(12) INTERNATIONAL APPLICATION PUBL (19) World Intellectual Property Organization International Burau Zz WIPO!|PCT (43) International Publication Date 16 May 2019 (16.05.2019) D UNDER THE PATENT COOPERATION TREATY (PCT) ANA (10) International Publication Number WO 2019/090389 Al (1) International Patent Classi C228 23/00 (2006.01) (C228 3724 (2006.01) ation 2B 3/42 (2006.01) (C228 3108 2006.01), Intern: sal Application Number: PCT/AU2018/051203, International ing Date: (08 November 2018 (08.11.2018) (25) Filing Language: English (26) Publication Language: English G0) Priority Data: 2017904565 10 November 2017 (10.11.2017) AU Applicant: BHP BILLITON NICKEL WEST PTY LTD IAU/AUL, NiW Perth Office, L41, 125 St Georges Tee, Perth, Westem Australia 6000 (AU), oy (7%) Inventors: CLOUT, Richard; c/o BIIP Billiton Nicket ‘West Pty Lid, NiW Perth Office, Level 41, 25 St Georges cy @n ‘Tenace, Per, Wester Australia 6000 (AU), STEWART, John; cio BHP Billiton Nickel West Ply Lid, NiW Perth OF fice, Level 41.25 St Georges Terrace, Perth, Western Aus- tralia 6000 (AU), ‘Agent: PHILLIPS ORMONDE FITZPATRICK; Level 16, 333 Collins Sureet, Melbourne, Vietoria 3000 (AU), Designated States unless otherwise indicated, for every Kind of national protection available), AE, AG, AL, AM, AO, AT, AU, AZ, BA, BB, BG, BH, BN, BR, BW, BY. BZ. CA. CH, CL. CN, CO, CR, CU, CZ, DE. DI, DK, DM. DO, DZ, EC, FE, EG, ES, Fl, GB, GD, GE, GH, GM, GT, HN, HR, HU, ID, IL, IN, IR, 1S, 10, JB KE, KG, KH, KN, KP. KR, KW,KZ,LA,LC,LK,LR,LS,LU, LY, MA, MD, ME, MG, MK, MN, MW, MX, MY, MZ, NA, NG, NI. NO NZ. (OM, PA, PE, PG, PH, PL, PT, QA, RO, RS, RU, RW, SA, SC, SD, SE, 8G, SK, SL, 8M, ST, SV, S¥, TH, TJ, TM, TN, TR, TT, TZ, UA, UG, US, UZ, VC, VN, ZA, ZM, ZW (64) Title: PRODUCTION OF HIGH PURITY NICKEL SULFATE wo 2019/090389 A1 lll 67) Abstract: A process for producing high purity nickel sulfate, preferably having a purty of 299.8%, more preferably 299.98%, suitable for use in batery manufacture or nickel plating is described. The process involves selectively removing nownickel metal impurities from a nickel sulfate solution, preferably a sub-saturated nickel sulfate solution, obtained for example from nickel powder, bby ion exchange using a nickel pre-loaded ion exchang (IX) resin which adsorbs non-nicke! metal impurities from the solution to form ‘a substantially non-nickel metal impurities free nickel sulfate soluioa from which the high punt aickel sulfate can be recovered. The recovered nickel sulfate can be crystallised to remove the high pusity product, [Continued on next page}WO 2019/090389 A. |MIINNITI NNN HH 00 A (84) Designated States fanless otherwise indicated, for every ind of regional protection available): ARIPO (BW, Gli, UG, ZM, ZW), Eurasian (AM, AZ, BY, KG, KZ, RU, TI, ‘TMD, European (AL, AT, BE, BG. CH, CY, CZ, DE, DK. EE, ES, Fl, FR, GB, GR. HR. HU, IE. IS, IT, LT, LU, LV, MC, MK, MT, NL, NO, PL, PT, RO, RS, SE, SI. SK, SM, ‘TR), OAPI (BF, BI, CF, CG, Cl, CM, GA, GN, GO, GW, KM, ML, MR, NE, SN, TD, TO), Published: = wth international search report grt. 213)10 15 20 25 35 WO 2019/090389 PCT/AU2018/051203 Title of Invention Production of High Purity Nickel Sulfate Technical Field ‘The invention relates to a process for the production of high purity nickel sulfate from a nickel powder leach in sulfuric acid. Background of Invention Nickel sulfate is used in electroptating and electroless piating as well as being a material for secondary batteries. There is a need for high purity nickel sulfate that is substantially free of impurities including copper, iron and cobalt for such uses. Currently, purification of nickel sulfate is by organic solvent extraction techniques which typically involve an acid extractant and neutralising agent, for example, sodium hydroxide, to faciitate extraction of the impurities. However, the recovered nickel sulfate product is contaminated with sodium which is dificult to remove. ‘Thus alternative methods for nickel sulfate purification are desirable. A reference herein to a patent document or any other matter identified as prior art, is not to be taken as an admission that the document or other matter was known or that the information it contains was part of the common general knowledge as at the priority date of any of the claims, ‘Where any or all of the terms "comprise", "comprises", "comprised" or "comprising" are used in this specification (including the claims) they are to be interpreted as specifying the presence of the stated features, integers, steps or components, but not precluding the presence of one or more other features, integers, steps or components, ‘Summary of invention In one aspect, the invention provides a process for producing high purity nicke! sulfate, preferably having a purity of 299.8%, more preferably 209.98%, suitable for use in a battery or nickel plating, comprising the step of: selectively removing non-nickel metal impurities from a nickel sulfate solution, preferably sub-saturated acidic nickel sulfate solution for example obtained from nickel powder, by ion exchange using a nickel pre-loaded ion exchange (IX) resin which adsorbs non-nickel metal impurities from the solution to form a substantially non-nickel metal impurities free nickel sulfate solution from which the high purity nickel sulfate can be recovered10 15 20 25 30 35 WO 2019/090389 PCT/AU2018/051203 2 Desirably. the nickel sulfate solution comprises trace amounts of non-nickel metal impurties. Suitably, the nicket sulfate solution is a sub-saturated nickel sulfate solution. More suitably, the nickel sulfate solution is non-nickel metal impurity depleted sub- saturated nickel sulfate solution. More suitably still the nickel sulfate solution is acidic. Preferably, the nickel sulfate solution is an acidic non-nickel metal impurity depleted sub-saturated nickel sulfate sotution which comprises trace amounts of non-nickel metal impurities, Preferably, the step of selectively removing the trace amounts of non-nickel metal impurities involves buffering the nicket sutfate solution prior to ion exchange (IX) with one or more basic nickel compounds to a pH optimised for selectivity and stability of non-nicket metal impurity loading onto the nickel pre-loaded ion exchange resin, Desirably, the process further comprises the step of recovering the high purity nickel sulfate from the substantially non-nickel metal impurities free nickel sulfate solution, preferably in the form of crystalline alpha nickel sulfate hexahydrate. Preferably, the niokel sulfate solution is an acidic sub-saturated nickel sulfate solution, and the method comprises prior to the selective removal step, the additional steps of: generating the acidic sub-saturated nickel sulfate solution which comprises the one or more non-nickel metal impurities: and removing bulk non-nickel metal impurities from the acidic sub-saturated nickel sulfate solution to form the non-nickel metal depleted nickel sulfate solution comprising a sub- saturated concentration of nickel sulfate and trace amounts of one or more non-nickel metal impurities In a preferred embodiment, the process is preferably a batch process, comprising the steps of: @ generating an acidic sub-saturated nickel sulfate solution which comprises one ‘or more non-nickel metal impurities; (i) removing butk non-nickel metal impurities from the acidic sub-saturated nickel sulfate solution to form an acidic sub-saturated non-nickel metal impurity depleted nickel ‘sulfate solution comprising a sub-saturated concentration of nickel sulfate and trace amounts of the one or more non-nickel metal impurities; (ii) selectively removing the trace amounts of non-nicke! metal impurities from the non-nickel metal impurity depleted nickel sulfate solution using a nickel pre-loaded fon exchange (1X) resin to remove the non-nickel metal impurity from the solution to form a substantially non-nickel metal impurities free sub-saturated nickel sulfate solution;10 15 20 28 30 WO 2019/090389 PCT/AU2018/051203 3 (iv) recovering the high purity niokel sulfate from the substantially non-nickel metal impunties free sub-saturated nicket sulfate solution, preferably in the form of alpha nickel sulfate hexahydrate, particularly crystalline alpha nickel sulfate hexahydrate. ‘Suitably, selective removat of the trace amounts of non-nickel metal impurities involves buffering the acidic sub-saturated non-nickel metal depleted nickel sulfate solution prior to ion exchange (IX) with one or more basic nickel compounds to a pH optimised for selectivity and stability of non-nickel metal impurity loading onto a nickel pre-loaded ion ‘exchange resin. Leaching {n another aspect, the invention provides a process. preferably a batch process, for leaching nickel sulfate from nickel powder comprising the steps of: (leaching a stoichiometric excess of the nickel powder with sulfuric acid to form an acidic sub-saturated solution of dissolved nickel sulfate and one or more non-nickel metal impurities, together with unieached nickel powder; (i) separating the acidic sub-saturated nickel sulfate solution from the unleached nickel powder to provide a discharge solution which is a substantially solid-free acidic sub- saturated nickel sulfate solution; and optionally repeating steps ()) and (i) one or more times, wherein the one or more additional leaching steps () are carried out with sulfuric acid, preferably using the unleached nickel solid separated in step (i). Preferably, the acidic sub-saturated solution of dissolved nickel sulfate and one or more non-nickel metal impurities, together with unteached nickel powder. is a pregnant leach solution. it should be understood that the pregnant leach solution is a solution is a solution of metal laden water