Accepted Manuscript

Beneficiation of an iron ore fines by magnetization roasting and

magnetic separation

Jianwen Yu, Yuexin Han, Yanjun Li, Peng Gao

PII: S0301-7516(17)30205-3
DOI: doi:10.1016/j.minpro.2017.09.012
Reference: MINPRO 3098
To appear in: International Journal of Mineral Processing
Received date: 13 November 2016
Revised date: 14 September 2017
Accepted date: 20 September 2017

Please cite this article as: Jianwen Yu, Yuexin Han, Yanjun Li, Peng Gao , Beneficiation
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 ACCEPTED MANUSCRIPT

Beneficiation of an iron ore finesbymagnetization roasting and magnetic

separation

Jianwen Yu*, Yuexin Han*, Yanjun Li, PengGao

College of Resources and Civil Engineering, Northeastern University, Shenyang 110819, P.R.

China

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*Both authors contributed equally to this work:

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Prof. Yuexin Han, E-mail address:dongdafulong@mail.neu.edu.cn

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Dr. Jianwen Yu, E-mail address:neu_mpc237@163.com.NU
Abstract: The utilization of abundant low-grade iron ores is potentially important to many

countries in the word, especially to China. These iron ores contain many detrimental impurities
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and are difficult to upgrade to make suitable concentrates for the blast furnace. In this paper, the

beneficiation of a low-grade hematite ore fines containing carbonates with magnetization roasting
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and magnetic separation was proposed and studied. The hematite and siderite are almost
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completely converted into magnetite by 8 wt.% coal at roasting temperature of 800 °C for 8 min.
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Under the optimized conditions, a high grade magnetic concentrate containing 65.4 wt.% iron with

an iron recovery of 92.7% was achieved. Meanwhile, the effects of roasting temperature, reaction
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time and coal to ore ratio on the magnetic properties of roasted materials were investigated using a

vibration sample magnetometer (VSM). The results show that the magnetic susceptibility and

magnetism saturation of hematite ore can be highly increased due to the selective conversion of

hematite and siderite into magnetite caused by magnetization roasting which facilitates their

separation from non-magnetic minerals.

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Keywords: Low-grade iron ore; Magnetization roasting; Magnetic properties; Phase

transformation; Magnetic separation.

1. Introduction

Hematite (α-Fe2O3) is widely distributed in various rocks and is one of the most common and

abundant iron oxide minerals in soil (Zhang 2007). However, it cannot be used in iron and steel

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industry without preliminary beneficiation due to its low grade. Many researchers have

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investigated the separation of iron minerals from gangue minerals by froth flotation process

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(Hanumantha and Narasimhan, 1985; Luo et al., 2016), reverse anionic flotation of quartz (Wang
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and Ren, 2005; Shrimali and Miller, 2016), and magnetic separation (Song et al., 2002). After

years of development and engineering practice, magnetization roasting followed by low-intensity

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magnetic separation has been proven as an effective solution, both technologically and

economically, when upgrading refractory iron ores (Zhu and Li, 2014; Li et al., 2015). Some such
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successful examples are the use of magnetization roasting followed by magnetic separation to treat
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zinc calcines (Peng et al., 2012; Li et al., 2012), cyanide tailings (Zhang et al., 2012), iron ore
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tailings (Li et al., 2010) and some refractory iron ores (Li and Zhu, 2012; Zhu et al., 2010; Luo et

al., 2014; Qi and Yu, 2011; Chun et al., 2015) for the recovery of iron. Meanwhile, the chemical
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and structural changes of iron ore samples versus the temperature during the magnetizing roasting

process have been identified: The transformation of iron ores starts at the temperature between

120 °C and 140 °C with the free moisture removal (Strezov et al., 2011); the dehydroxylation of

limonite occurs between 250 °C and 350 °C, and the decomposing of siderite happens between

490 °C and 630 °C (Jang et al., 2014; Gialanella et al., 2010; Feng et al., 2011; Li et al., 2011; Han

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et al., 2013; Zhang et al., 2002). Finally, the reduction of hematite to magnetite occurs at around

