Page Header

Effect of Time Stepping in the Filtering Process on the Synthesis of Nickel Sulfate Powder from Blast Furnace Ferronickel

Aprilio Muhammad Fulesa, Yuli Setiyorini, Fakhreza Abdul, Sungging Pintowantoro


The demand for nickel manganese cobalt (NMC)-type batteries is increasing along with the need for global electric vehicles, such as electric cars. Nickel used in the manufacture of NMC batteries is Nickel (II) sulfate hexahydrate (NiSO4.6H2O). Therefore, it is necessary to study how to synthesize nickel sulfate powder from blast furnace ferronickel to provide an alternative source of nickel sulfate and increase the added value of blast furnace ferronickel products. This study aims to analyze the effect of variations in the time difference of stepped filtering sludge on the precipitated filtrate. This study uses a nickel source from the ferronickel derived from the sintering and smelting process using a Mini Blast Furnace to synthesize nickel sulfate. First, the ferronickel was ground and sieved to pass 50 mesh size. Then, the leaching process was performed using a mixture of 120 mL H2SO4 (2M) and 30 mL H2O2 (30%) with a stirring speed of 200 rpm for 6 h for each 2 g ferronickel. Next, the precipitation process was carried out using CaCO3 powder to pH 3.01 at 90 °C. The precipitation solution was held at 90 °C for 24 h, and stepped filtering of the precipitate formed with variations of 2, 4, 6, and 8 h (the total time is kept the same, i.e., 24 h). The crystallization results were then washed and dried at 70 °C for 2 h. Based on X-Ray Fluorescence (XRF), the best results were obtained in stepped filtering variation every 8 h with 50.23% Ni content and 90.5% Ni separation efficiency. Based on XRD, the nickel sulfate powder product has the compound NiSO4.6H2O. In addition, nickel sulfate products also contain CoSO4, one of the compounds needed to manufacture NMC batteries. However, nickel sulfate powder products still contain impurity compounds like FeSO4 and CaSO4.


[1] D. Armstrong McKay, A. Staal, J. Abrams, R. Winkelmann, S. Cornell, I. Fetzer, and T. Lenton, “Global warming of 2 °C risks triggering multiple climate tipping elements,” presented at the AGU Fall Meeting Abstracts, New Orleans, USA, Dec. 13–17, 2021.


[2] D. Liu, L. Xu, U. H. Sadia, and H. Wang, “Evaluating the CO2 emission reduction effect of China’s battery electric vehicle promotion efforts,” Atmospheric Pollution Research, vol. 12, no. 7, Jul. 2021, Art. no. 101115, doi: 10.1016/j.apr. 2021.101115.


[3] A. Gomez-Martin, F. Reissig, L. Frankenstein, M. Heidbüchel, M. Winter, T. Placke, and R. Schmuch, “Magnesium substitution in Ni-Rich NMC layered cathodes for high-energy lithium ion batteries,” Advanced Energy Materials, vol. 12, no. 8, Feb. 2022, Art. no. 2103045, doi: 10.1002/ aenm.202103045.


[4] E. Kartini, M. Fakhrudin, W. Astuti, S. Sumardi, and M. Z. Mubarok, “The study of (Ni,Mn,Co) SO4 as raw material for NMC precursor in lithium ion battery,” in the International Conference on Advanced Material and Technology (ICAMT) 2021, vol. 2708, no. 1, 2022, doi: 10.1063/ 5.0122596.


[5] F. Abdul, H. V. Suryandaru, N. D. Saputra, and S. Pintowantoro, “The effect of sulfuric acid concentration on the leaching process of crude Fe-Ni obtained from mini blast furnace process,” in the 4th International Conference on Materials and Metallurgical Engineering and Technology (ICOMMET) 2020, 2021, vol. 2384, no. 1, doi: 10.1063/5.0071478.


[6] T. Havlík, “Chapter 4 - Equilibrium in Aqueous Solutions,” in Hydrometallurgy, T. Havlík, Ed., Sawston, England: Woodhead Publishing, pp. 60–95, 2008, doi: 10.1533/9781845694616.60.


