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WO2008138038A1 - Lixiviation à faible eh avec recyclage du soufre - Google Patents

Lixiviation à faible eh avec recyclage du soufre Download PDF

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Publication number
WO2008138038A1
WO2008138038A1 PCT/AU2008/000645 AU2008000645W WO2008138038A1 WO 2008138038 A1 WO2008138038 A1 WO 2008138038A1 AU 2008000645 W AU2008000645 W AU 2008000645W WO 2008138038 A1 WO2008138038 A1 WO 2008138038A1
Authority
WO
WIPO (PCT)
Prior art keywords
leach
nickel
process according
cobalt
slurry
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/AU2008/000645
Other languages
English (en)
Inventor
Daniel Arthur Kittelty
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BHP SSM Indonesia Holdings Pty Ltd
Original Assignee
BHP Billiton SSM Development Pty Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from AU2007902547A external-priority patent/AU2007902547A0/en
Application filed by BHP Billiton SSM Development Pty Ltd filed Critical BHP Billiton SSM Development Pty Ltd
Publication of WO2008138038A1 publication Critical patent/WO2008138038A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching processes
    • C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
    • C22B23/043—Sulfurated acids or salts thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00—Obtaining copper
    • C22B15/0063—Hydrometallurgy
    • C22B15/0084—Treating solutions
    • C22B15/0089—Treating solutions by chemical methods
    • C22B15/0093—Treating solutions by chemical methods by gases, e.g. hydrogen or hydrogen sulfide
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates to a new hydrometallurgical method of leaching nickeliferous lateritic ores, to recover nickel and cobalt values.
  • the present invention provides a method of acid leaching nickel and cobalt containing laterite or partially oxidised laterite ores together with a reducing agent, such as sulfur dioxide, to obtain a low Eh leach which leads to the conversion of the majority of any iron present in the iron (III) state to the iron (II) state. This leads to a process where the sulfur present in the leach may be recycled while producing a more environmentally acceptable residue.
  • Laterite nickel and cobalt ore deposits generally contain oxidic type ores, limonites, and silicate type ores, saprolites in the same deposits.
  • the higher nickel content saprolites tend to be commercially treated by a pyrometallurgical process involving roasting and electrical smelting techniques to produce ferronickel.
  • the power requirements and high iron to nickel ore ratio for the lower nickel content limonite and limonite/saprolite blends makes this processing route too expensive, and these ores are normally commercially treated by a combination of pyrometallurgical and hydrometallurgical processes, such as the high pressure acid leach (HPAL) process or the Caron reduction roast- ammonium carbonate leach process.
  • HPAL high pressure acid leach
  • Heap leaching is a conventional method of economically extracting metals from low grade ores and has been successfully used to recover materials such as copper, gold, uranium and silver. Generally it involves piling raw ore directly from ore deposits into heaps that vary in height. The leaching solution is introduced on to the top of the heap to percolate down through the heap. The effluent liquor is drained from the base of the heap and passes to a processing plant where the metal values are recovered.
  • Heap leaching has been proposed in recovery processes for nickel and cobalt and is described for example in U.S. patent 5,571 ,308 and 6,312,500, both in the name of BHP Billiton, but it has not yet been used commercially. However, it offers promise of a low capital cost process, eliminating the need for expensive and high maintenance, high pressure equipment required for the HPAL process.
  • the Eh is typically maintained at a sufficiently high level that the iron is predominantly in the iron (III) state during the actual leach.
  • the Eh during an acid leach process of a laterite ore is in the range of from 600-900 mV.
  • the solids residue from such processes may be environmentally unfriendly, as they may contain a large proportion of iron as jarosite.
  • Jarosite is not a stable compound and slowly releases acid as it weathers, which could have negative environmental impacts.
  • the present invention aims to overcome or at least alleviate one or more of the difficulties associated with the prior art by developing a process where iron is converted to the iron (II) state during a laterite leach process, which will result in a more environmentally acceptable residue, while recycling the sulfur for further use in the leach process.
  • iron is converted to the iron (II) state during a laterite leach process, which will result in a more environmentally acceptable residue, while recycling the sulfur for further use in the leach process.
  • the present invention relates to a process that involves a low Eh leach of nickel and cobalt containing laterite ores.
  • the process involves leaching the ores in the presence of a reducing agent to lower the Eh of the leach process, which leads to conversion of the majority of iron in the iron (III) state to the iron (II) state, and allows the integration of sulfur recycling into the process.
  • the present invention resides in a process for leaching nickel and/or cobalt containing laterite or partially oxidised laterite ore, including the steps of: a) providing a laterite or partially oxidised laterite ore; b) leaching the ore in a leach step with an acid in the presence of a reducing agent to produce a leach discharge containing nickel and/or cobalt values; c) recovering the nickel and/or cobalt from the leach discharge leaving a nickel and/or cobalt barren discharge liquor; and d) treating the discharge liquor to recover at least a portion of any sulfur as sulfur dioxide and/or sulfuric acid; wherein the reducing agent is present in a sufficient amount to lower or maintain the
  • the process is particularly applicable to pressure, atmospheric or heap leach processing of laterite ores or combinations of these processes.
  • the leach discharge is a slurry and the process of the invention includes a solid/liquid separation step where a solid residue is separated from the slurry to produce a nickel and/or cobalt rich product leach solution.
  • the nickel and/or cobalt may be recovered directly from the leach slurry by resin-in-pulp techniques.
  • the leach step may be conducted as a heap leach process.
  • the laterite ore may be piled in one or more heaps and the acid, together with the reducing agent, allowed to percolate through the heap or heaps to produce the leach discharge containing the nickel and/or cobalt values.
  • a plurality of heaps may be established and leached in a counter current process.
  • the leach discharge recovered from the heap leach process is generally a solution containing the nickel and/or cobalt values.
  • the presence of the reducing agent in the leach step lowers the Eh of the leach resulting in the majority of the iron (III) present being converted to iron (II) state.
  • the reducing agent in the leach step is generally a sulfur containing compound or gas, which in a preferred embodiment, is sulfur dioxide.
  • the sulfur dioxide recovered following treating the barren discharge liquor may be recycled for use as the reducing agent in the leach step.
  • other sulfur containing components could be used such as metabisulfite, dithionite and thiosulfate.
  • the nickel and/or cobalt may be recovered from the product leach solution by adding a sulfiding agent to a product leach solution to precipitate the nickel and cobalt as sulfides, leaving a nickel and cobalt barren discharge liquor.
  • the nickel and/or cobalt could be recovered from the product leach solution by other known processes, such as ion exchange or solvent extraction techniques, and leave a nickel and/or cobalt barren discharge liquor.
  • the nickel and/or cobalt barren discharge liquor includes other ions such as ferrous iron, aluminium and magnesium.