generated from stockpile leaching and heap leaching for example. A pregnant each solution is an acidic solution and may comprise one or more organic and/or inorganic acids. Preferably, the process is carried out as a batch process. ‘The nickel powder thought to be leached by the sulfuric acid in accordance with the following equation Nica) + He8s aq) > Hata) + NiSOnfaqy Other non-nickel metal impurities are co-leached by the acid, together with the nickel sulfate. Typically, the one or more non-nickel metal impurities include one or more of Ca, Al, Na, P, Si, K, Mg, Mn, Se, Cr, Co, Fe, Cu, Zn, As, Ru, Pb, Hr, Pd, Ag, Cd, Sb, Ir, Pt, Au and Bi. The most significant impurities tend to be varying amounts of Co, Cu, Cr, K, Ca, Na, Zn and/or Fe. However, the impurities in most appreciable quantities are usually Co, Cu and/or10 15 20 28 30 35 WO 2019/090389 PCT/AU2018/051203 4 Fe. Where chemically possible, various metal oxidation states species can be present in the leach solution, for example, iron can be present in the ferric or ferrous form. In order to reduce extemal metal ion contamination, preferably, the sulfuric acid used in the process for leaching is prepared using demineralised water. This is thought to reduce the contaminant burden to impurities arising from sulfuric acid leaching of nickel powder. This means that metal contaminants that are found in mains water are avoided In one embodiment, the nickel powder for leaching may be provided directly from @ nickel powder leach plant. Thus, itis desirable that the nickel sulfate process is carried out in proximity to a nickel powder leach plant, In such a case, the raw material nickel powder can ‘conveniently been provided to the nickel sulfate processing plant directly from the discharge of wet metals driers in the nickel powder leach plant. Alternatively, the nickel powder raw material can be provided by transport from an altemative source; however, this would be expected to atid to the overall processing cost. Preferably, the nickel powder used in the process described has an average particie size of from about 4 micron to about 1200 microns, more preferably from 10 microns to about 41000 microns, more preferably stil from about 100 microns to about 900 microns. in some ‘embodiment, itis believed that coarser paiticies leach more slowly such that there is a preference for less coarse paiticies where faster leaching is desirable. ‘The nickel powder raw material may have a purity of from about 98% to about 100%, However, the nickel powder preferably has a purity of 289.8% nickel. Such nickel powder may be obtainable by any industrial process capable of generating nickel powder having such Purity. One example of a suitable process is nickel powder production from a process involving hydrogen pressure reduction. Preferably, the leaching process is carried out at a temperature of from about 50 °C to about 100 °C, most proferably from about 70 °C to about 96 °C, most preferably stil at about 80°C. Suitably, the process temperature is achieved and/or maintained by steam healing, for ‘example, by a steam heating coil provided in the leach tank. Steam may be conveniently provided from a close by refinery. A sub-saturated nickel sulfate solution comprises dissolved nicket in a concentration which is about 70%to about 99% of the theoreticat nickel sulfate saturation concentration Under the particular leaching conditions used. Preferred sub-saturated solutions are of from ‘about 90% to about 98% nickel sulfate, more preferred sub-saturated solutions are of from about $2% to about 97%, with solutions of about 95% of the theoretical nickel sulfate saturation concentration being most preferred. Suitably, the pregnant leach solution is a sub- saturated nickel sulfate solution that comprises dissolved nicket in a concentration that is about 70% to about 99%, more preferably from about 92% to about 97%, most preferably about 95% of the theoretical nickel sulfate saturation concentration. Suitably, the sub-5 10 15 20 28 30 35 WO 2019/090389 PCT/AU2018/051203 5 saturated nickel sulfate sotution is acidic. The degree of nickel sulfate saturation in the leach solution is dependent on factors including the pH of the acid used, the temperature of the leach solution and/or the rate of evaporation from the leaching solution. it should be understood that the leaching sulfuric acid concentration and/or the process temperature may be controlled to in order to produce a discharge solution which is sub-saturated at about 95% of the saturation limit of nicket sulfate at under the processing conditions used. For example, at @ leaching process temperature of about 80°C, a nickel sulfate saturation of about 95% is readily achievable using an optimised acid concentration and processing conditions as described herein. Advantageously, operating close to saturation, particularly at higher temperatures, for example, 80°C, minimises evaporation duty in downstream process crystallisation stages, and eliminates the need for a pre-evaporator reducing capital and processing costs. In preferred embodiments, the initial concentration of sulfuric acid used in leaching step ()) is from about 150 g/l and about 350 g/L, more preferably from about 200 g/t. and about 300g/L, more preferably still from about 250 g/L to about 290g/L, most preferably about 280 g/L (which corresponds to about 150 mi. of sulfuric acidAvater), Preferably nickel powder is preferably provided/maintained at a loading of between about 850 g/L and 1200 g/L, more preferably, from about 950 g/L to about 1100 g/L, most preferably about 1000 g/L. (mass of nickel per litre of sulfuric acid). Suitably, the nickel in the sulfuric acid has a pulp density, that is amount of solids in a Pulp of nickel in acid, in the range of about 500 to about 1500 g/, more preferably from about {600 to about 200 g/L, more preferably stil from about 750 g/L to about 850 g/L, with a particularly preferred pulp density being about 800 gil, for example al a pH of between about and about 3.5, in preferred embodiments, the process occurs at about atmospheric pressure or at a positive gauge pressure. in particular, at least leaching step () may be carried out at about atmospheric pressure or more preferably at a positive gauge pressure. Ina preferred embodiment, during step () the nickel solid and sulfuric acid are agitated In one embodiment, the leaching and/or separation, that is, steps ()) and/or (i), may be carried out under geration, for example, under a compressed air atmosphere, for example, having a flow rate of about 0.1 to about 9.5 Limin, more preferably 1 ~ 5 Limin, most preferably about 1 Limin. Lower flow rates, for example, ¢ 3.5 Limin, are preferred as higher flow rates tend to result in increasing amounts of evaporation of the leaching acid which results in premature saturation of nickel sulfate in the discharge solution. In some embodiments, the process is carried out anaerobically, for example using No sparging10 15 20 28 30 35 WO 2019/090389 PCT/AU2018/051203 6 As hydrogen is evolved as a side product of the leaching process, the process desirably further comprises the step of removing the evolved hydrogen gas, for example, by flushing the local environment around the leaching location with steam, for example, a snuffing steam, and/or by operating the leaching process at a positive gauge pressure to prevent air ingress. It will be understood that the flush is maintained in the vicinity of at least the leach tank vapour space. As hydrogen gas evolution may be ongoing until the leaching reactions reach equilibrium it may be beneficial to provide the steam flush and/or positive gauge pressure to further steps of the process, particularly, the filering and bulk impurities removal steps also described herein. A preferred steam flush is a steamvair mixture ‘comprising from about 50% to about 80% steam, A steam flush providing a minimum of 70 vol% steam atmosphere is particularly desirable. Jn embodiments including the step of removing the evolved hydrogen gas, itis desirable, that the process further comprises the step of scrubbing the hydrogen steam flush off gas generated to remove acid mist and particulates prior to atmospheric discharge. Further desirably, the process includes the step of carrying out at least the leaching step under a nitrogen blanket to prevent a potentially explosive hydrogen/air mixture forming, In some embodiments, where hydrogen evolution is ongoing, the separating step (ji) and/or additional bulk impurity removal steps also described herein can further be carried out Using a steam flush and/or under a nitrogen blanket to minimise the risk of formation of an explosive environment. Desirably. when leaching step () has been completed, the unleached solid nickel is separated from the sub-saturated pregnant leach solution, for example, by fering or by decanting. Decanting is a particularly preferred separation method as conveniently leaves the Unreached nickel in place for easy commencement of a subsequent leach batch where fresh acid is simply to be added in the next batch. Thus, itis preferable that discharge solution decanting takes place after a suitable period for settling has elapsed. Completion of the leaching step can be identified by observation that the pregnant leach solution has a predetermined pH, or that the leaching step has been allowed to process for a predetermined period of time. The leaching process can be terminated at any point by addition of a suitable ‘amount of a neutralisation agent which is suitable to neutralise the excess free acid to provide a solution of a desired pH. Thus, in some embodiment, step (i) is allowed to proceed until the pregnant leach solution has a pH of from