434 Ind. Eng. Chem. Res.

1988,27,434-439

Registry No. NiO, 1313-99-1; H2,

1333-74-0.
Literature Cited
Bartholomew, C. H. J . Catal. 1976,45, 41.
Bartholomew, C. H.; Pannell, R. B. J . Catal. 1980, 65, 390.
Cimino, A.; Shiavello, M. J. Catal. 1971,20, 202.
Farrauto, R. J. AZChE Symp. Ser. 1974, 70, 9.
Gavalas, G. R.; Phichitkul, C.; Voecks, G. E. J . Catal. 1984,88, 54.
Levenspiel, 0. Chemical Reaction Engineering; Wiley: New York,
1983; Chapter 12, pp 367-371.
Martin, G . A.; Ceaphalan, N.; Moutgolfier, P. d. J. Chim. Phys. 1973,
70. 1422.
Pannell, R. B.; Chung, K. S.; Bartholomew, C. H. J. Catal. 1977,46,
340.
Ross, J. R. H.; Steel, M. C. F.; Zeini-Isfahani, A. J . Catal. 1978,52,
280.
Shalvoy, R. B.; Reucroft, P. J.; Davis, B. H. J . Vac. Sci. Technol.
1980, 17, 209.
Vedrine, J. C.; Hollinger, G.; Minh, 0. T. J . Phys. Chem. 1978, 82,
1515.
Wen, C. Y. Ind. Eng. Chem. 1968, 60, 34.
Wu, M.; Hercules, D. M. J . Phys. Chem. 1979, 783, 2003.
Received for review March 20, 1987
Revised manuscript received October 26, 1987
Accepted November 14, 1987

Sorption of SO2 on Metal Oxides in a Fluidized Bed

Bekir Zuhtu Uysal,*+Inci Aksahin,*and Hayrettin Yucelf
Chemical Engineering Department, Jordan University of Science and Technology, Zrbid, Jordan, and
Chemical Engineering Department, Middle East Technical University, Ankara, Turkey

A preliminary experimental study is described in which a low concentration of SO2 (0.2% v/v) is
removed from air at temperatures between 358 and 640 K by reaction with bauxite and red mud,
which consist of several metal oxides in a lab-size fluidized bed reactor of 5-cm diameter. CuO on
activated alumina, a well-known sorbent for SOz,was also tested in the same system for comparison.
A model based on the two-phase theory of fluidization was used to simulate the sorption process.
It was shown that a kinetic rate expression for sorption of SO2 on a single metal oxide to yield a
metal sulfate can also be used for mixtures of metal oxides by defining an overall apparent rate
coefficient and an overall consumption coefficient for active sites. The work indicated that bauxite
and red mud could also be considered as potential sorbents like CuO for SO2sorption in a typical
range of stack gas temperatures.

