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ABSTRACT
Doheim, M.A., Tarshan, M.M. and E1-Gendy, M.M., 1978. Fluidized-bed thermal treat-
ment of phosphate rock: effect of operating variables. Int. J. Miner. Process., 5:183---19'7
The presence of huge amounts of low- and intermediate-grade phosphate ore and the
need for high-grade ore for industry, necessitates the availability of economic and effi-
cient upgrading techniques. The fluidized-bed technique is most suitable for upgrading,
by thermal treatment, of ores having high percentages of organic matter, carbonates,
and moisture. In this work, studies were carried out on the process of thermal upgrading
of phosphate rock in a fluidized-bed furnace of 10-cm diameter. The studies involve the
effect of the important operating variables such as process temperature, air-flow rate,
calcine quenching temperature, and the attrition of phosphate particles. A run-of-mine
intermediate-grade phosphate ore was used. Batch and continuous runs were carried out
and the ore was calcined and washed.
It was found that the increase in process temperature favourably affects the % up-
grading of the ore, but this should be studied in close connection with the economic
aspects, especially in the case of ores with low carbonaceous matter contents. The fluid-
izing air-flow rate, and thus, the hydrodynamic condition of the bed, slightly affects the
upgrading process. The use of high air-flow rates increases the extent of attrition of phos-
phate particles. The quenching temperature of the calcine was found to have no effect on
the process product, within the range investigated.
INTRODUCTION
and it involves the removal of physically and chemically bound water, organic
matter, and easily volatilized substances. The calcining process is usually
carried out at a higher temperature so that the carbonates in the phosphate
are decomposed. The phosphate after roasting is more liable to flotation,
whereas after calcination, with formation of Ca and Mg oxides, the pH of
the pulp would be too high for flotation. Poor phosphate rock, having high
percentages of carbonaceous materials (organic carbon), calcareous materials
(calcite, dolomite), and moisture, is best thermally treated in fluidized-bed
furnaces. This treatment, at the calcination temperature, is sufficient for
highly upgrading the ore, especially low-silica ores. Fluidized-bed calcining is
also used to defluorinate phosphate rock at a temperature of about 1300°C
to make it suitable for animal feed.
The present work is concerned with the thermal treatment of an intermedi-
ate-grade phosphate ore in a fluidized-bed furnace. The intermediate-grade
ore is intended to be processed at intermediate conditions so that the data
obtained can be more representative. The study involves the effect of the
important operating variables such as process temperature, air-flow rate, and
the calcine quenching temperature on the process. The effect of air-flow
rate on the phosphate attrition was also studied. Batch and continuous runs
were carried out.
PREVIOUS WORK
the phosphatic beds, which may amount to 3.5%, interfere with the produc-
tion of triple superphosphate and they are now successfully removed by
roasting in fluidized beds at temperatures below 760°C (Priestly, 1967). A
5-m diameter three-compartment Fluosolids reactor is used. This percentage
of carbonaceous material furnishes most of the fuel required for the process.
Batch and continuous-circuit beneficiation of western phosphate ore has
been reported (Town et al., 1967). Two flow sheets were developed; the
first involved roasting, attrition scrubbing, sizing to remove a concentrate,
grinding of the oversize, desliming, and flotation; in the other flow sheet
the roasting step was eliminated. Roasting was carried out in fluidized beds.
Fluidized-bed roasting of phosphate rock at 700 ° C to obtain A1 and Fe phos-
phate has been reported (Anonymous, 1966). Calcining of phosphate ores
in a fluidized bed at higher temperatures than 760°C converts the carbonates
to oxides which can be leached out in a washing process (Priestly, 1967).
Studies on the upgrading of the carbonaceous Nile Valley phosphate by cal-
cination of the calcitic samples have been reported by Orphy et al. (1969}.
At the Eleventh International Mineral Processing Congress (Seminar..., 1975)
several authors tackled the beneficiation problems of calcareous phosphate
ores using flotation, leaching, and calcination. No concern was given to the
fluidized phosphate particle attrition and its consequent effect on bed behav-
iour and process performance.
The present study provides data on the important operating variables of
the thermal treatment process for upgrading the phosphate rock, particular-
ly on the attrition behaviour of the fluidized phosphate particles. These
data should be useful and essential in designing and operating larger-scale
units.