about 0 to about 4, more preferably a pH of about 1 to about 3.5, most preferably a pH of about 3. in other embodiments, the leaching step ()) may proceed for a period of from about 2 to about 20 hours, more preferably from about & to about 24 hours, more preferably stil from about 9 to about 12 hours, most preferably for about 10 hours,10 15 20 25 30 35 WO 2019/090389 PCT/AU2018/051203 7 Desirably. on termination, the pregnant leach solution comprises from about 130 g/L to about 210 g/L nickel, more preferably from about 140 g/L to about 200 g/t. nickel, more preferably still from about 150 g/l to about 195 g/L nickel, and most preferably about 192 g/L. ‘Typically under the processing conditions described herein, for example, when leaching is carried out at 80°C, a solution pH 3 generally corresponds to a nickel sulfate solution concentration of 192 g/t. Terminating the leaching process at about pH 3 is preferred as it provides a batance between (i) terminating at a lower pH, but requiring a much great amount of neutralisation agent to neutralise the excess free acid, and (i) terminating at a higher pH, which means the reaction is far slower and would take much longer and so would require increased capital for larger reaction tanks where the total process throughput is fixed. As used herein, the term about represents a plus/minus deviation on a vaiue corresponding to 4% in the context of pH measurements and 5% of concentration values. mi val Ina related aspect, the method further comprises the step of removing the bulk non- nickel metal impurities from the discharge solution. Thus, in one embodiment, the process further comprises the steps of (precipitating substantially all of the non-nickel metal impurities as an insoluble on-nickel metal impurity precipitate; and (i) removing the precipitate from the discharge solution to form a non-nicket metal impurty-depleted discharge solution comprising @ sub-saturated solution of nickel sulfate and trace amounts of the one or more non-nickel metal impurities, Suitably, the precipitation step may include the step of oxidising one or more non= nickel metal impurities in the discharge solution, Such an oxidation step is preferably carried ‘out prior to the precipitation step. Oxidation of one or more of the metal impurities can assist in formation of metal species which precipitate at a more desirable pH, for example, the pH of ‘operation. For example, oxidation converts iron from ferrous to ferric whereby ferric hydroxide and other impurities can be more conveniently precipitated at about pH 5. Suitably, the precipitated non-nickel metal impurities comprise non-nickel metal hydroxides which are formed when the pH of the discharge Solution is sufficiently increased to a level where such hydroxides can form. Suitably, the sulfuric acid may comprise one or more oxidising agents, for example, oxygen, preferably supplied by sparging the sulfuric acid with air, Where an oxidising agent is used, preferably it comprises a source of oxygen, for example, air, such as {an air sparge. For example, wherein the oxidising step is carried out in an aeration tank, air ‘can be sparged through the discharge solution. if necessary, the precipitating step can be executed by discharge solution to @ pH of about 3 to about 7, preferably to a pH of about 4.5 to about 5. more preferably to a pH of about 5. A particularly preferred precipitation pH is about 5. easing the pH of the10 15 20 28 30 35 WO 2019/090389 PCT/AU2018/051203 8 Suitably, the pH of the discharge solution may be increased by the addition of one or more basic compounds, preferably one or more basic nickel compounds. most preferably nickel hydroxide. Nickel hydroxide is suitable to raise the pH of the acidic sub-saturated solution (e.g. a pregnant leach solution) or the discharge solution to about pH 5 to about pH. 5.5, with reasonable neutralisation kinetics and efficiency. This is achievable with sufficient leach residence time. if a higher pH is required for impurity precipitation, preferably, an ammonia solution is used to increase the pH further. However, in preferred embodiment, alkali bases, in particular, sodium or potassium hydroxide bases are avoided as these bases typically leads to alkali contamination in the final product which can be burdensome to remove. Preferably, the process further inoludes the step of separating the non-nickel metal impurities precipitate from the discharge solution to form a non-nickel metal impurity-depleted discharge solution. In one embodiment, the non-nickel metal impurity-depleted discharge Solution js a non-nickel metal hydroxide-depleted discharge solution. it will be understood that on-hydroxide solid materials, such as solid nickel powder, are also advantageously removed in the separating step. Means for separation include any suitable separation means, for example, decanting, centrifuging or fttering. Preferably, the non-nickel metal impurity- depleted discharge solution is fitered to remove any remaining solids prior to storage in the ton exchange (IX) feed tank and/or prior to ion exchange (IX). Suitably, the non-nickel metal impurity-depleted discharge solution is held in the ion exchange (IX) feed tank prior to the fon exchange processing. Suitably, fiter sludge recovered from fitting is preferably transferred to a refinery final thickener for further processing or disposal Preferably, after non-metal impurity separation, the discharge solution has a pH of from about 3 to about 7, more preferably about 4 to 6, most preferably a pH of about §. Preferably, the bulk impurity removal process is associated the additional step of acid mist scrubbing to scrub off or remove any hydrogen gas evolved at this stage of the process. Most preferably, this scrubbing step is completely separate to the off-gas scrubbing used during leaching thereby ensuring hydragen and oxygen do not mix in corresponding off-gas scrubbers. Hf necessary, the steps of the bulk impurity removal process may be carried out by flushing the local environment around the leaching location with snuffing steam and/or a positive gauge pressure to prevent air ingress as described above. If necessary, the bulk Impurity removal process may also include the step of canying out the leaching step under a nitrogen blanket to prevent the hydrogen mixing with air to form an explosive environment as described above. Jon exchange purification10 15 20 25 30 35 WO 2019/090389 PCT/AU2018/051203 9 {in another aspect, the invention provides a process for producing high purity nickel suitable for use in battery manufacture or nickel plating, preferably having a purity of 299.98% nickel sulfate, comprising the steps of: selectively removing non-nickel metal impurities from a nickel sulfate solution by ion ‘exchange (IX) by subjecting a solution of nickel sulfate comprising dissolved nickel sulfate ‘and one or more non-nickel metal impurities to a first round of ion exchange using a resin pre- loaded with nickel, whereby non-nickel metal impurities in the nickel solution are selectively retained by the resin to generate a first IX discharge solution which is a clean nickel sulfate solution substantially free of non-nickel metal. {n a particularly preferred embodiment, the invention provides a process for producing 4 high purity nickel sulfate solution suitable for crystallisation of high pusity, preferably 299,98% purity nickel sulfate hexahydrate, comprising the steps of: (© providing a nickel sulfate solution, preferably being a substantially solid-free acidic sub-saturated nickel sulfate solution, comprising dissolved nickel sulfate and one or more non-nickel metal impurities, preferably a pregnant leach solution, more preferably obtainable by a process as defined in any one of claims § to 19; (® selectively removing non-nicke! metal impurities from a nickel sulfate solution by ion exchange (IX) by subjecting a solution of nickel sulfate, comprising dissolved nickel sulfate and one or more non-nicket metal impurities to a first round of ion exchange using a resin pre-ioaded with nickel, (i) whereby non-nickel metal impurities in the nickel solution are selectively retained by the resin to generate a first IX discharge solution which is a clean nickel sulfate. Solution substantially free of non-niokel metal Preferably, the nickel sulfate solution is an acidic sub-saturated nickel sulfate, more preferably an acidic sub-saturated non-nicket metal impurty-depleted discharge solution more particularly, such as one which has been subjected to a bulk non-nickel metal impurity removal process as described herein. in a particularly preferred embodiment, the nickel sulfate solution is a pregnant leach solution which may be obtainable by the leaching processes described herein. Suitably, the nickel sulfate solution from which the non-nickel metal impurities are removed is a subsaturated nickel sulfate solution, preferably having a nickel concentration of about 100 g/t. to about 215 g/L nickel. Preferably, the sub-saturated nickel sulfate solution has an initial concentration of nickel in the range of from about 130 g/L to about 210 g/L nickel, more preferably from about 180 g/L. to about 200 g/L nickel, more preferably still from about 175 g/l to about 195 g/t nickel, and most preferably about 190 g/L. ‘Typically, the non-nickel metal impurities are present, for example, in trace amounts, particularly ifthe nickel sulfate solution has been subject to a bulk non-nickel metal impurity10 15 20 28 30 35 WO 2019/090389 PCT/AU2018/051203 10 removal process. Suitably. the non-nickel metal impurities include divalent metal cations, for ‘example, divalent cobalt, iron and/or copper ions, preferably cobatt ions. Suitably, the non-nickel metal