850 °C (Jang et al., 2014).But in this investigation, we mainly introduce the relative contents of

iron recovery and magnetic properties as well as phase conversion for magnetization roasting, and

an iron ore fines containing iron carbonate minerals obtained from Donganshan Iron Ore Mine

was studied purposely to achieve its utilization.The carbonate minerals such as siderite as well as

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ankerite easily adsorbed on the surface of quartz and hematite, thus the quartz and hematite had a

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same or similar surface property, thus they could not be separated effectively in the reverse

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flotation (Luo et al., 2016(a); Luo et al., 2016(b); Luo et al., 2016(c)). Subsequently, a
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step-flotation (the first-step flotation is the froth flotation of siderite, by which some siderite was

separated; the second-flotation was the reverse flotation of quartz, by which the quartz was
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discarded) seemed to be a potential strategy to improve the separation between quartz and

hematite, but it didnot solve the problem of siderite adsorption on the surface of quartz and
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hematite. Therefore, the iron grade and recovery of iron concentrate produced by the combined
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process of gravity separation, low-intensity magnetic separation and high-gradient magnetic

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separation followed by step-flotation were both lower than 65wt.% (Yin et al., 2011; Shao 2011(a);

Shao 2013(b)).
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At present, about 2.0 million tons of iron ores containing carbonates are stockpiled by Anshan

Iron & Steel Group per year due to lack of processing technology. These carbonate-containing iron

ores not only pollute environment and give rise to security risks, but also occupy huge land for the

construction of iron ore disposal sites, which could increase the production cost of iron ore

dressing plants. So, it is very important and necessary to develop a new technology to deal with

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such type iron ores.

For this purpose, the beneficiation of a low-grade hematite ore fines containing carbonate

minerals with magnetization roasting and magnetic separation was proposed for the first time.

Therefore, the magnetization roasting of iron ore sample was studied extensively. Meanwhile, the

effect of magnetization roasting on magnetic properties of the roasted materials was characterized

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by VSM analysis combined with XRD analysis and Fe mineral phase analysis.

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2. Experimental

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2.1 Materials NU
The iron ore sample used in this research was obtained from Donganshan Iron Ore Mine

located in Liaoning Province, China. The sample with 85 wt.% passing 0.074 mm was air-dried.
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The iron ore sample was characterized using chemical analysis and XRD, and the results are

shown in Table 1 and Fig. 1, respectively. The content of valuable metal Fe is 34.6 wt.%, and the
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main phase structures of the sample are hematite (Fe2O3) and quartz (SiO2). Some other minerals
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such as magnetite and siderite cannot appear in the XRD pattern due to their low content (lower
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than 5%). Meanwhile, its iron phase analysis indicates that iron elements in the ore are distributed

in hematite (64.76%), magnetite (27.29%), carbonate (6.45%, mainly exist in siderite and ankerite)
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and iron silicate minerals (in total 0.42%) as well as in iron sulfide minerals (in total 0.29%)

(Table 5).

The bituminous coal obtained from Jilin Coal Mining Co., Ltd was used as reducing agent,

which was pulverized and screened to -2 mm. The proximate analysis of the bituminous coal is

given in Table 2, and the fixed carbon is 67.83%.

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2.2 Magnetization roasting and magnetic separation

The bituminous coal was mixed well-distributed with hematite ore for the magnetization

roasting in the muffle furnace (KJ, model KSL-1200X-J). After roasting, the roasted samples were

cooled to room temperature by water quenching to avoid re-oxidation.

In the magnetic separation tests, a Davis Tube Tester (model ø50) was employed. The roasted

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materials were ground to 85 wt.% passing 38 μm in a ball mill (XMQ-Φ240×90), the flow rate

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of water was 1.2 L/min, the stroke rate was 75 strokes/min and the magnetic field intensity was set

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to 0.12 T. After the magnetic separation, the non-magnetic product was the tailing, while the
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magnetic product was iron concentrate. Both of the products were filtered, dried, weighed, and

analyzed for Fe, from which the mass balances were made to obtain the iron recoveries. The
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overall experimental flow sheet is presented in Fig. 2.

2.3 Structural and vibrating sample magnetometer analysis

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The solid phase structure was analyzed by X-ray diffraction (X’ Pert PRO MPD) with Cu Kα
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radiation, and the operating voltage and current were 40 kV and 40 mA, respectively. The
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diffraction angle was scanned from 10° to 70°.

