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. 2025 Feb 4;15:4197. doi: 10.1038/s41598-025-88448-9

Removal of iron and manganese from acidic aqueous solution by pyrite and pyrite-calcium sulfite

Xu Zhang 1,2,✉, Yajing Wang 1,2,✉, Gesang Nima 3, Ziqian Wang 1, Caifeng Huang 1
PMCID: PMC11794849  PMID: 39905187

Abstract

Pyrite and calcium sulfite were used to remove iron and manganese from an acidic aqueous solution. The concentration of Fe was decreased to be smaller than 0.05 g/L in 60 min when pyrite and air were added into the acidic aqueous solution, but the concentration of Mn in the solution remained unchanged. After the process of iron removal, calcium sulfite and air were used to remove manganese ions from the solution, and the efficiency of manganese ion removal was larger than 75% in 240 min (with less than 0.05 g/L Fe and 0.5 g/L Mn in the solution). Meanwhile, experiments were conducted to simultaneously remove iron and manganese from artificially simulated acidic leaching solution of laterite nickel ore. When the proposed method was used to purify the leaching solution of laterite nickel ore, Fe3+ and Mn2+ ions were effectively removed from the acidic solution, and the recovery efficiency of nickel and cobalt was greater than 98%.

Keywords: Iron removal, Manganese removal, Pyrite, Goethite, Laterite nickel ore

Subject terms: Chemical engineering, Geochemistry, Mineralogy, Solid Earth sciences, Engineering

Introduction

Iron and manganese are very important chemical elements in the Earth’s environmental cycle, and are extensively present in minerals1,2. In the process of mineral resource development and valuable metal extraction, iron and manganese inevitably dissolve into the solution with the main metal, especially during the acid-leaching process of ores. It is essential step to remove iron and other impurities from the leaching solution to prepare pure metal compounds or other products. Hence, the removal of iron and other impurity ions plays a very important role in the process of hydrometallurgy3. A simple method employed to remove iron and manganese ions from the leaching solution has a certain industrial significance for a hydrometallurgical process.

Laterite ore contributes to about 70% of the world’s land-based nickel resources (As of 2023, the total nickel reserves across the world amounted to around 130 million metric tons.)4,5. After the leaching process of laterite nickel ore, iron and manganese are the main impurity ions in the leaching solution6,7. Precipitation is one of the most common methods utilized to separate, purify, and recover metals. In the solution, iron ions usually need to be converted into Fe (III) to form jarosite, goethite, hematite, and other precipitates to achieve the purpose of iron removal8. In an acidic solution, manganese mainly exists in the form of Mn (II). To remove manganese ion from an acidic solution, it is necessary to oxidize Mn (II) into Mn (III) or Mn (IV), and precipitate it in manganese dioxide, manganous oxide, or hydroxy manganese oxide9. A complex solution environment is often required to selectively remove iron and manganese from the leaching solution of laterite nickel ore.

We introduced a process for the removal of iron and manganese from the leach solution of laterite nickel ore using pyrite as a mediator10. The process was based on the iron removal method by goethite, interface reaction of pyrite in solution, and oxidation reduction potential of manganese ion in solution. Early reports on the process of iron removal by goethite demonstrated that when the Fe (III) concentration was more than 2 g/L, it was difficult for Fe (III) to directly hydrolyze into goethite in aqueous solution. However, Fe (II) could be precipitated in the form of goethite during the oxidation reaction process. Table 1 shows some differentmethods of iron and manganese removal from solutions. Pyrite (FeS2) can react with oxygen or Fe (III) in solution as a reducing substance. Some investigations on pyrite oxidation and pyrite photocatalysis suggested that oxygen could interact with pyrite to form active oxygen17–19. A complex redox reaction system is appeared acting around pyrite particles by the possible reaction, ionic behavior, and active oxygen in the solution. Based on this complex system, we investigated the removal of iron and manganese from acidic aqueous solution by pyrite and pyrite-calcium sulfite. Furthermore, the effects of pyrite dosage, pH, air volume, temperature, and use of pyrite-calcium sulfite on the simultaneous removal of iron and manganese were investigated, and parameters of the optimum process were determined. Meanwhile, experiments were conducted to simultaneously remove iron and manganese from artificially simulated acidic leaching solution of laterite nickel ore.