impurities in the nickel sulfate solution are selectively retained by the resin in exchange for pre-loaded nickel and/or hydrogen ions. Preferably, the subjecting step inckudes the step of buffering the nickel sulfate solution prior to ion exchange (IX) with one or more basic nickel compounds, preferably to @ pH optimised for selectivity and stability of non-nickel metal impurity loading onto the nickel pre- loaded ion exchange resin. In particular, a preferred amount of nickel hydroxide is sufficient to neutralise acid released by the resin in exchange for nickel during nickel preloading so that, the pH of the pre-IX and post-IX solutions are substantially equivalent, preferably within 10% of the relevant pH unit. The precise optimised pH may depend on factors including the ‘chemistry of the resin used but will be readily be determinable as shown in the examples provided herein, Preferably, prior to ion exchange, the nickel sulfate solution has an initial pH of pH <6, preferably a pH of from about 4.5 to about 6, more preferably, a pH of about 5 to about 5.5, most preferably, a pH of about Suitably, after ion exchange, the nickel sulfate solution has a final pH of pH <6, preferably a pH of from about 4.5 to about 6, more preferably, a pH of about 5 to about 5.5, most preferably, a pH of about 5 Desirably, the first and one or more additional rounds of ion exchange are camtied out ata temperature of from about 50 °C to about 95 °C, more preferably from about 70 °C to about 90 °C, most preferably at about 80°C. Suitably the resin is capable of extracting metal ions from solution, More suitably stil, the resin is capable of selective removal of metal ions fram solution, Selective removat means, ‘one or more metal ions are removed from the solution in preference to different metal ions which remain in solution at a given pH/operating conditions. Desirably, the resin is a cation exchange resin. The resin may be comprised of one or more polymers based on at least one monovinylaromatic compound and/or at least one polyvinylaromatic compound. itis preferable when chelating resins for the purposes of the invention are polymers composed of for example, styrene, divinylbenzene and ethylstyrene, The resin is preferably in bead form. In a particularly preferred embodiment, the resin is a macroporous crosslinked polystyrene based resin, which is preferably acidic or otherwise capable of extracting metal ions from solution such as the nickel sulfate solutions, as described herein. In one embodiment, the resin is a metal chelating resin which comprises one oF more metal chelating functional roups. Preferably, the resin comprises organophosphorus functional groups which are capable of selectively complexing with certain metal ions, for example, under certain pH conditions. Desirably such functional groups include phosphoric, phosphonic or phosphinic5 10 15 20 28 30 35 WO 2019/090389 PCT/AU2018/051203 W acid based functional groups. An example of a phosphoric acid based resin is one comprising di-2-ethylhexytphosphat (O2EHPA) functional groups (Lewatit VP OC 10266). An example of a phosphonic acid based resin is one comprising aminomethyl phosphonic acid functional ‘groups (Lewatit TP-260@), An example of a phosphinic acid based resin is one comprising bis-(2,4,4-trimethylpentyl-) phosphinic acid functional groups (Lewatit TP-272®). Preferably, the resin is not a TP-207 resin Preferably, the resin is provided in two or more columns arranged in a lead/lag configuration, whereby the fag column can act as () a polishing column when the impurity breakthrough of the lead column becomes undesirably, or as @ new lead column where the ‘original led column is subject to regeneration thereafter becoming the lag column. Desirably, the first IX discharge solution is transferred to a crystallisation plant. in prefoadin Control of solution pH is critical to the optimum selectively and efficiency of the fon ‘exchange resin. increasing the pH of the preloading feed solution typically results in increased nickel loading. However, if the pH is too high, undesirable species precipitation may occur and/or impurity ioading may cease or decrease to unacceptably low levels. It ‘should be understood thal fresh and preloaded resin has available hydrogen fons for ‘exchange with suitable metal ions. As the hydrogen ion exchange reaction releases two hydrogen ions for each divalent metal (I) ion taken up by the resin, the acidity of discharge/effiuent from the fon exchange column tends towards increased acidity over time ‘such that the equilibrium pH tends to be greater than the initial pH. in some embodiment, a pronounced increase in acidity may be undesirable as this may have a negative effect on the resin's ability to selectively uptake the non-nickel metal impurities, for example, cobalt in the case where a TP272 resin is used and/or may inhibit nickel preloading/uptake by the resin. ‘Therefore, methods for controlling and/or buffering the solutions are important. Ina preferred embodiment, the pre-foading step involves introducing nickel ions to the resin in fresh form (protonated) under conditions whereby hydrogen ions on the fresh resin are exchanged for the introduced nickel ions, The nickel ions are typically provided in the form of a nicke! pre-load solution. Preferably, the process for selectively removing non-nickel metal impurities from a nickel sulfate solution further comprises the step of preloading the resin of the first round of ion exchange (IX) with nickel ions. Pre-loading with nickel reduces the hydrogen ion availabilty and thus assists in preventing as great an increase in equilibrium pH compared to that observed where fresh resin is used, Desirably, as further pH contro! may be desirable, one or more buffering agents can be used to control the pH at a value that ensures impurity, particularly Co impunity, loading stability and optimum selectively. Preferably, the ion exchange process includes the step of buffering the acidity of the solution passing through the ion exchange resin which increases5 10 15 20 28 30 35 WO 2019/090389 PCT/AU2018/051203 12 with time. Using nickel hydroxide as base/buffer advantageously avoids pH decrease during ion exchange avoids and avoids the introduction of alkali or ammonium contaminant during pH adjustment. Furthermore, the formation of ammoniacal nickel complexes is avoided during the pre-loading by avoiding ammonia pH adjustment; avoiding formation of nickel hydroxide precipitates at higher pH (pH > 6); minimising degradation and loss of resin functional groups by operating at relatively fow pH <6; and providing for minimum washing requirements. Preloading feed solution & pH control ‘Suitably, the resin of the first round of ion exchange is preloaded with nickel using a nickel pre-loading feed solution, which is preferably a portion of the first IX discharge solution, or an altemative source of filtered clean nickel sulfate solution, preferably in the presence of nickel hydroxide for pH adjustmentibuffering. Suitably, the pH of the pre-loading feed solution, for example, the first IX discharge solution, may be buffered/increased to a desired pH by the addition of one or more basic, ‘compounds, preferably basic nickel compounds, most preferably nickel hydroxide. Nickel hydroxide is suitable to raise the pH of an acidic sub-saturated nickel sulfate Solution to from about pH 5 to about pH 5.5. At higher pH, the nickel and/or other species may begin to precipitate. Most preferably, the resin is pre-loaded using clean nickel sulfate in the presence of nickel hydroxide for pH adjustment/buffering, Preferably, the preloading feed solution pH is from about pH 4.6 to about pH 6, more preferably from about pH 4.0 to about pH 5. in this latter pH range minimal nickel precipitation occurred while maximising nickel loading onto resin. In embodiments using TP 272 resin, the preferted preloading feed pH is from about 4.5 to about 6, more preferably from 4.5 t0 about 5.5, most preferably the preloading feed pH is about 5. For TP 272 resin in particular, using a pre-loading feed having a pH greater than about 5.5 tends to adversely affect Co impurity removal by the column. itis preferred that alkali bases such as sodium hydroxide, potassium hydroxide or ammonium hydroxide bases are avoided as the may lead to contamination in the final nicket sulfate product In preferred embodiment, the pre-loading step involves introducing @ clean nickel sulfate solution substantially free of non-nickel metal impurities. in other embodiments, the resin may be preloaded using an alternative source of fitered clean nickel sulfate solution. Preferably, the process involves the step of fitering the first IX discharge solution or altemative source of solution prior to preloading. Fittering prior to pretoading advantageously removes residual solids, for example, resin particles, Desirably, the nickel pre-loading is maximised using a maximum strength nickel pre- loading feed, preferably, a maximum strength clean nickel sulfate solution as described herein, Preferably, the nickel pre-loading feed solution has an initial concentration of nickel in the range of from about 130 g/t to about 210 g/L nickel, more preferably from about 150 g/L5 10 15 20 28 30 35 WO 2019/090389 PCT/AU2018/051203 13 to about 200 g/L. nickel, more preferably stil from about 175 g/L to about 195 g/L nickel, and most preferably about 190 g/L. MOH. Desirably a portion of the first IX discharge solution is used to generate nickel hydroxide and/or to preload the resin of the first round of ion exchange (IX) with nickel. in a preferred embodiment, the nickel hydroxide base is generated from a portion of the IX purified clean nickel sulfate solution, which