The vibrating sample magnetometer used was a VSM Model 7410 (Lake Shore, USA). Once
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the room temperature sample had been positioned correctly, the magnetic field was increased

incrementally until 20.0 kOe. Subsequently, it was decreased and then back up again to 20.0 kOe,

thus a complete hysteresis loop for the samples was given (Barani et al., 2011). Besides, if a

magnetization versus field curve shows evidence of both paramagnetic and ferromagnetic

components, then it is possible to construct a Honda-Owen plot and separate the two aspects of the

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magnetization. This involves plotting the magnetic susceptibility of the samples against the

reciprocal of the field in the dM/dH = a region. This plot would show a linear relationship, with

the y-intercept being the magnetic susceptibility, χ, of the paramagnetic component. As χ for a

paramagnetic material is constant, the paramagnetic fraction of the total sample magnetization can

be calculated, and this can be subtracted from the total magnetization of the sample to obtain the

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ferromagnetic magnetization (Barani et al., 2011; Wu et al., 2012).

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3. Results and discussion

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3.1 Magnetization roasting and magnetic separation
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In the magnetization roasting process, the main factors of affecting roasted materials quality

were reduction temperature, roasting time as well as the coal to ore ratio. In order to determine the
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appropriate roasting process parameters, the effects of reduction temperature, roasting time, and

the coal to ore ratio on Fe content and recovery in magnetic fraction were studied. The results are
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given in Figs.3-5.
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As shown in Fig. 3, with the increase of roasting temperature, the iron recovery of the iron
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concentrate increased until it reached the maximum value at 800 °C and then declined slightly

when the temperature increased further. The maximum iron recovery was about 90.90% with a
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grade of 65.22 wt.% Fe. Meanwhile, the grade of the iron concentrate declined as increasing

roasting temperature. This result might be due to the fact that the reduction of hematite to

magnetite or the decomposition of siderite into magnetite was incomplete at low temperatures

because of the limited reaction rate (Zhang et al., 2012). At high temperatures, the gasification of

solid carbon accelerated and then speeded up the conversion of hematite or siderite to magnetite.

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While parts of the iron oxide could be transformed to weakly magnetic wustite (FeO) and fayalite

(Fe2SiO4) (Xie 2001; Zhang 2007; Xue 2008) if the temperature was too high, which subsequently

deteriorated the recovery of iron from gangue minerals in magnetic separation process.

Fig. 4 shows the effect of roasting time on Fe content and recovery in magnetic fraction. The

consequence could be figured out that, both of the grade and recovery of iron in concentrate

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increased continuously with the prolonging of roasting time until reaching the maximum value

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around 8 min and then declined quickly. This observation might be contributed to the magnetic

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conversion was not adequate if the roasting time was too short, and the formed or original
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magnetite could be re-oxidized if the roasting time was over long even at suitable temperature,

which were detrimental to the low-intensity magnetic separation (Cui et al., 2002).
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Fig. 5 exhibits the effect of coal to ore ratio on Fe content and recovery in magnetic fraction.

As the increase of coal dosage, the recovery of iron in concentrate increased until it reached the
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maximum value and then decreased gradually, while the grade increased slowly. This result might
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be due to that hematite could not be reduced to magnetite completely when the coal is insufficient
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even if the completed composition of siderite into magnetite occurred, resulting in a low iron

recovery and grade. However, when the coal was excessive, some new generated or original
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magnetite could be reduced to ferrous oxide which is weakly magnetic, going against the

following magnetic separation, and leading to a decreased iron recovery.

It is known that from Fig. 5, the iron concentrate with a grade of 65.4 wt.% and a recovery of

92.7% was obtained. The chemical analysis for the compositions of iron concentrate is given in

Table 3.

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It is implied in Table 3 that the grade of iron concentrate is qualified for the requirements of

companies, and the contents of impurities like S and P are much low by 0.01 wt.% and 0.02 wt.%,

respectively. It can be used as a high-quality raw material for iron smelting. The content of SiO2

(quartz) is 7.77 wt.%, indicating that iron and quartz were fine-disseminated complexly together,

and they were hard to be completely separated.

