldart Group C
(cohesive powder). A mass of 0.66-kg cornstarch powder
was charged into the equipment, which gave a bed height of
approximately 0.02 m. For wet granulation, an aqueous
solution of 10% hydroxypropylecellulose (HPC-L) was
used as a binder.

3.1. Fluidization behavior of cornstarch

2.3. Experimental procedure and operating conditions


Table 1 lists the operating conditions. Granulation experiments were conducted as follows:
(1) The powder sample (cornstarch) was fed into the
cylindrical air distributor (vessel).
(2) The air distributor was rotated and fluidization air was
supplied.
(3) Binder liquid was sprayed onto the powder bed.
(4) After a predetermined amount of binder was sprayed,
drying of granules was conducted until the moisture
content decreased to less than 1%.
2.4. Evaluation of granules
The size and size distribution of the granules were
measured by a laser diffraction particle size analyzer
(SALD-2100, Shimazu). The degree of compression was
measured based on the following equation
C

PA
 100 %
P

Fig. 3 shows the pressure drop plotted against airflow


velocity under different rotating conditions. The pressure
drop increased to a peak at minimum fluidization velocity
(umf) and then showed a constant pressure drop regardless
of a further increase in air velocity. Due to the radial
acceleration, the pressure drop increased with an increase
in the centrifugal force. At all rotational speeds, the
pressure drop did not show a linear increase before reaching the minimum fluidization velocity. This was because
the initial cornstarch powder formed some agglomerates
and was also compressed due to the high centrifugal force
while idling. Thus, a higher-pressure drop through the
powder bed was recorded until each powder uniformly
fluidized at the minimum fluidization velocity.
From Fig. 3, it can be seen that fine cohesive cornstarch
powder (Geldart Group C) can be uniformly fluidized
without any channeling. This figure also confirms the
possibility of handling fine powder in a rotating fluidized
bed.
Fig. 4 shows the relationship between the minimum
fluidization velocity and the rotational speed. The minimum fluidization velocity increased approximately linearly
with rotational speed. This agrees well with the equation

where P and A indicate the tapped and bulk densities,


respectively. Both densities were measured by using a
Powder Tester (Hosokawa Micron).
The flowability of the granules was measured by using
a discharge tester. This involved feeding 0.02 kg of
granules into a glass funnel (largest ID of the top part
is 50 mm, ID of the sleeve pipe is 5 mm) and subjecting
the powder to mechanical vibration. The time required to
completely discharge the powder was measured and used
as the indicator of flowability. In the literature, the angle
of repose measurement has been widely used; however,
this method was impossible to apply to cornstarch powder. The main reasons were that the cornstarch powder

Fig. 3. Pressure drop against airflow velocity.

S. Watano et al. / Powder Technology 131 (2003) 250255

253

Fig. 5. Temporal change in mass median diameter and geometric standard


deviation.

Fig. 4. Relationship between minimum fluidization velocity and centrifugal


acceleration.

based on a theoretical model proposed by Kao et al. [8]


given by
"
#1=2

qf qg  qf dg3 x2 C3
umf qf dg
C2 2

33:7
0:0408
l
C1
l2
C1
 33:7

C2
C1

where
C1 r02 1=ri  1=r0 ;
C3

r02

C2 r0 lnr0 =ri ;

ri2 =2

It is believed that particles contacting the cylinder wall


experience a direct centrifugal force, whereas other particles
away from the wall also transmit the centrifugal force due to
particle collisions and slip. Details will be reported in a
subsequent paper, which analyzes the particle movement
and force transmission by using a discrete element method
(DEM).
The results in Fig. 4 imply that the behavior of cohesive
cornstarch powder in the rotating fluidized bed is almost the
same as the behavior of Geldart Group A powders [6]. Also,
this result suggests that the adhesion force between fine
powders is negligible under a high centrifugal force field as
shown in Fig. 2.

contrast, the geometric standard deviation increased initially,


followed by a decrease (size distribution became narrow)
with operational time. At the initial stage of granulation,
granulated and original cornstarch particles co-existed, leading to a wide size distribution. As time elapsed, the powder
was gradually and uniformly granulated to reduce the size
distribution. In practice, coarse granules were never produced and ungranulated fine powders were never seen after
600 s of operation. These results occurred due to the
movement of individual cornstarch powder particles in the
high centrifugal force field.
Fig. 6 shows the temporal change in the compressive
degree of the granules. The compressive degree decreased
with time, indicating an increase in the tapped density of the
granules. Due to granulation, an increase in granule density
and improvement of flowability were achieved (as shown in
the next figure).
Fig. 7 shows the change in flowability by measuring the
time required for powder discharge. The required time was
decreased rapidly with operational time, showing that the
flowability was greatly improved. When the operation time
was 600 s, the discharge time was only 7 s. It is noteworthy
that this is almost the same time required for 100 Am

3.2. Microgranulation
Fig. 5 shows evolution of the mass median diameter and
geometric standard deviation of granules. The mass median
diameter increased gradually with time, implying that the
adhesion between individual cornstarch particles was occurring due to liquid bridges generated by the binder mist. By

Fig. 6. Temporal change in compressive degree.

