An Analysis of Radial Segregation for Different Sized Spherical Solids in Rotary Cylinders

N. NITYANAND, B. MANLEY, and H. HENEIN Rotary reactors such as ball mills, driers, mixers, blenders, and kilns are extensively used in chemical and metallurgical industries to process billions of tons/year of granular solids. Longitudinal and radial segregation of the feed and/or product due to size, shape, and density differences of the feed or product are often encountered in these unit operations. This paper presents some observations of radial segregation due to size differences of spherical solids for slumping, rolling, cascading, cataracting, and centrifuging beds. The mechanism by which spherical beads segregate radially is a combination of percolation and flow. The kinetics of radial segregation for rolling beds is observed and quantified using high speed photography. The rate of segregation is shown to be a function of the cylinder rpm but is independent of bed depth. Furthermore, the larger the size ratio of coarse to fines, the faster the rate of segregation. The scale-up of the segregation process is investigated using two cylinders, 0.2 m ID 0.2 m L and 0.4 m ID 0.4 m L. Both the size ratio of the solids and the Froude number are the scale-up criteria for the rate of radial segregation. The former is related to the packing characteristics of loosely packed beds when rolling and to the effective radius of rotation of particles when cataracting or centrifuging.

I.

INTRODUCTION

ROTARY reactors are commonly used in the chemical and metallurgical industries to process granular and powdered solids. The many and varied applications of these reactors include ball mills for comminution, driers, mixers, blenders, and kilns. In each of these unit operations granular solids are set in motion radially in the reactor. The design and mode of operation of rotary reactors in the metallurgical industry vary depending on the application. In general, though, rotary kilns tend to have length to diameter ratios, (L/D), greater than 10/1. They are operated continuously with not more than 20 pct solids (by volume). The burden moves down the kiln by virtue of its rotation (up to Fr = 10 -3) and inclination (up to 5 pct). Driers, on the other hand, are operated with higher loadings (about 30 pct), higher Froude numbers (-10-2), and may not be inclined. They are operated continuously and have an L/D as low as 3/1. Ball mills generally have L/D's up to 2/1 and are operated at Fr of 0.5 to 0.75, with 50 pet loadings. They are not inclined but are operated continuously. Finally, mixers and blenders are commonly batch operated with Fr ranging between driers and ball mills. The type of bed motion used, slumping, rolling, cascading, cataracting, or centrifuging,~ varies with the application and the type of reactor. For example, in ball mills cataracting is preferred, while in the sintering of iron oxides both cascading and rolling actions are required. In the processing of oxide dispersion strengthened composites, cascading would be the preferred mode of bed behavior to completely mix metal and ceramic powders. In all of these systems, the feed material may consist of more than one component, each having a different density and its own size and shape distribution. As solids travel through the reactors, they may undergo physical and chemical changes. In the
N. NITYANAND, formerly a Graduate Student, B. MANLEY, formerly an Undergraduate Student, and H. HENEIN, Associate Professor, are with the Department of Metallurgical Engineering and Materials Science, Carnegie-Mellon University, Pittsburgh, PA 15213. Manuscript submitted June 27, 1985. METALLURGICALTRANSACTIONS B

calcination of limestone, the size distribution of the feed may be broadened by degradation and fines generation. For other applications such as the direct reduction of iron, coal, iron ore, and flux with varying shape, size and density are charged to a rotary kiln. Due to these differences, segregation occurs often resulting in poor reactor performance, an unacceptable product, or poor energy efficiencies. The aim of this work is to quantify the effect of material, design, and operating variables on radial segregation. This work deals with segregation due to size differences of spherical solids applicable to the design and operating variables of kilns and driers. An experimental technique to be described in this paper was developed to quantify the kinetics of segregation and to identify the mechanism and scaleup of the radial segregation phenomenon.
II. PREVIOUS W O R K

Radial and axial segregation have been observed in horizontal rotary devices by numerous workers. T M In radial segregation finer or denser particles are found to form a horizontal core in the b e d , 2-9'14 whereas in axial segregation either alternate bands of coarse and fine particles could form down the length of the bed, or the fine particles could form two end bands at the cylinder walls in the center of the cylinder axis. 9-14 Most of the studies on segregation have been conducted on cascading beds. Segregation, like mixing, was reported to be a first order kinetic process which is indicative of a random or diffusional process. 2'n'~5 These studies relied on a statistical approach to analyze the segregation process. Furthermore, a sampling thief was used in these studies. This sampling technique would locally disturb the solids bed thereby skewing the results. Finally, the number of samples that may be taken using a sampling thief is limited due to significant bed depletion of solids. Radial segregation occurs faster than axial segregation. Numerous workers have found that axial segregation reached steady state only after 500 to 10,000 revolutions. 9'12-~5The work of Rogers and Clements ~2showed that
VOLUME 17B, JUNE 1986--247

radial segregation was well established following 10 cylinder revolutions. Reuter, 2 working with mixtures of coal and iron ore, reported radial segregation to be complete after two revolutions. It is therefore clear that axial segregation will have the radially segregated bed as its initial condition. Therefore, the configuration of the bed and the rate of segregation as a result of radial segregation must be determined as a prerequisite to any study on axial segregation. There are three mechanisms by which segregation occurs: percolation, flow, and vibration 1~ Percolation takes place when the size of the voids between the particles is large enough to allow smaller particles to trickle through them. This type of segregation is a function of the packing characteristics of the bed, the particle shape, and size. Segregation by flow occurs when granular solids are set in motion over an inclined surface. Coarse particles travel down an inclined surface farther than fine particles and spherical particles flow easier than angular particles. Segregation by vibration typically occurs when a mixture of coarse and fine particles is subjected to prolonged vibration. Smaller particles would segregate to the bottom while the larger particles would segregate to the top. In this investigation no vibration was imparted to the system; thus, segregation would occur predominantly by the percolation and/or the flow mechanisms.