is the first IX discharge solution. Suitably, the clean nicket sulfate solution substantially free of non-nickel metal impurities may be a portion of the first IX discharge solution as desoribed above, Alternatively, the nickel hydroxide could be produced from a bleed of a nickel powder refinery process, for example, a Sherritt Gordon Process, via ammonia steam stripping process to generate nickel hydroxide Desirably, the amount of nicket hydroxide provided is sufficient to neutralise acid released by the resin in exchange for nickel during nickel preloading. A preferred amount of nickel hydroxide is one that can substantially stabilise the pH pre-ioading feed solution such that the pH of the solution a column of resin is substantially the same as the pH of the solution discharging from the column of resin. in embodiments using TP 272 resin, the preferred preloading feed pH is from about 4.5 to about 6, more preferably from 4.5 to about 5.5, most preferably the preloading feed pH is about 5, For TP 272 resin, using a pre-loading feed having a pH greater than about 5.5 tends to adversely affect Co impurity removal by the ‘column. In preferred embodiments, the process for selectively removing non-nicket metal impurities from a nickel sutfate solution further comprises the step of generating the nickel hydroxide for pH adjustment/buffering from clean nickel sulfate solution, Preferably the process further comprises subjecting the first IX discharge solution to a ‘second round of ion exchange using nickel preloaded resin to provide a second IX discharge solution being a polished IX discharge solution. ‘Suitably, the second round of fon exchange may be used where impurity break through is observed in the first IX discharge solution Resin regeneration Suitably, the process further comprises the step of regenerating the resin used in ion ‘exchange, preferably on observation that () loading of substantially all of the non-nickel metal impurities onto the resin has been achieved or (i) break through of the non-nickel metal impurity in the first IX discharge solution. in a preferred embodiment, cobalt breakthrough in the IX column discharge solution can signity that resin regeneration or replacement is required.10 15 20 25 30 35 WO 2019/090389 PCT/AU2018/051203 14 Desirably. the method further comprises the step of replacing or regenerating the resin Used in the ion exchange rounds. Desirably, the requirement for replacement or regeneration of the resin may be determined for example on observation that loading of substantially all of the non-nicket metal impurities onto the resin has been achieved andior that the non-nickel metal impurity concentration begins to increase in the first IX discharge solution Suitably, regenerating resin which has been used in ion exchange involves the steps of washing the resin free of entrained nickel with an aqueous solution of acid, preferably sulfuric acid, preferably having a pH of about pH 4 to about pH 5; Gi) stripping retained non-nicket metal impurities from the resin using an aqueous acid solution, preferably sulfuric acid, preferably at a concentration of from about 0.25 M to ‘about 2.5 M acid, more preferably from about 1.0 M to about 2.0 M acid, wherein the stripping step exchanges the resin retained non-metal impurities for hydrogen ions in the acid, thereby loading hydrogen ions onto the resin to provide resin in the hydrogen form; (ii) removing excess acid from the resin by washing with water, preferably demineralised water; (v)__pre-loading the resin with nicket by fushing the resin with a nickel pre-toading ‘feed solution wherein the pre-loading exchanges at least a portion of the hydrogen ions. loaded onto the resin for nicket ions in the nickel pre-load feed, thereby loading nickel ions ‘onto the resin to provide resin in nickel pre-loaded form. Preferably, step (iv) is carried out as described above. Suitably, nickel pre-loading feed solution has @ pH about pH 4.5 to about pH 6, more preferably from about pH 4.0 to about pH 5. In this latter pH range minimal nickel precipitation ‘occurred while maximising nickel loading onto resin As discussed above, itis desirable that the nicket pre-loading feed solution is a clean nickel sulfate solution, more preferably being a portion of the first IX discharge solution, It should be understood that the clean nickel sulfate solution and the first IX discharge solution described herein is an acidic sub-saturated nickel sulfate solution, preferable obtainable by a leaching process as described herein In a particularly preferred embodiment, the nickel pre-loading feed solution further ‘comprises a buffering amount of nicket hydroxide. In one embodiment, a buffering amount of nickel hydroxide is one which is sufficient to optimise for selectivity and stability of non-nickel metal impurity loading onto the nickel pre-loaded ion exchange resin Desirably, the nickel pre-loading feed solution comprising nickel sulfate and/or nickel hydroxide is preferably fitered prior to the pre-loading step.10 15 20 25 30 35 WO 2019/090389 PCT/AU2018/051203 15 A silightly acidic pH for the wash, for example, a pH of about 3 to about 6, more preferably from about 4 to about 5. avoids dissolution of the active resin component which would lead to a loss of ion exchange capacity. in the case of TP 272, a pH of about 4 to about 5 is particularly suitable to preserve the resin, Advantageously, the wash sulfuric acid may be recycted to a leach acid solution for reuse Desirably, the strip solution comprising the removed impurities is transferred to a waste collection tank. Crystalfisation In particularly preferred embodiments, the clean nickel sulfate solution preferably being the first IX discharge solution, is crystallised to form high purity nickel sulfate orystals, preferably, nickel sulfate hexahydrate orystals, for example, in the alpha form. Suitably, in the process of the invention the sub-saturated nickel sulfate solution is an acidic pregnant leach solution, for example, obtainable from a nickel sulfate leaching process as defined herein, and which has been subjected to buik impurity removal and trace impurity removal via fon exchange as described herein, Suitably, the clean nickel sulfate solution may be fitered prior to crystatiisation In another aspect, the invention provides a process for producing high purity nickel suitable for use in battery manufacture or nicke! plating, preferably having a purty of 209.98% nickel sulfate, comprising the steps of: ( providing a solution sub-saturated with nickel sulfate and comprising one or more non-nickel metal impurities {i removing the bulk of the one oF more non-nickel metal impurities by raising the pH of the sub-saturated nickel sulfate solution by adding a basic nickel compound, preferably nickel hydroxide, to the sub-saturated nickel sulfate solution and separating the non-nickel ‘metal impurities from the solution in the form of precipitated insoluble non-nickel metat hydroxides; (ii) selectively removing remaining trace non-nicke! metal impurities from the sub- saturated nickel sulfate solution using one or more rounds of ion exchange purification involving at least a first round of fon exchange using a resin pre-loaded with nickel to forrn a fist IX discharge solution comprising nickel sulfate and a reduced amount of non-nicke! metal impurities which is a clean nickel sulfate solution being a substantially non-nickel metal impurities free sub-saturated nickel sulfate solution: (iv) recovering high purity nickel sulfate from the substantially non-nickel metal impurities free sub-saturated nicke! sulfate solution, preferably in the form of alpha nickel sulfate hexahydrate10 15 20 28 30 35 WO 2019/090389 PCT/AU2018/051203 16 Suitably, there is provided a process for producing high purity nickel suitable for use in battery manufacture or nickel plating, preferably having a purity of 209.98% nickel sulfate, ‘comprising the steps of () providing a solution sub-saturated with nickel sulfate and comprising one or more non-nickel metal impurities, preferably a pregnant leach solution, more preferably obtainable by a process as defined herein; Gi) removing the bulk of the one or more non-nickel metal impurities by raising the pH of the sub-saturated nickel sulfate solution by adding a basic nickel compound, preferably nickel hydroxide, to the sub-saturated nickel sulfate solution and separating the non-nickel metal impurities from the solution in the form of precipitated insoluble non-nickel metal hydroxides: (id selectively removing remaining trace non-nicke! metal impurities from the sub- saturated nickel sulfate solution using one or more rounds of ion exchange purification involving at least a first round of fon exchange using a resin pre-loaded with nickel to form a first IX discharge Solution comprising nickel sulfate and @ reduced amount of non-nicket metal impurities which is a clean nickel sulfate solution being a substantially non-nickel metal impurities free sub-saturated nickel sulfate solution; (iv) recovering high purty nickel sulfate from the substantially non-nickel metal impurties free sub-saturated nicket sulfate solution, preferably in the form of alpha nickel sulfate hexahydrate Preferably, the process further comprises the optional step of oxidising non-nickel ‘metal impurities in the sub-saturated nickel sulfate solution prior to the step of raising the pH. of the sub-saturated nickel sulfate solution to induce precipitation of insoluble non-nicket ‘metal impurities. Suitably, the insolubie precipitate is formed by increasing the pH of the discharge solution to a pH of about to about 7, preferably to a pH of about 4.5 to about §.5, more preferably to a pH of about 