WO2001062989A1 - Procede de recuperation de nickel et/ou de cobalt - Google Patents

Procede de recuperation de nickel et/ou de cobalt Download PDF

Info

Publication number
WO2001062989A1
WO2001062989A1 PCT/AU2001/000179 AU0100179W WO0162989A1 WO 2001062989 A1 WO2001062989 A1 WO 2001062989A1 AU 0100179 W AU0100179 W AU 0100179W WO 0162989 A1 WO0162989 A1 WO 0162989A1
Authority
WO
WIPO (PCT)
Prior art keywords
nickel
ions
cobalt
hydroxide
alkaline agent
Prior art date
Application number
PCT/AU2001/000179
Other languages
English (en)
Inventor
Leslie Troman
Original Assignee
Anaconda Nickel 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
Application filed by Anaconda Nickel Ltd filed Critical Anaconda Nickel Ltd
Priority to AU2001235241A priority Critical patent/AU2001235241A1/en
Publication of WO2001062989A1 publication Critical patent/WO2001062989A1/fr

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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
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • 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
    • C22B23/0476—Separation of nickel from cobalt
    • C22B23/0492—Separation of nickel from cobalt in ammoniacal type solutions
    • 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
    • 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
    • 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
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • 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 method for the recovery of nickel and/or cobalt. More particularly, the method of the present invention relates to the recovery of nickel and/or cobalt from nickel laterite ores or concentrates.
  • US Patent 5855858 describes a hydrometallurgical process for the extraction, and subsequent recovery of nickel and cobalt from ores or concentrates, that utilises an intermediate separation step to selectively precipitate nickel and cobalt as a mixed nickel/cobalt hydroxide.
  • the nickel/cobalt hydroxide is then leached in a two stage, ammonium sulphate solution leach, with the two subsequent leach solutions being treated in separate solvent extraction circuits to separate and selectively recover cobalt, magnesium or nickel respectively.
  • the nickel and cobalt is subsequently recovered from the solvent extraction solutions by electrowinning.
  • An additional claim is that solvent extraction is conducted at up to about 60°C and is beneficially conducted with magnesium in the feed solution to solvent extraction to enhance the separation between cobalt and nickel.
  • the separation factor between cobalt and nickel is critical to ensure production of a commercially acceptable quality of nickel and cobalt cathodes.
  • the requirement for two separate trains of leaching and solvent extraction, as well as the requirement to extract magnesium and nickel via solvent extraction, serves to increase the complexity and cost of the process. Additionally, the requirement for relatively low metal concentrations in the leach solution, which is subsequently advanced to solvent extraction, adds considerably to the size and cost of the equipment required.
  • a method for the recovery of nickel and/or cobalt from nickel and cobalt containing ores or concentrates comprising the steps of: subjecting a nickel and cobalt containing ore or concentrate to acid pressure leaching thereby forming a process solution containing nickel ions, cobalt ions and residual ions of one or more impurity metals;
  • the step of treating the process solution containing nickel ions, cobalt ions and undesired metal ions with one or more alkaline agents to induce the precipitation of a mixed metal hydroxide of nickel and cobalt and the impurity metals comprises the following sub-steps:
  • the resulting mixture is part neutralised to pH 3 with calcrete or limestone, then subjected to counter current decantation to produce the process solution containing nickel ions, cobalt ions and ions of one or more undesired metals.
  • the method of the present invention comprises the additional steps of:
  • the method of the present invention comprises the additional step of: adding a fourth alkaline agent to the supernatant solution to raise the pH of such to about 8.5 to cause undesired metal ions, such as manganese ions, to precipitate as manganese hydroxide.
  • the first alkaline agent may be a metal oxide or hydroxide or carbonate.
  • the first alkaline agent is calcrete, or limestone.
  • the second alkaline agent may be a metal oxide or hydroxide.
  • the second alkaline agent is magnesium hydroxide or oxide.