III.

EXPERIMENTAL

The experiments were carried out in two laboratory cylinders with an L / D of 1/1 having dimensions of 0.2 m ID 0.2 m L and 0.4 m ID x 0.4 m L. The cylinders were placed on two horizontal rollers. One was coupled to a variable speed drive motor, while the second was adjustable to accommodate cylinders of various diameters. On each of the two cylinders, one of the clear glass endplates had a hole in the center for easy access to the bed. The cylinders were designed with a variable wall insert to allow variation of the wall roughness and hence the bed/wall frictional characteristics. In all the experiments described in this work, bed/wall friction was always maintained such that no slipping occurred between the solids bed and the cylinder wall. For most of the experiments described in this work, the inside of the cylinder was lined with corrugated cardboard. The size of these corrugations was 2.4 mm high and 4 mm apart. Although the corrugations were running along the length of the cylinder, they were not observed to impart any lifting action to any of the solids tested in the cylinder. However, due to the resiliency of the cardboard, the smallest spheres used in this study could be lodged firmly between the corrugations. The rotational speeds used in these experiments varied from 1.4 to 100 rpm and the observations reported on the rate of segregation apply to a rolling bed and to the low Froude numbers of a cascading bed where the bed is not crescent-shaped. A digital tachometer and an infrared sensor were used to measure the rotational speed of the cylinder. The tachometer was calibrated and found to be accurate to within --- 0.25 rpm. Spherical acrylic beads were used as the charge material in the cylinders. The beads were of uniform color for each of the three sizes tested. This allowed easy identification of the particles when analyzing the high speed movies and
248--VOLUME 17B, JUNE 1986

when making observations of the bed. The bead sizes were 9.5 mm, 6.4 mm, and 4 mm. Therefore, segregation experiments were carried out in the two cylinders at varying bed depths and rotational speeds using different combinations of the beads to yield size ratios of 2.4, 1.6, and 1.5. Visual observations of the rate of segregation were made for varying volume pcts of the finer component (10 to 49 pct) in the 0.2 m ID cylinder. For this range of the finer fraction and for all three size ratios, the segregation mechanism observed and more recently quantified TMwas independent of the volume pct of the finer fraction. Thus the volume pcts of finer components used for the segregation rate experiments were 20, 20, and 14 pct for the size ratios 2.4, 1.6, and 1.5, respectively. These volume fractions were chosen to facilitate subsequent quantification of the data from the high speed movies. In order to study the end wall effects and the configuration of the segregation core, a sampler was constructed to allow a portion of the bed to be removed for observation. For these experiments, Velcro | rather than the corrugated cardboard, was used to line the inside of the cylinder. At 30 pct fill, no slipping was observed between the solids bed and the Velcro | wall. The sampler was constructed of two plexiglas | side plates which were positioned vertically and were separated by a metal strip conforming to the internal curvature of the cylinder wall. The outside curvature of the metal strip was covered with Velcro | fiber tape to allow it to stick against the Velcro | hook wall, while the inside curvature of the strip was covered with Velcro | hook material to maintain the same frictional characteristics as the remainder of the wall of the cylinder. A 16 mm high speed movie camera operated at 100 frames per second was used to record the segregation phenomenon. At the start of the segregation kinetics experiment, a well-mixed condition was achieved (Figure l(b)) by cascading the binary mixture of beads. The rotational speed of the cylinder was then decreased to the desired rpm where the bed was rolling. In the rolling mode fine particles moved within the bed to form the segregated core. Filming was continued until the segregation process had reached a steady state. Subsequent analysis of the film was carried out on a film analyzer. IV. RESULTS AND DISCUSSION

A. Effect of Bed Behavior

Observations of bed motion and segregation were made in the 0.2 m ID 0.2 m L cylinder containing all three sizes of beads. Different radial segregation patterns occurred at different types of bed behaviors. Representative photographs are shown in Figures l(a) through l(d). When the active layer of solids flows over the passive region of the bed (i.e., a rolling bed), the finer particles form a core in the central part of the bed (Figure l(a)). Similar patterns were observed for slumping beds. For the rolling mode shown in Figure l(a), the 6.4 mm particles seem to be well mixed with the 9.5 mm particles, while the 4 mm particles have formed a central segregation core. When binary mixtures of the 9.5 mm and 6.4 mm beads and of the 6.4 and 4 mm beads were tested, the smaller sized beads always formed a central segregation core. The different segregation patterns observed with binary and ternary mixMETALLURGICAL TRANSACTIONS B

(a-) Rolling:

Central segregation core

(b) Cascading: Well mixed bed

~.---= "-

1F

~-

~1,..,

,i. r

..

