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Powder Technology 374 (2020) 190–200

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Powder Technology

journal homepage: www.elsevier.com/locate/powtec

Pelletization of synthesized magnetite concentrate obtained


by magnetization roasting of Indian low-grade BHQ iron ore
Sachida Nanda Sahu a,b,⁎, Prasanta Kumar Baskey a, Santosh Deb Barma a, Soumya Sahoo a,
B.C. Meikap b, Surendra Kumar Biswal a
a
CSIR- Institute of Minerals and Materials Technology, Bhubaneswar, Odisha 751013, India
b
Indian Institute of Technology, Kharagpur, West Bengal 721302, India

a r t i c l e i n f o a b s t r a c t

Article history: In India, the use of iron ore pellets in the blast furnace, electric arc furnace, or sponge iron production is contin-
Received 21 April 2020 uously optimized, considering different aspects of the production chain from the run of mining (ROM) to metallic
Received in revised form 16 June 2020 iron depending upon the industrial need and ore availability (recent aggressive iron ore mining auction 2020 in
Accepted 1 July 2020
India). The scarcity of high-grade iron ore resource and availability of the considerable quantity of low-grade iron
Available online 7 July 2020
ore fines, banded hematite quartzite (BHQ) ore in mines (mostly in Bihar, Odisha, Madhya Pradesh, and Karna-
Keywords:
taka), has to lead the way to beneficiate and utilize the concentrate as pellet feed for the steelmaking process.
Low-grade iron ore Banded iron ore such as BHQ is one of the potential resources of iron having a total iron content, i.e., Fe (T) of
Banded hematite quartzite 35–48 wt%, which is lying unutilized in most of the Indian iron ore mines. The challenge before the policymakers
Magnetization roasting and researchers is to think of a sustainable process technology to utilize these iron ore resources wisely. The con-
Pelletization ventional beneficiation of this type of siliceous BHQ iron ore resource having low iron content is not advisable.
Induration Therefore, pelletization of synthesized magnetite concentrate obtained from the magnetization roasting of
BHQ emerged as an alternative energy-saving and ore conserving process that may be scaled up and commercial-
ized for low-grade banded iron ores. The pelletization of magnetite concentrate is an independent heat hardening
process; thereby requirement of anthracite coal fines as a fossil fuel additive to maintain the temperature gradi-
ent from core to the periphery of the pellet can be avoided. Physical properties such as cold crushing strength
(CCS) and porosity of the pellets were optimized to study their suitability in the steelmaking process. In this re-
gard, characterization studies of the pellets were performed using X-ray diffraction (XRD), scanning electron mi-
croscope (SEM), optical microscope, and X-ray micro-computed tomography to understand the microstructural
properties of the pellets. The CCS of 255.8 kg/pellet and porosity of 25.42% were achieved at the optimized indu-
ration temperature and residence time of 1250 °C (50 °C to 80 °C less than conventional hematite pellet indura-
tion) and 10 min, respectively. The properties studied are encouraging and comparable with the pellet prepared
from the natural magnetite/hematite ore.
© 2020 Elsevier B.V. All rights reserved.

1. Introduction iron and steel industries if appropriately processed [2]. BHQ iron ore is
presumed to be a sedimentary rock either formed through a chemical
According to the Ministry of Steel Policy 2017 declared by the Indian or biochemical precipitate of Precambrian origin, consisting of
government, the requirement of low-grade iron ore is about 800 million interchanged iron-rich and iron-poor (amorphous silica-rich) layers
tons for the production of 300 million tons of steel by 2030 [1]. To meet [3]. In the Indian context, BHQ iron ore typically consists of around
this targeted steel demand, shifting the focus towards the utilization of 35–48 wt% of total iron content, i.e., Fe (T) alongside 40–45 wt% of
banded iron ore such as banded hematite quartzite (BHQ) is very crucial SiO2, and 0.5–2.5 wt% of Al2O3 [4]. Due to the complex nature and low
rather than depending on the high-grade ores which are on the verge of Fe content of BHQ, the separation of iron values from gangue impurities
depletion. BHQ iron ore resources are considered as a waste resource in using conventional physical processes is very challenging. For instance,
many parts of the world, especially in India. In a situation where the one of the significant challenges is to recover the iron values because of
availability of high-grade calibrated iron ore is insufficient, BHQ iron their liberation at a lower size fraction. To achieve the desired separa-
ore could act as an alternative and a potential raw material to many tion of iron values, converting hematite phase (available in BHQ) to
magnetite phase by the reduction-roasting process followed by the sep-
⁎ Corresponding author. aration of magnetic concentrates from roasted BHQ using low-intensity
E-mail address: [email protected] (S.N. Sahu). magnetic separator is one of the best ways for maximizing the iron

https://doi.org/10.1016/j.powtec.2020.07.004
0032-5910/© 2020 Elsevier B.V. All rights reserved.
S.N. Sahu et al. / Powder Technology 374 (2020) 190–200 191