EXPERIMENTAL
Materials
TABLE I
Component Weight%
CasP20 s 45.93
Carbonates 30.34
Insolubles 11.24
Oxides 2.29
Chlorides 0.70
Sulphates 1.96
Moisture 1.83
TABLE II
Umf values for phosphate rock at room temperature
--8 mesh phosphate ore and the Umf values are given in Table iI. The Vmf
values at higher temperatures were obtained from the values at room tem-
peratures through the use of a factor accounting for the change in air vis-
cosity (Singh et al., 1973). Air was used as the fluidizing gas.
Apparatus
Procedure
The work reported in this paper involves batch and continuous runs. In
batch runs a weighed charge of about 1 kg was dropped slowly into the fur-
187
I-Control valve •
2_Pressure gouge.
3_Silica gel dryer To cyclone and exhaust
4-Flow meter. =,
5- Water manometer. I
6_Chromet /Alumel ti'lermocouple. (
7- InsuLation.
8_ Furnace
9.Fluidized bed o.f phosphate rock. J
lO_Expanded sect,on k tO /~
1 l_ Distributor . I\ / I
..... \ / J
A)!up
Fig.1. Sketch showing the apparatus for thethermal treatment of ores.
naee, after which the furnace was switched on and regulated to the required
temperature level. While heating, air flow was allowed into the phosphate
bed at about the minimum fluidization rate. This assists in speeding up the
heating process and in uniformly heating the bed. After attaining the re-
quired temperature, the run was carried out at the specified conditions. The
calcined charge was left to cool inside the closed reactor. A sample was taken
for analysis and the calcine underwent a washing process for slaking and
washing out the oxides formed from carbonate decomposition. The washing
process was carried out manually. The calcine was stirred with water, left to
settle, and then the solution was decanted. A sample from the washed cal-
cine was analysed for its P2Os content.
During the continuous operation of the calcining furnace, a belt ore feeder
was used with its hopper loaded with --8 mesh phosphate rock. The dis-
charge gate was adjusted in accordance with the feed to give the required
188
solids flow rate. After reaching steady-state conditions, the calcined ore was
quenched in water at high temperature, and samples were taken for deter-
mining the P2Os c o n t e n t of the initial, calcined, and washed ores.
A volumetric m e t h o d (Vogel, 1961; E1-Shahat, 1964) was used for the
determination of the P205 c o n t e n t of the phosphate ore samples.
Effect of temperature
In studying the effect of temperature, a --8 mesh ore was used with a bed
weight of ab o u t 1 kg giving an H/D ratio of a b o u t 2.0 for the static bed (H=
height o f bed, D = diameter of bed}. The duration of the thermal t r e a t m e n t
was ab o u t 15 minutes at the different temperatures of 500, 600, 700, 800
and 900°C. The runs at 500, 600, and 700°C m ay be considered as roasting
and those at 800 and 900°C as mainly calcining. The results are given in
TABLE III
Table III. As can be seen, the P2Os content of the phosphate ore increased
from about 20 to 30%. The washing step in order to slake and remove the
oxides formed from carbonates decomposition, was most effective at 800°C.
The increase in P2Os content (A P205) was plotted against temperature, as
shown in Fig.2.
7.5
7.0
6,5
O~ 6.0 G
<3
D
5.5
Uf / Umf = 2
5.0
4.5
Z,.O
5'00 6'00 700 8'o0 '
9O0
Temperature °C
Fig. 2. Effect of process temperature on the thermal upgrading of phosphate ores.
The --8 mesh phosphate rock was calcined at different flow rates corre-
sponding to Uf/Umf values of 1, 2, 4, 6, and 8, (Uf = fluidizing-gas velocity)
at a process temperature of a b o u t 800 ° C and H/D of about 2. The results
are given in Table IV. It can be noticed that the P:Os content of the phos-
phate increased from 20 to about 30%, in some runs, by thermal treatment
and washing. A metallurigcal balance of some runs at different flow rates is
given in Table VII. The data in the table indicates that the P2Os content of
the elutriated fines is much less than the initial phosphate, indicating that
elutriation of fines contributes to the upgrading process. The effect of flow
rate can best be shown by plotting AP2Os against Uf/Umf a s given in Fig.3.
It can be seen that there is only a slight improvement in the P2Os content
of the calcine. This may probably be due to the particle/particle interaction
which causes attrition and size degradation of the fluidized phosphate. The
extent of this effect increases with flow-rate increase. This effect improves
the degree of liberation and makes the thermal-treatment process more effi-
cient.
