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10 Aug 2022

Two-step flotation and reverse flotation circuits of iron oxide and

its process minerology
Ying Hou

Song Lin

Guohui Fu

Zhuang Gai

et. al. For a complete list of authors, see https://scholarsmine.mst.edu/min_nuceng_facwork/1856

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Recommended Citation
Y. Hou et al., "Two-step flotation and reverse flotation circuits of iron oxide and its process minerology,",
Aug 2022.
The definitive version is available at https://doi.org/https://doi.org/10.21203/rs.3.rs-1930653/v1

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Two-step flotation and reverse flotation circuits of iron
oxide and its process minerology
Ying Hou
University of Science and Technology Liaoning
Song Lin
University of Science and Technology Liaoning
Guohui Fu
Anshan Iron and Steel Group
Zhuang Gai
Anshan Iron and Steel Group
Guang Yang
Anshan Iron and Steel Group
Ahmed Sobhy (  [email protected] )
Central Metallurgical Research and Development Institute

Article

Keywords: Magnetite, hematite, quartz, starch, two-step flotation, reverse flotation

Posted Date: August 10th, 2022

DOI: https://doi.org/10.21203/rs.3.rs-1930653/v1

License:   This work is licensed under a Creative Commons Attribution 4.0 International License. Read Full License

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Abstract
Mining operations usually provide ore of varying characteristics. Similarly, for Donganshan Sintering Plant, the charges
in iron oxide ore especially prior flotation process were investigated by conducting mineral liberation analyzer “MLA”.
This in-deep study of process mineralogy explored and analyzed the mechanism of difficulty to obtain high-efficient
flotation process. The MLA analysis results showed also that the main useful minerals in this ore are
magnetite/hematite, and the main gangue minerals is quartz, followed by chlorite and ankerite. In addition, two-step
“direct then reverse” and one step “reverse” flotation experiments were carried out and produced iron oxide concentrates
of 48.91% and 49.45% yield; 65.03% and 65.22% grade; 70.96% and 72.08% recovery respectively. Besides, the process
flow sheet was simplified with reduced reagent consumptions.

1. Introduction
Majority of iron ore reserves in China are low-grade, finally disseminated, and scattered reserves (Li et al., 2014). The
estimated national reserves are more than 20 billion tons (“Seven countries with the largest iron ore reserves in the world
in 2019,” n.d.), and one fifth of the estimated reserve is located in Anshan region, Liaoning (Jia et al., 2013). Large
proportion is low-grade, complex, difficult-to-separate carbonate-containing refractory iron ore (Li et al., 2016). With the
mining operation development, the carbonate contents increase in the iron ore produced at Donganshan Sintering plant,
which negatively affect the reverse flotation efficiency (Li et al., 2012). The current Donganshan Sintering Plant iron ore
contains mainly magnetite and hematite fine-grained particles, which are easy to lose in the flotation tailings (Li et al.,
2016).

A two-step flotation processes mainly for carbonaceous iron ore was developed and applied for Donganshan iron ore
(Pattanaik and Venugopal, 2018; Yin et al., 2010; Zhang et al., 2019), which is mainly divided into two parts; first by direct
flotation at neutral conditions and second by reverse flotation under alkaline condition (Fan et al., 2020; Filippov et al.,
2021; Silva et al., 2021; Zhang et al., 2019). Due to the change of the original mineral properties, it is worth exploring the
flotation process and its chemical reagent system of mixed magnetically separated particles. The flotation performance
is significantly affected by the amount of flotation reagents which has been studied extensively (Hou et al., 2020; Hou
and Sobhy, 2021; Sobhy et al., 2021; Tao et al., 2021; Zhang and Gao, 2022). Thus, in flotation circuit, unsuitable reagent
system leads to metal loss with reduced product quality. It is worth mentioning that iron reverse flotation is carried out by
floating the gangue minerals such as quartz while depressing the iron minerals in the slurry. The reagent system
comprises of pH regulators, depressants, activators, and collectors (Hou and Sobhy, 2021).