(c~) C a t a r a c t i n g :

Onset o f r e v e r s e segregation

(d) C e n t r i f u g i n g :

Reverse segregation

Fig. 1 - - R a d i a l segregation for different types of bed motion observed with 34 pct fill in the 0.2 m ID x 0.2 m L cylinder containing particle sizes for 9.5 ram, 6.4 ram, and 4 ram.

tures are believed to be related to the packing characteristics of the solids bed. Current research at Carnegie-Mellon University 18 is directed at testing this hypothesis and at relating bed packing and segregation to the experimental and mathematical modeling studies of packing reported in the literature. 19-24 When the bed is cascading (Figure 1(b)), no radial segregation of the ternary mixture is visible, but at higher rpm's (Figures l(c) and l(d)), radial segregation is again observed. In this instance, though, finer solids, 6.4 mm and 4 mm beads, segregate to the walls of the cylinder. Hence, it has been termed reverse segregation in this work to differentiate it from the segregation core associated with rolling and slumping beds. The extent of reverse segregation is more pronounced under centrifuging conditions. It is clear from Figure l(d) that the particles have been graded with the finest adjacent to the wall and the coarsest farthest from the wall. The reason for the different pattern of segregation when rolling and centrifuging is clear from a fundamental understanding of bed behavior. 25 Bed motion is a function of the ratio of centrifugal and gravitational forces applied on the solids, the Froude number. The critical rpm at which solids begin to centrifuge is a function of the cylinder diameter and
METALLURGICAL TRANSACTIONS B

the particle size of the charge. This relation is given by: nc = - /T

[ll

where nc is the critical rotational speed and g is the gravitational acceleration. The effective radius of rotation, R ', is given by the distance between the center of rotation of the cylinder and the center of a particle at the wall of the cylinder. If each of the three particle sizes shown in Figure 1 is rotated separately in the 0.2 m ID cylinder, the nc calculated from Eq. [1] is 96.1, 95.3, and 94.7 rpm for the 9.5, 6.4, and 4 mm particles, respectively. This clearly shows that the smallest particles are easiest to centrifuge because their effective radius of rotation is the largest. With the cylinder rotating at 94.7 rpm, the 9.5 and the 6.4 mm particles would have Froude numbers of 0.97 and 0.987, respectively. With all three particle sizes placed together in the cylinder at a given rotational speed, it follows that the Froude number would still be largest for the smallest sized particles, the 4 mm beads. Hence, the smallest sized beads will segregate to the wall at high rotational speeds or when the bed starts cataracting. They will be the effective wall for the coarser sized beads. Thus the critical rotational
VOLUME 17B, JUNE 1986--249

speed of the coarser beads must correspondingly increase with the decreasing effective radius of rotation. To illustrate: if the finest beads form a monolayer against the wall, the 6.4 mm beads would rotate with an effective radius of rotation of 0.0945 m when loosely packed against the 4 mm beads. The corresponding Froude number is 0.948 at 94.7 rpm, the n~ of the smallest beads, a significant decrease from the 0.987 calculated with the cylinder containing only the 6.4 mm beads. This result would not change significantly for a different degree of packing of the intermediate sized beads. With the cylinder rotating at 94.7 rpm and all three bead sizes in the cylinder, the coarsest beads would have a Fr of 0.87 with the smaller two sized beads layering at the wall of the cylinder. Therefore, at large rotational speeds (i.e., cataracting and centrifuging beds), radial segregation is predicted to occur in a layered structure as was observed experimentally (Figures l(c) and l(d)).

i_

/ x

Vliit

, : , :.,gJw

B. End-Wall Effects and Characteristics of the Segregation Core

For the remainder of this work, experiments were conducted with the bed rolling or lightly cascading. The latter bed mode occurs at relatively low rpm's and high bed depths where the upper portion of the bed has a net velocity into the freeboard of the cylinder but the active layer is still in contact with the passive region of the bed. To ensure that observations of the segregation phenomenon at the cylinder end-wall were representative of the entire bed, sampling of the bed along the cylinder axis was conducted using the sampler already described and the 0.2 m ID cylinder. The steady-state configuration of the central segregated core was first examined. The cylinder was rotated at the desired speed for a period of approximately five minutes to allow the radial segregation core to come to equilibrium. The cylinder rotation was then stopped and the sampler inserted against the upper portion of the wall facing the surface of the bed. The cylinder was rotated until the sampler was inserted into the bed. The sampler containing a 5.8 cm thick slice of the bed was then removed from the cylinder and the ends of the slice were photographed. The large particles which had formed the active layer were stripped away to reveal the top of the segregation core which was also photographed. The procedure was repeated once with the sampler adjacent to the end plate and then with the sampler mid-way into the cylinder axis. These slices of the bed taken at the end and center of the small cylinder covered half of the axial length of the cylinder. A representative set of observations is presented in Figure 2. Observing the cross section of the segregation core through the end plates of the cylinder and of the sampler reveals that the core assumes a shape similar to that of the bed as shown in Figure 2. The core is positioned just below the active layer of the bed when rolling. In the slumping mode since there is no active layer per se, the core resides virtually at the bed surface. Observing cross sections x, y, and z in Figure 2, it is clear that the end-wall effects decrease the size of the segregation core at the end of the cylinder, while its shape and position remain unaffected. By studying the width of the top of the segregation core after removal of the coarse particles from the bed surface, it is seen that the end-wall effects occur only
250--VOLUME 17B, JUNE 1986