Table1.

Some methods of iron and manganese removal from solutions.

liquor pH, Temperature and time in the operation Precipitation efficiency The method References
[Me]total(g/L) [Ni](g/L) [Co] (g/L) pH Temperature time Me removal Ni
loss		 Co
loss
Fe 14.0 0.63 – 2.5–3.0 95 °C 260min > 92% 4.12% – Removal of iron via goethite precipitation by the Vieille Montgane technique 11,12
Fe 1.88 1.63 0.115 3.7–3.8 90–95 °C 80min > 99% 1.6% 0.4–1.6% Using NH4OH as a precipitating agent to removal iron as jarosite and goethite phases 13
Fe 24.9 4.1 0.20 4.0 90 °C 120min > 95% 4% 7% Using an oxidative hydrolysis technique targeting goethite precipitation from a synthetic laterite leach solution containing Fe, Ni and Co 14
Mn 0.328 0.153 0.068 1.5 25 °C 90min 97% < 1%  < 2% Manganese precipitation from nickel laterite leached solution by ozone oxidation 15
Mn 9.15 31.3 1.67 pH = 7, pH = 2 50 °C 120min 99.5% 1.7% 11% Using O2 to convert Mn2+to MnO2 at pH = 7 (Ni and Co were precipitated in the solid residues) and sulfuric acid to leach Ni and Co at pH = 2 16
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Experimental method

Pyrite and artificially simulated acidic leaching solutions were used in the present study. The sample of pyrite was obtained from Guizhou Province of China and milled into a size smaller than 150Inline graphic m. The chemical analysis of the sample, which was used in the next experiments, showed 49.08% Fe, 43.63% S, and 2.57% SiO2. The main component of the sample was pyrite, which was determined by X-ray diffractograms. All reagents used in the experiments were provided by the company of Sinopharm Chemical Reagent Co., Ltd, and analytical grade. Distilled water is used in the experiments. The following reagents were used to prepare artificially simulated leaching liquids: NiSO4·6H2O (≥ 98% purity), CoSO4·7H2O(≥ 99% purity), Fe2(SO4)3 (≥ 99% purity), MnSO4·H2O (≥ 99% purity), and Al2(SO4)3·18H2O (≥ 99% purity). H2SO4 (≥ 99% purity) and CaCO3 (≥ 99% purity) were used to adjust the pH changes during the experiments. The experiments were conducted in a 250-ml glass reactor. A certain amount of pyrite and 200 ml of simulated liquid were added into the reactor, and air was introduced into the mixed liquid through the air pump. A rotameter was used to control the gas velocity and a constant-temperature water bath was used to control the temperature16. The value of pH was monitored during the process and was measured by a pH meter (Rex laboratory PHS-25, a combination electrode). The concentration of iron and manganese ions in the solution was determined by ICP (Thermo Fisher iCAP PRO, USA) during the experiments. The crystal structures of the selected samples were determined using X-ray diffractograms (XRD, Bruker D8 Advance, DEU). SEM–EDS (TESCAN MIRA LMS, CZE) and XPS (Thermo Scientific K-Alpha, USA) the results were used to investigate the process of removing iron and manganese ions in the experiments.

The removal efficiency of Fe or Mn was determined using the following arithmetic formula:

graphic file with name M2.gif 1

where ε stands for the removal efficiency of Fe or Mn. Ci and Ct represent the concentration of Fe or Mn initially and after a period of reaction, respectively. The recovery efficiency of Ni or Co was determined using the following equation:

graphic file with name M3.gif 2

where E denotes the recovery efficiency of Ni or Co. CI and CT represent the concentration of Ni or Co initially and after a period of reaction, respectively.

Results and discussion

Figure 1 shows the X-ray patterns of the sample of pyrite. The result of Fig. 1 shows that It is mainly in the form of FeS2 in the sample. Table 2 presents the chemical compositions of the artificially simulated acidic leaching solutions that were used in the study. The initial pH of the artificially simulated acidic leaching solutions was controlled at 1.8 ± 0.1. Figure 1 shows the X-ray patterns of the sample of pyrite.

