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Abstract
To recover heavy minerals from the Athabasca oil sands tailings, a roasting step is necessary to burn off the residual bitumen.
However, most of the previous researchers, using a roasting step, did not seem to be able to separate the Fe-bearing titanium
minerals (ilmenite and leucoxene) from the Fe-free titanium minerals (rutile and anatase). An investigation was therefore carried out
to study the changes in magnetic properties after roasting to the types of minerals contained in the oil sands tailings. Ilmenite,
hematite, and a rutile concentrate (LR Rutile) produced from the oil sands tailings (containing mainly leucoxene and rutile), were
used in the study. It was observed that the magnetic susceptibility of ilmenite increased after either oxidation or reduction roasting at
some intermediate temperatures and roasting time. For hematite, reduction roasting increased its magnetic susceptibility and oxi-
dation roasting did not seem to have any effect. Reduction roasting of the LR Rutile resulted in an increase in its magnetic sus-
ceptibility, and this increase was mainly due to the contaminating Fe-bearing minerals (leucoxene). Upgrading of the LR Rutile was
possible either by using low intensity magnetic separation following reduction roasting, or by using high intensity magnetic sepa-
ration directly.
Ó 2002 Elsevier Science Ltd. All rights reserved.
Keywords: Oil sands (A); Tailings (A); Magnetic separation (B); Roasting (C)
2. Experimental 1.9 A. The transverse slope ðhÞ of the separator was set
at 14.5°. The magnetic susceptibility v of a material
2.1. Materials tested in the Frantz Isodynamic Separator is expressed
as (McAndrew, 1957):
Ilmenite (TiO2 FeO) and hematite (Fe2 O3 ) minerals sin h
were used in the tests, together with a rutile concentrate v¼
KI 2
produced previously from the oil sands tailings by
Lakefield Research Ltd. The latter will be referred to as where K is a constant and I is the electric current that
LR Rutile in this paper. The ilmenite and hematite, results in a 50%:50% split of the test sample at the exit
originating from St. Urbain, Quebec (Canada) and Hoyt chute of the separator. K was found to be 3:15 106
Lake, Michigan (USA), respectively, were purchased when using ferrous ammonium sulfate, Fe(NH4 )2 -
from WardÕs Natural Sciences Ltd. Lumps of the (SO4 )2 6H2 O (v ¼ 32:4 106 m3 /kg), and copper
ilmenite and hematite were crushed with a laboratory sulfate, CuSO2 5H2 O (v ¼ 5:88 106 m3 /kg), as stan-
jaw crusher, followed by a Brinkmann pulverizer. The dards to calibrate the separator. To measure the mag-
180 þ 74 lm size fractions were screened out for the netic susceptibility of a sample, the sample powder was
roasting tests. X-ray diffraction spectra of the ilmenite separated in the Frantz Isodynamic Separator at diffe-
and hematite showed that these were high purity mine- rent applied electric currents. The recovery of the mag-
rals. The LR Rutile, on the other hand, assayed 75.5% netic fraction was then plotted against the applied
TiO2 , 18.7% Fe2 O3 , 1.03% Al2 O3 , and 1.94% SiO2 . A current, from which the current corresponding to 50%
mineralogical analysis indicated that it contained about recovery was found. This was then used to calculate the
10–17% rutile (anatase), and the remaining titanium was magnetic susceptibility v using the above equation.