I t is generally accepted that emission of sulfur oxides
from combustion of fossil fuels causes a serious air pollu-
tion problem. The control of sulfur dioxide emissions
becomes more important due to the trend of using in-
creasing amounts of high sulfur coal to meet energy re-
quirements. A great number of processes have been pro-
posed for removal of sulfur oxides from flue gases, and they
are summarized in several references (Slack, 1971; Kohl
and Riesenfield, 1979).
All of the proposed processes for flue gas desulfurization
can be classified into two basic categories: throwaway
processes and recovery processes. In each category, the
processes can be further classified into wet or dry pro-
cesses. Wet throwaway processes such as alkali or lime-
limestone scrubbing have been preferentially developed
on a commercial scale. However, dry recovery processes
are thought to be more advantageous over wet systems
since they may permit flue gas treatment a t elevated
temperatures, avoiding flue gas reheating which is usually
required for a wet process to maintain plume buoyancy.
On the other hand, the dry recovery processes might have
the usual problems of large-scale handling of regenerable
solids, mainly high investment costs due to the complex-
ities of the regeneration system and excessive losses of
sorbent due to attrition.
Recently, a significant amount of work has been done
to develop dry recovery processes based on sorption of
sulfur oxides on metal oxides (Bienstock et al., 1961;
Thomas et al., 1969; Lowell et al., 1971). In a study by
Tracor Corporation (Thomas et al., 1969; Lowell et al.,
1971) the oxides of 48 metals were screened to determine
which were best suited for the removal of sulfur oxides
from flue gases by chemical reactions. The screening was
Jordan University of Science and Technology.
t Middle East Technical University.
0888-5885/88/2627-0434$01.50/0
based on the thermodynamic requirement for efficient SO2
removal and product regeneration. Oxides of Ti, Zr, Hf,
V, Cr, Fe, Co, Ni, Cu, Zn, Al, Sn, Bi, Ce, Th, and U were
selected as a result of this screening process. Further
screening of metal oxides by consideration of their reaction
rates with SO2in a flue gas atmosphere showed that oxides
of Cu, Cr, Fe, Ni, Co, and Ce would have economically
feasible reaction rates with SO2. After further evaluation
of factors such as sorption reaction stoichiometry, forma-
tion of product layers which affect the reaction rate, and
SO, partial pressure over the sorption product, oxides of
copper and iron were selected as the most promising.
Of the potential metal oxide sorbents for SO2 removal,
CuO received the most attention. Laboratory-scale work
on copper oxide impregnated into porous alumina has been
conducted by the US. Bureau of Mines (McCrea et al.,
1970). The results showed that sulfate formation goes
essentially to completion at temperatures of about 450 "C.
The regeneration by the reducing gases such as hydrogen
and methane could be accomplished at much lower tem-
peratures.
Work on a copper oxide process has also been conducted
by Shell in the Netherlands (Dautzenberg and Nader,
1971). This process, which has been named the shell flue
gas desulfurization (SFGD) process, also uses CuO on an
alumina support. Two fixed bed units are used in the
process. One is used for gas purification and the other
undergoes regeneration by use of hydrogen, carbon mon-
oxide, or methane. Both steps are accomplished at about
400 "C.
The main object of this study was to test the possibility
of using bauxite and red mud for SO2 sorption. Bauxite
mineral and red mud-a byproduct of aluminum
plants-contain oxides of metals such as iron, titanium,
and aluminum which can be considered to be potential
sorbents for SOz. Copper impregnated on activated alu-
1988 American Chemical Society
 Ind. Eng. Chem. Res., Vol. 27, No. 3, 1988 435

