Studying the Pelletization of Rosseta Ilmenite ... - doiSerbia

Science of Sintering, 44 (2012) 113-126
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doi: 10.2298/SOS1201113E
UDK
Studying the Pelletization of Rosseta Ilmenite Concentrate With
Coke Breeze Using Molasses and Reduction Kinetics of
Produced Pellets At 800-1150 O C
N.A. El-Hussiny, M.E.H. Shalabi *)
Centeral Metallurgical Research and Development Institute. Cairo, Egypt.
Abstract:
Ilmenite ore fine and coke breeze as reduced material which were pelletized with
different amounts of molasses were studied in this investigation. The produced pellets at
optimum condition were reduced in nitrogen atmosphere at temperature range 800 - 1150 o C
to determine the controlling mechanism. The reduction indicated that the reduction rates
increased as the temperature increased and the controlling mechanism of reaction rate is
solid-solid reaction
Keywords: Ilmenite - reduction kinetic- pelletization, Reduction of ilmenite by coke breeze.
1. Introduction
The reduction of iron titanium concentrate with anthracite as reducing agent was
investigated at temperature 1000-1300 o C. The results indicated that the degree of reduction of
FeO to Fe and TiO 2 to Ti 2 O 3 increased with time and temperature, also the reduction rate is
directly proportional to time at 1000 o C, while at higher temperature the reduction becomes
diffusion controlled [1].
Some investigators [2] studied the reduction of synthetic ilmenite with graphite. It
was found that the reaction has been observed to initiate near 860 o C at the contact points
between the reactants, while up to 1020 o C solid state reduction appears to be the main
reaction mechanism. Above this temperature(1020 o C), it was observed a rate of reaction
increased due to the change of mechanism to gaseous reduction of ilmenite by regenerated
CO.
The reduction kinetics of mixtures of synthetic ilmenite and graphite powder in the
temperature range 980 o C-1100 o C in N 2 and CO 2 atmospheres was studied and the results
observed that the initial rate of reduction was explained in term of solid-solid reaction
between graphite and ilmenite, while in the latter stage of the reduction is gas solid reaction
[3]
When the prepared pellets from mixtures of synthetic ilmenite and graphite were
heated in argon at 1000 to 1100 o C, it was found that no measurable reaction was obtained at
1000 °C but the rate was high at 1100 °C. It was showed that an inflection in the reduction
curve at about 2 pct weight loss at 1050 and 1100 o C was due to the difficulty in nucleating
iron [4].
The carbothermic reduction of Panzhihua ilmenite (FeTiO 3 ) were studied extensively
at temperature ranges from 900 o C to 1400 o C [5]. The results indicated that the reduction
_____________________________
*) Corresponding author: shalabimeh@hotmail.com