Fig. 2--Photographs of the surface of the segregated core and of its cross section at various axial positions in the 0.2 m ID cylinder using 9.5 and 4 mm beads.

over a short distance of 2 cm from the end plate. Furthermore, from Figure 2 it is clear that the segregation core is composed predominantly of the finer sized beads throughout the axis of the cylinder. End-wall effects were also investigated during the process of segregation. Starting with a well-mixed bed of 9.5 mm and 4 mm beads, the bed was rotated in the rolling mode for less than one revolution. The structure of the cross section of the bed at the end-wall and of the surface of the segregation core along the cylinder axis are visible in Figure 3. Viewing the cross section through the end plate, it is clear that the finer beads have begun to segregate to the central core. The finer beads are also visible in the remainder of the bed, particularly at the top right (i.e., the upper part of the bed when rotated). The surface of the bed is covered with coarse particles. Along the axis of the cylinder, this layer of coarse particles was removed to reveal the surface of the segregation core. As in the cross-sectional view, fines segre-

g%

.~..-, .~

Fig. 3 - - Cross section and axial view of the segregation core prior to its equilibrium posntion. The cylinder was rotated in a counter clockwise direction. METALLURGICALTRANSACTIONSB

gate to the center and are still visible at the surface of the bed, while in the lower part of the bed, few fines are visible. This clearly shows that the segregation process is not complete. Also, as in Figure 1, it appears therefore that the end-wall effect is one of reducing the number of finer particles at the end walls of the cylinder. This result is relevant to the onset of axial segregation where, in industrial reactors, dams and discharge ports could affect the flow and hence the residence time of finer solids. However, the phenomenon responsible for the radial segregation which is visible through the end-wall of the cylinder is representative of the entire bed. Hence, for the experiments on the kinetics of segregation a correction must be made of the number of finer beads visible through the end-wall as this cannot be controlled from one experiment to another.

C. Mechanism of Segregation
It was observed in the study of the end-wall effect that radial segregation was complete within less than one cylinder revolution. Hence, in order to quantify the kinetics of segregation, a 16 mm HYCAM operating at 100 frames/sec was used to film the events from the end-wall. These filming studies constitute the first detailed and recorded observation of radial segregation. A typical sequence of events is shown in Figure 4 where the beads of different sizes are differentiated by color. In this sequence, a binary mixture of 9.5 mm and 4 mm beads are rotated at 2.84 rpm in the 0.2 m ID cylinder with 23 pct fill. Many common features of the segregation process were observed from viewing a number of films. These will be briefly described below and illustrated using Figure 4 whenever possible. The bed may be divided into two distinct regions, the active layer and the passive region as has been postulated earlier. 4 In the active layer, particles move from the upper part of the bed to the lower part, where there is relative motion between the particles in this layer and the cylinder. On the other hand, particles move with the cylinder rotation in the passive region. The void fraction in the active layer is greater than in the passive region due to the motion of the particles. As fine particles are carried into the active layer from the passive region, they percolate between the voids of the coarse particles. As the fine particles travel down the active layer, they remain in contact with the passive region. This results in finer solids falling into the voids between the coarse solids of the passive layer while in the upper region of the bed. Due to the continuous rotation of the cylinder, these fine particles reenter the active layer and continue to proceed down the active layer toward the lower part of the bed. This process continues with a corresponding build-up of fines moving in and out of the active layer until these fines pass into the lower half of the active layer. Here the net mass flux of solids is into the passive region due to the cylinder rotation. The fines will subsequently reemerge in the active layer once they are placed by the cylinder rotation in the upper half of the active layer and will reenter the passive region within the central part of the bed, slightly recessed from the bed surface. As more fine particles enter the active layer from the well mixed bed, the central core of the fines increases in size. Hence, the midpoint of the active layer is the point of initiation of the segregation core.
METALLURGICAL TRANSACTIONS B

Very few of the finer beads ever travel with the active layer to the bottom surface of the bed. Hence, once the fine particles report to the central core, their subsequent movement is restricted to within the radius of the core. This results in an annulus of the bed cross section which becomes depleted very quickly of fines. This is clearly visible in Figure 4, where the formation of the annulus progresses more visibly with increasing time. From our observations of the high speed films, as soon as the bottom point of the active layer (the point where the lower surface of the bed meets the cylinder wall) reached the apex of the bed, the segregation process was essentially complete. That is, the shape, size, position, and composition of the core appeared to reach equilibrium. For the case shown in Figure 4, this time of segregation is only 4.1 seconds. In this instance, as well as in all experiments in this work, the segregation core was composed of the finer beads, was slightly recessed from the surface of the bed, had a crosssectional shape similar to that of the bed, and its size was proportional to the amount of the finer solids at the endwall. The coarser fraction always formed the surface of the bed. Clearly, this would result in poor heat transfer to the finer solids in kilns and driers. From observing the films, the percolation mechanism is clearly responsible for the separation of fine and coarse particles in the active layer. Here, the voids between the coarse particles are greater in size than in the passive region. The fine particles fall between the coarse until they are just above the passive region. As the fine and coarse particles move down the active layer, further segregation occurs by the flow mechanism. Coarse particles traveling farther than the fine particles results in a segregation core void of coarse solids. Earlier observations with angular solids indicated that the core contained both fine and coarse particles at the maximum bulk density of the mixture. 4 Clearly, the particle shape strongly affects the dynamic frictional force of the fine and coarse solids. Further research is necessary to elucidate and quantify these effects.

