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Selective Nickel Leaching from Nickel and Cobalt Mixed Sulfide

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Selective Nickel Leaching from Nickel and Cobalt Mixed Sulfide Materials Transactions ©2018 The Japan Institute of Metals and Materials Selective Nickel Leaching from Nickel and Cobalt Mixed Sulfide Using Sulfuric Acid+1 Hiroshi Kobayashi+2, Hirofumi Shoji, Satoshi Asano and Masaki Imamura NIIHAMA RESEARCH LABORATORIES, SUMITOMO METAL MINING CO., LTD., Niihama 792-0002, Japan Sumitomo Metal Mining Co., Ltd. (SMM) has gradually increased the mixed sulfide (MS: mixture of nickel and cobalt sulfides) production from nickel laterite ore as raw material for the SMM’s unique Matte Chlorine Leach and Electro-winning (MCLE) process over the past decade. This process has significant cost advantages because it is capable of selectively and effectively leaching nickel from MS; however, chlorine leaching requires expensive corrosion-resistant facilities. A new process that could be operated using lower-cost facilities has therefore been desired. To meet its development needs, this study evaluated a process for nickel-selective leaching from MS, which is similar to the existing process for refining of ZnS. The process uses sulfuric acid, which does not require high-cost facilities. However, selective nickel leaching from MS, which was the process development goal, could not be achieved. This result is quite different from the case of selective Zn leaching from ZnS. The mechanism of nickel leaching from MS using sulfuric acid was identified. It was shown that nickel-selective leaching using sulfuric acid is difficult because of the formation of elemental sulfur and NiS2 precipitates on the MS surface that interfere with the leaching reaction. [doi:10.2320/matertrans.M2018080] (ReceivedAdvance March 7, 2018; Accepted June 15, 2018; Published July 23, 2018) Keywords: mixed sulfide, sulfuric acid, iron(III) sulfate, nickel selective leaching, NiS2 1. Introduction neutralization of sulfate ions from selective nickel leaching from MS. We examined the possibility of applying a proven Nickel matte and mixed sulfide (MS, i.e., a mixtureView of selective zinc leaching process2,3,4) from sphalerite (name of nickel and cobalt sulfide) are made by rough refining from ore where the main component is ZnS) by sulfuric acid. nickel sulfide ore or nickel oxide ore. These intermediate We then examined selective nickel leaching from MS using products are used as raw materials for commercial nickel sulfuric acid. As shown in the leaching eq. (1), zinc is production. In particular, production from MS has become leached selectively fromProofs sphalerite by sulfuric acid and increasingly popular because MS is made by hydro- sulfide ions are simultaneously oxidized, mainly up to metallurgical processes, which are lower in cost than elemental sulfur, by potential control. pyrometallurgical processes used to produce nickel matte. 0 ZnS þ H2SO4 þ 1=2O2 ¼ ZnSO4 þ H2O þ S ð1Þ As a raw material, MS is used for various kinds of oxidative nickel leaching processes, including: 1) chlorine leaching by However, the reaction in eq. (1) is very slow because of chlorine gas; and 2) pressure leaching by oxygen gas. the reactivity of the redox pair (O2/H2O). To promote this (1) Chlorine leaching is a well-known selective nickel reaction it is necessary to substitute the redox pair (O2/H2O) leaching process with high efficiency, which has been with another pair, which has higher reactivity.4) We define the widely used for nickel cathode production.1) However, substitutable redox pair as an oxidation medium. for safe and environmentally friendly production, As an oxidation medium, the redox pair (Fe3+/Fe2+)is facilities require expensive corrosion-resistant materials generally used for reaction promotion because Fe ions are for handling chlorine gas. These conditions place easily removed from sulfate solution. Equation (2) and unfavorable restrictions on the location of facilities eq. (3) show the break down reaction of selective zinc from the point of material supply. leaching from sphalerite in sulfate solutions. (2) Pressure leaching is an energy efficient method, which 0 ZnS þ Fe2ðSO4Þ3 ¼ ZnSO4 þ 2FeSO4 þ S ð2Þ involves the use of oxidative heating of MS by air blowing and does not require expensive corrosion- 2FeSO4 þ H2SO4 þ 1=2O2 ¼ Fe2ðSO4Þ3 þ H2O ð3Þ resistant equipment. However, for complete oxidation Some of the sphalerite reacts with sulfuric acid as shown in of sulfur up to the sulfate ions, this method features eq. (4), as a result, zinc is leached to yield hydrogen sulfide. high operation costs for sulfate ions neutralization, ZnS þ H2SO4 ¼ ZnSO4 þ H2S ð4Þ particularly for applications to rechargeable nickel battery or nickel powder production processes. On the sulfur side, sulfate ions are yielded from sphalerite On the basis of these issues, the development of new and elemental sulfur as shown in eqs. (5), (6), and (7). refining processes, which have lower costs and lower ZnS þ 2O2 ¼ ZnSO4 ð5Þ environmental impact, is highly desired. Hence, we 0 S þ H2O þ 3=2O2 ¼ H2SO4 ð6Þ investigated processes that could reduce the costs of excess 0 S þ 4H2O þ 3Fe2ðSO4Þ3 ¼ 6FeSO4 þ 4H2SO4 ð7Þ fi +1This Paper was Originally Published in Japanese in J. Japan Inst. Met. When sulfate ions are generated from sul de or elemental Mater. 