254

S. Watano et al. / Powder Technology 131 (2003) 250255

Fig. 7. Temporal change in time required for powder discharge


(flowability).

diameter spherical glass beads to discharge through the


same funnel. From this result, it is easy to see that the
flowability of cohesive cornstarch was greatly improved by
the microgranulation process.
Fig. 8 shows scanning electron microscopy (SEM) pictures of granules. Since cornstarch does not dissolve into
water, each cornstarch particle maintained its original shape
even when forming granules. In addition, each cornstarch
particle regularly adhered to another particle, forming
spherical granules.
Fig. 9 confirms the effects of centrifugal acceleration on
granule bulk (apparent) density after 600 s of processing.
With an increase in centrifugal acceleration, the granule
bulk density increased gradually. Due to fluidization, granules experience a high impaction force, resulting into the
formation of well-compacted granules.
The granule size and density are determined by a balance
of the adhesion force and separation force experienced by
the granules. When the centrifugal force is increased, the
separation force becomes large, leading to a decrease in the
granule size and an increase in the granule density. Also, a
high centrifugal force results in a high fluidization air
volume to maintain uniform fluidization. This leads to an
increase in drying efficiency and granule growth rate.
These results indicate that we have succeeded in developing a method for microgranulation of cohesive fine

Fig. 9. Effects of centrifugal acceleration on the granule bulk density.

powders, with a dramatic improvement in flowability, an


increase in density and a sharpening of the particle size
distribution. In the manufacturing processes of particulate
materials, problems due to the cohesiveness of fine powder
are well known. Our system can overcome these problems
by granulating the cohesive fine powders just enough to
meet the requirement for smooth transportation, accurate
weighing, better handling and the further work, we will
investigate the powder flow and the granule growth mechanism in the rotating fluidized bed.

4. Conclusions
A novel rotating fluidized bed has been developed and
applied to fluidization of cohesive fine powder (cornstarch
powder, mass median diameter of 15 Am), which is normally categorized as a Geldart Group C powder. However,
uniform fluidization was obtained in the rotating fluidized
bed and the minimum fluidization velocity was well-predicted by using a model for a Geldart Group A powder. By
spraying a binder into the fluidized powder, microgranulation was achieved. The flowability of cohesive fine cornstarch powder was dramatically improved and a narrower
size distribution of particles was observed. This method can
be extended to improve the handling and processing of other
fine cohesive powder, which are used in transportation,

Fig. 8. SEM photographs of cornstarch granules.

S. Watano et al. / Powder Technology 131 (2003) 250255

dispersion and synthesis of composite materials in many


different industries.
List of symbols
A
Bulk density in Eq. (2), kg/m3
dg
Granule diameter, m
C
Compressive degree defined by Eq. (2)
D50
Mass median diameter, Am
N
Rotational speed, s 1
P
Tap density in Eq. (2), kg/m3
P1
Pressure drop across powder bed and air distributor, Pa
P2
Pressure drop across air distributor, Pa
ri
Radius of inner surface of granule bed, m
r0
Radius of rotating fluidized bed, m
t
Processing time, s
u
Air flow velocity, m/s
umf
Average minimum fluidization velocity, m/s
l
Air viscosity, kg/ms
DP
Pressure drop, Pa
qf
Air density, kg/m3
qg
Granule density, kg/m3
rg
geometric standard deviation
x
Angular velocity, rad/s

255

Acknowledgements
This work was partially supported by grant CTS
9985618 from the National Science Foundation and award
# 01-2042-007-24 from the New Jersey Commission of
Science and Technology. The authors also wish to acknowledge Mr. Yozo Kamata for his help in doing the granulation
experiments.

References
[1] D. Geldart, Powder Technol. 7 (1973) 285.
[2] Y. Mawatari, T. Koide, Y. Tatemoto, T. Takeshita, K. Noda, Adv.
Powder Technol. 12 (2001) 157.
[3] N.J.K. Kuipers, E.J. Stamhuis, A.A.C.M. Beenackers, Chem. Eng. Sci.
51 (1996) 2727.
[4] R. Chirone, L. Massimilla, Chem. Eng. Sci. 49 (1994) 1185.
[5] Q. Zhu, H. Li, Powder Technol. 86 (1996) 179.
[6] G.H. Qian, I. Bagyi, I.W. Burdick, R. Pfeffer, H. Shaw, J.G. Stevens,
AIChE J. 47 (2001) 1022.
[7] R.N. Dave, C.Y. Wu, B. Chaudhuri, S. Watano, Powder Technol. 112
(2000) 111 125.
[8] J. Kao, R. Pfeffer, G.I. Tardos, AIChE J. 33 (1987) 858.

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