recovery [2]. The so-obtained synthesized magnetic concentrates can induration. Fourier transform infrared spectroscopy (FTIR) was
then be used for the preparation of magnetite-based pellets using the employed to study the pellet characteristics, and the FeO% from the
pelletization technique. In general, pelletization of iron ore is a process core to the periphery of the pellet was determined. It was observed
where the feed is a mixture of high-grade hematite/magnetite ore that the core of the pellet is high in FeO% than that of the periphery. It
mixed with binder and coke breeze as additives to form pellets for the was due to the oxidation rate, which decreases with an increase in tem-
production of iron and steel [5]. Such types of initiatives can eradicate perature because of the decomposition of the MHA binder [16].
the crises of high-grade iron ore demand as pellet feed material as All over the world, pelletization (a form of agglomeration of iron ore
well as support the utilization of low-grade banded iron ores to meet fines) studies of both hematite and magnetite iron ore were mostly con-
the targeted steel production in the forthcoming years. ducted using either high-grade ore from the mines or the beneficiated
In recent years, studies based on the reduction-roasting of low-grade concentrate from the processing plants. To evaluate the quality of indu-
iron ore followed by the magnetic separation for the production of the rated pellet for its end use in the iron-making process, characterization
desired grade of magnetite concentrate for making pellets is a hot such as CCS, microscopic analysis, and mineralogical phase change are
topic [6]. Different researchers have studied the reduction-roasting pro- the essential factors. For example, the increase in the porosity of the in-
cess and reported that it requires above 600 °C temperature to convert durated pellet beyond specific value decreases the CCS of the pellet,
the low-grade iron ore from weakly magnetic minerals to magnetic which can cause more production of fines during transportation and
minerals in a reduced atmosphere at elevated temperature [7–10]. screening, and hence, not suitable in the subsequent process. Some-
However, controlling the temperature parameter plays an important times, results show an increase in the strength of the pellet due to the
role and should not exceed the desired temperature range; otherwise, decrease in the fayalite (a compound of iron silicate) formation and
it leads to the formation of paramagnetic wustite, which is undesirable un-oxidized-magnetite. It concludes that there is always a relationship
[2]. The synthesized magnetic concentrate thus obtained from the mag- between the mineral phases with the physical strength of the pellet
netization roasting process is then subjected to an agglomeration pro- [17–19].
cess called pelletization. In the India scenario, many pellet plants are To minimize the use of fossil fuel consumption (since anthracite coal
running based on the magnetite ore as feed material for making pellets fines are used as additives in hematite ore pelletization) in the pelletiza-
and then utilized in the steelmaking process. In industrial practice, it is tion plant, also to increase the utilizing of the low-grade iron ores such
reported that the magnetite ore pelletization is much easier than that as BHQ for the production of synthesized magnetite concentrate (used
of the hematite ore pelletization because of the absence of clay and frag- as raw material for the pellet in the study), magnetization roasting pro-
ile goethite minerals in it. Some researchers also reported the benefits of cess has emerged as a novel technique. In this paper, an effort has been
using magnetite ore for pelletization (an oxidation processes) where made and successfully executed by pelletizing the synthesized magne-
the magnetite concentrate obtained is subjected to a disc pelletizer to tite concentrate without using anthracite coal fines as an additive in
form the raw or green pellet. The green pellet is then subjected to a maintaining the temperature gradient from core to periphery of the pel-
straight grate-kiln for induration/heat hardening. Physical parameters let. In-depth study of pelletizing the synthesized magnetite concentrate
like cold crushing strength (CCS) and porosity were also studied to were taken care of, and green pellets were prepared and indurated at
understand the indurated pellet quality with the activation energy different times and temperatures for optimizing the parameters of in-
[3,11–13]. Researchers have also studied the effect of the organic binder terest. Experiments were conducted keeping in view of minimizing
during the pelletization process and compared the physical properties the adverse environmental effect (by not using anthracite coal fines as
of pellets with those made of inorganic binder (bentonite). They additives in pelletization), as well as optimizing the strength and micro-
found that applying organic binders alone is not sufficient to improve structural properties of the pellet required for industrial applications. All
the quality of pellets and require the addition of bentonite in combina- the commercial pelletization plants in India use hematite ore as raw ma-
tion to a certain percentage to achieve desirable strength [11]. The in- terial for pellet feed in the presence of anthracite coal fines as an addi-
vestigation was also carried out on the utilization of both activated tive to maintain the overall temperature gradient inside the pellet,
bentonite and sodium-based bentonite as a binder for pelletization of which ultimately affects the pellet physical (porosity & CCS), micro-
high-grade barite iron ore concentrate. The quality and the average structural, and metallurgical properties. In this context, authors have
strength of the sodium-based bentonite were found higher than that potentially tried to avoid the use of anthracite coal fines (that could af-
of the activated bentonite being used [14]. fect the environment by increasing the carbon footprints) in the pellet-
During the pelletization of the magnetite iron ore, the temperature ization of synthesized magnetite concentrate and evaluate the pellet
requirement is around 1250 °C, which is almost 80 °C less than that of properties as desirable by industries. The temperature requirement in-
the hematite ore pelletization. It is because the diffusion bonding of side the pellet was compensated by the exothermic reaction and in-
magnetite pellets (which enhance CCS of the pellet) is more during in- situ heat generation caused by the conversion of the magnetite phase
duration than that of the hematite ore pellet at low temperature. Be- to the hematite phase during induration. Sustainability of the novel pro-
cause of this, in hematite ore pelletization, coke fines are required to cess of synthesized magnetite concentrate pelletization and thereby
give the in-situ heat for maintaining the compressive strength of the saving the energy requirement (by reducing the consumption of fur-
pellet. From the experimental data, it was observed that around 2% of nace oil as well as anthracite coal fines as additives) were supported
the carbon was optimum for giving the required strength to the hema- by the physical and microstructural properties of the indurated pellets.
tite pellet. More addition of carbon values reduced the hematite to mag- Various characterization techniques such as Optical microscopy, X-Ray
netite in a lesser quantity and increased the porosity of the pellet [15]. Diffraction (XRD), Scanning Electron Microscopy (SEM), and X-ray
The green ball strength and production of fewer fines mostly depends microcomputed tomography (X-Ray micro-CT) were incorporated.
on the type of binder used in the pellet making. Reportedly, it was
found that the use of sodium-based bentonite as an inorganic binder 2. Raw materials
has a better binding property and produce fewer pellet fines in the pel-
let making process. Apart from bentonite, researchers have also looked 2.1. Feed characterization
into the possibility of using other binders in the pelletization process
like MHA (a special kind of binder), which was prepared by the Central For the present investigation, the BHQ iron ore sample received from
South University in China and mostly aimed to determine the oxidation the Barbil region of Odisha, India, was used. The preparation procedures
and sintering characteristics of the pellet. Magnetite concentrate con- of the magnetite concentrate from the BHQ sample and its characteriza-
taining Fe (T) of 66.40 wt% was used by them to make the pellet. The de- tion are already reported in our previous published work [2]. However,
gree of oxidation was evaluated by calculating FeO% before and after for the ease of readers, these results are discussed comprehensively for
192 S.N. Sahu et al. / Powder Technology 374 (2020) 190–200