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3.2 Magnetic properties of iron ore sample after roasting

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The saturation magnetism (Ms), an important parameter for magnetic separation, is estimated

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from the hysteresis loops and shows in Figs. 6-8.NU
Fig. 6 shows the saturation magnetism for raw ore and roasted samples at different

temperatures. It was obvious that compared with the magnetization of raw ore (8.9 emu/g), the
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magnetization of the roasted samples was enhanced. With increasing in roasting temperature from

650 °C to 750 °C, saturation magnetism was increased from 16.0 to 35.1emu/g. Further increasing
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in roasting temperature to 800 °C, the saturation magnetism slightly increased to 37.3 emu/g, and
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then almost kept it constant. Therefore, it was concluded that the coal was decomposed to
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reducing gas at large when the temperature was around 750-800 °C, which efficiently converted

the hematite and siderite into magnetite.

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Fig. 7 shows the saturation magnetism of roasted samples for different time. It is seen from Fig.

7 that the saturation magnetization increased to the maximum value of 37.3 emu/g when the

roasting time up to 8 min. Further extending the time, it turned to decrease. Short time was

insufficient for the complete conversion of hematite and siderite into magnetite, and over long

time might make the new-generated or original magnetite re-oxidized.

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Fig. 8 shows the saturation magnetism of roasted samples with different coal to ore ratios.

With increasing in coal to ore ratio from 4 wt.% to 8 wt.%, saturation magnetism was increased

from 31.0 to 37.3 emu/g. Further increasing the coal to ore ratio, the saturation magnetism was

increased negligibly.

The saturation magnetism value includes paramagnetic and ferromagnetic minerals (Barani et

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al., 2011). Honda-Owen plot was drawn to calculate the magnetic susceptibility of paramagnetic

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and ferromagnetic fractions in the total saturation magnetism.

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Fig. 9 shows Honda-Owen plot for raw ore (marked as A) and roasted samples at temperatures
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of 700 °C, 800 °C and 900 °C (marked as B, C and D, respectively). Table 4 shows the magnetic

susceptibility of paramagnetic and ferromagnetic components of the samples. It can be seen

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clearly that the magnetic susceptibility of ferromagnetic and paramagnetic fractions were changed

after roasting treatment with coal. With the increasing in roasting temperature to 800 °C, the
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magnetic susceptibility of the paramagnetic fraction was decreased from 4.91 to 1.67 (10-6m3/kg),
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correspondingly the magnetic susceptibility of ferromagnetic fraction was dramatically increased

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from 3.89 to 35.23 (10-6m3/kg). With further increasing in roasting temperature up to 900 °C, the

total magnetic susceptibility and the ferromagnetic percentage of the sample just slightly
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increased.

3.3 Phase transformation of iron ore sample after roasting

Fig. 10 shows the XRD traces for roasted samples at different temperatures. Compared with

the XRD pattern of raw ore (Fig.1), it is clear to see that most of hematite (Fe2O3) in the raw ore

was converted to magnetite (Fe3O4) after roasting with bituminous coal. According to the

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characteristic diffraction peak value of hematite, there was a certain amount of hematite in the

samples roasted at 650 °C and 750°C yet (Fig. 10d and c). As the roasting temperature was further

raised up to 800°C or 900°C, the characteristic diffraction peak of hematite in roasted samples

disappeared (Fig.10b and a), indicating that the reduction of hematite to magnetite was almost

completed. It is noteworthy that the phases of wustite (FeO) and fayalite (Fe2SiO4) are not found

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in the XRD patterns of roasted samples, which means that the magnetite is not over reduced to

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wustite at above suitable conditions. Perhaps such a short roasting time (8 min) is insufficient to