D. Kinetics of Segregation
In order to utilize fully the information recorded by filming the segregation process, a technique was developed to obtain quantitative data from the films. This involved counting the number of finer beads in the annulus at a particular film frame and repeating the process at specified time intervals in the film (i.e., every 50 frames or about 0.5 second). This annulus was determined to be the simplest area for counting particles to yield information about the kinetics of the segregation process. The data collected reflect the depletion of fine particles from the annulus of the bed during the formation of the segregation core and are directly correlated to the flow of fines into that core. The start of the segregation was determined from the film as that frame where decreasing rotational speed of the cylinder first became apparent. This was explicitly achieved by advancing the film frame by frame and measuring the circular displacement of the cylinder after each frame to the point where it matched that of the final cylinder rotational speed. Other workers reported the kinetics of the segregation process to follow first order kinetics. 2'12'15This may be described mathematically by the equation: log N = log No + kt [2]

VOLUME 17B, JUNE 1986--251

.....

"-

;_:~-e:':

~ ~,.~.~:~

.~_-~"

0.513

(sec)

1.02S

(sec)

"
.. .' ~ ,~

~'~

. ~ . . . , ~ " . . o.-t
=

~__.,,.~..,,,_~

.,_.

~:

1.538

(sec)
m ~

2.050

(sec)

"~,,,

~,

.,,

.,,~

-,,

~1'

-.'~,4'~5,,

"

~',,,

"

llw~.
t = 3. 075 ( s e c )

t ; 2. 563 ( s e c )

~,,

t = 3.588

(sec)

t = 4. 100 ( s e c )

Fig. 4 - - High-speed photographs illustrate segregation phenomenon in a rotating granular bed for a mixture of 20 pct by volume of finer (4 mm) component. 252--VOLUME 17B, JUNE 1986 METALLURGICAL TRANSACTIONS B

where N and No are the number of fine particles in the annulus at any time t and initially at t = 0, respectively, while k is a constant of proportionality. This equation indicates that if first order kinetics is obeyed, then plotting the logarithm of the number of fines vs time should produce a straight line. Figure 5 shows such a plot for some typical experimental runs. The curved lines clearly indicate that the first order kinetic model does not apply. Furthermore, first order kinetics imply that the bed should turn over a number of times before segregation is complete. In this study, segregation was always complete within one turn of the contents of the bed. Hence, radial segregation is not a random or diffusional process as has been indicated by previous workers. 2.12.15 This is further substantiated from a careful observation of the segregation process on the high speed films. There was no motion of fine or coarse particles in relation to each other within the annulus of the bed (Figure 4). Any movement of fine particles into the segregation core occurred in the active layer. Furthermore, the dissection of the bed for low rotational speeds, 2.4: 1 size ratios, and percent fill higher than twenty indicated that the fines came into the active laye" at the top of the bed (from the annulus) and none traveled to the bottom to be deposited back into the annulus (Figure 3). Thus, all fines transferred to the active layer from the annulus due to the rotation of the cylinder were deposited immediately in the segregation core. Consequently, because the fines are assumed to be evenly distributed in the annulus (from the cascading state) and because the rotational speed is held constant, it follows that the rate of fines entering the segregation core should be constant as long as fine particles remain in the annulus. This type of behavior corresponds to zero order kinetics where:
dm/dt = S

For illustration, one of the runs plotted in Figure 5 is replotted in Figure 6 according to [4]. Excellent agreement is observed between the experimental data and the kinetic model indicating that radial segregation obeys zero order kinetics. The fact that all particles leaving the annulus report to the' segregation core suggests that the total time of segregation should be equal to the time required to pass the entire annulus through the active layer. This corresponds to the time necessary to rotate the cylinder by an angle equal to that

RPM 5 7 1 rev/min Bed Depth 7 . 8 4 c m Regression Coefficient: 0.98 Slope -18.06 Segregotion Time t: 5 . 8 4 sec Criticol Time tc: 4 . 4 8 sec

\
i

15

[3]

and
X = No + St 200f r F 1 1

t (sec)

[4]
T

Fig. 6 - - P l o t of number of beads (N) in the annulus as a function of segregation time (t) 0.2 m ID cylinder and 2.4:1 particle size ratio.

. , de symool ~-f
9 2.4

r.p.m. % cylinder (rev/min)fill I.D.(m)

5.71 35

I
I,z 8 0 ~ ~ '

0.2
0.2

1.6

1.94

1.5 1.5

2.85 3.74

25 28

0.2
0.4

= 5o r
4 "=' 30 v -

t (sec)
Fig. 5 - - R a d i a l segregation kinetics plotted according to first order kinetics.