ready reference in this section. Initially, the BHQ sample obtained from synthesized magnetite concentrate (15 kg feed per batch) in the pres-
the mine was subjected to a laboratory jaw crusher and, thereby, ence of sodium-based bentonite as the binder (0.5% of the concentrate
crushed to below 10 mm size. The representative sample of raw BHQ wt.). The green pellet prepared was subjected to a screening periodi-
was collected after the coning-quartering method and subsequently cally to obtain a near sized −12.5 + 10 mm pellet for induration. The
used in all the experiments. The chemical and mineralogical character- average drop numbers of green pellets were found to be 20–25 drops
ization of the raw BHQ sample was conducted to determine the mineral to break the pellet (determined by taking 50 nos. of green pellets). A
compositions and their distribution over the iron matrix. The methodol- laboratory oven (Cole-Parmer Stabletemp) was used at 110 °C for 3 h
ogy used for the determination of detailed chemical composition, phase to remove the moisture content of the green pellet. The dry pellets are
liberation and optical mineralogy of the sample was done using wet then subjected to the induration process; carried out in a muffle furnace,
chemical analysis method (IS 1493), XRD (X'pert Pro, PANalytical), as shown in Fig. 2(a). After induration, the compressed air was used for
and Optical Microscopy (DM2500 P, Leica). The detailed chemical com- cooling the pellet to below 50 °C, and the pellet was removed from the
positions of the head sample and the synthesized magnetite concen- furnace. Indurate pellet characteristics were carried out to investigate
trate are shown in Table 1. its suitability as iron-making material in the subsequent sections. For a
It was observed that the BHQ head sample contains Fe (T) of 47.15% better understanding of the phase transformations and microstructural
in association with the other major gangue minerals such as SiO2 properties, the indurated pellet sample was analyzed using XRD, SEM,
(28.31%) and Al2O3 (1.65%). The particle size analysis is shown in optical microscopy, and X-ray micro-CT.
Fig. 1(a), which indicates that 13.52% of the particles in the iron ore
head sample are below 45 μm, whereas 62.09% of particles are above
1.0 mm. At the same time, the size analysis also has shown a uniform
distribution of the Fe (T) in the range of 1–2% of the head sample. The 3. Results and discussion
crystalline mineral phases were investigated qualitative and quantita-
tive using XRD, which was recorded at 2θ (from 6° to 80°) at a scan Making pellets using the magnetite concentrate obtained from low-
speed of 1°/min. From XRD analysis, the presence of mineral phases grade BHQ iron ore by magnetization roasting process has industrial ap-
such as hematite, goethite, gibbsite, quartz, and kaolinite was observed plications and would impart positive environmental impact. Therefore,
in the BHQ head sample, as shown in Fig. 1(b). Furthermore, the per- looking into the present scenario of iron ore demand and supply chain
centage contribution of the individual mineral phases was calculated management, agglomeration technologies such as sintering/pelletiza-
using Rietveld refinement technique and approximated as: 63% hema- tion have to be added to steel plant so that beneficiation concentrates
tite (H); 7% goethite (G); 27% quartz (Q); 1.5% gibbsite (Gi); and 1.5% can be used as feed material. The focus must be on reducing the air/
kaolinite (K). The optical microscopic study is shown in Fig. 1(c) and water pollution and solid-waste handling by lowering the generation
(d), which confirms the presence of hematite (H), goethite (Go), Kaolin- and stockpiling of the low/lean grade iron ore resources, which is the
ite (K), quartz (Q), and gibbsite (Gi) in the BHQ matrix. In Fig. 1(c), the need of the hour [20].
appearance of hematite grains all over the surface of the sample fraction Moreover, the magnetite-based pelletization process is more advan-
can be seen, resembling a massive structure in the BHQ head sample, tageous than those using goethite/hematite iron ore (particularly in the
whereas in Fig. 1(d), the fraction of the head sample showing the hema- Indian context) in terms of energy and use of fossil fuel. The fragile and