In this work, the mixed magnetically separated particles at Donganshan Sintering Plant were subjected to two-step
flotation and reverse flotation circuits for comparison purpose. Besides, with the assistance of Advanced Mineral
Identification and Characterization System (AMICS), the process mineralogy characteristics were studied, and the
mechanism of high-efficiency flotation was given.

2. Materials And Methods

2.1. Materials
The experimental sample is a representative flotation feed, which is a mixture of particles after low-intensity and high-
gradient magnetic separation from Donganqian Sintering Plant, Anshan, Liaoning, China. The as-received sample was
dried to remove the moisture contents, split into small portions, and sealed in plastic bags for later usages.
2.2. Sample characterization

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For accurate characterization, 100 grams representative samples were classified by sizing into three closed sizes using
74 µm and 38 µm standard sieves. The samples were homogenized by mixing and then mounted in epoxy, then polished.
The polished samples were subjected to carbon-spray by C-ion sputter evaporator to ensure conductivity on the sample
surface.

The full characterization was carried out by conducting AMICS, which combines advanced image analysis to segment
particles of mineral phases boundary, element analysis with Sigma 500 and scanning electron microscopy SME for high
quality imaging of 300x magnification, and X-ray microscopy with hybrid mode options of backscattered electrons
(XBSE) with the QUANTEX EDS system for advanced analytical microscopy. The measurements were performed under
the following parameters; an accuracy of 0.56 µm pixels, a probe current of 10 nA, and an acceleration voltage of 20 kV
for the total electron beam. The background is then epoxy resin (BSE grayscale value < 35) and metal as the upper limit
(BSE grayscale value > 255). The backscatter electron (BSE) set up was accomplished by image gray scale calibration,
and the resulting data is processed by AMICS Process software.
2.6. Experimental methods
Laboratory flotation experiments were conducted using temperature controlled XFG-ⅡI flotation machine with a 1.5 L cell
at 35oC temperature, 33.3% solids, and 1920 rpm rotor speed. Unless otherwise stated, the sample suspensions pH was
adjusted to 11.5 by adding pH regulators (NaOH) for 3 min, and then the starch was mixed for 3 minutes. CaO was
added for 3 minutes to activate the quartz to accommodate the adsorption of TD-II anionic collector for 2 minutes. The
flotation time was kept constant at 3 minutes. The froth was scraped manually by using a plastic blade. The
concentrates and tailings were dried, weighed, and analyzed for the total iron grade and recovery.

3. Results And Discussion

3.1. Two-step flotation circuit
As an open circuit, direct flotation experiments were conducted using 0.8 kg/t starch and 0.2 kg/t TD-II collector to float
magnetite/hematite at pH 11.5. Then reverse flotation at 11.5 pH was conducted using 0.5 kg/t starch, 0.8 kg/t calcium
oxide, and 0.8 kg/t TD-II collector, and 0.4 kg/t TD-II collector for each scavenging step, and the results are shown in
Table 1. It is clear from Table 1 that the final grade of 66.28% with 64.90% recovery was obtained.

Table 1
Open circuit results of two-step flotation process.
Product Name Yield (%) Total Fe grade (%) Total Fe Recovery (%)

Final Concentrate 44.53 66.28 64.90

First Tailings 10.61 43.22 9.72

Scavenging I 5.43 44.43 5.30

Scavenging II 3.42 33.23 2.50

Scavenging III 3.11 23.79 1.63

Second Tailings 32.90 22.05 15.95

Total (Feed) 100.00 45.48 100.00

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The closed flotation circuit using the same operation conditions mentioned in the open-circuit process with using 0.4
kg/t TD-II when required in each scavenging step at pH 11.5 as illustrated in Fig. 1, the final concentrate of 48.91% yield,
65.03% total iron, and 70.96% recovery was accomplished.
3.2. Flotation feed characterization
3.2.1. Mineral composition
SEM, EDS energy spectrum, and AMICS analysis system showed that the main valuable minerals in the flotation feed of
Donganshan Sintering Plant are magnetite / hematite minerals, and the main gangue minerals are quartz, and a wide
variety of other minerals. The mineral content of each of which is shown in Table 2.