mina, a well-known sorbent for SO2 and on which some
fundamental studies have been carried out (Koballa and
Dudukovic, 1970; Yates and Best, 1976; Best and Yates,
1977; Cho and Lee, 1983), was also used for SO2 sorption
for comparison. As a contacting device, a fluidized bed
reactor was used. The fluidized bed reactor, in addition
to some obvious advantages as a gas-solid contactor, al-
lowed use of fine powders of red mud, thus avoiding the
formation of pellets which would be required in a fmed bed
operation.
Theory
Reaction Mechanism for Sorption of SO2on Metal
Oxides. When sulfur dioxide reacts with metal oxides in
the presence of oxygen at temperatures below the decom-
position temperature of the sulfate, the principal product
is sulfate and the overall reaction for a bivalent metal can
be written as
Me0 + SO2 + 1/202
F! MeS04 (1)
A great number of mechanisms may be postulated for this
reaction (Koballa and Dudukovic, 1970; Yates and Best,
1976; Best and Yates, 1977; Cho and Lee, 1983). One
possible reaction scheme that explains the empirically
determined rates (Cho and Lee, 1983) is as follows:
S02(g)+ MeO* $
z MeO-S02* (2)
kd
l/202(g) +L LO* (3)
k,
MeO-S02* + LO* MeO-S03* +L (4)
MeO-S03* A MeS04 (5)
It should be pointed out that actual reaction scheme may
be more complex than that given above because chemistry
of metal-oxygen-sulfur systems can involve multiple ox-
idation states, sulfite formation, disproportionation of
sulfites to sulfates and sulfides to sulfate decomposition,
and catalytic oxidation of SO2 to SOB. However, at the
temperatures involved, reactions such as sulfite formation
and catalytic oxidation of SO2 to SO3 are expected to be
unimportant, and the above reaction scheme is assumed
to be adequate to predict the system behavior.
Considering the reaction mechanism expressed by eq 2-5
and assuming that the sulfate formation step is rate de-
termining, then the rate expression can be written as
rA = k,(MeO-S03*) (6)
Other steps are assumed to be in equilibrium
(MeO-S02*)
K1 =
(MeO*)(S02)
(7)
where K , = K1K2K3k,(02)1/2(MeO*)0, C A = (SO,), XR =
fractional conversion of MeO*, and (MeO*)o = initial
concentration of MeO*. The rate of consumption of the
active site, MeO*, can be expressed as (Yates and Best,
1976)
dX,/dt = Kd(1 - x,) (11)
where Kd is an overall consumption rate coefficient of
MeO*. Integration of eq 11 gives
1 - XR = exp(-Kdt) (12)
Inserting eq 12 in eq 10 yields
rA = K r C A exp(-Kdt) (13)
Furthermore, it is worth adding that for the particle sizes
and the conditions involved the intraparticle resistance is
negligible by the criteria of pore diffusion (Levenspiel,
1972; Smith, 1981).
Modeling of Fluidized Bed. In recent years, a great
number of models for fluidized beds have been developed,
and extensive information about these models can be
found elsewhere (Grace, 1971,1986; Rowe, 1972; Kunii and
Levenspiel, 1977; Yates, 1983).
The model employed in this research is based on the
two-phase theory of fluidization. An approach similar to
the Orcutt model (Yates, 1983) with slight modifications
is used due to its simplicity and ability of satisfactory
predictions of performance.
Basic assumptions involved in the derivation of the
model are as follows:
1. All the gas in excess of that required to incipiently
fluidize the bed passes through the bed as bubbles, which
are uniform in size and equally distributed throughout the
bed.
2. Interfacial area per bubble volume, a; overall mass-
transfer coefficient, kbe; and fraction of fluidized bed oc-
cupied by bubbles, 6, are all independent of the height of
the bed.
3. The gas in bubble phase is considered to be in plug
flow.
4. The gas in emulsion phase is considered to be per-
fectly mixed.
5. There are no particles and, therefore, no adsorption
in bubble phase.
6. Gas density is considered to be approximately con-
stant.
For a differential height along the bed, mole balance for
the bubble phase, assuming pseudo steady state, can be
written as
-Puos, dCA, = k b e ( C A h - CAe)ClhS, dZ (14)
Mole balance in the emulsion phase gives
(1 - P)UOS,C, - (1 - P)UOS,C, +
LHfkb,U(CA, - dZ = r A ( 1 - 6)s&f
c~.)6s, (15)

Integration of eq 14 yields

K3 =
(MeO-S03*) (L) CAb = CA, + (C, - C4)e-yz (16)
(MeO-S02*) (LO*)
where
Elimination of concentrations of sorbed species in eq 6-9
gives * = -Izbea6
rA = K1K2K3k,(02)1/2(S02)(MeO*) P UO
Substitution of eq 16 in eq 15 and then integration give
The concentration of O2 can be taken as constant if it is
in large excess; thus, the rate expression becomes
r A = K,cA(1 - x,) (10)
436 Ind. Eng. Chem. Res., Vol. 27, No. 3, 1988
Substitution of the rate eq 13 in eq 17 gives the emul- Table I. Chemical Analyses (Weight Percent) of Sorbents
sion-phase concentration and Alumina Support on Dry Basis
alumina bauxite red mud
ignition loss 0.1 12.75 7.45
SiQz 0.03 7.23 16.85
A1203 98.5 56.49 16.96
Fe203 0.035 18.46 37.69
Combination of eq 16 and 18 gives the bubble-phase con- Ti02 22.12 4.73
v205 0.008
centration as a function of height: pzo5 0.005
CaO 1.17 3.76
Na20 0.05 10.27
COZ 1.4
H20 1.59