  • these ions may be removed or recovered by crystallising them as their sulfates by cooling or refrigerating the discharge liquor. Alternatively, they may also be crystallised by subjecting the discharge liquor to evaporation. Additional sulfuric acid may be added to assist in the crystallisation process.
  • the solid crystallised sulfates may then be separated from the discharge liquor and heated within the range from 550 °C to 800 °C in the presence of elemental sulfur to produce metal oxides and sulfur dioxide gas.
  • the metal oxide will generally be considered as reject material, but may in some circumstances, be retained for further processing or other commercial uses.
  • the sulfur dioxide gas that is produced in this step can be recycled to the start of the leach step as a source of the reducing agent, together with the remaining discharge liquor.
  • some of the sulfur dioxide gas may be used for sulfuric acid generation for use in the leach process or the crystallisation step.
  • the process is particularly applicable to processing laterite ores.
  • the limonite component of the laterite ore is first leached with sulfuric acid under low Eh conditions to produce a primary leach slurry and then the saprolite component is added to the primary leach slurry to complete leaching of the ore and to aid in neutralising the leach slurry.
  • the pH of the leach slurry can be further adjusted with a base, such as limestone, to precipitate any ferric iron that may remain to form a neutralised leach slurry.
  • the as mined ore mixture of limonite and saprolite may be leached together, or the separated limonite and saprolite components may be leached in parallel, or any combination thereof.
  • the processing of the saprolite and limonite component may be tailored to optimise ore handling costs and/or sulfuric acid usage.
  • the leach slurry is at least partially neutralised as outlined above.
  • the neutralised leach slurry preferably undergoes a solid/liquid separation step such that the solid residue is separated from the leach slurry to form a neutralised product leach solution.
  • nickel and cobalt are recovered from the product leach solution by adding a sulfiding agent such as hydrogen sulfide or sodium hydrosulfide to the product leach solution to form a sulfide slurry, and precipitated from the sulfide slurry as nickel and/or cobalt sulfides, leaving a nickel and cobalt barren discharge liquor.
  • the dissolved iron in the product leach solution is in ferrous form, it will not precipitate as a sulfide, and so remains in the discharge liquor, to be disposed of with other metals as metal oxides following crystallisation of ions remaining in the discharge liquor, and does not become an impurity in the mixed nickel and/or cobalt sulfide.
  • the nickel and/or cobalt may be recovered from the product leach solution by other known techniques such as solvent extraction and ion exchange.
  • the nickel and cobalt may also be recovered directly from a leach slurry by resin-in-pulp techniques.
  • the discharge liquor which is substantially free of nickel and cobalt following the nickel and/or cobalt recovery step, can then be cooled or refrigerated to crystallise any ferrous iron, aluminium, magnesium and other ions that remain in solution as their respective sulfates either separately or as a mixture of sulfates. Additional sulfuric acid could be added at this stage to assist in the crystallisation process. Further solid/liquid separation could then be employed to remove the solid crystallised sulfates.
  • An alternative to cooling or refrigerating the discharge liquor to crystallise the metal sulfates is to subject the discharge liquor to an evaporation step to produce the metal sulfates.
  • the remaining discharge liquor together with condensed vapour is then recirculated as part of the leach solution in the leach step.
  • the crystallised metal sulfates may then be reduced to their metal oxides and sulfur dioxide gas generated by heating the metal sulfates in the presence of elemental sulfur in a reducing atmosphere. This is preferably done at a temperature within the range of from 550°C to 850°C. Additional energy may be required for this step, as even though the reactions for the expected elements are exothermic, the dehydration of the precipitated solids may require additional heat.
  • the remainder of the discharge liquor can then be recycled to the leach step.
  • the discharge liquor can be combined with all, or a portion of the sulfur dioxide gas to form the leach solution for the leach process, with the sulfur dioxide acting as the reducing agent to produce the low Eh leach conditions.
  • a portion of the sulfur dioxide gas may be used to generate sulfuric acid as required, to supplement the acid used for the leach step, or for use in the crystallisation step.
  • the process of the invention provides the benefit in that the metal oxides that are recovered are more environmentally acceptable than say, for example jarosite, and may be used for alternative commercial purposes. Further, a significant proportion of the sulfur that would normally be lost to tailings is recovered and reused within the leach process, minimising raw materials costs and further reducing waste discharge.
  • Figure 1 shows a proposed flowsheet for the process of the invention.
  • Figure 2 is a graph showing the higher iron level in the product leach solution at lower leach Eh levels.
  • Figure 3 is a graph showing the percentage of iron precipitated at various Eh levels.
  • Figure 1 illustrates a low Eh leach step (1 ) where an ore (3) is leached in multiple separate tanks.
  • the limonite component of the laterite ore is leached with sulfuric acid in the presence of a reducing agent in the first tank (5) to produce a primary leach slurry, which is then transferred to the second tank (7) where the saprolite component is added to undergo further leaching and partially neutralise the leach slurry.
  • Limestone (9) is added to the primary leach slurry (1 1 ) to complete neutralisation of the leach slurry.
  • the solid leach residue (13) is then separated from the neutralised leach slurry (15) leaving a neutralised product leach solution.
  • a sulfiding agent (17) such as hydrogen sulfide or sodium hydrosulfide is added to the neutralised product leach solution (19) precipitating nickel and cobalt sulfides to form a sulfide slurry (21 ).
  • the nickel and cobalt sulfide solids are separated off (23) leaving a discharge liquor barren of nickel and cobalt (25).
  • the barren discharge liquor then undergoes a cooling and/or refrigeration step (27) to crystallise any ferrous iron, aluminium, magnesium and/or other ions that remain in the solution as their sulfates either separately or as a mixture of sulfates.
  • the crystallised sulfate solids are then heated with elemental sulfur in a reducing atmosphere (29) to produce metal oxides (31 ) and sulfur dioxide gas (33).
  • An alternative to cooling/refrigeration is to subject the discharge liquor to an evaporation process (35) where the solids are crystallised as sulfates. The remaining discharge liquor is condensed (37) for recycle to the leach process.
  • Sulfuric acid generated in the process may be combined with the recycled discharge liquor and the remaining portion of the sulfur dioxide gas in a mix tank (39) and recycled for use as the low Eh leach solution (40) in the leach step (1 ).
  • Figure 2 illustrates a process where the saprolite slurry has been added to the limonite slurry and demonstrates that at lower Eh levels (45OmV) the iron from the saprolite can be seen to leach. This is due to the iron being in the ferrous form, from which it is unable to precipitate.
  • Figure 3 further illustrates that at higher Eh levels (for example 80OmV) results in a higher percentage of the iron precipitating from the solution, which will usually be in the form of jarosites and goethites. At lower Eh (45OmV) less iron precipitates as the iron will be substantially in the ferrous form.
  • Eh levels for example 80OmV
  • Table 2 gives the metal recoveries when the leach conditions were typical atmospheric acid leach conditions.
  • Table 3 shows the metal extractions obtained when using the low Eh ferrous ion producing conditions. Clearly the saprolite leach results under these conditions results in a significant improvement of both cobalt and nickel extraction.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