Fig. 1.

Fig. 1

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XRD of the sample of pyrite (Cu target, 5°/min).

Table 2.

Chemical compositions of the artificially simulated acidic leaching solutions used in the study.

Liquid pH Fe3+ (g/L) Mn2+ (g/L) Ni2+ (g/L) Co2+ (g/L) Al3+ (g/L)
L1 1.7 3.04 1.98 – – –
L2 1.8 3.05 1.96 1.58 – 0.85
L3 1.9 3.05 1.97 1.58 0.26 0.85
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Removal of iron and manganese from acidic aqueous solution by pyrite or pyrite-calcium sulfite

The effects of pyrite dosage (10 g/L, 15 g/L, 20 g/L, 25 g/L), pH (2.0 ± 0.1, 2.5 ± 0.1, 3.0 ± 0.1, 3.5 ± 0.1), air volume (0.8 L/min, 1.6 L/min, 2.4 L/min, 3.2 L/min), and temperature (25 °C, 35 °C, 45 °C, 55 °C) on the simultaneous removal of iron and manganese were investigated. Liquid L1 was used in the test. During the experiment, we added the sample of pyrite and air in the liquid and control the pH at a certain stable value. A mixed emulsion of calcium carbonate and deionized water was used to control the pH. We found that iron ions could precipitate rapidly in the solution, but the concentration of manganese ions remained unchanged. Figure 2 exhibits the effects of the above-mentioned parameters on iron removal. Figure 2a reveals the effects of pyrite dosage on the removal of iron ions from liquid L1. When no pyrite was added to the liquid L1, the iron ions in the solution were not removed. And the removal efficiency of Fe increased very quickly when pyrite was added to the liquid L1 under the experimental conditions of pH = 2.5 ± 0.1, air volume of 2.4 L/min, and temperature of 25 °C. The removal efficiency of Fe was enhanced with the growth of pyrite dosage and reached more than 95% after 30 min of the reaction due to the pyrite dosage beyond 15 g/L. It is worth mentioning that the method of adding pyrite for Fe removal had better advantages than other traditional methods such as adding jarosite, goethite, or hematite for Fe removal. Figure 2b displays the results of the effects of pH (2.0–3.5) on the removal efficiency of Fe from the liquid L1. It is generally believed that pH is an important parameter for the removal of iron ions from solutions and the value of pH will significantly affect the efficiency of iron removal14,20,21. However, after adding pyrite and air to remove iron from the liquid L1, the removal efficiency of Fe could achieve a high value (larger than 98%) in 90 min in the pH range 2.0–3.5. When the value of pH was greater than 3.0, the removal efficiency of Fe reached 99% in 60 min. Figure 2c and d show the results of the effects of air volume and temperature on the removal efficiency of Fe, respectively. When air was not added to the solution, the iron ions in the solution were not removed. The reactions between Fe3+ and FeS2 or CuFeS2 have been reported in many research papers22–26. The removal rate of iron ions in the solution was significantly affected by air volume and pyrite dosage. The removal efficiency of Fe reached 95% in 30 min, when the air volume was more than 2.4 L/min. Figure 2d indicates that the temperature has an obvious impact on the removal efficiency of Fe within the initial 10 min of the experiments, and the temperature effect begins to weaken after 30 min of the experimental reaction.

Fig. 2.

Fig. 2

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Effects of pyrite dosage, pH, air volume, and temperature on the removal of iron ions from the liquid L1: (a) effects of pyrite dosage on the removal of iron ions from the liquid L1 (pH = 2.5 ± 0.1, air volume = 2.4 L/min, and temperature = 25 °C), (b) effects of pH on the removal of iron ions from the liquid L1 (pyrite dosage = 15 g/L, air volume = 2.4 L/min, and temperature = 25 °C), (c) effects of air volume on the removal of iron ions from the liquid L1 (pyrite dosage = 15 g/L, pH = 2.5 ± 0.1, and temperature = 25 °C), (d) effects of temperature on the removal of iron ions from the liquid L1 (pyrite dosage = 15 g/L, pH = 2.5 ± 0.1, and air volume = 2.4 L/min).