  • the third alkaline agent may be a metal oxide or hydroxide.
  • the third alkaline agent is calcium hydroxide.
  • the fourth alkaline agent may be a metal oxide or hydroxide.
  • the fourth alkaline agent is calcium hydroxide.
  • the method of the present invention comprises the step of:
  • an organic extractant is used in the step of substantially separating the cobalt ions from the nickel ions by solvent extraction in an alkaline medium.
  • a suitable extractant is an organic phosphorous acid, more specifically an organic phosphinic acid extractant.
  • the extractant is bis (2,4,4-trimethylpentyl) phosphinic acid, known commercially as CYANEX 272.
  • Figure 1 is a schematic representation of a precipitation phase and a leaching phase of a production plant for the production of nickel according to the method of the embodiment
  • Figure 2 is a schematic representation of a solvent extraction phase of the production plant of Figure 1 ;
  • Figure 3 is a schematic representation of a cobalt removal phase of the production plant of Figure 1 ;
  • Figure 4 is a schematic representation of a hydrogen reduction phase of the production plant of Figure 1.
  • Ore containing nickel and cobalt is crushed, optionally upgraded to a concentrate, and subjected to acid leaching.
  • the solution from the acid leach is partially neutralised to approximately pH 2.8 to 3.0 by the addition of calcrete or limestone, thereby rejecting the majority of iron, chromium and aluminium from the solution.
  • a counter current decantation circuit is then used to produce a process solution containing nickel ions, cobalt ions with some residual undesirable metal ions, such as iron, aluminium, chromium, zinc, copper and manganese.
  • the solution from the counter-current decantation circuit is partially neutralised to a pH of about 5 using a limestone or calcrete slurry. This causes the residual iron, aluminium and chromium to precipitate as hydroxides.
  • the hydroxides, along with some nickel and cobalt may then be removed along with the gypsum from the neutralised slurry by thickening prior to leaching and return prior to or at the counter current decantation circuit.
  • the clarified liquor is reacted with magnesium hydroxide or oxide at a pH of about 7 to 7.5 to precipitate approximately 90% of the nickel, cobalt and some other impurity metals, such as zinc and copper, as a mixed hydroxide.
  • the mixed metal hydroxide is transferred to a vacuum belt filter for washing, prior to being leached using ammonium sulphate solution from the nickel hydrogen reduction process, which will be discussed subsequently.
  • the leach step residual iron and manganese are reduced to acceptable levels. Excess water generated by the leaching process is removed by evaporation from the process stream to maintain a high nickel tenor.
  • the process liquor is then contacted with an extractant, such as Cyanex 272, to extract sufficient cobalt and impurity metals such as zinc and copper to allow hydrogen reduction to be used to selectively precipitate nickel, whilst retaining any residual cobalt in solution. That is, the nickel to cobalt ratio is increased from about 12 to 1 to at least 50 to 1.
  • the organic phase is then stripped of the extracted metals, leaving a sulphate solution rich in cobalt and impurity metals such as copper, zinc and iron.
  • the nickel is then recovered by hydrogen reduction, before being processed into briquettes or being sold as a powder.
  • ammonium sulphate leaching solution quality is maintained by taking a bleed stream of the solution remaining after nickel reduction to an ammonia recovery process in which an alkaline agent, preferably calcium hydroxide, is reacted with the ammonium sulphate to regenerate ammonia, and reject the sulphate as gypsum, with the slurry so produced being returned to the counter current decantation circuit to recover any residual nickel and cobalt values.
  • an alkaline agent preferably calcium hydroxide
  • FIGs 1 to 4 there is shown a production plant for the production of nickel according to the method of the embodiment comprising a precipitation phase 10, a leaching phase 12, a solvent extraction phase 14, a cobalt removal phase 16 and a hydrogen reduction phase 18.
  • Ore containing nickel and cobalt is crushed, optionally upgraded to a concentrate, and subjected to acid leaching.
  • the acid leach of the ore is conducted in pressurised vessels at a temperature of between 240°C and 290°C, but more generally between 255°C and 275°C and at a pressure of between 4500 kPa and 6500 kPa.