5, and separating the precipitate to form a non-nickel metal impurities depleted, preferably a non-nickel metal hydroxides-depleted sub-saturated nickel sulfate solution and which has been subjected to bulk impurity removal and trace impurity removal via ion exchange as described herein. Suitably, the clean nickel sulfate solution may be filtered prior to crystallisation. Desirably, recovering step (iv) involves erystallising the non-nickel metal impurity depleted sub-saturated nickel sulfate solution to form high purity nickel sulfate crystals, preferably nickel sulfate hexahydrate crystals, more preferably alpha nickel sulfate hexahydrate crystals. Crystalline alpha nickel sulfate hexahydrate is particularly desirable as itis the industry standard for applications such as battery manufacture and nickel plating, including electroless and electoplating,5 10 15 20 25 30 35 WO 2019/090389 PCT/AU2018/051203 7 In a preferred embodiment, the sub-saturated nickel sulfate solution is an acidic, pregnant each solution, for example, obtainable by leaching nickel powder in sulfuric acid, for ‘example, by a process as defined herein. ‘Suitably, the selectively removal step (ji) is an ion exchange process as defined herein. Preferably, the orystatising step is carried out at a temperature of from about 45 °C to about 65 °C, preferably from about 50 °C to about 60 °C, most preferably at about 53°C. and/or under a pressure of about 10 kPa absolute, preferably forming alpha erystalline nickel sulfate hexahydrate Suitably, the crystallising step is carried out in an evaporative crystalliser, for example, ‘a mechanical vapour recompression type crystalliser, preferably a draft tube baffle corystalliser. Suitably, the process further comprises the step of separating the crystals from the nickel sulfate solution, for example, dewatering using a fier, centrifuge or oycione. Preferably, the process further comprises the step of drying the crystals to provide dry high purity nickel sulfate hexahydrate, for example, in a fluid bed dryer. Plant In another aspect, the invention provides a processing plant capable of producing high Purity (299.8%, more preferably 299.98%) nickel sulfate from nickel powder comprising: (an acidic nickel leach module for generating sub-saturated pregnant leach solution comprising nickel sulfate and non-nickel metal impurities, preferably configured for batch leaching; (i) downstream of the acidic nickel leach module, a bulk non-nickel metal impurity removal module for precipitating the bulk of the non-nickel metal impurities, preferably configured to oxidise oxidisable non-nickel metal impurities in the pregnant ieach solution; Gi) downstream of the bulk non-nickel metal impurity removal module, a trace non-nickel metal impurity ion exchange removal module for removing trace amounts of non- nickel! metal impurity to form a purified sub-saturated nickel sulfate solution substantially free of non-nickel! metal impurity, preferably configured for one or more rounds of ion exchange in leadilag configuration; and optionally, (iv) downstream of the trace non-nickel metal impurity ion exchange removal module, a nickel sulfate crystallisation module for crystallisation of high purity nickel sulfate crystals from the purified sub-saturated nickel sulfate solution substantially free of non-nicket ‘metal impurity, preferably configured to crystallise alpha-nickel sulfate hexahydrate. Desirably, the plant further comprises a nickel hydroxide formation module for preparation of nickel hydroxide for use as an acid neutraliser and/or as a pH buffer in the10 15 20 28 30 35 WO 2019/090389 PCT/AU2018/051203 18 production of the high purity nickel sulfate, wherein the nickel hydroxide formation module is in communication with the bulk non-nicke! metal impurity removal module and/or the trace non-nickel metal impurity ion exchange removal module for providing nickel hydroxide solution thereto. Preferably, the nickel hydroxide formation module comprises a closed circuit for forming a nickel hydroxide solution such that ammonia and/or NaOH used for neutralisation and pH adjustment during nickel hydroxide preparation is isolated from the bulk non-nicket metal impurity removal module andior the trace non-nickel metal impurity ion exchange removal module thereby avoiding contamination of nickel sulfate solutions. ‘Suitably, the bulk non-nickel metal impurity oxidiser module is in communication with a source of oxidant, for example, air, and a source of nickel hydroxide acid neutraliser and/or as «4 pH buffer preferably from the nickel hydroxide formation module as described herein, Ina preferred embodiment, the plant further comprise a hydrogen gas mitigation module associated with at ieast module () and/or module (i) for management of hydrogen ‘985 evolved during processing, Suitably, the hydrogen gas mitigation module comprises a source of a steam flush for management of hydrogen evolved during the process. Preferably, the hydrogen gas mitigation module is configured to generate and maintain a steam flush comprising about 70 ‘vol% steam, The hydrogen gas mitigation module comprises a scrubber for scrubbing acidic mist from the off gas prior to venting to the atmosphere, In a preferred embodiment, the hydrogen gas mitigation module further comprises means for processing nickel leaching under a positive gauge pressure to prevent air ingress. Suitably, the hydrogen gas mitigation module further comprises a means for providing a blanket of nitrogen gas over at least module (i) and/or module (i) to assist in the prevention of the formation of a potentially explosive hydrogenvair mixture. Preferably, the plant is configured to provide sulfuric ackd from a refinery to the plant, wherein the plant is configured to provide sulfuric acid to the acidic nickel leach module for leaching nickel sulfate from nickel powder and/or sulfuric acid ion exchange removal module for ion-exchange stripping during regeneration. The plant is provided with a means for producing and/or providing demineralised water which is used to prepared required acid dilutions and wash for the ion exchange steps. Preferably, the plant further comprises a nickel sulfate dewatering module for removing the bulk of solute from nickel sulfate crystals downstream of the nickel sulfate crystallisation module Suitably, the plant further comprises a nickel sulfate crystal dryer module to dry the crystals to a high purty nickel sulfate hexahydrate product in powder form,5 10 15 20 28 30 35 WO 2019/090389 PCT/AU2018/051203 19 Ina preferred embodiment, the plant further comprises a high purity nickel sulfate product packaging module. Preferably, the plant is configured to recycle condensates from one or more plant modules, for example, heating coils in the leaching module, the product dryer module, and/or the crystallisation module for reuse. Suitably, the plant further includes one or more off-gas scrubbers, for example, associated with the acidic nickel leach module, the bulk non-nickel metal impurity oxidiser module and/or the bulk non-nickel metal impurity removal module for capture of gases and the nickel sulfate crystallisation module to capture nickel sulfate dust. In another aspect, the invention provides for a use of nickel hydroxide as an acid eutraliser and/or a pH buffer in a process for preparing high purity nickel sulfate, preferably having a purity of 299.8%, more preferably 299.98% nickel sulfate suitable for use in battery manufacture or nickel plating including electroplating and electroless plating, in another aspect, the invention provides for a use of nickel hydroxide as an acid neutraliser and/or a pH buffer in an ion exchange purification process for selective removal of on-nickel metal impurities from a nickel sulfate solution, preferable an acidic sub-saturated nickel sulfate solution, more preferably, an acidic sub-saturated nickel sulfate solution from which butk non-nickel metal impurities have been removed, In another aspect, the invention provides for a use of nickel hydroxide as an acid neutraliser and/or a pH buffer in nickel suifate solution, preferable an acidic sub-saturated hickel sulfate solution to precipitate non-nickel metal impurities in as insoluble non-nickel ‘metal impurities, for example, non-nickel metal hydroxides, in another aspect, the invention provides for a use of a nickel pre-loaded ion exchange resin to selectively remove non-nickel metal impurities from a nickel sulfate solution, preferable an acidic sub-saturated nickel sulfate solution, more preferably, an acidic sub- saturated nickel sulfate solution from which bulk non-nickel metal impurities have been removed. Suitably, the resin is a phosphoric acid, a phosphonic acid or phosphinic acid resin, In another aspect, the invention provides for a use of a nitrogen gas blanket to prevent formation of explosive air and hydrogen mixtures over an acidic nickel leach evolving hydrogen. {in another aspect, the invention provides for a use of a sub-saturated nickel sulfate solution in a process for the preparation of high purity nickel sulfate, preferably having a purity 0f 299.8%, more preferably 299.98% nickel sulfate, and preferably wherein the sub-saturated nickel sulfate solution is a pregnant leach solution, for example, obtainable by a process according to the invention.10 18 20 25 30 35 WO 2019/090389 PCT/AU2018/051203 20 In another aspect, the invention provides for high purity nickel sulfate obtainable by a process according to the invention. tn another aspect, the invention provides for a use of high putity nickel sulfate as defined in herein in the manufacture of an energy storage device, for example, a battery or capacitor andior in a nickel plating