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degree of ilmenite increases with increasing temperature and the reaction initiates at 860 o C.
Ilmenite concentrate with graphite were reduced under argon gas at temperature
between 1250 °C and 1350 °C. The results indicated that the reduction of Fe 3+ to Fe 2+ , Fe 2+ to
Fe and Ti 4+ to Ti 3+ took place within 50% reduction during which a secondary oxide phase
was formed and replaced the natural ilmenite. Also, the reduction of Ti 3+ to Ti 2+ took place
after 50% reduction, which altered the composition of the secondary oxide phase by
decreasing its oxygen content. Reduction of Ti 2+ took place while the oxygen deficient
TiO (1−x) phase formed. Formation of any titanium carbide or oxycarbide phases depended on
the completion of the reduction which was not possible at the specified temperatures [6]
The results of experimental data on reduction of ilmenite with char coal in a rotary
reactor showed that the rate controlling steps are solid-solid reaction during initial stages and
diffusion of carbon monoxide through product layer during later stages of reaction. The
activation energies for the two heterogeneous reactions are estimated to be 25 and 35 kcal/
mol for solid-solid and gas-solid reactions, respectively [7].
Some authors [8] indicated that the carbothermic reduction of ilmenite up to 1200 °C
proceed through the formation of a series of oxides (Ti n O 2n−1 ) and iron metal. Also, the
results showed that the metallization percentage reached up to 99% for a period of 6 h at
1200 °C using particle size a 200 mesh (−74 μm).
The reduction of Bama ilmenite concentrate by graphite under argon gas ambient
from 850 to 1400 °C were studied [9]. The results showed that the reduction degree of Bama
ilmenite is enhanced with increasing temperature and the molar ratio of carbon to oxygen, and
that the reaction rate varies with temperature and reduction time simultaneously. The high
content of impurities in Bama ilmenite evidently bates the reduction of ilmenite. Forming the
enrichment zone of manganese prevents complete reduction of Fe 2+ . The reduction products
are mostly reduced iron, rutile, reduced rutiles, Ti 3 O 5 and pseudobrookite solid solution. The
reduction kinetics shows that the reduction temperature is a key factor to control reaction rate.
The reduction of briquettes prepared mixtures of Rossetta ilmenite and coke breeze
in nitrogen atmosphere at 800 – 1200 ºC were studied [10]. The results indicated that the
reduction degree of the ilmenite increased with the increase stoichiometric ratio of carbon
which required converting all FeO & Fe 2 O 3 to Fe and TiO 2 convert to Ti 3 O 5 . The reduction
degree of the briquettes increased with temperature rise. The sample reduced at 1200 ºC
illustrated that the product contain α Fe and Ti 3 O 5 , rutile (TiO 2 ) and pseudobrokite. At 800 ºC
the products formed were ilmenite, rutile, anatase and traces of hematite.
The carbothermal reduction of ilmenite concentrate and graphite pellets was studied
in hydrogen, argon, and helium [11]. Reduction was studied in isothermal and temperatureprogrammed
reduction experiments in a tube reactor with continuously flowing gas. CO, CO 2 ,
and CH 4 contents in the off-gas were measured online using infrared sensors. The main
phases in the ilmenite concentrate were ilmenite and pseudorutile. The reaction started with
the reduction of pseudorutile to ilmenite and titania , followed by the reduction of ilmenite to
metallic iron and titania. Titania was reduced to Ti 3 O 5 and even more to Ti 2 O 3 , which was
converted to titanium oxycarbide. Reduction was faster in hydrogen than in helium and argon,
which was attributed to involvement of hydrogen in the reduction reactions. The formation of
titanium oxycarbide in hydrogen started at 1000 °C and was completed in 300 minutes at
1200 °C, and 30 minutes at 1500 °C. The formation of titanium oxycarbide in argon and
helium started at 1200 °C and was not completed after 300 minutes at 1300 °C.
This work aimed to study the reduction kinetic of Rosseta beach ilmenite concentrate
in the form of pellets with coke breeze in nitrogen atmosphere.

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2. Materials and Experiments
2.1. Materials
2.1.1. Ore Characterization
A representative sample of Rosetta beach ilmenite concentrate was provided by the
black sands project of Nuclear Material Authority (NMA) used for all experiments during this
work. The Rosetta ilmenite concentrate ore contains about 43.6% TiO 2 , 27.5% FeO and
20.9 %Fe 2 O 3 . The size of Rosetta ilmenite ore used in this investigation was less than 0.075
mm.
X- ray analysis of Rosetta ore concentrate (Fig. 1) indicated that the components of
Rosetta ilmenite concentrate are ilmenite FeTiO 3 , pseudorutile Fe 2 Ti 3 O 9 , hematite Fe 2 O 3 and
small quantity of rutile.
Fig. 1. XRD analysis of Rosetta ilmenite ore concentrate
2.1.2. Coke Breeze
The chemical composition of used coke breeze used contain 90.6 % fixed carbon,
1.16% volatile matter, 8.24% ash and 0.75 humidity. The coke breeze fines used in this work
have size less than 0.075 mm.
2.2. Experimental Procedures
2.2.1. Preparation of Sample
Preparation of samples for the briquette process was carried out by mixing of ilmenite
ore concentrate with 1.5 stoichiometric ratio of carbon [10] to convert all FeO & Fe 2 O 3 to Fe
and TiO 2 convert to Ti 3 O 5 according to the following reactions:
FeO + C → Fe + CO (1)
Fe 2 O 3 + 3C → 2Fe + 3CO (2)
3 TiO 2 + C → Ti 3 O 5 + CO (3)