METALLURGICAL TRANSACTIONS B

VOLUME 17B, JUNE 1986--253

bounding the arc along the cylinder wall which is covered by the bed. This critical time, to, may be calculated from the following equation:
tc ~

-O OOk

I X

IX
-0 05 r

l\

~ I i BED DEPTH % FILL (cm) 9 579 25

60 1JR - H] cos- 7rn

I
[5]

~"

9 8 z9

38
~z

-~ '~
' ~ -0 15-

--X
m~ ~

9 ,o.54

For a number of trials, the critical time did not agree well with the measured segregation times since the bottom portion of the bed did not contain fine particles at time zero. This situation is brought about at the start of the experiment by the collapse of the cascading bed to form the rolling bed when the rotational speed is reduced. A cascading bed has a steeper angle of inclination than a rolling bed. Thus, during the transition from cascading to rolling the top of the bed falls through the active layer to the bottom of the bed. As it passes through the active layer, the fines begin to report to the segregation core and a portion of the bottom of the bed is free from fines at the start of the segregation process. This situation is illustrated in Figure 7. Hence segregation times and the rate of segregation may be different for two identical experiments. Since it is not feasible in our experimental apparatus to reproduce exactly the cascading and transition conditions for every experiment, the rate of segregation was corrected by the critical time of segregation. Furthermore, this normalized rate of segregation accounted for the different starting number of finer solids in the annulus. The resulting function, S,, is given by: S.
-

Intercept of line - 0 0 I Slope of line: - 0 0 3 Regress=on coeff 0 99

'g - o 2 o -

,\\
== -o 35o

'X
-040-45 I 25 I I I I 50 75 I00 125 ROTATIONAL SPEED(RPM)
~O

\
'X I \ 150
175

-0 5(

St Note

[6]

Fig. 8 - - N o r m a l i z e d slope v s cylinder rpm for a size ratio of 2.4:1 in the 0.2 m ID cyhnder for three bed depths.

S. was determined for various pct fills, rpm's, particle size ratios, and cylinder diameters. Rotational Speed and Bed Depth: S. was found to be a linear function of rotational speed and to be independent of bed depth or percent fill as shown in Figures 8 through 11. These results are from experiments performed on the two cylinders containing different bed depths and size ratios. Each data point in Figures 8 through 11 was determined from an analysis of high speed movies as already described.

-0 00[

r~,.

BED DEPTH

% FILL

oosL\ I "~
I N

9 5~9
~
"'X N~ X

z3
35

-o.,o~I -O. IE F

.,o89

~72

s5

Intercept of line -0 02 Slope of line - 0 0 2 Regression coeff 0 9 9

(~ ~ c a s c a d i n g

-02.=

r
V

.\."
\
I 25
I 1 I I 5,0 75 I00 125 ROTATIONAL SPEED (RPM)

-045N = No+St

-05(
St

I 150

175

S N - Note Fig. 7 - - S c h e m a t i c of the difference between the actual time oT segregation, t, and the critical time of segregation, to. 254--VOLUME 17B, JUNE 1986

Fig. 9 - - N o r m a l i z e d slope v s cylinder rpm for a size ratio of 1.6:1 in the 0.2 m ID cylinder for three bed depths. METALLURGICAL TRANSACTIONS B

-000

BED DEPTH (cm)

-00~ " ~ 9 6.02

% FiLL 25 _

9
- 0 IC

7.74 9 9 34

35 45

Intercept of hne.-O 0 2 q-0 I~ . ~ Slope of hne - 0 0 2 -

-o zc
LIJ

~
W N

- 0 2~

_.5 -o.3c
- 0 35

frO

-0 4C

-045--

- 0 5C i )

2.5

I I I I I 50 75 I00 125 150 ROTATIONAL SPEED (RPM)

17.5

Fig. 10--Normalized slope v s cylinder rpm for a size ratio of 1.5:1 in the 0,2 m ID cylinder for three bed depths.