tite grains mixed with massive goethite mineral phase alongside minor ultrafine nature of goethite/hematite ore with a high loss on ignition
constituents of impurities (quartz, kaolinite, and gibbsite) was (LOI) makes goethite/hematite pelletization more difficult than magne-
observed. tite ore pelletization. The occurrence of LOI in these iron ores comes
from the weathering and presence of associated clay minerals in it.
2.2. Experimental method However, researchers have also studied that the presence of clay min-
erals in the iron ore attracted more water molecules because of its neg-
For the production of synthesized magnetite concentrate, the mag- ative surface charge causing a swelling effect in the beneficiation
netization roasting of BHQ iron ore followed by the magnetic separation process. On the other hand, the exothermic reaction occurred during
of roasted BHQ was performed as per our previously published method- the induration of the magnetite ore pellet has an added advantage of
ology [2]. In this process, the BHQ sample was reduced using reductant using it as a pellet feed material rather than hematite [21]. We at
at 1100 °C in a laboratory-scale muffle furnace (HTF 18/27, Carbolite CSIR-IMMT, Bhubaneswar, found that the iron ore sourced from the
Gero) as shown in Fig. 2(a). The reductant used was one of the non-cok- mines of the Joda-Barbil region of Odisha is structurally more weath-
ing coals obtained from the eastern part of India. The proximate analysis ered, and having high clay contents, which causes a severe swelling
of the non-coking coal sample is shown in Table 2. problem during grinding in the ball mill of beneficiation plant producing
After the magnetization roasting process, the reduced or roasted pellet grade concentrate. The presence of high LOI (more than 2% in the
BHQ sample was separated from burnt coal ash using a hand-magnet. form of kaolinite) in the pelletization of hematite iron ore causes the
Subsequently, the ash-free roasted BHQ ore was ground to below 45 generation of high-pressure steam during the induration and thereby
μm using wet milling in a laboratory-based ball mill and subjected to a causing cracking of pellets and generation of more fines. Due to the
low-intensity magnetic separator (approximately 1500 G) to separate self-pelletizing phenomena, the induration of synthesized magnetite
the synthesized magnetite concentrate from the non-magnetic frac- iron ore is less energy-intensive (in-situ exothermic reaction and oxida-
tions. The Fe (T) content in the synthesized magnetite concentrate ob- tion of magnetite to hematite) and economically favourable (no anthra-
tained after the reduction roasting process of BHQ ore was found to be cite coal fines is used).
66.42% (as shown in Table 1). Noteworthy to mention that the benefit Researchers have studied the oxidation phenomena of natural mag-
of using magnetite concentrate in pelletization is that there is no need netite ore extensively [22], but pelletization of synthesized magnetite
to use anthracite coal fines (used 1% by weight in hematite ore pelleti- ore produced from the reduction roasting of banded iron ores have
zation in plant practices) as additives for maintaining temperature gra- not been explored yet. This study can find a way forward for developing
dient from core to periphery of the pellet due to in-situ heat generation countries like India where availability/scarcity of high-grade lumpy iron
during an exothermic reaction. The synthesized magnetite concentrate ore is an inherent problem. The physical characteristics of indurated
produced was then utilized as a pellet feed material using a labora- pellets such as CCS, porosity, mineralogical behavior, and porosity dis-
tory-scale disc pelletizer (Fig. 2(b)) of 1 m diameter wherein bentonite tribution were studied accordingly. The head or raw sample with inter-
was used as a binder during the pelletization process. The pellet feed mediate (green balls/pellets) and final (indurated pellets) products are
containing 10% moisture was prepared by spraying water into the shown in Fig. 3.
S.N. Sahu et al. / Powder Technology 374 (2020) 190–200 193