Table 2
Mineral quantitative analysis results of flotation feed.
Mineral Magnetite/ Quartz Chlorite Ankerite Illite Pyroxferroite Calcite Ferrohypersthene
Name
hematite

Wt (%) 62.99 29.97 2.55 1.48 0.72 0.35 0.35 0.18

Mineral Oligoclase Pyrite Apatite Dolomite Orthoclase Siderite Other Total

Name

Wt (%) 0.15 0.14 0.12 0.11 0.11 0.03 0.75 100.00

Table 2 shows that 62.99% of the flotation feed consists of magnetite and hematite valuable minerals, and 29.97%
quartz as gangue mineral followed by other impurities. Pulsar minerals such as chlorite (turquoise) and ankerite (iron
dolomite) are about 2.55% and 1.48%, respectively. Sulfur-containing minerals are mainly yellow iron ore (pyrite),
phosphorous-containing minerals are mainly phosphorite (apatite), and their contents are 0.14% and 0.12%, respectively.
The content of iron carbonate ore (siderite) is only 0.03%.
3.2.2. Size distribution of major mineral grains
The particle size of the flotation feed at Donganshan Sintering Plant is 87.61% finer than 0.074 mm particle size. The
particle size distribution of the main minerals in the flotation feed is analyzed by the AMICS test system, and the results
are shown in Fig. 2.

Figure 2 shows that the particle sizes of magnetite/hematite and quartz in the flotation feed are coarser, the granularity
of chlorite is finer than that of magnetic/hematite and quartz, and the particle size of iron dolomite is the finest. It can be
seen from the analysis that during grinding, magnetic/hematite and quartz are not easily ground, while chlorite and
ankerite are easily ground and muddy phenomena occur, which will have a greater impact on subsequent flotation
separation.
3.2.3. Major mineral liberation characteristics
The degree of liberation of minerals directly affects the subsequent flotation performance, and in order to further
understand the liberation characteristics of the main valuable minerals (magnetite/hematite), primary gangue quartz,
and other minerals, the degree of liberation of magnetic/hematite, quartz, turquoise and iron dolomite were analyzed. As
can be seen from Table 3, the 100% mineral liberation of magnetic/hematite, quartz, turquoise and ankerite are 76.38%,
75.4%, 50.16%, and 66.13% respectively in the flotation feed.

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In the flotation feed, the mineralogical characterization of the magnetite/hematite particle of 88.66% purity contains
6.58% quartz, while the quartz gangue mineral particle of 93.34% purity consists of 4.79% magnetite/hematite (Table 4).
Besides, 71.83% and 86.24% purity turquoise and ankerite contain 16.33% and 5.22% magnetite/hematite respectively in
addition to 5.88% and 3.11% quartz respectively (Table 4).

Table 3
Degree of liberation of main minerals in the flotation feed.
Mineral Name liberation degree (%)

0%<x < = 25% 25%<x < = 50% 50%<x < = 75% 75%<x < 100% 100%

Magnetite/hematite 1.74 3.14 5.8 12.94 76.38

Quartz 4.79 3.69 5.89 10.23 75.4

turquoise 19.19 9.36 9.01 12.28 50.16

Ankerite 7.24 5.57 8.94 12.12 66.13

Table 4
Mineralogical characterization of the particles of the main minerals in the flotation feed.
Mineral Name Magnetite/hematite Quartz Turquoise Ankerite Others Total

Contents 88.66 6.58 2.37 0.27 2.12 100

4.79 93.34 0.56 0.11 1.2 100

16.33 5.88 71.83 1.05 4.91 100

5.22 3.11 0.58 86.24 4.85 100

The X-ray microscopy with hybrid mode options of backscattered electrons for mineral map images shown in the Fig. 3
indicate the advanced particle segmentation of magnetic/hematite, quartz, chlorite, ankerite, and other minerals. Figure 3
shows also those main minerals are not fully liberated

From Magnetite / hematite, quartz, chlorite and ankerite mineral liberation results shown in the Figs. 3 and 4, it can be
seen that the chlorite mineral liberation is the lowest in comparison to other minerals, and both magnetite/hematite and
quartz have the same degree of liberation (Fig. 4).
3.3. Reverse flotation circuit
The issue with the two-step flotation plant circuit is the high iron carbonate (siderite) content in Dong'anshan mixed
magnetically separated concentrates, but the current analysis shows that there is only 0.03% of siderite in the flotation
feed, which is no longer the main mineral affecting flotation indicator. The main impact on the flotation performance
became associated with the amount of chlorite and ankerite in the flotation feed as well as the quartz content.