[7] C. Shi, X. Zuo, and B. Yan, “Selective recovery of nickel from stainless steel pickling sludge with NH3-(NH4)2CO3 leaching system,” Environmental Technology, pp. 1–14, Apr. 2022, doi: 10.1080/09593330.2022.2056085.


[8] S. Yang, P. Zhang, F. Lai, S. Ling, Y. Huang, K. Liu, F. Zheng, H. Wang, X. Zhang, and Q. Li, “New strategy of electrochemical precipitation to metals separation in spent NCM cathode materials for direct regeneration,” Electrochim Acta, vol. 431, Nov. 2022, Art. no. 141144, doi: 10.1016/j.electacta.2022.141144.


[9] V. Miettinen, J. Mäkinen, E. Kolehmainen, T. Kravtsov, and L. Rintala, “Iron control in atmospheric acid laterite leaching,” Minerals, vol. 9, no. 7, Jun. 2019, Art. no. 404, doi: 10.3390/ min9070404.


[10] K. Petkov, V. Stevanova, L. Stamenov, and P. Iliev, “A study of the partial precipitation process of solutions obtained during autoclave dissolution of pyrite concentrate,” Journal of Chemical Technology and Metallurgy, vol. 52, no. 2, pp. 270–276, 2017.


[11] L. Cassayre, B. Guzhov, M. Zielinski, and B. Biscans, “Chemical processes for the recovery of valuable metals from spent nickel metal hydride batteries: A review,” Renewable and Sustainable Energy Reviews, vol. 170, Dec. 2022, Art. no. 112983, doi: 10.1016/j.rser.2022.112983.


[12] H. Han, W. Sun, Y. Hu, H. Tang, and T. Yue, “Magnetic separation of iron precipitate from nickel sulfate solution by magnetic seeding,” Hydrometallurgy, vol. 156, pp. 182–187, Jul. 2015, doi: 10.1016/j.hydromet.2015.07.001.


[13] H. Han, W. Sun, Y. Hu, T. Yue, L. Wang, R. Liu, Z. Gao, and P. Chen, “Induced crystallization of goethite precipitate from nickel sulfate solution by limonite seeding,” Hydrometallurgy, vol. 174, pp. 253–257, Dec. 2017, doi: 10.1016/j.hydromet. 2017.03.001.


[14] Z. T. Ichlas, M. Z. Mubarok, A. Magnalita, J. Vaughan, and A. T. Sugiarto, “Processing mixed nickel cobalt hydroxide precipitate by sulfuric acid leaching followed by selective oxidative precipitation of cobalt and manganese,” Hydrometallurgy, vol. 191, Jan. 2020, Art. no. 105185, doi: 10.1016/ j.hydromet.2019.105185.


[15] O. A. Nasser and M. Petranikova, “Review of achieved purities after li-ion batteries hydrometallurgical treatment and impurities effects on the cathode performance,” Batteries, vol. 7, no. 3, Sep. 2021, Art. no. 60, doi: 10.3390/ batteries7030060.


[16] N. Pandey, S. K. Tripathy, S. K. Patra, and G. Jha, “Recent Progress in hydrometallurgical processing of nickel lateritic ore,” Transactions of the Indian Institute of Metals, vol. 76, no. 1, pp. 11–30, Jan. 2023, doi: 10.1007/s12666-022- 02706-2.


[17] S. Pintowantoro, P. C. Panggabean, Y. Setiyorini, and F. Abdul, “Smelting and selective reduction of limonitic laterite ore in mini blast furnace,” Journal of The Institution of Engineers (India): Series D, vol. 103, no. 2, pp. 591–600, Dec. 2022, doi: 10.1007/s40033-022-00348-8.


[18] F. Abdul, S. Pintowantoro, and A. Maulidani, “Analysis the effect of charcoal mass variation to Ni content, sinter strength and yield on sintering process of limonitic laterite nickel ore,” Key Engineering Materials, vol. 867, pp. 25–31, Oct. 2020, doi: 10.4028/ KEM.867.25.


[19] S. Pintowantoro, K. Oktandria, R. A. M. Pasha, and F. Abdul, “Variation of oxygen flow rate on nickel and iron content in the oxidation refining process of crude Fe-Ni from Mini Blast Furnace (MBF),” in the 4th International Conference on Materials and Metallurgical Engineering and Technology (ICOMMET) 2020, vol. 2384, no. 1, 2021, doi: 10.1063/5.0071487.