Table 1
Chemical composition of raw BHQ iron ore head (−10 mm size) and synthesized magnetite concentrate sample.

Details Fe (T) % SiO2% Al2O3% LOI % Na2O % P2O5% TiO2% CaO % K2O % MnO2%

BHQ head sample 47.15 28.31 1.65 1.36 0.03 0.04 0.13 0.09 0.04 0.30
Synthesized magnetite concentrate 66.42 6.68 0.28 Approximately 0.71% constituents (without LOI) are in trace quantity

3.1. Effect of induration temperature on the cold compressive strength was also achieved at induration temperature and RT of 1300 °C and 5
(CCS) of the pellet min, respectively, which may not be suitable from the economic point
of view. The results collectively indicate that the RT of the pellet indura-
Cold compression strength (CCS) indicates the ability of pellets to tion must be more than 5 min to achieve the required strength of indus-
withstand the load during their handling/stockpiling and a load of bur- trial standard at 1250 °C. The effect of higher RT on CCS is discussed in
den material in the reduction furnace. Generally, blast furnace needs the next section (3.2). The temperature was fixed at 1250 °C as an opti-
pellets with CCS values in the range of 250–260 kg/pellet. In this mum induration temperature, as shown in Fig. 4.
study, the synthesized magnetite concentrate was subjected to pelleti-
zation in a laboratory disc pelletizer. Then the green pellet formed 3.2. Effect of residence time (RT) on the cold compressive strength of the
(−12.5 + 10 mm size) was subjected to induration (heat hardening) pellet
in the high-temperature muffle furnace at different fired temperatures.
The effect of the induration temperature inside the furnace was studied The induration process was conducted with varying RT after achiev-
from 1000 °C to 1300 °C, maintaining a temperature interval of 50 °C at ing the optimum firing/induration temperature (1250 °C) to evaluate
5 min of fixed residence time (after obtaining firing temperature). The the effect of RT on the CCS. Experiments were conducted systematically,
indurated pellets were then cooled below 50 °C and subjected to a and it was observed that the RT is directly proportional to the CCS of the
CCS Tester (SET-T-2000, Shanta Engineering) to determine the CCS of pellet. Optimizing RT could help in obtaining desired pellet strength,
the pellet, as shown in Fig. 4. which in turn would help the pellet in sustaining the thermal burden,
Experiments show that the strength of the pellet was increased thereby producing fewer fines due to its high physical strength (primar-
slightly (at 1050 °C) and then decreased suddenly at 1100 °C. The de- ily CCS of the pellet) during the blast furnace charging. The optimum
crease in the strength of the pellet is probably due to the phase transfor- value of CCS would also help in minimizing the generation of undesir-
mation of the iron phase minerals from magnetite to hematite during able broken pellets due to the pellet-pellet collision during transporta-
the oxidation process, as reported by previous researchers [22]. How- tion. Here, the RT of the pellets were varied from 5 to 15 min, and CCS
ever, beyond 1100 °C, the CCS of the pellet increased significantly with of the pellet was measured. A plot of CCS against the temperature at
increasing temperature up to 1250 °C. This increase in the strength of varying RT is shown in Fig. 5. The CCS at 10 and 15 min RT was measured
the pellet at 1250 °C is due to the particle-particle fusion (sintering of to be 255.8 and 270.5 kg/pellet, respectively, under the optimum indu-
particles) inside the pellet. Despite increased strength, it was observed ration temperature of 1250 °C. These values of CCS are very optimistic,
that the obtained CCS at an induration temperature of 1250 °C is 245 acceptable, and industry-friendly as it falls under the standard industrial
kg/pellet, which is less than a minimum requirement of CCS (250 requirements (250–260 kg/pellet), and can be utilized for the iron mak-
kg/pellet) [18] in real plant practices. However, CCS of 250 kg/pellet ing process. The results indicate that the minimum induration

Fig. 1. Feed characterization BHQ iron ore. (a) Size distribution (b) XRD analysis (c,d) Optical microscopic study [2].
194 S.N. Sahu et al. / Powder Technology 374 (2020) 190–200

Fig. 2. (a) Laboratory-scale muffle furnace and (b) Laboratory-scale disc pelletizer available at CSIR-IMMT, Bhubaneswar.

temperature and RT for the pelletization of synthesized magnetite RT. Initially, the porosity of 29.98%, 29.52%, and 29.45% was achieved
concentrate were 1250 °C and 10 min, respectively, to achieve 255.8 at 1000 °C temperature with the RT of 5, 10, and 15 min, respectively.
kg/pellet of CCS. From Fig. 7, it can be seen that the porosity of the indurated pellet