In this view of the low content of iron carbonate ore, there is no need to use the two-step flotation circuit. Therefore, this
paper recommends a reverse flotation circuit for the East Anshan difficult-to-upgrade mixed magnetically separated
particles, trying to obtain a better separation performance while simplifying the process with lower reagent
consumptions.

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The suggested flotation process conditions based on an extensive investigation in a previous work by the authors are:
11.5 pH value, 1 kg/t of starch, 0.3 kg/t of calcium oxide, and 0.4 kg/t of TD-II in the rougher flotation step, then 0.3 kg/t
of TD-II at pH 11.5 in the cleaner flotation step, while the three scavenging steps were carried out at 11.5 pH value. The
open circuit produced a final concentrate of 32.15% yield, 65.63% grade, and 47.39% recovery as shown in Table 5. While
the closed-circuit process test at the same conditions as illustrate in Fig. 5 produced a concentrate of 49.45% yield,
65.22% grade, and 72.09%.

Table 5
Open circuit results of reverse flotation process.
Product Name Yield (%) Total Fe grade (%) Total Fe Recovery (%)

Final Concentrate 32.15 65.63 47.39

Scavenging I 7.19 51.23 8.27

Scavenging II 3.50 43.68 3.44

Scavenging III 3.50 37.03 2.88

Final Tailings 53.70 31.54 38.03

Total 100.00 44.53 100.00

3.4. Comparison between two-step and reverse flotation circuits

The two-step and reverse flotation results are shown in Table 6. It shows that the product quality of the reverse flotation
circuit is comparable to the two-step circuit with 0.54% higher yield, 0.19% higher grade, and 1.12% higher recovery with
reducing the reagent consumptions by 0.3 kg/t starch, 0.5 kg/t calcium oxide, and 0.7 kg/t TD-II. Furthermore,
simplifying the processes with reducing the dosage of flotation reagents has a greater advantage.

Table 6
Two-step and reverse flotation circuit
Process Product Name Yield (%) Total Fe grade (%) Total Fe Recovery (%)

Two-step flotation circuit First Tailings 9.20 38.52 7.90

Concentrate 48.91 65.03 70.96

Second Tailings 41.90 22.62 21.14

Feed 100.00 44.82 100.00

Reverse flotation circuit Concentrate 49.45 65.22 72.08

Tailing 50.55 24.71 27.92

Feed 100.00 44.77 100.00

Comparison Concentrate + 0.54 + 0.19 + 1.12

4. Conclusions
The most significant conclusions are as following:

1. The two-step flotation circuit of Donganshan mixed magnetically separated concentrate produced of 44.82% grade
produced a final product 48.91% yield, 65.03% grade, and 70.96% recovery.
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 2. The two-step flotation circuit solves the problem of high iron carbonate content in Donganshan flotation feed, but
for the current analysis presence of 0.03% siderite is no longer the main mineral affecting flotation performance, and
the main minerals that affect the performance are chlorite and ankerite with low degree of liberation.
3. The reverse flotation circuit of a giving flotation feed of 44.77% grade can produce a concentrate of 49.45% yield,
65.22% grade, and 72.08% recovery.
4. The reverse circuit with greater advantages simplified, improved the performance, and reduced the reagent
consumptions.

Declarations
The authors have no competing interests to declare that are relevant to the content of this article.

Data availability
The datasets generated and/or analyzed during the current study are not publicly available due to institutional roles and
confidential conditions but are available from the corresponding author on reasonable request.

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Figures

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Figure 1

Flow-chart of closed-circuit test of two-step flotation.

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Figure 2

Particle size analysis of main minerals

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Figure 3

AMICS images of mineral map after particle mode analysis of flotation feed sample.

Figure 4

The comparison of degree of mineral liberation.

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Figure 5

Flow chart of closed-circuit process.

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