81 (2017) 320­326. sulfur in the leaching reactions shown as eqs. (5), (6), and +2Corresponding author, E-mail: [email protected] (7), the leaching cost of these reactions increases because 2 H. Kobayashi, H. Shoji, S. Asano and M. Imamura MS Table 1 Compounds’ ratio of MS and Sphalerite (ZnS). Medium Air䚸O2 䠄Fe3+䠅 Electrolytic effluent 䠄Including Sulfuric acid䠅 Electro- Autoclave winning Residue Impurity Leach-soln. removal Ni electrolyte S0 E-Ni0 Fig. 1 Concept of nickel electro-winning process from nickel sulfate solution. Particle Distribution (μm) Sample D10 D50 D90 MS 1.5 7.4 24.5 Sphalerite large amounts of oxidant is necessary for leaching and 1.0 8.2 21.5 (ZnS) neutralizing of sulfate ions. Thus, it is industrially very important to control these reactions to achieve the lowest ratio. If nickel is selectively leached from the MS according toAdvance leaching reaction shown in eqs. (8), (9), and (3), which are the same as zinc in the eqs. (1), (2), and (3), it will be possible to produce nickel cathode material from MS cheaply, as shown in Fig. 1. 0 NiS þ H2SO4 þ 1=2O2 ¼ NiSO4 þ H2O þ S ð8Þ Fig. 2 Particle size distribution curve of MS and Sphalerite (ZnS) samples. 0 NiS þ Fe2ðSO4Þ3 ¼ NiSO4 þ 2FeSO4 þ S ð9Þ 2FeSO þ H SO þ 1=2O ¼ Fe ðSO Þ þ H OView 4 2 4 2 2 4 3 2 (3) Furthermore, eqs. (6), (7), and (10) for MS leaching 2. Samples and Experimental Procedure reactions proceed in the same manner as those for sphalerite. The promotion of these reactions also requires large amounts 2.1 Sulfide samplesProofs of oxidant and neutralizing reagents, necessitating their MS produced by Coral Bay Nickel Corporation6) was used control. for the sulfuric acid leaching tests. The MS was ground in a planetary ball mill to a D90 value of less than 20 µm before NiS þ 2O2 ¼ NiSO4 ð10Þ use. D90 is the diameter at which the cumulative distribution As for sphalerite, hydrogen sulfide is generated in the MS accounts for 90% in the particle size distribution. High purity leaching reaction, as shown in eq. (11). sphalerite produced from Osarizawa mine in Akita prefecture was also used for comparison. The sphalerite was ground by NiS þ H2SO4 ¼ NiSO4 þ H2S ð11Þ hand to a D90 value of less than 20 µm. The compositions of In this report, we defined the sulfate ion ratio yielded in the MS and sphalerite are shown in Table 1. These compositions MS leaching versus sulfur content in the MS source as a were determined by inductively coupled plasma mass sulfur oxidation ratio in the leaching reaction. We also spectrometry (ICP-MS) analysis and x-ray diffraction defined the reactions, in which nickel is selectively leached (XRD) measurements. Furthermore, Fig. 2 shows the particle and sulfide ions are oxidized up to elemental sulfur, as shown size distributions of the two samples. in eqs. (1), (2), and (3), as selective nickel leaching reactions. Iron(III) sulfate heptahydrate (reagent grade 1) and For example, if the nickel leaching rate from MS or the nickel(II) sulfate hexahydrate (special grade reagent) zinc leaching rate from sphalerite is higher than the sulfur produced by Wako Pure Chemical Industries Ltd. were used. oxidation ratio, nickel or zinc is selectively leached versus These reagents were used as the oxidation medium and as a sulfur. Thus, we define the value of the nickel leaching rate synthetic solution source for leaching, respectively. from MS or the zinc leaching rate from sphalerite divided by the sulfur oxidation ratio as an index of selective leaching. 2.2 Leaching reaction and its evaluation An index of selective leaching greater than 1 indicates higher 2.2.1 Comparative tests of sulfide leaching selectivity of the leaching reaction. We define reactions with First, we performed tests to simulate the reactions shown higher index values as reactions with high selectivity. To in eqs. (2) and (8) to confirm the difference between the develop the above nickel cathode production process, we leaching behavior of MS and sphalerite. As a starting aimed to clarify the nickel leaching mechanism of MS in solution, iron(III) sulfate was dissolved so that its sulfuric acid leaching. Incidentally, in studies of selective concentration in the aqueous solution was 0.26 kmol/m3. nickel leaching from nickel sulfide by sulfuric acid, there has This iron(III) sulfate concentration was determined to be been a report on electrolytic oxidation of a nickel sulfide 1.5% of the dissolved solution as an oxidation medium, anode5); however, there have been no reports on control of considering its removal from the leaching solution after the the leaching parameters.
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