3.3. Effect of induration temperature on the porosity of the pellet

The porosity is an essential factor for the direct reduction of (DRI) of


the iron ore pellet in the kiln/blast furnace (BF) applications. Primarily
for the processes like DRI/BF, the distribution of the pores inside the pel-
let plays a significant role in its reduction to metal values. For better re-
ducibility inside the DRI kiln/BF, the porosity of the pellet between the
range of 25–26% is required [23]. To obtain better reducibility and re-
quired metal values, the porosity of the pellet was determined using a
standard porosity measuring procedure (IS 11348). A plot between dif-
ferent indurated temperatures against the porosity of the pellet is
shown in Fig. 6. Initially, at 1000 °C induration temperature and 5 min
RT, the porosity of the pellet was found to be 29.98%, which is higher
than the required porosity values (25–26%). Therefore, the required
CCS of the pellet could not be obtained at 1000 °C temperature.
With increasing the indurated temperatures up to 1100 °C, it was
observed that the porosity of the pellet was further increased to nearly
31%, possibly due to the phase transformation of the pellet from magne-
tite to hematite. However, beyond 1200 °C temperature due to particle-
particle fusion, there was a decrease in the porosity of the pellet. At RT 5
of min, the indurated pellet porosity of 28.6% and 26.82% were obtained
at 1250 °C and 1300 °C temperature, respectively. This result is slightly
higher than the required values of the indurated pellet porosity for
industrial applications. Optimizing the residence time could be an alter-
native method to decrease the pellet porosity to the desired standard
(25–26%), which has been discussed in the next section (section 3.4).

3.4. Effect of residence time on the porosity of the pellet

The RT at each induration temperature was varied between 5 and 15


min to understand the effect on the pellet porosity. The results show
that the porosity of the pellet was changed marginally on varying the

Table 2
Proximate analysis of coal samples on an air-dry basis. Fig. 3. Photographs of (a) Head BHQ sample (−10 mm) (b) BHQ sample after
magnetization roasting (c) Magnetite concentrate after LIMS (d) Green pellet (e)
Type Moisture % Volatile matter % Ash % Fixed carbon % Indurate pellet at 1250 °C and 10 min of residence time (RT).
Non-coking coal 9.46 28.46 26.84 34.74
S.N. Sahu et al. / Powder Technology 374 (2020) 190–200 195

Fig. 4. Temperature vs. CCS at 5 min of residence time (RT).


Fig. 6. Temperature vs. porosity at 5 min of residence time (RT).

decreased slightly with an increase in the RT. The decrease in the pellet
magnetic separation, the synthesized magnetite concentrate obtained
porosity was caused by particle-particle fusion. It may be noted that the
was subjected to pelletization at different temperatures and RT to opti-
pellet RT is the time at which the pellet is fired with the preset temper-
mize the process parameters. Since pelletization is an oxidation process,
ature. The measured value of the pellet porosity at 1250 °C and 10 min
the magnetite phase present in the pellet after induration converted
RT, was found to be 25.42%, which is acceptable for DRI and BF
to the hematite phase minerals, which can further be confirmed from
applications.
Fig. 8(b).

3.5. Phase transformation study of the indurated pellet 3.6. Optical microscopic study of the indurated pellet

It was evident that the synthesized magnetic concentrate obtained Understanding the effect of mineralogical behavior on the physical
after the magnetization roasting followed by the magnetic separation parameters such as CCS and porosity of the indurated pellet, the optical
process majorly consisted of magnetite iron phase mineral alongside microscopic study was carried out using an optical microscope
some quartzite as a gangue mineral. For visualization, the phase analysis (DM2500 P, Leica). The microscopic study of the indurated pellet is
of the synthesized magnetite concentrate and the indurated pellet (ob- very crucial because CCS and porosity depend on the particle-particle
tained at 1250 °C induration temperature and 10 min RT) was investi- fusion that occurred during the induration process, can be identified mi-
gated using the XRD technique (major mineral phases are identified), croscopically. The particle-particle fusion/sintering occurs by the energy
as shown in Fig. 8. Comparatively, to Fig. 1(b), it can be seen that the ma- released from the exothermic reaction, increases the process tempera-
jority of hematite iron phase minerals present in the raw BHQ ore was ture, and helps in maintaining temperature gradient from core to
converted to the magnetite mineral phase, as shown in Fig. 8(a). This periphery of the pellet. From the microscopic study shown in Fig. 9(a)
conversion of hematite to magnetite phase depends on the reduction and (b), it can be observed that the fusion between the particles has oc-
time, temperature, and reductant percentage of the process. It was curred uniformly, and distributed evenly from the periphery to the core
also reported in our published work that if the reduction time of the of the pellet. At 1250 °C induration temperature and 10 min RT, the syn-
BHQ ore was increased beyond optimized conditions, then there was a thesized magnetite pellet was self-sufficient to generate the required
formation of wustite iron phase mineral, which is undesirable due to amount of heat to fuse the particles among themselves and converted
its less affinity towards low-intensity magnetic separator [2]. After the to the hematite phase. However, the periphery of the pellet was more
exposed to the high temperature than that of the core, making the un-
even distribution of pores. Therefore, the core of the pellet is more po-
rous (Fig. 9(b)) than that of the periphery (Fig. 9(a)).