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2.2.2. Production of the Pellets
The pellets were prepared in a disc pelletizer of diameter 400 mm, collar height 100
mm, angle of inclination 52 o , disc rotating speed 17 rpm and residence time 10-30 min. The
200 g of mixture of ilmenite with 1.5 stoichiometric coke breeze as shown in equation 4 were
fed to the pelletizer.
The stoichiometric amount of coke breeze = X(100)/Y (4)
Where X - stoichiometric amount of carbon, Y - Percentage of carbon in coke.)
The predetermined amount of water (9%) with molasses (3-10%), were then sprayed onto the
rolling bed of material in the disc pelletizer. At the end of the tests, a pellet sample was
collected and screened to collect the (7-10 mm diameter) fraction which was taken as a
measure of the productivity of the pellet as shown in equation number 5
P p =W 1 /W 2 * 100 (5)
Where: P p is the productivity of the pellets (7 -10 mm size), %.
W 1 is the weight of the pellets (7 -10 mm size), g
W 2 is the weight of the charge fed to disc pelletizer, g
The produced green pellets were dried in air for three days, to ensure the evaporation
of water used during the pelletization process. The average compressive strength of pellets is
measured by compressing at least 10 pellet samples (7-10 mm diameter) between parallel
steel plates until they break. The mean value for the tested pellets gives their compressive
strength. The dried granules were then subjected to use in sinter mix.
The produced pellets were subjected to mechanical tests (Drop damage resistance test
[12-14] and compressive strength tests [15].
2.2.3. Reduction Procedures
The reduction of produced pellets was done on thermo gravimetric apparatus in
nitrogen atmosphere (A schematic diagram of thermo gravimetric apparatus is shown in Fig.
2. It consisted of a vertical furnace, electronic balance for monitoring the weight change of
reacting sample and temperature controller. The sample was placed in an Alumina crucible
which was suspended under the electronic balance by Ni-Cr wire. The furnace temperature
was raised to the required temperature and maintained constant to ± 5 ºC. Then samples were
placed in hot zone. The weight of the sample was continuously recorded at the end of the run;
the samples were withdrawn from the furnace and kept in the desiccators.
Fig. 2. Schematic diagram of
the apparatus

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The percentage of reduction was calculated according to the following equation
number 6.
Percent of reduction =[ (W o -W t ) (100)(16)/28]/ Oxyge (mass) (6)
Where W o the initial mass of sample after removal of moisture.
W t mass of sample after each time, t.
Oxygen (mass) indicates the mass of oxygen percent in ilmenite ore concentrate in form FeO &
Fe 2 O 3 and oxygen loss due to convert TiO 2 to Ti 3 O 5 .
3. Results and Discussions
3.1. Effect of Molasses Addition on the Properties of Green and Dried Pellets
The effect of using different amount of molasses (2- 10 % molasses), with constant
amount of water (9 %), on the properties of produced green and dried pellets were studied
where the following conditions were kept constant (residence time in the disc pelletizer 10
min, disc rotating speed 17 rpm, inclination angle of disc pelletizer 50°). Figs 3-7 indicated
that as the amount of molasses increases up to 8% the productivity of the produced pellets
increases. This is due to the viscosity of liquid sprayed on the pellets increased with
increasing the amount of molasses.
75
70
Productivity percentage
65
60
55
50
45
40
0 2 4 6 8 10 12
%, of molasses added
Fig.3. Effect of changing molasses percentage on the productivity percentage of green pellets.
The increase of molasses from 8 to 10% the productivity of the pellets decreased, this
may be due to the sticky of pellets together and formation of large pellets having size more
than 10 mm.

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4.5
4
drop damage resistance.
3.5
3
2.5
2
1.5
1
0 2 4 6 8 10
%, of molasses added.
Fig. 4. Effect of changing molasses percentage on the drop damage of the green pellets (10
min. pelletization time.
Also it is clear that increasing the percentage of molasses increases the drop damage
resistance and compressive strength of the green and dried pellets as shown in Figs 4-7. This
may be attributed to the fact that increasing molasses addition leads to an increase in the
contact points between the particles of the ilmenite and coke breeze and a decrease in the
distance between them [16].
255
245
Crushing strength, g/pellet.
235
225
215
205
195
185
0 2 4 6 8 10
%, of molasses added.
Fig. 5. Effect of changing molasses percentage on the crushing strength of the green pellets
(10 min. pelletization time).