  • the residence time in the autoclave is nominally 60 minutes.
  • the leach is conducted so as to have excess acid to result in an acid concentration of approximately 20 to 50 gL "1 at the completion of the leach.
  • the precise quantity of acid added is dependent on the chemistry of the feed.
  • the slurry feed density is generally in the range of 30-45 wt% generally dependent on slurry rheology.
  • a quantity of limestone or calcrete is added to the leach residue slurry prior to the counter-current decantation circuit to raise the pH to about 3 that will precipitate the majority of the iron and other impurity metals prior to the feed to counter- current decantation
  • a counter current decantation circuit (not shown) is then used to produce a process solution containing nickel ions, cobalt ions and ions of other impurity metal ions.
  • a quantity of calcrete 20 or limestone is added to the solution to increase the pH to approximately 5, causing the precipitation of iron, aluminium and chromium as hydroxides thereof.
  • the slurry so produced is subjected to thickening 22, the thickener overflow 23 in turn being subjected to filtration 24.
  • the thickener underflow 25 is passed to a recycle leach 27, then back to the counter current decantation circuit (not shown).
  • a quantity of magnesium oxide hydroxide 26 sufficient to precipitate about 90% of the nickel and cobalt, is added to the filtrate in the primary precipitation stage 28 causing the precipitation of the nickel and cobalt as a mixed metal hydroxide.
  • the mixed metal hydroxide is passed to a thickener 30, with the thickener underflow 32 being subjected to filtration 34.
  • the thickener overflow 36 is subjected to a secondary precipitation 39 with calcium hydroxide 37 being added to raise the pH to approximately 8.0 and thereby cause precipitation of the remaining nickel and cobalt as hydroxides.
  • the mixed metal hydroxide slurry 41 is advanced to a thickener 40.
  • the thickener overflow 44 is subjected to a tertiary precipitation 45, calcium hydroxide 42 being added to raise the pH to approximately 8.5 and thereby cause the precipitation of manganese as manganese hydroxide.
  • the resultant slurry 47 is returned to the counter-current decantation circuit.
  • the solution 50 from the filtration 34 is returned to the primary precipitation 28, whilst the solids 52 are advanced to the leaching phase 12.
  • the solids 52 are mixed with ammoniacal ammonium sulphate solution 54 of concentration approximately 500 to 650 gL "1 , the leached slurry 55 being subjected to evaporation 56 and thickening 58.
  • the thickener underflow is subjected to filtration 59, with the filtrate being returned to the thickener 58, and the filter cake being transferred to recycle leach 27.
  • the thickener overflow 60 is subjected to filtration 62, the filtrate 64 being passed on to the solvent extraction phase 14, and the filter cake being transferred to recycle leach 27.
  • the filtrate 64 containing both nickel and cobalt diamine sulphates is mixed with an organic phase 66 containing an organic extractant 68, such as bis(2,4,4-trimethylypentyl) phosphinic acid.
  • organics are removed from the raffinate, leaving nickel as nickel diamine sulphate 70.
  • the organic phase is subjected to scrubbing 71 with aqueous cobalt sulphate solution 73, and stripping 72.
  • Organics are removed from the stripping liquid to leave cobalt sulphate 74, which is passed to the cobalt removal phase 16, as can be seen in Figure 3.
  • the organic phase is then recycled back to extraction.
  • the nickel diamine sulphate 70 is then pre-heated 74 before being subjected to hydrogen reduction 76.
  • the ammonium sulphate solution 54 generated in the hydrogen reduction phase 18 is recycled to the leaching phase 12.
  • the slurry containing the metallic nickel is filtered 80, and the metallic nickel so collected dried 82, briquetted 84, sintered 86 in an atmosphere of nitrogen and hydrogen and, finally, packaged 88.
  • the method of the present invention may be conducted as a series of batch processes, it is envisaged that the method of the present invention will be conducted as a continuous process.
  • the method of the present invention is adapted to recovery of nickel and/or cobalt from ores or concentrates thereof without the use of hydrogen sulphide, without the production of significant ammonium sulphate by-product and with greatly reduced ammonia consumption. Modifications and variations such as would be apparent to the skilled addressee are considered to fall within the scope of the present invention.