L'invention concerne un procédé de lixiviation du minerai de latérite contenant du nickel et/ou du cobalt ou du minerai de latérite partiellement oxydé. Ledit procédé comprend les étapes consistant : a) à fournir un minerai de latérite ou un minerai de latérite partiellement oxydé; b) à lixivier le minerai lors de la lixiviation à l'aide d'un acide en présence d'un agent réducteur, pour produire un lixiviat résiduel contenant du nickel et/ou du cobalt; c) à récupérer le nickel et/ou le cobalt du lixiviat résiduel en produisant une liqueur résiduelle stérile en nickel et/ou cobalt; et d) traiter la liqueur résiduelle afin de récupérer au moins une partie du soufre présent sous la forme de dioxyde de soufre et/ou d'acide sulfurique; l'agent réducteur étant présent en une quantité suffisante pour abaisser ou maintenir la valeur d'Eh de l'étape de lixiviation de telle sorte que la majeure partie du fer (III) présent dans le procédé de lixiviation est convertie à l'état de fer (II).
PCT/AU2008/000645 2007-05-14 2008-05-12 Lixiviation à faible eh avec recyclage du soufre Ceased WO2008138038A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AU2007902547A AU2007902547A0 (en) 2007-05-14 Low Eh Leach with Sulfur Recycle
AU2007902547 2007-05-14