process including electroplating and electroless plating In another aspect, the invention provides for an energy storage device, for example, a battery or capacitor, comprising nickel sulfate obtainable by a process according to the invention, In another aspect, the invention provides for a product comprising plated nickel derived from comprising nickel sulfate obtainable by a process according to the invention. Brief Description of Drawings Figure 1 illustrates a process flow diagram for an exemplary embodiment of the production of high purity of nickel sulfate as described herein; Figure 2 illustrates the particle size distribution (PSD) of the nickel powder sample Used in the bench scale experiments: Figure 3(A) ~ (G) illustrate the results of bench scale experiments relating to the effect of pulp density on leaching: (A) Effect of pulp density on nickel powder dissolution in tests maintained at pH 0 and 1. Tests were maintained at 80 °C. with a compressed air aeration rate of 5 Limin. All tests were operated for a period of 10 hours; (8) Impact of Pulp density on leaching rate at pH 1, 80°C; (C) Comparison of Nickel concentration for tests operated under anaerobic conditions at 290 g/t. sulfuric acid, 80 °C; (D) Impact of Pulp density on Neutralisation Rate under anaerobic conditions: (E) Comparison of particle size distribution for tests operated under anaerobic conditions at 290 g/t sulfuric acid, 80 °C; (F) Impact of Pulp density on Ni Extraction for Anaerobic conditions with batch acid addition; (G) impact of Pulp Density on NNi Extraction Rate for Anaerobic conditions with batch acid adkiton; Figure 4(A) (D) ilustrate the results of bench scale experiments relating to the effect of pH on leaching: (A) Effect of operational pH on nickel powder dissolution. Tests were maintained at 80 °C, with a compressed air aeration rate of 5 Limin. All tests were operated {for a period of 10 hours with 1000 g/L nickel powder present; (8) Comparison of simple free hydrogen ion concentration and total nickel dissolution: (C) Comparison of total nickel dissolved and total sulfuric acid added over ail 34 tests, excluding anomalies of tests 7, 8 and 42; (D) Aerobic Impact of Leaching Time on pH Figure 5(A) ~ (C) iustrate the results of bench scale experiments relating to effect of aeration rate on leaching; (A) Impact of aeration rate and nitrogen on nickel powder dissolution at 80 °C, 1000 g/t nickel powder and pH 1.0. Red data point is Nz-sparged test;10 15 20 28 30 35 WO 2019/090389 PCT/AU2018/051203 21 (®) Impact of aeration rate on measured solution evaporation; (C) Effect of Aeration rate on Ni Extraction Rate; Figure 6(A) ~ (E) itustrate the results of bench scale experiments relating to effect of pH on impurity teaching; (A) Comparison of pH: (8) Comparison of free acidity; (C) ‘Comparison of Nickel; (0), Comparison of Cobalt (E) and Comparison of Copper (F) in tests ‘operated under anaerobic conditions at 237, 256, 275 and 293 g/t. sulfuric acid. Note that Cu and Co are reported in mg/L compared to Nickel (g/L); Figure 7(A) & (B) illustrate the results of bench scale experiments relating to effect of temperature on leaching: (A) Impact of temperature on nickel powder dissolution at pH 1.0, 1000 g/L nickel and 5 L/min aeration, Red data points represent tests undertaken using uncoated impellors; (B) Effect of Temperature on Leaching Rate: Figure 8(A) ~ (G) ilustrate the results of bench scale experiments relating to batch ‘acid leaching; (A) Impact of acid loading on nickel powder dissolution at €0 °C with 1000 g/L nickel and 5 Limin aeration, (B) Neutralisation with time for acid joading tests at 80 and 100 °C; (©) Nickel concentration over time during tests operated under near-optimal conditions (D) Solution pH over time in near optimal tests. Tests were operated at 80°C, 1000 g/t. nickel and 4 L/min aeration; (E) Aerobic Batch Acid Addition Ni Extraction Rate; (F) Impact of acid loading on nickel extraction rate; (G) Batch acid adaition pH profile; Figure 9(A) ~ (H) illustrate the results of bench scale experiments relating to the effect of acid concentration on impurity leaching for Co, F, Cr, K, Ca, Na, Cu, Zn respectively: Selected impurity element concentrations throughout experiments. Note that Cu is reported in ug/L (ppb), compared to all other elements in mg/L. (ppm); Figure 10 illustrates a comparison of iron, copper and zinc concentrations to pH Note that Cu and Zn are reported in ug/L. (ppb), Fe reported in mg/l. (ppm): Figure 11(A) & (B) illustrate the resutts of bench scale experiments relating to the effect of agitation on leaching: (A) Comparison of Nickel concentration; (B) pH for tests operated under anaerobic conditions at 290 git sulfuric acid, 80 °C; Figure 12(A) - (E) illustrates a schematic of the IX process of the invention and results of bench scale experiments relating to the effect of preloading of resin on IX; (A) ‘schematic of the IX process of the invention; (B) pH isotherms with fresh TP272 without pH ‘control showing the effect of ulilizing the ion exchange resin TP 272 without pre-toading; (C) Ni pre-loading with Ni sulphate solution (ntial 20 g/L Nd; (D) Ni loading pH profile with various nickel concentration in the feed solutions (80 °C); (E) Ni pre-loading kinetics for pH 5 and 6 at 80°C: Figure 13(A) ~ (K) illustrates the results of bench scale experiments relating to the effect of non-preloaded resin and comparison to nickel pre-loaded resin; (A) Comparison of initial solution pH with final pH after equilibrium loading; (B) Metal loading (36) pH isotherms10 15 20 28 30 WO 2019/090389 PCT/AU2018/051203 22 with fresh TP 272 vs. final pH without pH control; (C) Metal loading (mg/g resin) pH isotherms with fresh TP 272 vs. final pH without pH control; (D) Metal loading (mg/g) pH isotherms with Ni pre-loaded resins at pH 6 with nickel hydroxide: (E) Metal loading (%6) pH isotherms with Ni pre-loaded resins at pH 5 with nickel hydroxide; (F) Ratfinate metal concentrations; (G) Metals in the neutralised synthetic PLS; (H) Metal loading (mg/g) pH isotherms with Ni pre- loaded resins at pH 6 with ammonium hydroxide; (P) Metal loading (%) pH isotherms with Ni pre-loaded resins at pH 6 with ammonium hydroxide; (J) Raffinate metal concentrations; (K) Final equilibrium pH vs. initial pH using the Ni preloaded resins and the synthetic PLS with pH pre-adjusted with nickel hydroxide: Figure 14(A) ~ (D) illustrates (A) pH isotherm profile for TP 272; (B) pH isotheam profile for Cyanex 272 resin; Figure 15(A) ~ (D) illustrates the results of bench scale experiments relating to cobalt stripping kinetics: (A) Ni and Co loading (maya) vs. loading time; (B) Ni and Co loading (%) vs. loading time; (C) Mass balance of Ni and Co loading; (D) Metal stripping (%) vs. stripping time; Figure 16 illustrates the results of bench scale experiments relating to the effect of pH (HS0, concentration) on % metal stripping; Figure 17(A) ~ (H) illustrates the results of bench scale experiments relating to the results based on air dry mass; (A) Metal loadings (%) vs. resin / solution ratio; (B) Metal loading (mg/g) vs. resin / solution ratio (g/mL); (C) Metal in raffinate vs. resin / solution ratio; (D) Co distribution isotherms on air dry resin basis; (E) Comparison of Co distribution isotherm curves based on air dry and estimated dry resin mass; (F) Langmuir model Fitting 4 linear part by taking 6 data points; (G) Langmuir modet Fitting 2: linear part by taking 8 data points: (H) Freundlich isotherm equation fitting: linear part by taking 8 data points; () ‘Comparison of Ni and Co loadings and variation of equilibrium pH; Figure 18 illustrates the results of bench scale experiments relating to the total exchange capacity vs. stabilly test cycles; Figure 19(A) — (E) ilustrates the results of bench scale experiments relating to the variation of exchange capacity; (A) Metat loadings on the resin vs. cycles; (B) Co behaviour in the stabilty tests; (C) Ni behaviour in the stabilty tests; (D) Fe behaviour in the stability tests; (©) Cu behaviour in the stability tests;5 10 15 20 25 30 35 WO 2019/090389 PCT/AU2018/051203 23 Figure 20(A) ~ 20(E) illustrates the results of bench scale experiments relating to the ‘effect of consecutive loading and sampling; (A) Variation of raffinate metal concentrations with pH; (8) Variation of metal loadings with pH based on aqueous assays; (C) Metal loading efficiency (%) vs. pH with TP 207; (D) Raffinate metat concentrations vs. pH with TP 207; Metal mass loading vs. pH with TP 207; Figure 21(A) & (B) illustrates the results of bench scale experiments relating to the loading kinetics with TP 207; (A) Raffinate metals vs. time with TP 207; (B) Metal joadings vs time with TP 207; Figure 22(A) - 22(D) illustrates the results of bench scale experiments relating to loading distribution isotherms for TP 207; (A) Metal loading (%) vs. solution / resin ratios: (B) Raffinate metal concentration with solution / resin ratios: (C) Metal loading at various A/ Resin (TP 207) ratios; (D) Fe distribution isotherm with resin TP 207; Figure 23 illustrates the results of bench scale experiments relating to the elution of ‘TP In particular to elution acidity isotherms with TP 207; Figure 24(A) - 24(C) illustrates the results of bench scale experiments relating to IX — Amberlite IRC 748 resin; (A) Metal loading efficiency vs. pH with IRC 748 resins; (B) Raffinate metals vs. pH with IRC 748 resin; (C) Metal loadings on resin vs. pH with IRC 748 resin; Figure 26 illustrates the results of bench scale experiments relating to IX ~Purolite; (A) Metal loading pH isotherms with Purolite $910 resin; Figure 26(A) - 26(C) illustrates the resutts of bench scale experiments relating to SX ~ cyanex 