Abstract

L'invention concerne un procédé de récupération de nickel et/ou de cobalt à partir de minerais ou concentrés contenant du nickel et du cobalt. Ce procédé consiste à : soumettre un minerai ou un concentré contenant du nickel et du cobalt à une séparation par lixiviation acide sous pression, formant ainsi une solution de procédé contenant des ions nickel, des ions cobalt et des ions résiduels d'un ou plusieurs métaux impurs;traiter la solution de procédé contenant les ions nickel, cobalt et ions métalliques d'impuretés résiduelles avec un ou plusieurs agent(s) alcalins, afin d'induire la précipitation d'un hydroxyde de métal mélangé de nickel, de cobalt et de certains métaux impurs; séparer l'hydroxyde mélangé de la solution surnageante; séparer par lixiviation l'hydroxyde de métal mélangé au moyen d'une solution de sulfate d'ammonium ammoniacale, en vue de produire une solution de complexes aminés de nickel et de cobalt et de rejeter ainsi la majorité des ions impurs; séparer presque entièrement les ions cobalt des ions nickel par solution solvante dans des conditions alcalines; soumettre la phase aqueuse contenant principalement du nickel à une réduction par l'hydrogène, afin de produire du nickel métallique et du sulfate d'ammonium; et recycler ledit sulfate d'ammonium ainsi obtenu, lors de l'étape de séparation par lixiviation du sulfate d'ammonium.
PCT/AU2001/000179 2000-02-22 2001-02-22 Procede de recuperation de nickel et/ou de cobalt WO2001062989A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2001235241A AU2001235241A1 (en) 2000-02-22 2001-02-22 Method for the recovery of nickel and/or cobalt

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AUPQ5782A AUPQ578200A0 (en) 2000-02-22 2000-02-22 Method for the recovery of nickel and/or cobalt
AUPQ5782 2000-02-22

Publications (1)

Publication Number Publication Date
WO2001062989A1 true WO2001062989A1 (fr) 2001-08-30

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003056045A1 (fr) * 2001-12-21 2003-07-10 Falconbridge Limited Elimination de chrome de solutions de lixiviation au cours de la lixiviation acide a haute pression de minerais lateritiques
WO2009149522A1 (fr) * 2008-06-13 2009-12-17 Poseidon Nickel Limited Procédé rhéologique pour la récupération hydrométallurgique de métaux de base à partir de minerais
CN103103354A (zh) * 2011-11-13 2013-05-15 深圳市环境友好金属材料工程技术研究开发中心 由废弃crt屏幕荫罩循环回收超细镍粉的生产方法
CN103290219A (zh) * 2012-02-22 2013-09-11 新兴重工湖北三六一一机械有限公司 一种石煤钒矿混合焙烧后的浸出溶液的除杂方法
CN103740938A (zh) * 2014-01-13 2014-04-23 合肥融捷金属科技有限公司 无皂化溶剂萃取法回收碳酸钴生产废水中钴的方法
AU2011236124B2 (en) * 2010-10-21 2014-10-30 Murrin Murrin Operations Pty Ltd Method for the Control of Ammonium Sulphate Addition in the Hydrogen Reduction of Base Metals
EP2860271A4 (fr) * 2012-06-12 2015-11-11 Sumitomo Metal Mining Co Procédé de neutralisation
CN106544505A (zh) * 2015-09-16 2017-03-29 金发科技股份有限公司 一种萃取剂组合物及其制备方法与应用
CN113474069A (zh) * 2019-03-26 2021-10-01 住友金属矿山株式会社 从含镍和钴的氢氧化物制造含镍和钴的溶液的制造方法
CN114212827A (zh) * 2021-12-31 2022-03-22 湖南烯富环保科技有限公司 一种除氢氧化锰中钙和/或镁杂质的方法
WO2022183243A1 (fr) * 2021-03-02 2022-09-09 The University Of Queensland Précipitation de métaux
CN115491513A (zh) * 2022-09-08 2022-12-20 西北矿冶研究院 一种含铜钴镍固危废综合回收铜、钴、镍的工艺

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1988009389A1 (fr) * 1987-05-20 1988-12-01 Meq Nickel Pty. Ltd. Separation et extraction de nickel et de cobalt dans les systemes ammoniacaux
WO1996041029A2 (fr) * 1995-06-07 1996-12-19 Cominco Engineering Services Ltd. Extraction hydrometallurgique, assistee par des chlorures de nickel et de cobalt a partir de minerais sulphures
US5855858A (en) * 1993-07-29 1999-01-05 Cominco Engineering Services Ltd. Process for the recovery of nickel and/or cobalt from an ore or concentrate
WO1999009226A1 (fr) * 1997-08-15 1999-02-25 Cominco Engineering Services Ltd. Extraction hydrometallurgique au chlorure de nickel et de cobalt a partir de minerais sulfures ou lateritiques