in the form of leucoxene (xFe2 O3 yTiO2 ). The LR Ru-
tile was used directly without size treatment since its 3. Results and discussion
dominant particle size was about 120 lm, and its 80%
passing size was 145 lm. 3.1. Effect of roasting on the magnetic properties of
Charcoal was used as a reducing agent in the reduc- ilmenite
tion roasting tests. This was an Antelope Ranch char-
coal supplied by The Weight Products Co. The charcoal Most of the ilmenite roasting studies reported in the
was screened and the 850 þ 250 lm size fraction was literature were carried out under a reducing atmosphere
used. The use of coarse sized charcoal provided a simple and in the temperature range of 800–1400 °C. Nell
indicator for the maintenance of a reducing environment (2000) recently gave an overview of the phase chemistry
during roasting since the un-reacted charcoal could be in the production of high-titanium slag from ilmenite
screened out. using reduction roasting. The roasting temperatures
were mostly above 800 °C. El-Guindy and Davenport
2.2. Procedures (1970) studied the kinetics and the mechanisms of
ilmenite reduction with graphite in the temperature
The roasting tests were performed in a laboratory range up to 1400 °C. They observed that reactions were
muffle furnace. The furnace was heated to a predeter- initiated near 860 °C at the contact points between the
mined temperature before the samples were introduced. reactants. Up to 1020 °C, solid state reduction appeared
A ceramic crucible, measuring 7.6 cm in diameter and to be the main reaction mechanism, and above this
9.0 cm in depth, was used. Oxidation roasting was temperature the reaction mechanism was gaseous re-
conducted in the crucible open to air. Reduction roast- duction of ilmenite by regenerated CO. Grey and Reid
ing was performed by heating a blend of 1 g charcoal (1974) studied the reaction sequences in the reduction of
and 5 g mineral (i.e., a weight ratio of 1:5). This ratio ilmenite above 1000 °C. Pre-oxidation of ilmenite at
was used in most of the reduction roasting tests, al- about 1000 °C leads to the formation of rutile plus a
though a ratio of 1:10 was also used in some tests. The Fe2 TiO5 –FeTi2 O5 –Mn2 TiO5 solid solution. The final
mineral and charcoal mixture was placed at the bottom reduction product consists of a mixture of metallic iron,
of the crucible and was covered by a small ceramic reduced rutile and a Fe2 TiO5 –FeTi2 O2 –Ti3 O5 solid so-
hemisphere. The crucible was not completely sealed. lution. El-Tawil et al. (1996) reported the reduction
The magnetic susceptibilities of the samples were roasting of ilmenite ore with carbon in the presence of
measured with a Frantz Isodynamic Separator. The sodium carbonate between 1000 and 1200 °C. They
electric current in the magnetizing coil of the separator observed that the addition of sodium carbonate of up to
could be adjusted from 0 to 1.9 A. The magnetic field 30 wt.% of the ore enhanced the reduction efficiency.
strength of the separator was measured with a DC The maximum metallization of iron obtained at 1200 °C
Magnetometer (supplied by AlphaLab Inc.) and the was about 85%, while the rest of the iron existed in the
maximum was found to be 1.2 T at the current setting of form of sodium iron titanate.
Z. Cui et al. / Minerals Engineering 15 (2002) 1121–1129 1123
the high dosage it did not (Fig. 11). This seemed to in-
dicate that at the low dosage, the charcoal may have
been completely consumed after prolonged heating and
the partially reduced hematite started to re-oxidize. In
fact, during the tests, it was observed that there was no
charcoal left after more than 30 min of heating at the
low charcoal dosage of 1:10.
Figs. 12 and 13 show the magnetic susceptibility of
hematite as a function of roasting temperature. They
again indicate that the lower limit of temperature was
about 500 °C. X-ray diffraction analysis of the reduced
Fig. 11. Comparison of reduction roasting of hematite at different hematite shows that some of the hematite phases have
charcoal dosages. Charcoal and hematite were blended at a ratio of been changed into maghemite (c-Fe2 O3 ), resulting in
either 1:5 or 1:10. significant increase in magnetic susceptibility. In fact,
Fig. 14 shows that there is a good correlation between
the magnetic susceptibility of the roasted hematite and
the magnetic susceptibility of the hematite started to the peak intensity ratio corresponding to maghemite and
drop after a long heating at the low dosage, whereas at hematite.
Z. Cui et al. / Minerals Engineering 15 (2002) 1121–1129 1127
Table 1
Magnetic susceptibility of the LR Rutile
Treatment Condition Magnetic susceptibility 106 m3 /kg
After treatment After separation at 0.4 T
Magnetic fraction Non-magnetic fraction
Original sample 0.46 0.66 0.05
Oxidation roasting 800 °C, 30 min 0.13 0.16 0.03
Reduction roasting 800 °C, 30 min, charcoal:rutile ¼ 1:10 0.58 1.15 0.05
1128 Z. Cui et al. / Minerals Engineering 15 (2002) 1121–1129
4. Conclusions
Acknowledgements
The magnetic properties and the magnetic separation
behavior of ilmenite, hematite and a rutile sample (LR The authors are grateful to the financial support
Rutile) produced from Athabasca oil sands tailings were provided to this project by the Alberta Energy Research
studied and the following conclusions can be drawn: Institute and by Syncrude Canada Ltd. We also appre-
ciate the valuable advice from and discussions with Mr.
1. Oxidation roasting increased the magnetic suscepti- John Oxenford and Mr. Julian Coward during the
bility of ilmenite within the temperature range of course of this project.
500–1000 °C. Below 500 °C, the magnetic suscepti-
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