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120
100
drop damage resistance.
80
60
40
20
drop no
0
0 2 4 6 8 10
%, of molasses added.
Fig. 6. Effect of changing molasses percentage on the drop damage resistance of the dry
pellets after 3 days (10 min. pelletization time).
650
600
Crushing strength, g /pellet.
550
500
450
400
350
300
0 2 4 6 8 10
%, of molasses added.
Fig. 7. Effect of changing molasses percentage on the drop damage resistance of the dry
pellets after 3 days (10 min. pelletization time).
3.2. Effect of Time of Pelletization on the Properties of Green and Dried Pellets
The effect of time of pelletization (5-25 min.), on the properties of produced green
and dried pellets, were studied where the following conditions were kept constant (the amount
of molasses=8% with 9% water, disc rotating speed 17 rpm, inclination angle of disc
pelletizer 50°). Results illustrated in Figs. 8-12, Fig. 8 indicated that as the residence time of

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pelletization increase to 20 min the productivity of the produced pellets increases to
maximum value. The decrease in productivity at time more than 20 min may be due to the
flushing away of some water during their growth. [12,17].
90
85
Productivity percentage
80
75
70
65
60
55
0 5 10 15 20 25 30
Time of pelletization,min.
Fig. 8. Effect of changing the time of pelletization on the productivity percentage of green
pellets, (8% molasses added).
Fig. 9 indicated that as increasing the time of pelletization more than 15 min. the
drop damage resistance decreased this fact may be the flashing amount of water during the
growth of pellets [18].
6.5
8% molasses added
6
Drop damage resistance.
5.5
5
4.5
4
3.5
0 5 10 15 20 25
Time of pelletization, min.
Fig. 9. Effect of change the time of pelletization on the drop damage resistance of green
pellets

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Fig. 10 illustrated as the time of pelletization increase the crushing strength of
produced green pellets increased.
Figs. 11 and 12 shows the effect of time of pelletization on the drop damage
resistance and crushing strength of the dried pellets, from which it is clear that the damage
resistance approximately constant and = 100 as the time of pelletization increased, while the
compressive resistance of dried pellets increased as the time of pelletization increased.
400
8% molasses added
Crushing strength, g /pellet.
350
300
250
200
0 5 10 15 20 25
Time of pelletization, min.
Fig. 10. Effect of change the time of pelletization on the crushing strength of green pellets.
150
8 % molasses
Drop damage resistance.
100
50
0 5 10 15 20 25
Time of pelletization, min.
Fig. 11. Effect of change the time of pelletization on the drop damage resistance of dry
pellets for 3 days.

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800
750
8 % molasses.
Crushing strength,g /pellet.
700
650
600
550
500
450
0 5 10 15 20 25
Time of pelletization,min.
Fig. 12. Effect of change the time of pelletization on the crushing strength of dry pellets for 3
days
3.2.2. Effect of Temperature on the Reduction Degree
Experiments were performed in the temperatures ranges of 800 to 1150 ºC. Plots of
the reduction percentage of ilmenite by coke breeze as a function of time are shown in Fig.
13. It is clear that the reduction rates increased with increasing temperature. At high reduction
temperatures (more than 1000 ºC), with increasing temperature, the oxygen removal
increased. Also, it is clear that the reduction rates was faster in the first period and then
decreased at the end of period.
120
100
800 0C
900 0C
1000 0C
1100 0C
1150 0C
Reduction percentage, %.
80
60
40
20
0
0 20 40 60 80 100
Time of reduction,min.
Fig. 13. The relation between the time of reduction and reduction percentage for pellets
containing 8% molasses after drying for 3 days.