3.7. Scanning electron microscope (SEM) analysis of the indurated pellet

The microstructural analysis was carried out on the representative


sample of synthesized magnetite pellets to study the induration effect
on the CCS and porosity using an SEM (JSM-6510, JEOL). The pellets ob-
tained at optimized conditions (indurated at 1250 °C for 10 min RT)
were used for this study. The SEM images in Fig. 10(a, b) and (c, d) indi-
cate the microstructure of the core and periphery of the pellet, respec-
tively. It can be seen from Fig. 10 that the particle-particle fusion at
the periphery of the pellet is more as compared to the core. The ob-
served phenomenon is because of the decrease in the penetration of
heat along the radius of the pellet. Therefore, the surface of the pellet
is more exposed to high temperature than that of the core. On the
other hand, the regular bigger fused shape of the particles is found to
be formed at the periphery of the pellet. In addition to this, the bigger
Fig. 5. Temperature vs. CCS at different residence times (RT). fused grains at the periphery are significantly more abundant in nature
196 S.N. Sahu et al. / Powder Technology 374 (2020) 190–200

Fig. 7. Temperature vs. porosity at different residence times (RT).

Fig. 8. XRD analysis of the (a) magnetite concentrate and (b) pellet indurated at 1250 °C at 10 min residence time (RT), where Hematite: H, Quartzite: Q, Magnetite: M.

and have a lesser distribution of pores causing less generation of air- at plant practices, the anthracite coal fines are used in the pelletization
born fines. The desired specification of CCS, porosity, and lesser air- of hematite iron ore concentrate on maintaining the temperature gradi-
born fines generation was achieved by the microstructural changes ent between the core and periphery of the pellet. However, our present
that occurred at the interior of the pellet. It is worth mentioning that investigation revealed that the pellet produced from synthesized

Fig. 9. Optical microscopic analysis of the pellet indurated at 1250 °C for 10 min residence time: (a) periphery of the pellet; (b) core of the pellet.
S.N. Sahu et al. / Powder Technology 374 (2020) 190–200 197

Fig. 10. SEM analysis of the pellet indurated at 1250 °C and 10 min residence time (RT): (a, b) core of the pellet; (c, d) periphery of the pellet.

Fig. 11. X-ray micro-CT images of pellet indurated at 1250 °C and 10 min residence time: (a) 3D image of the pellet; (b) hemispherical internal 3D view of the pellet; (c) 3D image showing
the porous structure of the inside pellet; (d) internal image of the pellet having porous at the core of the pellet.
198 S.N. Sahu et al. / Powder Technology 374 (2020) 190–200

Fig. 12. Hematite ore pelletization process.

magnetite concentrate (without the addition of anthracite coal fines) distribution of the pores inside the pellet in a non-destructive method
acquired similar physical properties as that of the hematite ore of X-Ray micro-CT (Sky Scan-2211, Bruker) was investigated.
pelletization. Fig. 11(a–d) shows the 3D images of both the external and internal
microstructure of the indurated pellets. Fig. 11(a, b) indicates the over-
3.8. X-ray microcomputed tomography analysis of the pellet all 3D microstructure of the pellet spherically and hemispherically,
whereas Fig. 11(c, d) shows the distribution of the porous structure at
The percentage of the pellet porosity mostly controls the strength the core of the pellet. It can also be observed in Fig. 11(c, d) that the
and reduction capability of the pellet. Therefore, the study of the core of the pellet is more porous than that of the periphery of the pellet.

Fig. 13. Magnetite ore pelletization process.


S.N. Sahu et al. / Powder Technology 374 (2020) 190–200 199

Table 3
Qualitative assessment of the proposed process flowsheet for the commercial application.

Factors Hematite iron ore pelletization (1) Synthesized magnetite iron ore Remarks
pelletization (2)

Consumption of Furnace oil (FO) 15–18 l per ton of fired/indurated pellet 10–12 l per ton of fired/indurated pellet Reduction in fossil fuel as well as CO2 emission in
(2)
Requirement of anthracite coal 1–1.5% per ton of fired/indurated pellet NIL Reduction of CO2 emission as well as import
fines in pelletization substitution in (2)
Presence of clay minerals High LOI which has a negative impact in NIL High LOI causes the generation of the undesirable
pelletization cracked pellet (below 5 mm)
Presence of ultrafine goethite High goethite increases the Blaine NIL Increase in Blaine number causes difficulties in
minerals number (>3000cm2/g) in ball mill pelletization because of the fragile nature of
grinding goethite
Energy in phase conversion Pelletization is endothermic Pelletization is exothermic due to Exothermic pelletization is a self-sufficient process
oxidation of synthesized magnetite to and requires less heat energy
hematite
Induration temperature Around 1300–1330 °C Around 1200–1250 °C Approximate 80–100 °C less in synthesized
magnetite pelletization