S~ze Bed Depth (cm) Roho Symbol -005 16 iO o ,, 9.71 1315 8.71 11.51

% Fill 16 2B 16 25

-0

~4

~
9

Size Raho - 0 151

,ote,oop, o,,,oe I -? ol I -o
S,ope o, ,,~ I -o
0 99

I
L

I-0

~g -o z o
LIJ n_

Regression coeff I

[ 0 99 I

-OZ5
0 ~J N

-o so

-035

k
-O 4 0

N ~

In all instances zero order kinetics prevailed. The straight lines drawn in Figures 8 through 11 are least square regressions of the normalized slopes. The excellent fit of the straight line function between S, and rpm confirms that radial segregation is a zero order kinetic process. Secondly, the rate of segregation increases with increasing rotational speed, while the rate of segregation is independent of bed depth. This also confirms the mechanism of segregation described earlier in that deeper beds will require a longer time to segregate but will do so at the same rate as shallower beds. At low bed depths, less than 15 pct fill, in the 0.2 m ID cylinder, a different radial segregation pattern was observed. While the behavior of the coarser and finer fractions in the active layer occurred as described earlier, fine particles percolated between the voids of coarse in the passive region. This resulted in a nonstationary central segregation core and has been attributed to circumferential wall effects. With the 9.5 mm beads, a 15 pct fill represents a bed of only 3 to 4 particles deep. The bed was observed to have larger sized voids, allowing the finer beads in the passive region to move relative to the walls of the cylinder. Due to this movement, it was not possible to quantify segregation at low bed depth. These observations have two interesting implications. First, they clearly show that percolation can occur in the passive region, which supports the percolation mechanism postulated by Henein et al. 4 for the formation of a second segregation core at the top of the bed. 3 This second core is believed to be responsible for the onset of slipping. Second, these observations imply that the cylinder diameter to particle size ratio may be a scale-up criterion. ~8 Particle Size R a t i o : Donald and Roseman ~5have reported effects of particle size ratios on the segregation kinetics. Their study indicated that the greater the size differences of the particles, the faster the segregation. They observed that size ratios of 1.2:1 did not allow enough voidage for finer particles to percolate. Also, that the rate of segregation increased with increasing size ratio. The slopes of the least square fitted lines in Figures 8 through 11 are presented in Table I. The results are similar to those of Donald and Roseman in that the rate at which segregation takes place in either the 0.2 m ID or the 0.4 m ID cylinders increases as the size ratios increase. C y l i n d e r D i a m e t e r a n d S c a l e - u p : It is evident from Figures 8 through 11 and from Table I that for the same size ratio of 2.4:1 the rate of segregation is faster in the 0.4 m ID cylinder than in the 0.2 m [ D cylinder. Figures 9 and I1 and Table I reveal the same trend for the 1.6:1 size ratio. An understanding of bed motion is helpful to explain these trends. At the same rotational speed the ratio of centrifugal to gravitational forces will be higher for larger cylinders. Figure 12 presents the normalized slope vs the Froude number for all the experimental data in Figures 8 through 11. It
Table I. Slope of the S . vs RPM Regressed Lines

-o 4s

Cylinder -o 5c
25

50

-/'5

I00

125

__ dc/d f
150 1"7

ROTATIONAL SPEED (RPM)

Fig. 11 --Normalized slope vs cylinder rpm for the size ratio of 2.4:1 in the 0.4 m ID cylinder for two bed depths.

2.4 1.6 1.5

0.2 m ID -0.028 -0.026 -0.024

0.4 m ID -0.050 -0.030 --

METALLURGICAL TRANSACTIONS B

VOLUME 17B, JUNE t986--255

O~

V.

CONCLUSIONS

~
-% v

-0.1

(B) o

(B) 9

uJ - 0 2 n

o --J if) ~ -03

1"4

.J

~
o z

-04
&

-0 5

0004

0008

0.012

0016
NUMBER

002

0024

FROUDE

Fig. 12--Scale-up of the rate of segregation for several dc/d: in the 0.2 m ID (A) and 0.4 m ID (B) cylinders.

is evident from Figure 12 that for a given size ratio and Fr, S, will be the same regardless of cylinder size. Hence the scale-up criteria for segregation from this study are the size ratio of coarse to fine solids and the Froude number. Figure 12 also reveals that the smaller dJd:, the smaller S,. In the limit it may be expected that S, will approach zero as the dc/d: decreases to where no segregation occurs. Similarly, it seems intuitive that as d~/d: increases, S, would reach a limiting value. Current research will delineate these limits. ]8 Finally, the relationship between S, and Fr is not linear. As the Fr increases, the rate of segregation seems to reach a minimum value for each size ratio. As Fr is further increased, it is expected that the segregation rate will decrease until Sn will be zero for a well-mixed cascading bed. A least square regression of the experimental results was conducted on each dJd: ratio. The resulting equations are: S, = - 2 . 4 8 Fr ~ S, = - 2 . 0 3 Fr ~ S, = - 2 . 0 1 Fr ~ for for for

dJd: = dc/d: = dc/d: =

2.4/1 1.6/I 1.5/1

[7] [8] [9]

1. Radial segregation is a function of bed behavior. For slumping, rolling, and low cascading beds, the finer solids segregated to the central core of the bed. Higher cascading beds result in a well mixed bed, while for cataracting and centrifuging a layered structure of particles occurs at the cylinder walls. Finer particles are closest to the wall and the coarsest particles are farthest away from the wall. 2. The reverse pattern of radial segregation is attributed to the decreasing effective radius of rotation for larger sized particles. This results in a smaller Froude number for a constant cylinder rpm. 3. The central segregation core was found to be of the same shape as the solids bed. It was composed predominantly of the finer solids and was recessed from the bed surface by a layer of the coarser particles. 4. Radial segregation occurred by the percolation and flow mechanisms, and the kinetics of segregation follows zero rather than first order kinetics. 5. The rate of segregation was found to be directly proportional to the cylinder rpm but independent of bed depth for the experimental results reported in this work. Furthermore, it was observed that the larger the size ratio of coarse to fine, the faster the rate of segregation. The rate of segregation increased greatly for small increases in rpm's at low rotational speeds, but at high rpm's the rate of segregation did not significantly increase. 6. The scale-up criteria for radial segregation are de~d:and Fr. The former is believed to be related to the packing characteristics of the coarser fraction, while the latter represents the same segregation rate at the same ratio of centrifugal to gravitational forces imposed on the rotary device. 7. This analysis constitutes a new quantitative technique to measure the rate of radial segregation which can be used to measure the effects of bed behavior, particle size, shape, and density differences and to access the design of lifters, mixers, and protrusions in rotary reactors for the break-up of the radial segregation.