Table 11. Physical Properties of Sorbents and Alumina

A mole balance a t the exit of the reactor gives SUDDO~~
CA,dt = pcA,lZ=H, + (l - P)cAelZ=H, (20) alumina bauxite red mud
particle size, m m (Sauter mean) 0.0738 0.150 0.076
Substituting eq 18 and 19 in eq 20 yields the exit gas SOz particle density, g/cm3 1.52 2.46 1.16
concentration solid density, g/cms 3.55 2.95 3.12
-X porosity 0.57 0.17 0.63

av pore radius,i
surface area, m2 g 84.9
94.4
9.79
68.2
96.8
79.4

where
x = VHf (22)
Hydrodynamic parameters and mass-transfer coefficients
required in the models are estimated as follows:
The minimum fluidization velocity, Umf,is calculated
by Leva's equation (Yates, 1983):
dp1.82(P, - p,)0.94$.94
umf= (1.1 x 10-3) (23)
p,0.@-Qe8
The terminal velocity of the particles, Ut, is found by
using empirical correlation of Kunii and Levenspiel (1977).
The average bubble diameter is calculated by using
Kunii and Levenspiel's (1977) correlation.
The height of the bed is calculated by
The fraction of fluidized bed occupied by bubbles is
found from
The fraction of inlet gas entering the bubble phase is
calculated as
The interfacial area per bubble volume is
a = 6/db (27)
The overall mass-transfer coefficient is calculated by
using Sit and Grace's (1981) equation
which takes into account enhancement of mass transfer
due to bubble interactions in freely bubbling beds. The
effect of sorption on the mass-transfer coefficient is ne-
glected since the SO2 concentration is low.
Experimental Section
Apparatus. The experimental system which consists
of mainly a fluidized bed reactor, gas handling and me-
tering equipment, and a gas chromatograph is shown
schematically in Figure 1. The fluidized bed reactor was
a stainless steel tube of 5-cm inside diameter and 40-cm
length. It was fitted with a perforated brass gas distrib-
utor. The distributor was designed according to the me-
thod outlined by Kunii and Levenspiel (1977) to give a
uniform flow through openings. It had 69 holes of 1-mm
diameter. The column was heated by nichrome heating
wire, and the temperature in the bed was measured by a
thermocouple. The reactor was insulated by glass wool
lagging. The gas mixture was heated in a furnace preheater
before being fed into the reactor. There was a cyclone at
the top of the reactor to collect and return back the en-
trained particles. The exit gas was taken from the top of
the cyclone and was given to the chromatograph (Perkin-
Elmer Model F-20H) after passing through a double-pipe
cooler.
Materials. Three types of sorbents, CuO impregnated
on alumina, bauxite, and red mud, were tested as sorbents.
The chemical analyses of the sorbents and their important
physical properties are given in Tables I and 11.
CuO impregnated on alumina was prepared according
to a procedure given by Yates and Best (1976) and Cho
and Lee (1983). A concentrated solution of C U ( N O ~ ) ~ . ~ H ~ O
in distilled water were prepared. The alumina particles
previously activated at 750-850 K for 6 h were immersed
in this solution for 48 h. The impregnated alumina was
removed from the solution and washed with distilled water
to remove any of the solution trapped between the par-
ticles. These particles were dried at 353 K for 48 h, and
heated to 723 K, and vented to air for further 24 h to
decompose Cu(NO& to CuO. The percentage of copper
in the final product was determined by idometric methods
(Kolthof and Elvin, 1961). This procedure gave about 6%
(weight) Cu on the sorbent.
Procedure. The system was operated semibatchwise
with a single charge of particles. The bed was first loaded
with an amount of sorbent to give a static bed height of
5 cm. The flow rate of air was set to the desired value, and
after steady-state temperature was reached, SOz was in-
troduced at such a rate as to give an inlet SOz concen-
tration of 0.2% (v/v). The velocity was set equal to 11.1
 Ind. Eng. Chem. Res., Vol. 27,No. 3, 1988 437
Temperature
Controller

TO Atmosphere

TO GOS

oln

P
n l I I I I I
0 1 2 3 4 5 6
Preheoter Time x s
Figure 3. Breakthrough curves for bauxite. Symbols show exper-
imental data, and lines show model equation.

h
Rotameters

I f 1

U I
SO2 Ail

Figure 1. Schematic diagram of the experimental setup. 0-491 K

0.2i; ~ - - - - 5 0 8K
613 K
IO

01 I I I I I
0 1 2 3 4 5
Time x s
Figure 4. Breakthrough curves for red mud. Symbols show ex-
perimental data, and lines show model equation.