A CCS of 255.8 kg/pellet was observed where the pores inside the pellet substantial quantity of energy is saved during magnetite ore pelletiza-
are concentrated significantly at the core. However, with an increase in tion due to the exothermic nature of the magnetite oxidation [22,25].
the fired temperature, the porous structure gradually concentrated at This helps in avoiding the usage of anthracite coal fines during the
the core of the pellet and then disappears due to particle-particle fusion pelletization process, thereby promoting the reduction of carbon foot-
at a higher temperature. prints. The fossil fuel requirements in term of furnace oil (FO) during
firing is also reduced to a lower value which makes the process more
4. Process feasibility: benefits and recent plant practices environmentally friendly. A typical practice of magnetite ore pelletiza-
tion in India is shown in Fig. 13.
In recent trends, utilizing the low/lean-grade iron ore resources
through beneficiation followed by pelletization of iron ore concentrate 4.1.3. Qualitative assessment between hematite and synthesized magnetite
is considered as a boon to iron and steel making industries. Improved ore pelletization
physical strength & metallurgical properties make iron ore pellets an al- In this study, we have compared the process benefits and complica-
ternative feed material for blast furnace in comparison to calibrated tions and tried to utilize the low-grade BHQ ore using pelletization in
lump ore (CLO), considering a sustainable utilization of high-grade the iron making process. A qualitative assessment of the proposed pro-
iron ore resources. cess flowsheet for the commercial application was carried out and
shown in Table 3.
4.1. Iron ore pelletization and process complications As per the assessment of the pelletization processes, one can able to
identify the process benefits while using the synthesized magnetite iron
All over the world, iron ore industries are practising pelletization of ore concentrate. On the other hand, the physical properties studied
beneficiated iron ore either in the form of hematite or magnetite con- were at par the properties required for the iron making process without
centrate. Added to this, iron ore pelletization is one of the essential pro- compromising the environmental impact.
cesses for the iron and steelmaking industries and mine owners for
sustainable and effective use of their raw materials [22,24]. However, 5. Conclusion
the impact of iron ore beneficiation and pelletization on the environ-
ment plays a vital role in terms of fossil fuel consumption, an increase In this paper, a novel technique has been studied for making synthe-
in the carbon footprints, and generations of considerable air-born dust sized magnetite-based iron pellets in the absence of anthracite coal fines
particles. as an additive for iron and steelmaking processes. The magnetite con-
centrate produced from magnetization roasting of BHQ iron ore
4.1.1. Pelletization of hematite iron ore and process complications followed by low-intensity magnetic separation has proven to be the
In Indian hematite iron ore pelletization, industries are facing the promising technique and could act as an alternative to the conventional
negative effect due to the presence of unwanted clay as well as ultrafine pelletization process. It has been observed despite the low iron content
goethite mineral, which increases the loss on ignition (LOI) and Blaine of the banded ore, the CCS and porosity of 255.8 kg/pellet and 25.42%,
number of the pellet feed concentrate above the acceptable limit [20]. respectively, were achieved at the optimized conditions, which are
Because of this, there were problems with the generation of more indu- very encouraging and comparable with industry standards. The parti-
rated pellet fines (below 5 mm), the formation of the hairline cracks in cle-particle fusion at the periphery and core of the pellet under optimal
the pellet, and release of considerable amount of air-born dust particles induration conditions act as a driving force and are responsible for re-
during the screening and transportation of the indurated pellet. The re- quired CCS and porosity. The present study has unfolded the dynamic
quirement of pulverized anthracite coal fines in the hematite ore pellet- potency of synthesized magnetite pelletization. It could act as a poten-
ization is another reason for the increase in the carbon footprints in the tial footstep towards the effective utilization of low-grade banded iron
overall pelletization process. The schematic process flowsheet for he- ore resources as well as conservation of high-grade calibrated iron ore
matite ore pelletization is shown in Fig. 12. available at the Indian iron ore mines in the pilot-scale as well as in
large scale.
4.1.2. Pelletization of synthesized magnetite iron ore and process benefits
Pelletization of magnetite ore involves oxidation at lower temper- Credit author statement
ature followed by sintering to maintain the required physical and
metallurgical properties for the subsequent iron making process Sachida Nanda Sahu: Conceptualization, Manuscript preparation.
such as blast furnace or direct reduction of iron processes. A Prasanta Kumar Baskey: Data Collection, Manuscript preparation.
200 S.N. Sahu et al. / Powder Technology 374 (2020) 190–200

Santosh Deb Barma: Data analysis, Manuscript preparation. [8] J. Kou, T. Sun, D. Tao, Y. Cao, C. Xu, Coal-based direct reduction and magnetic sepa-
ration of lump hematite ore, Mining, Metall. & Explor. 31 (2014) 150–161.
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Surendra Kumar Biswal: Manuscript preparation. iron ore tailings: part 1. The recovery of iron from iron ore tailings using magnetic
B. C. Meikap: Manuscript preparation. separation after magnetizing roasting, J. Hazard. Mater. 174 (2010) 71–77.
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binders, Powder Technol. 210 (2011) 23–28.
[12] O. Sivrikaya, A.I. Arol, An investigation of the relationship between compressive
The authors declare that they have no known competing financial strength and dust generation potential of magnetite pellets, Int. J. Miner. Process.
interests or personal relationships that could have appeared to influ- 123 (2013) 158–164.
[13] H. Zhang, J. Fu, J. Pan, F. Zhang, Z. Guo, Isothermal oxidation kinetics of artificial mag-
ence the work reported in this paper. netite pellets, Journal of Wuhan University of Technology-Mater. Sci. Ed. 33 (2018)
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