The concentration of Fe in the liquid L1 could be reduced to smaller than 0.05 g/L in 60 min with the method of adding pyrite and air into the liquid L1. But the concentration of Mn in the solution remained unchanged during the experimental reaction in 90 min. To further remove manganese ions from the liquid L1, a mixed suspension of calcium sulfite and deionized water (1.2 g of calcium sulfite and 10 ml of deionized water) was added to remove manganese ions from the solution, after 30 min of the liquid was treated with pyrite and air. Some researchers have studied the oxidant system of SO2/O2 in aqueous solutions and reported that the oxidant system of SO2/O2 could cause the oxidation of Mn2+ to MnO2 or Mn2O3 (the oxidation of Mn2+ to Mn4+ or Mn3+). During the experiments, 1.2 g of calcium sulfite was used for every 200 ml of the liquid L1, and the mixed suspension of calcium sulfite and deionized water was slowly added dropwise in 200 min. Figure 3 shows the removal efficiency of Mn using calcium sulfite and air after adding pyrite and air for 30 min. The method of adding calcium sulfite and air in the liquid could effectively decrease the concentration of manganese ions in the liquid L1 and the removal efficiency of manganese ion was greater than 75% after 240 min (with less than 0.05 g/L Fe and 0.5 g/L Mn in the solution).

Fig. 3.

Fig. 3

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Removal of manganese ions from the liquid L1 using calcium sulfite and air (pyrite dosage = 15 g/L, pH = 3.0 ± 0.1, calcium sulfite dosage = 6 g/L, air volume = 2.4 L/min, and temperature = 25 °C).

Analysis and reaction mode of iron and manganese precipitation in the experiments

Removal of iron and manganese ions from the solution using pyrite and pyrite-calcium sulfite is a very complex chemical process. The experimental process can be divided into two following parts: part (a) the process of iron ions removal from the liquid L1, and part (b) the process of manganese ions removal from the liquid L1. There are many chemical reactions in part (a) and part (b). The free energy values in the equations cited from HSC chemistry 6.0.

The following reactions are those that occur in part (a)27–30:

graphic file with name M4.gif 3
graphic file with name M5.gif 4
graphic file with name M6.gif 5
graphic file with name M7.gif 6

The following reactions are those that occur in part (b)31–34:

graphic file with name M8.gif 7
graphic file with name M9.gif 8
graphic file with name M10.gif 9

Based on the chemical reactions in the solution and the redox potential of the solution, the diagram of Eh–pH is described in Fig. 4. From the Eh–pH of Fe3+/FeS2/O2, it can be observed that there is a transition pH range between 2 and 4, where the Fe2+/FeOOH can react at low redox potentials. As the reaction between Fe3+/FeS2, Fe2+ was generated around the pyrite particles in the solution, and then it reacted with oxygen to form precipitate, which was the mechanization of the method of the rapid Fe removal from the solution. The Eh–pH of Mn2+/SO2(CaSO3)/O2 exhibits that Mn2+ could react with oxygen in the solution at a transition pH range between 2 and 4. Owing to the extremely low solubility of oxygen in the solution, it was not easy to oxidize Mn2+ and form manganese oxide precipitates at a pH range between 2 and 4. Some studies have indicated that SO2(CaSO3)/O2 can be utilized as an oxidant to cause the oxidation of Mn2+ to form the precipitates of MnO2 and Mn2O3. These studies suggested that HSO3− could react with oxygen to generate HSO5−, and HSO5− was a strong oxidizing agent for oxidizing low-valence manganese ions to high-valence manganese ions32,34.

Fig. 4.

Fig. 4

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The Eh–pH diagram of Fe3+/FeS2/O2 and Mn2+/SO2(CaSO3)/O2: (a) the Eh–pH of FeS2/O2 in the removal process of Fe (Fe3+ = 0.1 mol/L) at 25 °C, (b) the Eh–pH of SO2(CaSO3)/O2 in the removal process of Mn (Mn2+ = 0.1 mol/L) at 25 °C.