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the formation of wustite (FeO) and fayalite (Fe2SiO4).
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In order to definitely understand the iron minerals phase conversion, quantitative iron minerals

phase analysis is necessary, and the results are shown in Table 5. It can be seen that a temperature
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of 800 °C seems to be a critical value, at which the fractions of magnetite and hematite were 91.17%

and 6.03%, respectively. At temperatures above 800 °C, the fractions of magnetite and hematite
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almost remained unchanged. This result might be due to that hematite cannot be reduced to
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magnetite completely if its particle size is too coarse, i.e., the surface of the hematite particle was
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reduced to magnetite, but the inner was still hematite crystal lattice. It is worth noting that the

fractions of iron carbonates (mainly exist in siderite and ankerite) decreased until it reached the
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minimum value at 800 °C and then remained almost constant when the temperature increased

further. This result might be contributed to the decomposition of siderite into magnetite in a

reducing atmosphere (Yan et al., 2012(a), Yan et al., 2012(b); Luo et al., 2016;

Baldauf-Sommerbauer et al., 2017; Lin et al., 2017; Baldauf-Sommerbauer et al., 2016; Bai

et al., 2011; Zhu et al., 2016), while the decomposition of ankerite hardly occurred at such low

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roasting temperatures (lower than 900 °C) and short roasting time (8 min) (Gu 1990; Chen et al.,

2014). Meanwhile, the results are greatly in agreement with above analysis.

4. Conclusions

The results of this study indicate that magnetization roasting pre-treatment had a significant

effect upon magnetic properties of hematite ore. The magnetic susceptibility and magnetism

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saturation of hematite ore could be highly increased due to the selective conversion of hematite

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and siderite into magnetite caused by selective reduction roasting. The optimized magnetization

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roasting conditions were obtained as following: roasting at 800 °C for 8 min with 8 wt.% coal.
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Enhancing the magnetism saturation and magnetic susceptibility means that an effective

magnetic separation can be achieved. A high grade concentrate containing 65.4 wt.% iron with an
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iron recovery of 92.7% was achieved by magnetic separation with a grinding fineness of 85 wt.%

passing 38 μm. The results demonstrated that the application of magnetization roasting in iron ore
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beneficiation was prospective to the efficient exploitation and utilization of refractory iron bearing
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resources.
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Acknowledgements

The authors are grateful to the financial support provided to this project by the National
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Science Foundation of China (51674064 and 51674065), and program for the Fundamental

Research Funds for National University, Northeastern University (Grant No. N140108001 and

N150106003).

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Zhu, D., Zhao, Q., Qiu, G., 2010. Magnetizing roasting-magnetic separation of limonite ores from

Anhui province in east China. Journal of University of Science and Technology Beijing 32(6),

713-718. (In Chinese)

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Zhu, Q., Li, H., 2014. Status quo and development prospect of magnetizing roasting via fluidized

bed for low grade iron ore. CIESC Journal 65(7), 2437-2442. (In Chinese)

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Figures for the manuscript:

Figure captions

Fig. 1 XRD pattern of raw ore

Fig. 2 Schematic diagram of the experimental flow sheet

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Fig. 3 Effect of roasting temperature on Fe content and recovery in magnetic

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fraction (roasting time: 8 min, coal to ore ratio: 8wt% (8g coal/100g ore))

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Fig. 4 Effect of roasting time on Fe content and recovery in magnetic fraction

(roasting temperature: 800 °C, coal to ore ratio: 8wt%)

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Fig. 5 Effect of coal to ore ratio on Fe content and recovery in magnetic fraction
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(roasting temperature: 800 °C, roasting time: 8min)

Fig. 6 Effect of roasting temperature on saturation magnetism of roasted samples

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(roasting time: 8 min, coal to ore ratio: 8wt%)

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Fig. 7 Effect of roasting time on saturation magnetism of roasted samples

(roasting temperature: 800 °C, coal to ore ratio: 8wt%)

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Fig. 8 Effect of coal to ore ratio on saturation magnetism of roasted samples

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(roasting temperature: 800 °C, roasting time: 8min)

Fig. 9 Honda-Owen plots for different samples

Fig. 10 XRD patterns of sample roasted at different temperature; (a) 900 °C, (b)

800 °C, (c) 750 °C and (d) 650 °C

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Fig. 1 XRD pattern of raw ore