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1988009389A1 (fr) * 1987-05-20 1988-12-01 Meq Nickel Pty. Ltd. Separation et extraction de nickel et de cobalt dans les systemes ammoniacaux
US5855858A (en) * 1993-07-29 1999-01-05 Cominco Engineering Services Ltd. Process for the recovery of nickel and/or cobalt from an ore or concentrate
WO1996041029A2 (fr) * 1995-06-07 1996-12-19 Cominco Engineering Services Ltd. Extraction hydrometallurgique, assistee par des chlorures de nickel et de cobalt a partir de minerais sulphures
WO1999009226A1 (fr) * 1997-08-15 1999-02-25 Cominco Engineering Services Ltd. Extraction hydrometallurgique au chlorure de nickel et de cobalt a partir de minerais sulfures ou lateritiques

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7318914B2 (en) 2001-12-21 2008-01-15 Falconbridge Limited Chromium removal from leach liquors produced during high pressure acid leaching of lateritic ores
WO2003056045A1 (fr) * 2001-12-21 2003-07-10 Falconbridge Limited Elimination de chrome de solutions de lixiviation au cours de la lixiviation acide a haute pression de minerais lateritiques
WO2009149522A1 (fr) * 2008-06-13 2009-12-17 Poseidon Nickel Limited Procédé rhéologique pour la récupération hydrométallurgique de métaux de base à partir de minerais
AU2011236124B2 (en) * 2010-10-21 2014-10-30 Murrin Murrin Operations Pty Ltd Method for the Control of Ammonium Sulphate Addition in the Hydrogen Reduction of Base Metals
CN103103354A (zh) * 2011-11-13 2013-05-15 深圳市环境友好金属材料工程技术研究开发中心 由废弃crt屏幕荫罩循环回收超细镍粉的生产方法
CN103103354B (zh) * 2011-11-13 2014-08-27 深圳市环境友好金属材料工程技术研究开发中心 由废弃crt屏幕荫罩循环回收超细镍粉的生产方法
CN103290219A (zh) * 2012-02-22 2013-09-11 新兴重工湖北三六一一机械有限公司 一种石煤钒矿混合焙烧后的浸出溶液的除杂方法
EP2860271A4 (fr) * 2012-06-12 2015-11-11 Sumitomo Metal Mining Co Procédé de neutralisation
AU2013275418B2 (en) * 2012-06-12 2017-03-09 Sumitomo Metal Mining Co., Ltd. Neutralization method
CN103740938A (zh) * 2014-01-13 2014-04-23 合肥融捷金属科技有限公司 无皂化溶剂萃取法回收碳酸钴生产废水中钴的方法
CN106544505A (zh) * 2015-09-16 2017-03-29 金发科技股份有限公司 一种萃取剂组合物及其制备方法与应用
CN113474069A (zh) * 2019-03-26 2021-10-01 住友金属矿山株式会社 从含镍和钴的氢氧化物制造含镍和钴的溶液的制造方法
CN113474069B (zh) * 2019-03-26 2023-04-07 住友金属矿山株式会社 从含镍和钴的氢氧化物制造含镍和钴的溶液的制造方法
EP3950085A4 (fr) * 2019-03-26 2023-05-10 Sumitomo Metal Mining Co., Ltd. Procédé de fabrication d'une solution contenant du nickel et du cobalt à partir d'hydroxyde contenant du nickel et du cobalt
WO2022183243A1 (fr) * 2021-03-02 2022-09-09 The University Of Queensland Précipitation de métaux
AU2022229686B2 (en) * 2021-03-02 2023-12-14 Pure Battery Technologies Limited Precipitation of metals
CN114212827A (zh) * 2021-12-31 2022-03-22 湖南烯富环保科技有限公司 一种除氢氧化锰中钙和/或镁杂质的方法
CN115491513A (zh) * 2022-09-08 2022-12-20 西北矿冶研究院 一种含铜钴镍固危废综合回收铜、钴、镍的工艺
CN115491513B (zh) * 2022-09-08 2023-11-17 西北矿冶研究院 一种含铜钴镍固危废综合回收铜、钴、镍的工艺

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