Besides particle/particle interaction, the flow-rate increase affects, par-
ticularly, the heat-transfer characteristics of the bed. The increase in flow
rate increases the mixing of solids (Baeyens and Geldart, 1974) and this
improves heat transfer and leads to temperature uniformity throughout the
T A B L E IV
T h e r m a l t r e a t m e n t o f p h o s p h a t e r o c k a t d i f f e r e n t flow rates at 8 0 0 ° C
Vf UflUmf Assay p e r c e n t
(l/rain.)
P20s corresponding
Ca3PiOs
20 1.02 1 9 . 9 0 .1 43.44
25.11 *= 54.81
2 6 . 2 4 *3 57.30
40 2.02 19.90 43.44
25.89 56.52
29.05 63.41
80 4.08 19.90 43.44
26.59 57.87
26.71 58.29
120 6.12 19.90 43.44
26.82 58.55
26.82 58.55
160 8.16 19.90 43.44
26.65 58.17
26.82 58.54
7C
6,5 ¸
v
L~ 6 . 0 o
0
<7
o
5.5
• = - 8 mesh
5.0
4,5 I I I I I I I I
1.0 2 3 a 5 6 7 8
Uf / Umf
bed. This is very important in the present case where the endothermic reac-
tion of CaCO3 decomposition is involved in the thermal-treatment process.
The washing process was effective up to a certain flow rate as shown in
Table IV. At high flow rates it becomes ineffective; this may be attributed
to the formation of appreciable amounts of phosphate fines. These fines are
washed away, during the washing process, due to the inefficiency of decan-
tation.
TABLE V
Coarse and fine fractions of treated phosphate rock at different flow rates and different
size cuts
T h e e f f e c t o f q u e n c h i n g t e m p e r a t u r e was s t u d i e d during t h e c o n t i n u o u s
o p e r a t i o n o f the calcining furnace. T h e q u e n c h i n g o f the calcined p h o s p h a t e
in w a t e r c o n v e r t s t h e c a l c i u m a n d m a g n e s i u m oxides, f o r m e d f r o m carbo-
193
15
;totes °'
Uf /Umf
=4
=6
m values of =8
0J
10
Y:
ol
I
2.6 2.4 21.2 2'0 1.8 1.6 1'.4 1',2 110 0.'8 0.16 0.~4 O.2
p a r t i c l e size , m m
Fig.4. E f f e c t o f gas f l o w o n t h e a t t r i t i o n o f p h o s p h a t e r o c k (--4 mesh).
Design considerations
15 v 1 Processed = 2
a I ores at =4
x / U f l Umf =6
Jvalues of =8
c
u
10
2_
[ I l L
2.6 214 212 210 II+8 I]6 11.4 1.2 1,0 O,B 01.6 0L4 0*.2
pclrticle s i z e , mm
Fig.5. Effect o f gas f l o w on the attrition of phosphate rock (--6 mesh).
T A B L E VI
Metallurgical balance of s o m e r u n s *a d u r i n g p h o s p h a t e r o c k c a l c i n a t i o n
2 *~ 4 6 8 2 4 6 8 2 4 6 8 2 4 6 8
Non-Calcined 930 930 930 930 100 100 100 100 19.9 19.9 19.9 19.9 100 100 100 100
ore
Calcined ore 645 637 638 562 69.35 68.49 68.78 60.43 25.89 26159 26.82 26.65 98.36 98.24 97.75 96.89
Elutriated 18 20 24 31 1.94 2.15 2.58 3.33 15.4 15.2 15.3 15.6 1.64 1.76 2.25 3.11
ore
Unaccounted 267 273 268 337 28.71 29.36 28.64 36.24 . . . .
lo~m*3
100.00 100.00 100.00 100.00 100.00 100.00 100.00 100.00
cD
c~
196
fluidized-bed systems, there are many problems which include: gas distribu-
tor plates, solid transfer system from a bed to a lower one, and the working
stability (Lago et al., 1967). A design procedure for multi-stage systems of
industrial application is given by Toei and Akao (1968). Their fluidized-bed
apparatus is characterised by having perforated plates instead of the conven-
tional overflow pipes (down-comers). Improved stability is expected with
the system having perforated plates.
CONCLUSIONS
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