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Fig. 2 Schematic diagram of the experimental flow sheet
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Fig. 3 Effect of roasting temperature on Fe content and recovery in magnetic fraction
(roasting time: 8 min, coal to ore ratio: 8wt.% (8g coal/100 g ore))
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Fig. 4 Effect of roasting time on Fe content and recovery in magnetic fraction
(roasting temperature: 800 °C, coal to ore ratio: 8 wt.%)
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Fig. 5 Effect of coal to ore ratio on Fe content and recovery in magnetic fraction
(roasting temperature: 800 °C, roasting time: 8 min)
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Fig. 6 Effect of roasting temperature on saturation magnetism of roasted samples
(roasting time: 8 min, coal to ore ratio: 8wt.%)
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Fig. 7 Effect of roasting time on saturation magnetism of roasted samples (roasting
temperature: 800 °C, coal to ore ratio: 8wt.%)
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Fig. 8 Effect of coal to ore ratio on saturation magnetism of roasted samples (roasting
temperature: 800 °C, roasting time: 8min)
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Fig. 9 Honda-Owen plots for different samples
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Fig. 10 XRD patterns of sample roasted at different temperature; (a) 900 °C, (b)
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800 °C, (c) 750 °C and (d) 650 °C

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Tables for the manuscript:

Table captions

Table 1 Main composition of raw ore (mass fraction, %)

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Table 2 Proximate analysis results of bituminous coal

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Table 3 Multi-elements analysis of iron concentrate

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Table 4 Magnetic susceptibility of paramagnetic and ferromagnetic fractions at

the field H= 100 kA/m in samples

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Table 5 Chemical phases of Fe and its distribution in raw ore and roasted samples
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Table 1 Main composition of raw ore (mass fraction, %)

Composition TFe SiO2 Al2O3 CaO MgO Mn K S P LOI
Percent 34.60 43.34 0.73 0.55 0.72 0.1 0.11 0.06 0.04 2.63

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Table 2 Proximate analysis results of bituminous coal

Fixed Carbon Volatile matter Ash content Moisture Fuel
(wt.%) (wt.%) (wt.%) (wt.%) Ratio
67.83 18.45 12.00 1.48 3.68

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Table 3 Multi-elements analysis of iron concentrate

Compositions TFe SiO2 S P As Cu Pb Zn K Na
Content/wt.% 65.43 7.77 0.01 0.02 <0.01 <0.01 <0.01 0.01 0.04 0.05

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Table 4 Magnetic susceptibility of paramagnetic and ferromagnetic fractions at the

field H= 100 kA/m in samples
Sample Roasting Magnetic susceptibility (10-6 m3/kg)
code temp.( °C) Total Paramagnetic Ferromagnetic
8.80 4.91 3.89
A --
100% 55.80% 44.20%
30.83 2.01 28.82

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B 700
100% 6.52% 93.48%
36.90 1.67 35.23

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C 800
100% 4.53% 95.47%

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37.55 1.57 35.98
D 900
100% 4.19% 95.81%
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Table 5 Chemical phases of Fe and its distribution in raw ore and roasted samples
Distribution (%)
Roasting temp.
In In In In In Total
(°C )
magnetite hematite carbonate sulfide silicate Fe
9.44 22.4 2.23 0.11 0.42 34.6
Raw ore
27.29 64.76 6.45 0.29 1.21 100
21.92 11.29 0.65 0.03 0.41 34.3

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650
63.91 32.92 1.89 0.09 1.2 100

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29.55 4 0.57 0.03 0.4 34.55
700
85.53 11.56 1.65 0.09 1.16 100

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30.27 3.22 0.52 0.03 0.41 34.45
750
87.87 9.35 1.51 0.09 1.19 100
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31.27 2.07 0.51 0.03 0.42 34.3
800
91.17 6.03 1.49 0.09 1.22 100
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31.46 1.98 0.52 0.03 0.41 34.4

850
91.45 5.76 1.51 0.09 1.19 100
D

31.51 1.78 0.53 0.03 0.42 34.27

900
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91.95 5.19 1.55 0.09 1.22 100

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Graphical abstract NU
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Highlights

1. The beneficiation of a low-grade hematite ore fines containing carbonates with magnetization

roasting and magnetic separation was proposed and studied.

2. The magnetic susceptibility and magnetism saturation of hematite ore can be highly increased

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due to the selective conversion of hematite and siderite into magnetite.

3. Magnetization roasting followed by magnetic separation can be applied effectively for the

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processing of carbonate-containing hematite ore.

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