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WO2008138038A1 true WO2008138038A1 (fr) 2008-11-20

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8147781B2 (en) * 2009-09-09 2012-04-03 Sheritt International Corporation Recovering metal values from a metalliferrous material
US20130291686A1 (en) * 2012-05-04 2013-11-07 Vale S/A Sulfide ore leaching process
CN104805282A (zh) * 2014-01-28 2015-07-29 广西银亿科技矿冶有限公司 一种红土镍矿硫酸熟化堆浸方法
CN109797295A (zh) * 2019-02-15 2019-05-24 四川大裂谷钒业有限公司 从含钴铁精矿中提钴的方法
EP3395968A4 (fr) * 2015-12-25 2019-07-10 Sumitomo Metal Mining Co., Ltd. Procédé d'élimination d'agent de sulfuration
WO2020073411A1 (fr) * 2018-10-08 2020-04-16 金川集团股份有限公司 Procédé d'extraction de nickel, de cobalt et de fer à partir de minerai de nickel latéritique de qualité inférieure
CN112662892A (zh) * 2020-12-15 2021-04-16 衢州华友钴新材料有限公司 一种酸浸液的掺杂高压镍铁分离方法
CN113502394A (zh) * 2021-05-26 2021-10-15 广东佳纳能源科技有限公司 一种钴或镍的中间品回收的方法
WO2023005404A1 (fr) * 2021-07-29 2023-02-02 广东邦普循环科技有限公司 Procédé de lixiviation et d'extraction d'un métal précieux et d'un élément sulfureux à partir d'une matte à faible teneur en nickel