Table 111. Saturation Capacities of the Sorbents

saturation capacity,
sorbent temp, K g S02/kg adsorbent
CuO on alumina 384 6.41
430 6.71
466 6.43
529 14.2
01 I I I I I I
bauxite 392 3.17
0 1 2 3 4 5 6 7
483 5.09
Time x s
641 9.24
Figure 2. Breakthrough curves for copper oxide on alumina. Sym- red mud 491 3.95
bols show experimental data, and lines show model equation. 508 5.28
613 5.98
cm/s in all runs. Throughout a run, gas samples were
taken from the reactor inlet and outlet streams and ana- of sorbents for suA-drdiox ie. It is c-served that at tem-
lyzed by the gas chromatograph using a Porapak Q column. peratures lower than about 473 K the breakthrough curves
A run was continued until the outlet concentration of SO2 converge to a single curve toward saturation. At tem-
became almost equal to the inlet concentration. peratures higher than about 523 K, the saturation capac-
ities of the sorbents increase appreciably.
Results and Discussion The saturation capacities of the sorbents were evaluated
Experimental data in terms of sulfur dioxide break- from experimental breakthrough curves by
through curves for the sorbents examined at various tem-
peratures are given in Figures 2-4. Theoretical model eq
21 is also plotted in these figures for comparison. Ex-
perimental breakthrough curves are more or less sigmoid where A is the area above the breakthrough curve. These
in shape, although there is some noticeable deviation from values are shown in Table 111. The sorption capacities
it particularly for bauxite and red mud. This is probably are in good agreement with those reported by Koballa and
due to differences in the activities of various metal oxides Dudukovic (1970) and Cho and Lee (1983). In the former
present in these materials. study, the saturation capacity of a sorbent containing 20%
The data show that as the temperature increases the Fe20, is reported to be 0.015 kg of S02/kg of adsorbent
breakthrough curves for all sorbents shift to the right, at 588 K and 0.008 kg of S02/kg of adsorbent at 533 K.
indicating a higher rate of sorption and sorption capacities These values are quite close to the values obtained in this
438 Ind. Eng. Chem. Res., Vol. 27, No. 3, 1988

10000 I I I J 10-

IO
IO 15 20 25 30 35
I/T x lo3, K -
Figure 5. Arrhenius plots of K, and Kd for CuO on alumina.

Table IV. Parameters in Arrheniue Equations for K , and

KA
Kr Kd
~ o - ~ A , , ER, i03A2, ED,
1 1 0 - 4
s-l kJ/mol s-l J/mol
IOlO 15 20 25 30
CuO on alumina 39.3 29.4 2.04 851.5 I / T XIO, K-
bauxite 201.0 38.1 2.95 4142
red mud 0.287 17.7 2.27 50.6 Figure 6. Arrhenius plots of K, and Kd for bauxite.

study for red mud containing 37.69% Fez03. In the latter

study, it is reported that CuO impregnated on alumina has
the saturation capacities ranging between 0.018 and 0.03
kg of SOz/ kg of adsorbent for the temperatures between 5 t +\
473 and 698 K.
The model eq 21 was solved numerically by computer
using a nonlinear regression analysis to calculate the kinetic
parameters K, and Kd. The analysis involved the mini-
mization of IO
IO 15 20 2.5 30
l/TxlO, K-

Figure 7. Arrhenius plots of K, and Kd for red mud.