272; (A) Metal extraction pH isotherms with 10% Cyanex 272 in Shellso! D70 at 80 ° and 1:1 A/O ratio; (B) Metal extraction in organic phase with 10% Cyanex 272 in Shetisol D70 at 80 ° and 4:1 A/O ratio; (C) Metals in raffinate vs. pH with 10% Cyanex 272 in Shelisol 70 at 80° and 1:1 A/O ratio; Figure 27(A) & 27(B) ilustrates the results of bench scale experiments relating to ‘column loading tests; (A) Column 4 metal loading profile; (B) Colurnn metal loading sampled ‘on the column top; Figure 28 illustrates the results of bench scale experiments relating to polishing/ioading experiments Raffinate Co assayed by ICP-MS vs. bed volume for the ‘samples from Column 3 ~ Polishing Runs with Column 1 raffinate solutions as feed at 3 different flow rates or residence time, Figure 29 illustrates the results of bench scale experiments relating to the effect of column washing in particular a column Co loading washing profile; Figure 30 illustrates the results of bench scale experiments relating to column washing in particular the elution profile at different acidities (HO, concentrations).10 15 20 25 30 35 WO 2019/090389 PCT/AU2018/051203 24 Figure 31 illustrates the results of bench scale experiments relating to column elution washing: Figure 32(A) - 32(E) itustrates the results of bench scale experiments relating to the effect of column tests; (A) breakthrough point of TP 272 resin; (B) cobalt breakthrough curve ‘comparison. Detailed Description Overall description of a preferred embodiment of the process A flowsheet to produce high purity nickel sulfate is shown in Figure 1 Nickel leach module A ‘Nickel powder 100 is teached in a batch process in a nickel leach module A. Nickel each module A comprises one or more leach acid solution preparation tanks 110, preferably a plurality of tanks, which are in fluid communication with the following sources of consumables: a source of steam andior nitrogen gas 180, a source of sulfuric acid 190, a source of demineralised water 120 for diluting the sulfuric acid to a desired concentration, and a source of nickel powder 100, for example directly from @ nearby nickel powder refinery. The tanks are adapted to include a source of steam for heating, for example, indirect steam. heating via heating coils associated with the tanks 110. Agitation is provided by the leach acid solution preparation tank agitators (not shown) which are associated with the tanks 140, The nickel leach module A also comprises a teach gas scrubber 170 for scrubbing hydrogen ‘evolved from leaching from the vapour spaces about the tanks 110. The leach gas scrubber 170 is configured to vent scrubbed off-gas 160 to the atmosphere. ‘The buik impurity removal module B comprises one oF more solution aeration vessels 190 which is in communication a source of oxygen/ai 200 for sparging into the vessels 190 to convert iron impurity in the discharge solution 140 from the ferrous to fersic oxidation state. The aeration vessels 190 are in fluid communication with a source of a nickel hydroxide slurry 390 which is generated in a nickel hydroxide preparation module C. The aeration vessels 190 are equipped with separate acid mist scrubber (not shown) to the leach tanks 110 to ensure hydrogen and oxygen do not mix in the off-gas scrubbers. The scrubber is configured to vent scrubbed off-gas 220 to the atmosphere. The vessels are in ‘communication with one or more solution polishing fiters 230 for removing any remaining solids fo generate a fitered non-nickel metal impurity depleted discharge solution 260 ready {for jon exchange which occurs in jon exchange module C. The polishing fiters 230 are ideally configured to operate in a duty/standby arrangement, and can be equipped with a backwash cycle and a solution filler sludge tank (not shown) and transfer pump (not shown). Module 810 18 20 28 30 35 WO 2019/090389 PCT/AU2018/051203 25 further comprises an IX feed tank (not shown) for holding fitered non-nickel metal impurity dopleted discharge solution 280 before IX. lon exchange module € ‘This module comprises one or more ion exchange (1X) columns 270 which ideally are arranged in a lead/iag configuration. A third column (not shown) may be provided offline {or regeneration which includes washing, stripping and pre-loading. The fourth colurnn (not ‘shown) may be installed as a spare. The columns will be loaded with suitable resin. An ion exchange discharge tank (not shown) is included in module C for holding resultant first IX discharge solution which is a clean nickel sulfate solution 310 substantially free of non-nickel ‘metal impurities. The tank is associated with one or more ion exchange discharge polishing fitters 400 for removing any carry-over resin or solids from the IX columns 270. A crystalliser plant feed tank (not shown) holds fered clean nickel sulfate solution 420 and is in uid ‘communication with the orystalliser 450 of a crystalliser plant E. The fluid line between the ‘one or more ion exchange discharge polishing fiters 400 and the crystalliser 460 configured to divert a small portion of the ftered clean nickel sulfate solution 420, a nickei hydroxide preparation module B and to an ion exchange nickel preload tank (not shown} to be held until 1X column 270 regeneration is required. The 1X columns 270 adapted to be in fluid communication with a source of acid, demineralised water and nickel preload solution from the nickel hydroxide preparation module B as well as an ion exchange waste tank (not shown). The one or more ion exchange discharge polishing filters 400 are in fluid ‘communication with a source of demineralised water 410 and the crystalliser 450. Leaching module A ‘Nickel powder 100 is leached in a batch process in a nickel leach module A which ‘comprises one or more leach acid solution preparation tanks 4140, preferably a plurality of tanks. The nickel powder 100 may be provided to the nickel powder leach plant A from a discharge of wel metals driers in a nickel leach plant before the powder is either packaged or converted in to briquettes. The batch process begins with the transfer of nickel powder 100 to the tanks 110. The target concentration of nickel powder in solution is 1000 git. This is @ significant excess in the amount of nickel than that stoichiometrically needed for the reaction, to ensure high reaction kinetics. Typically only approximately 10% of the nickel powder in the tanks 110 reacts during the batch cycle. The reaction proceeds are per the equation below. Nig) + H250s (aq) > Hacgy + NiSOxcaqy a In the leach acid solution preparation tanks 110, sulfuric acid 130 is continuously mixed with demineralised water 120 to generate acid of a target concentration. The acid dilution is exothermic and this step must be operated with caution. The tanks 110 are then fed5 10 15 20 25 30 35 WO 2019/090389 PCT/AU2018/051203 26 with a batch make-up of sulfuric acid solution 130 at a sulfuric acid concentration of approximately 280 g/L. The sulfuric acid solution 130 is transferred to the batch leach tanks 110 on demand using an acid solution pump (not shown). This acid concentration is controlled by addition of demineralised water 120 in order to have the discharge solution 140 ‘at 95% of the saturation limit of nickel sulphate at 80°C. The demineralized water 120 for acid ditution may be supplied by hydrogen plant demineralized water pumps (aot shown). ‘Operating close to saturation at 80°C minimises the evaporation duty of the crystaliser 450 in crystallisation module E, and eliminates the need for a pre-evaporator. Heating, preferably steam heating, is applied indirectly via heating coits (not shown) in the tanks 110, to maintain the tanks 110 temperature at 80°C. Agitation is provided by the leach acid solution preparation tank agitators (not shown). ‘The leaching process evolves hydrogen. To prevent the formation of an explosive ‘environment, the vapour space about the leach acid solution preparation tanks 110 is flushed with flush steam 150 and the tanks are preferably operated at a positive pressure to prevent ingress air. The flush steam (snuffing steam) 150 ideally maintains a minimum 70 vot% steam atmosphere in the vapour space about the tanks 110, The resultant hydrogen containing off ‘985 160 is processed by a leach off-gas scrubber 170 which captures acid mist and particulates before the scrubbed off-gas 180 is discharged via a stack (not shown). In an ‘emergency, where the tanks 110 are operating but the off-gas scrubber 170 fails, the vapour ‘space about the tanks 140 which are connected to a source of nitrogen (not shown) can be flooded with nitrogen 150 to form a nitrogen blanket which can prevent the formation of an explosive environment. At the completion of the leach, the residual acid concentration in the tanks 110 correlates to approximately pH 3, and the nickel sulfate in solution concentration approximately 192 g/L. The terminal nickel strength is determined by the amount of acid added to the batch (as there is a vast excess of nickel). The decision to terminate the reaction at pH 3 is a trade-off between () terminating at a lower pH, but requiring a much increased amount of nickel hydroxide 390 to neutralise the excess free acid, and (ji) terminating at a higher pH, meaning the reaction takes much longer and so would require increased capital for the farger reaction tank 140, given total throughput is fixed. At the end of the leaching process, agitation is stopped and the solids are settled The leach discharge solution 140 is decanted from the tanks 110 via a leach decant pump (not shown). Un-leached solids remain in the heel of the leach tanks 110 and are re- processed in the next batch of the leach cycle. ‘An exemplary leach batch cycle is shown below in Table 1