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1086075A (fr) * 1977-05-10 1980-09-23 Kohur N. Subramanian Reduction de melanges d'oxydes par lessivage
US4410198A (en) * 1981-04-30 1983-10-18 Versatron Research Corporation Human powered vehicle
US20060024224A1 (en) * 2004-08-02 2006-02-02 David Neudorf Method for nickel and cobalt recovery from laterite ores by combination of atmospheric and moderate pressure leaching
WO2006029443A1 (fr) * 2004-09-17 2006-03-23 Bhp Billiton Ssm Technology Pty Ltd Production de mattes de ferronickel ou de nickel au moyen d'un procede combine d'hydrometallurgie et de pyrometallurgie
US20060228279A1 (en) * 2005-04-07 2006-10-12 Finlay Campbell Process for recovery of nickel and cobalt from laterite ore

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1086075A (fr) * 1977-05-10 1980-09-23 Kohur N. Subramanian Reduction de melanges d'oxydes par lessivage
US4410198A (en) * 1981-04-30 1983-10-18 Versatron Research Corporation Human powered vehicle
US20060024224A1 (en) * 2004-08-02 2006-02-02 David Neudorf Method for nickel and cobalt recovery from laterite ores by combination of atmospheric and moderate pressure leaching
WO2006029443A1 (fr) * 2004-09-17 2006-03-23 Bhp Billiton Ssm Technology Pty Ltd Production de mattes de ferronickel ou de nickel au moyen d'un procede combine d'hydrometallurgie et de pyrometallurgie
US20060228279A1 (en) * 2005-04-07 2006-10-12 Finlay Campbell Process for recovery of nickel and cobalt from laterite ore

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8147781B2 (en) * 2009-09-09 2012-04-03 Sheritt International Corporation Recovering metal values from a metalliferrous material
US20130291686A1 (en) * 2012-05-04 2013-11-07 Vale S/A Sulfide ore leaching process
US9085812B2 (en) * 2012-05-04 2015-07-21 Vale S.A. Sulfide ore leaching process
CN104805282A (zh) * 2014-01-28 2015-07-29 广西银亿科技矿冶有限公司 一种红土镍矿硫酸熟化堆浸方法
EP3395968A4 (fr) * 2015-12-25 2019-07-10 Sumitomo Metal Mining Co., Ltd. Procédé d'élimination d'agent de sulfuration
WO2020073411A1 (fr) * 2018-10-08 2020-04-16 金川集团股份有限公司 Procédé d'extraction de nickel, de cobalt et de fer à partir de minerai de nickel latéritique de qualité inférieure
CN109797295A (zh) * 2019-02-15 2019-05-24 四川大裂谷钒业有限公司 从含钴铁精矿中提钴的方法
CN109797295B (zh) * 2019-02-15 2021-06-22 四川大裂谷钒业有限公司 从含钴铁精矿中提钴的方法
CN112662892A (zh) * 2020-12-15 2021-04-16 衢州华友钴新材料有限公司 一种酸浸液的掺杂高压镍铁分离方法
CN112662892B (zh) * 2020-12-15 2022-06-14 衢州华友钴新材料有限公司 一种酸浸液的掺杂高压镍铁分离方法
CN113502394A (zh) * 2021-05-26 2021-10-15 广东佳纳能源科技有限公司 一种钴或镍的中间品回收的方法
WO2023005404A1 (fr) * 2021-07-29 2023-02-02 广东邦普循环科技有限公司 Procédé de lixiviation et d'extraction d'un métal précieux et d'un élément sulfureux à partir d'une matte à faible teneur en nickel

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