where f j is the value of C,/C, calculated from eq 21 for
time t j and Fj is the corresponding experimental point.
The method employed in the nonlinear regression analysis
was a combination of Gauss and steepest-descent method
(Marguardt, 1959; Kuester and Mize, 1973).
Arrhenius plots of the rate coefficients K , and Kd are
given in Figures 5-7. From these plots, the values of
activation energies and preexponential factors in the Ar-
rhenius equations K, = Ale-ER/RTand Kd = A2e-ED/RT were
calculated and presented in Table IV.
Quite satisfactory fit of the theoretical breakthrough
curves with the experimental data shows that the model
equation and the kinetic expression give a realistic de-
scription of the process. However, it should be pointed
out that the rate constants determined for bauxite and red
mud are overall values including the contributions of all
the active metal oxides present in these materials.
The slight deviation of the theoretical breakthrough
curves from the data in the early part of the curves is
probably due to overestimation of the mass-transfer re-
sistance which considers bubble interactions. This is ex-
pected because the value of the mass-transfer coefficient
decreases due to bubble interactions, resulting in a higher
mass-transfer resistance. As time proceeds, the active sites
sorb SO,; hence, the rate of reaction decreases and
mass-transfer resistance becomes relatively smaller. This
leads to a better agreement between the experimental and
theoretical breakthrough curves for the longer times.
Conclusion
Sorption of SO2 on CuO impregnated on alumina,
bauxite, and red mud in a fluidized bed showed that these
materials can be considered as potential sorbents for SO,
in the typical range of stack gas temperatures. The study
of the effect of temperature indicated that the efficiency
of the reactor increases as temperature increases. The
kinetic rate expression for sorption of SO2on metal oxides
(Kobda and Dudukovic, 1970; Yates and Best, 1976; Best
and Yates, 1977; Cho and Lee, 1983) was verified to be
satisfactory for sorption of SO2 on CuO as well as mixtures
of metal oxides such as bauxite and red mud by the de-
fining overall apparent rate constant, K,, and overall
consumption coefficient of active sites, K,+ The fluidized
bed model developed by using the two-phase theory of
fluidization is found to represent fluidized bed sorption
process adequately. The results of the semibatch exper-
iments can establish the basis for the design of continuous
fluidized bed processes. The required residence time of
adsorbent particles and thus the flow rate of fresh ad-
sorbent particles in continuous fluidized bed processes can
be determined by using the results of the fluidized sorption

processes carried out in this study. Furthermore, model
suggested in this work can be helpful in adjusting the
design parameters of fluidized beds for the required con-
version or retention of SO2.
Nomenclature
A = area, m2
AI, A2 = preexpbnential factors, l/s
a = interfacial area per bubble volume,
CA = concentration of SO2 in air, moi/m3
CAb= concentration of SO2 in bubble phase, mol/m3
C
, = concentration of SO2 in emulsion phase, mol/m3
C
, = concentration of SO2 at the inlet of the fluidized bed,
moi/m3
,,C = concentration of SO2 at the exit of the fluidized bed,
mol/m3
d b = average bubble diameter, m
ER,ED = activation energies, J/mol
g = gravitational acceleration, m/s2
Hf = height of fluidized bed, m
Hmf= height of bed at minimum fluidization, m
K,, K2 = equilibrium constant, m3/kg
K3 = equilibrium constant, dimensionless
Kd = overall consumption coefficientof active sites to absorb
so29 l/s
K , = overall reaction rate constant, l/s
kbe = overall mass-transfer coefficient between bubble and
emulsion phases, m/s
k,, kd, k:, kd', k,', k2/, k, = reaction rate constants
L = active sites on sorbent for oxygen
MeO* = active site of metal oxide for SO2 sorption
(MeO*) = concentration of active sites
(MeO*)o = initial concentration of active sites
MW = molecular weight
Q = volumetric flow rate, m3/s
rA = reaction rate of SO2, mol/(m3-s)
S = saturation capacity, kg of S02/kg of sorbent
S, = cross-sectional area of the bed, m2
T = temperature, K
t = time, s
U,, = minimum fluidization velocity, m/s
U, = inlet gas velocity to the bed, m/s
Ut = terminal velocity of bubbles
W = weight of sorbent, kg
x = vHf, dimensionless
XR = fractional conversion of active sites to sorb SO2, di-
mensionless
z = distance from the distributor, m
Greek Symbols
a = ( Ubtyf)/ U,!, dimensionless
p = fraction of incoming gas entering bubble phase
Ind. Eng. Chem. Res., Vol. 27, No. 3, 1988 439
v = (kbaQ)/(SUo),m':
6 = fraction of fluidized bed occupied by bubbles, dimen-
sionless
emf = minimum fluidization voidage, dimensionless
pg = density of gas, kg/m3
pp = particle density, kg/m3
Registry NO.SO2,7446-09-5; CuO, 1317-38-0; AlzO3,1344-28-1;
Si02, 7631-86-9; Fe203,1309-37-1; TiOz, 13463-67-7; V205,
1314-
62-1; P206,1314-56-3; CaO, 1305-78-8 Na20, 1313-59-3; bauxite,
1318-16-7.
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Received for review April 23, 1987
Accepted October 28, 1987