The XRDs of precipitation after removing iron and manganese are shown in Fig. 5. Figure 5 suggests that the main components of these two precipitates are calcium sulfate and a small amount of pyrite. Due to the excessive addition of pyrite dosage, some pyrite particles were the remaining substance after the reaction. Calcium sulfate was the product generated by adjusting the pH of calcium carbonate. Figure 5 also suggests that amorphous iron compounds and amorphous manganese compounds are present in the precipitates. To further characterize the amorphous iron and manganese compounds of the precipitation, the results of the XPS analysis of the precipitates are displayed in Fig. 6. From Fig. 6a and c, we found that there are four peaks in the Fe 2p region, namely 706.3 ± 0.1 eV, 710.9 ± 0.3 eV, 719.0 ± 0.1 eV, and 724.4 ± 0.1 eV. The peak of 706.3 ± 0.1 eV agreed with the values reported in the literature for FeS235–37. The peaks of 710.9 ± 0.3 eV and 724.4 ± 0.1 eV were attributed to FeOOH38,39. The Mn 2p spectrum in Fig. 6b exhibits the method of only using pyrite and air in the experiment couldn’t remove manganese from the solution, which matches the experimental data well. Figure 6d shows the valence state of the manganese element and possible manganese compounds after the precipitation of Mn2+. The peaks of Mn 2p were 653.7 ± 0.3 eV and 641.5 ± 0.2 eV, which agreed with the values reported for MnO2 and Mn2O340–42. Figure 7 showed the principle and thermodynamic analysis of using pyrite to remove iron ions from the solution18,43. The free energy values in the equations of Fig. 7 cited from HSC chemistry 6.0.

Fig. 5.

Fig. 5

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XRD of precipitations in the conducted experiments (Cu target, 5°/min).

Fig. 6.

Fig. 6

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The XPS of the precipitates: (a) the Fe 2p spectrum of the precipitate after iron removal, (b) the Mn 2p spectrum of the precipitate after iron removal, (c) the Fe 2p spectrum of the precipitate after iron and manganese removal, (d) the Mn 2p spectrum of the precipitate after iron and manganese removal.

Fig. 7.

Fig. 7

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The principle and thermodynamic analysis of using pyrite to remove iron ions from the solution.

The experiment of iron and manganese removal from the liquid L1 was a complex chemical reaction process. The SEM mapping and EDS mapping of the precipitate after iron and manganese removal are shown in Figs. 8, 9. There were mostly three types of particles with different morphologies in this precipitation, namely large particles, clusters of debris, and needle-like particles. The EDS mapping suggested that the large particles were largely composed of S and Fe, and contained a small amount of O (≤ 15%). The results demonstrated that the large particles were pyrite (FeS2) and a few debris particles (FeO·OH) existed on the pyrite. The clusters of debris were chiefly composed of Fe and O and contained a small amount of S (≤ 10%) and Mn (≤ 4%). The clusters of debris were amorphous goethite (FeO·OH), pyrite (residual substance after reaction), and amorphous MnO2 and Mn2O3. The needle-like particles primarily consisted of S, Ca, and O, and these particles were gypsum minerals (CaSO4·2H2O). From the results of Eh–pH, XRD, XPS, SEM, and EDS, amorphous goethite was initially formed on the surface of pyrite and wrap the pyrite particles in the experiment. These reactions occurred on the surface of pyrite and changed the number and size of pyrite particles. During the manganese removal process, Mn2+ in the solution predominantly reacted with SO2(CaSO3)/O2 around the goethite particles, resulting in the generation of a certain amount of MnO2 and Mn2O3 among the goethite particles. The model of this reaction process during the experiment is shown in Fig. 10.

Fig. 8.

Fig. 8

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SEM images of the precipitate after iron and manganese removal.

Fig. 9.

Fig. 9

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EDS mapping of the precipitate after iron and manganese removal.

Fig. 10.

Fig. 10

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The process of iron and manganese removal during the experiment.