The exponents of the Froude number confirm the linear dependence of rotational speed observed in Figures 8 through 11. Furthermore, the decreasing coefficients with decreasing size ratio are believed to be related to the packing characteristics of the bed and to the size of voids between the coarse particles relative to the size of the finer particles. Further experimentation is required to verify these effects. It is important to emphasize that the rates of radial segregation of fines is extremely fast with segregation times of the order of seconds. This clearly implies that the configuration of a radially segregated bed will always form the initial condition for subsequent axial segregation which occurs in batch and continuous operations. Furthermore, with radial segregation occurring so quickly, mixing devices or protrusions must be placed at regular and frequent intervals longitudinally in a reactor. These mixing devices and protrusions must have a minimum height in order to reach the segregation core, if effective mixing is to be achieved. The tracer technique described in this study would provide a very effective quantitative tool to access the design of lifters and protrusions available in industry.
256--VOLUME 17B, JUNE 1986

NOMENCLATURE Fr H N No R R' S Froude number bed depth (cm) number of fine particles in the annulus at time t number of fine particles initially in the annulus radius of cylinder (cm) effective radius of rotation (cm) rate of segregation (finer particles/sec) normalized rate of segregation (cm -1) size of coarser particles (mm) size of finer particles (mm) gravitational acceleration (cm/sec 2) constant of proportionality rotational speed (rev/min) critical rotational speed (rev/min) time (sec) critical time
METALLURGICAL TRANSACTIONS B

S.

dc

d:
g k n nc t tc

ACKNOWLEDGMENTS The authors are grateful to Carnegie-Mellon University and to the National Science Foundation (NSF CPE8204522) for providing financial support for this work. Appreciation is also expressed to Mr. C. Able for his assistance in the design and construction of the experimental apparatus used in this study. Discussions with Mr. E. Sunnergren are also gratefully acknowledged. REFERENCES
1. H. Henein, J. K. Brimacombe, and A.P. Watkinson: Metall. Trans. B, 1983, vol. 13B, pp. 191-205. 2. G. Reuter: Doctoral Thesis, Rheinisch-West falischen Technischen Hoschule, Aachen, October 1985. 3. C.E. Sunnergren: Bethlehem Steel Co., Bethlehem, PA, unpublished research, 1974. 4. H. Henein, J. K. Brimacombe, and A. P. Watkinson: Metall. Trans. B, 1985, vol. 16B, pp. 763-74. 5. Ft. Muller: Aufbereitungs-Technik, 1966, vol. 5, pp. 274-85. 6. W. Weydans: Chem. lng. Tech., 1960, vol. 32, pp. 343-49. 7. C. von Sauer: Neue Hutte, June 1972, vol. 17, pp. 358-62. 8. M. Ullrich: Chemie. Ing. Tech., 1969, vol. 41 (16), pp. 903-07. 9. K.W. Carley-Macauly and M.B. Donald: Chemical Engineering Science, 1962, vol. 17, pp. 493-506.

10. M.B. Donald and B. Roseman: Brit. Chem. Eng., 1962, vol. 7(10), pp. 749-53. 11. K. Yamaguchi: Seramikkusu, 1971, vol. 6(1), pp. 47-54. 12. A.R. Rogers and J.A. Clements: Powder Technology, 1971/72-, vol. 5, pp. 167-78. 13. S.S. Weidenbaurn and C. E Bonilla: Chem. Eng. Progress, 1955, vol. 51(1), pp. 27J-36J. 14. H. Henein: Ph.D. Thesis, University of British Columbia, 1981. 15. B. Roseman and M. B. Donald: Brit. Chem. Eng., 1962, vol. 7(11), pp. 823-27. 1~ J.C. Williams and M.I. Khan: The Chemical Engineer, 1973, pp. 19-25. 17. J.C. Richards: "The Storage and Recovery of Particulate Solids," Institution of Chem. Engineers, Working Party Report, 1966. 18. B. Pollard and H. Henein: unpublished research, Carnegie-Mellon University, Pittsburgh, PA, 1985. 19. C.C. Furnas: Industrial and Engineering Chemistry, 1931, vol. 23(9), pp. 1052-58. 20. J. Eastwood, E.J.P. Matzen, M.J. Young, and N. Epstein: British Chemical Engineering, 1969, vol. 14(11), pp. 1542-45. 21. K. Karlson and L. Spring: Journal of Materials Science, 1970, vol. 5, pp. 340-44. 22. B.M. Zivanovic: Proceedings of the First International Conference on the Compaction and Consolidation of Particulate Matter, The Powder Advisory Centre, October 1972, pp. 37-40. 23. D.R. Hudson: Journal of Applied Physics, 1949, vol. 20, pp. 154-62. 24. E von Sommer and H. Soeder: Archiv .fur das Eisenhiittenwesen, 1963, vol. 34(1), pp. 1-8. 25. H. Henein, J. K. Brimacombe, and A. P. Watkinson: Metall. Trans. B, 1983, vol. 13B, pp. 207-20.

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