[20] S. Pintowantoro, F. Waluyo, Y. Setiyorini, V. Setyowati, A. Kawigraha, and F. Abdul, “Study of the effect of time variations on the leaching process of ferronickel products from mini blast furnace to yield elements of Fe, Ni, and Co for NiSO4.6H2O Synthesis,” Journal of Physics, vol. 2117, no. 1, Nov. 2021, Art. no. 012024, doi: 10.1088/1742-6596/2117/1/012024.


[21] B. A. Wills and J. A. Finch, “Introductionin Wills’ Mineral Processing Technology,” Elsevier, 2016, pp. 1–27. doi: 10.1016/B978-0-08-097053- 0.00001-7.


[22] H. E. Farrah, G. A. Lawrance, and E. J. Wanless, “Solubility of calcium sulfate salts in acidic manganese sulfate solutions from 30 to 105 °C,” Hydrometallurgy, vol. 86, no. 1–2, pp. 13–21, Apr. 2007, doi: 10.1016/j.hydromet.2006.10.003.


[23] G. P. Demopoulos, “Aqueous precipitation and crystallization for the production of particulate solids with desired properties,” Hydrometallurgy, vol. 96, no. 3, pp. 199–214, Apr. 2009, doi: 10.1016/j.hydromet.2008.10.004.


[24] A. J. Bard and L. R. Faulkner, Electrochemical Methods: Fundamentals and Applications. New York: Wiley, 1980.


[25] G. Azimi and V. G. Papangelakis, “Thermodynamic modeling and experimental measurement of calcium sulfate in complex aqueous solutions,” Fluid Phase Equilibria, vol. 290, no. 1–2, pp. 88– 94, Mar. 2010, doi: 10.1016/j.fluid.2009.09.023.


[26] B. Padh, P. C. Rout, G. K. Mishra, K. R. Suresh, and B. R. Reddy, “Recovery of nickel and molybdate from ammoniacal leach liquors of spent HDS catalysts using chelating ion exchange resin,” Hydrometallurgy, vol. 184, pp. 88–94, Mar. 2019, doi: 10.1016/j.hydromet.2019.01.001.


[27] F. Wirsching, “Calcium Sulfate,” in Ullmann’s Encyclopedia of Industrial Chemistry. Weinheim, Germany: Wiley-VCH Verlag GmbH & Co. KGaA, 2000. doi: 10.1002/14356007.a04_555.


[28] L. M. Roux, E. Minnaar, P. J. Cilliers, M. Bellino, and R. Dye, “Comparison of solvent extraction and selective precipitation for the purification of cobalt electrolytes at the Luilu refinery, DRC,” in The South African Institute of Mining and Metallurgy Base Metal Conference, pp. 343–364, 2007.


[29] B. A. Wills and T. Napier-Munn, “Introduction,” in Wills’ Mineral Processing Technology. Amsterdam, Netherlands: Elsevier, 2005, pp. 1–29, doi: 10.1016/B978- 075064450-1/50003-5.


[30] V. Yu. Gus’kov, D. A. Allayarova, G. Z. Garipova, and I. N. Pavlova, “Supramolecular chiral surface of nickel sulfate hexahydrate crystals and its ability to chirally recognize enantiomers by adsorption data,” New Journal of Chemistry, vol. 44, no. 41, pp. 17769–17779, 2020, doi: 10.1039/D0NJ03912H.


[31] Z. Zhu, Y. Pranolo, W. Zhang, W. Wang, and C. Y. Cheng, “Precipitation of impurities from synthetic laterite leach solutions,” Hydrometallurgy, vol. 104, no. 1, pp. 81–85, Jul. 2010, doi: 10.1016/j.hydromet.2010.05.003.


[32] W. Xiao, X. Liu, and Z. Zhao, “Kinetics of nickel leaching from low-nickel matte in sulfuric acid solution under atmospheric pressure,” Hydrometallurgy, vol. 194, p. 105353, Jun. 2020, doi: 10.1016/j.hydromet.2020.105353.

Full Text: PDF

DOI: 10.14416/j.asep.2023.06.002


  • There are currently no refbacks.