Removal of iron and manganese from the leaching solution of laterite nickel ore using pyrite-calcium sulfite

Fe3+ and Mn2+ are usually present in the acidic leaching solution of laterite nickel ore, and it is necessary to remove Fe3+ and Mn2+ from the solution to create favorable conditions for the subsequent process or obtaining high-quality nickel and cobalt compounds. The liquids L2 and L3 were the artificially simulated acidic leaching solutions used to simultaneously remove the iron and manganese from the acidic leaching solution of laterite nickel ore. The experimental steps were performed according to those described in the removal process of iron and manganese in Sect.  3.2. The removal process of iron continued for 30 min and that of manganese continued for 240 min. The experiments were carried out at pH = 3.5. The concentration of various ions in the solution was determined after 270 min of the experimental reaction. The results of iron and manganese removal and the recovery efficiency of nickel and cobalt from the liquids L2 and L3 are displayed in Fig. 11. The removal efficiency of iron from the liquids L2 and L3 was larger than 99.5% and that of manganese was about 78%. The recovery efficiency of nickel and cobalt from the liquids L2 and L3 was larger than 98% after 270 min. These results suggest that the method is feasible to obtain a good separation and purification result, especially in iron and manganese removal from the leaching solution of laterite nickel ore.

Fig. 11.

Fig. 11

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Iron and manganese removal and the recovery efficiency of nickel and cobalt from the liquids L2 and L3: (a) iron and manganese removal from the liquids L2 and L3, (b) the recovery efficiency of nickel and cobalt from the liquids L2 and L3.

Conclusion

Iron and manganese were effectively removed from the acidic leaching solution using pyrite and pyrite-calcium sulfite and air as auxiliary precipitation materials. This technique could be used to purify the acidic leaching solution of laterite nickel ore.

The main conclusions drawn from this study were as follows: (a) Adding pyrite and air in the experiment could remove Fe3+ quickly from the acidic solution, and the concentration of Fe3+ decreased from 3 g/L to smaller than 0.05 g/L within 30 min during the experiments; (b) Only using pyrite and air in the experiment could not remove Mn2+ from the acidic solution, and using calcium sulfite and air after iron removal could reduce the concentration of manganese ions in the acidic solution; (c) In the experiments, using pyrite-calcium sulfite and air could effectively precipitate the Fe3+ and Mn2+ from the acidic solution, and the recovery efficiency of nickel and cobalt was greater than 98% when proposed method was used to purify the leaching solution of laterite nickel ore.

Supplementary Information

Supplementary Information. (804.1KB, pdf)

Acknowledgements

The authors wish to acknowledge the following China research institutes for their financial and technical support: Yunnan Fundamental Research Projects (Grant No. 202401BC070019), Hebei Education Department (Project D2019108), Hebei GEO University (Project KBZ202305), Science and Technology Department of Tibet (XZ202101ZY0008G). The authors also acknowledge the reviewers for their constructive and thoughtful suggestions that contributed to improving the technical quality of this paper.

Author contributions

Xu Zhang: Conceptualization, Methodology, Validation, Formal analysis, Investigation, Writing-original draft, Project administration, Funding acquisition. Ya-Jing Wang: Conceptualization, Methodology, Validation, Formal analysis, Investigation, Writing-review and editing, Supervision, Funding acquisition. Gesang Nima: Investigation, Writing-review and editing, Supervision. Zi-Qian Wang: Formal analysis, Investigation. Cai-Feng Huang: Methodology, Validation, Project administration.

Data availability

Data will be made available on request. XU ZHANG be contacted if someone wants to request the data from this study. Email: zhxu1021@126.com.

Declarations

Competing interests

The authors declare no competing interests.

Footnotes

Publisher’s note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Contributor Information

Xu Zhang, Email: zhxu1021@126.com.

Yajing Wang, Email: wyjbs@hgu.edu.cn.

Supplementary Information

The online version contains supplementary material available at 10.1038/s41598-025-88448-9.

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Associated Data

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Supplementary Materials

Supplementary Information. (804.1KB, pdf)

Data Availability Statement

Data will be made available on request. XU ZHANG be contacted if someone wants to request the data from this study. Email: zhxu1021@126.com.

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