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3.2.3. Kinetics of Reduction of Ilmenite Ore
Applied model of solid-solid reaction as shown in equation number 4[19], on the
reduction of ilmenite ore concentrate.
[1-(1-R) 0.333 ] 2 = kt (7)
Where R is fractional reduction
t- is time mint and k is rate constant.
The results showed that this model gave straight line for all temperature as shown in Fig. 14.
1
0.9
0.8
800 0C
900 0C
1000 0C
1100 0C
1150 0C
0.7
(1-(1-R)^0.333)^2
0.6
0.5
0.4
0.3
0.2
0.1
0
0 20 40 60 80 100
Time of reduction,min.
Fig. 14. The relation between time of reduction, min. and [1-(1-R) 0.333 ] 2 for ilmenite pellets
containing 8% molasses.
0
-1
-2
Ln K
-3
-4
-5
-6
-7
-8
-9
6.5 7 7.5 8 8.5 9 9.5
1/T * 10^-4
Fig. 15. Relationship between ln k and 1/T for pellets containing 8% molasses and drying for
3 days.
The slope of these straight lines gave the constant rate for each reduction temperature.

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The logarithms (ln) of these constants were used to calculate the activation energies
(Fig. 15). From the slope of this straight line, it was found that the activation energy of this
reaction ≈ 159.4837 Kj /mole. This value corresponds solid diffusion control.
3.5.3 X-Ray Diffraction of the Reduction by Carbon
X- ray diffraction of the reduction of Ilmenite pellets with carbon using molasses as
binder material at 800°C, illustrated in Fig. (16). From which it is clear that the main phases
are psedorutile, pseudobrookite, rutile, small amount of iron and ilmenite. This may be due to
pseudorutile decomposes to pseudobrookite and rutile
Fe 2 Ti 3 O 2 → Fe 2 TiO 5 + 2 TiO 2
And hematite Fe 2 O 3 reduce by carbon formed CO and iron
Fe 2 O 3 + 3C → 2 Fe + 3 CO
And then Ilmenite is then reformed by recombination reduction process involving rutile.
Fe 2 TiO 5 + TiO 2 + CO → 2 FeTiO 3 + CO 2
X-ray diffraction of the reduction of ilmenite with carbon, using molasses as a binder at 100-
1100°C, is illustrated in Fig. (16), it is clear that the main phases are pseudobrookite, rutile
and iron. This may be due to Fe 2 O 3 reduced to Fe and CO according to the following reaction
Fe 2 O 3 +3 C → 2 Fe + 3CO
And pseudorutile is decomposes to pseudobrookite and rutile.
Fe 2 Ti 3 O 9 → Fe 2 TiO 5 + 2 TiO 2
Also these results are consistent with the reaction of Ilmenite to metallic iron and rutile
according to the general mechanism [20]
FeTiO 3 + CO → Fe + TiO 2 + CO 2
1150 0C c
a = pseudorutile
b = rutile
e = pseudobrokite
d e b d b
e
e e d d b
e e e e
e b
b
e
c = iron
d = ilmenite
e
1100 0C
d
c
e b
e
b
e
1000 0C
b
e
c
e
e
e
d
d
e
b b
d
d e
d e
b
d d
b e e d e
e
b
800 0C
a
d
b
a
d
be
b a
c
d
d a
b a b b
a
a d
b d
30
40
50
60
70
2Q
Fig. 16. X-ray diffraction of the reduced ilmenite with coke breeze pellets at different
temperature.

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4. Conclusions
1. The amount of molasses added to the mixture of ilmenite and coke breeze during the
pelletization played a very important role on the quality of the green and dried
pellets. The productivity of green pellets -10+7 mm increased as the amount of
molasses increased up to 8 %.
2. As the time of pelletization increase to certain time the quality of the produced
pellets improved.
3. The reduction rates increased with increasing temperature.
4. The activation energy of the carbothermic process of the pellets of ilmenite and coke
breeze using molasses as a binder in nitrogen atmosphere ≈ 159.4837 kJ /mole .
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16. B.K. Dhup .and S. Sarkar , TISCO, 17 , 4, (1970) 139-143.
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Садржај: Различити молски односи руде илменита (гвожђе и титанијум) и кокса као
редукционог средства су испресовани и изучавани у овом раду. Испресци добијени под
оптималним условима су редуковани у атмосфери азота у температурском интервалу
800 – 1150 o C да би се одредио контролни механизам. Резултати указују на то да
брзина редукције расте са порастом температуре и да је контролни механизам
реакције, реакција у чврстој фази.
Кључне речи: Илменит – кинетика редукције- испресци, редукција илменита коксом.