WO2020181745A1 - Procédé de séparation efficace de cobalt/nickel magnésium manganèse à partir d'une matière première de sel de cobalt/nickel brut - Google Patents

Procédé de séparation efficace de cobalt/nickel magnésium manganèse à partir d'une matière première de sel de cobalt/nickel brut Download PDF

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Publication number
WO2020181745A1
WO2020181745A1 PCT/CN2019/104293 CN2019104293W WO2020181745A1 WO 2020181745 A1 WO2020181745 A1 WO 2020181745A1 CN 2019104293 W CN2019104293 W CN 2019104293W WO 2020181745 A1 WO2020181745 A1 WO 2020181745A1
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WIPO (PCT)
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cobalt
nickel
magnesium
manganese
crude
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PCT/CN2019/104293
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English (en)
Chinese (zh)
Inventor
胡雷
陈宇乾
陈聪
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衢州华友钴新材料有限公司
浙江华友钴业股份有限公司
刚果东方国际矿业简易股份有限公司
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Publication of WO2020181745A1 publication Critical patent/WO2020181745A1/fr

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    • 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
    • C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00—Magnetic separation
    • 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
    • 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 invention belongs to the technical field of hydrometallurgy and relates to a method for efficiently separating cobalt/nickel magnesium manganese from crude cobalt/nickel salt raw materials.
  • Chinese patent CN108179272A discloses a method for separating cobalt and magnesium in the process of cobalt-nickel hydrometallurgy. It specifically includes: extracting and removing impurities from the cobalt-containing magnesium solution in the cobalt-nickel wet smelting process, and using a multivalent metal adsorption resin to selectively adsorb the cobalt metal ions in the cobalt-containing magnesium solution, thereby reducing the cobalt and magnesium in the solution Metal separation.
  • the process method removes most of the metal impurities through multiple extractions, and then uses the selective adsorption of the polyvalent metal adsorption resin to leave the magnesium metal ions in the solution, thereby achieving the purpose of removing magnesium.
  • the entire process is cumbersome and requires Multiple extraction steps achieve the purpose of impurity removal, increase the cost of impurity removal, and cannot achieve the purpose efficiently.
  • Chinese patent CN103088215B discloses a method for separating nickel-cobalt and manganese in raw materials with high manganese-cobalt ratio of nickel-cobalt-manganese. It specifically includes: mixing the high manganese-cobalt ratio nickel-cobalt-manganese raw material with the mixed solution of dilute sulfuric acid and sodium sulfite, adjusting the end point pH to 0-3.5, after full reaction, filtering and retaining the first filtrate and adding soluble persulfate to it, adjusting the end point The pH is 2-6.
  • a second filtrate containing nickel sulfate and cobalt sulfate is obtained by filtration, while manganese is oxidized and precipitated, thereby achieving the purpose of separating nickel and cobalt from manganese in the raw materials.
  • This method is divided into two steps: adding dilute sulfuric acid and sodium sulfite to dissolve cobalt and nickel and adding persulfate to precipitate manganese, and cannot achieve the purpose of separating cobalt, nickel, manganese and magnesium in one step.
  • the present invention provides a method for efficiently separating cobalt/nickel magnesium manganese from crude cobalt/nickel salt raw materials, which stably separates cobalt/nickel and magnesium manganese during the process of preparing metallic cobalt powder, and No loss of cobalt/nickel is caused, and the process of removing magnesium and manganese when the factory produces cobalt products is reduced, saving costs.
  • the technical solution adopted by the present invention is: a method for efficiently separating cobalt/nickel magnesium manganese from crude cobalt/nickel salt raw materials, which uses the crude cobalt/nickel salt as raw materials, slurries, adds a catalyst, and uses high temperature High-pressure hydrogen reduction process, that is, the hydrogen reduction reaction is carried out by controlling pH, catalyst, hydrogen partial pressure, temperature and reaction time. After the reaction is completed, the initial separation of cobalt/nickel magnesium manganese is achieved through reselection, and the obtained light manganese slag is subjected to magnetic separation to entrainment The fine-grained cobalt/nickel powder is recovered for use as a catalyst.
  • the obtained crude cobalt/nickel powder is acid leached to prepare a cobalt/nickel leachate.
  • the magnesium is removed by the resin to obtain a magnesium cobalt/nickel solution, or further extraction
  • the high-purity cobalt/nickel product solution is obtained after the deep removal of impurities and the resin for magnesium removal, and finally the deep separation of cobalt/nickel-magnesium-manganese is realized; in the high-temperature and high-pressure hydrogen reduction process, the pH is 0.5-7.0, and the catalyst includes But not limited to one or more of anthraquinone, Pd, Pd compounds, and cobalt/nickel powder, the hydrogen partial pressure is 0.5-10 MPa, the reaction temperature is 100-300°C, and the The reaction time is 1-48 hours.
  • the present invention is different from the existing hydrogen reduction slurry concept.
  • the H + generated by oxidation and a small amount of basic magnesium sulfate and basic magnesium carbonate contained in the crude cobalt salt raw material are used.
  • the reaction causes the magnesium and manganese impurities to enter the liquid phase to achieve the separation of cobalt, magnesium and manganese.
  • the high density and magnetic characteristics of the metal cobalt are then used.
  • the cobalt and manganese are separated through the combined selective separation of gravity and magnetic separation, eliminating the need to prepare metal cobalt products. , Adding additional processes to remove magnesium and manganese, shorten the process flow, reduce production costs, and make the process faster.
  • liquid-to-solid ratio of slurrying and mixing is 1-20:1.
  • the slurrying time is 1-60 min.
  • the density of cobalt/nickel powder used in the gravity separation magnetic separation is higher than that of manganese and magnesium, and the cobalt/nickel powder has magnetism, so as to realize the separation of cobalt/nickel magnesium manganese.
  • the acid used for the acid leaching of the crude cobalt/nickel powder acid leaching to prepare the cobalt/nickel product solution includes but not limited to carbonic acid, hydrochloric acid, and sulfuric acid.
  • magnesium cobalt/nickel solution is used as a raw material for preparing ternary materials.
  • the purpose of the further extraction and removal of impurities and the deep removal of impurities by resin is to remove nickel/cobalt, manganese and magnesium in the cobalt/nickel solution to obtain a high-purity cobalt/nickel product solution.
  • the resin used for removing magnesium from the resin includes but is not limited to D406.
  • the pH is 2-7
  • the hydrogen partial pressure is 0.5-5 MPa
  • the reaction temperature is 100-300° C.
  • the reaction time is 1-20 hours
  • the reaction temperature is 100-300°C.
  • the pH is 4-6
  • the hydrogen partial pressure is 1-2MPa
  • the reaction temperature is 100-200°C
  • the reaction time is 4-8 hours
  • the reaction temperature is 120- 160°C.
  • the demagnesium rate of the present invention is more than 99%, and the manganese removal rate is more than 99%;
  • the density of cobalt/nickel powder is higher than that of manganese and magnesium, and the cobalt/nickel powder has magnetism. While high-efficiency separation of cobalt/nickel-magnesium-manganese is achieved through gravity separation and magnetic separation, the cobalt/nickel product is also improved purity;
  • the present invention has simple process, high and stable removal rate of magnesium and manganese, low loss rate of cobalt, low cost, short flow and the like.
  • Figure 1 is a schematic flow diagram of the method of the present invention.
  • Example 1 A method for efficiently separating cobalt/nickel magnesium manganese from crude cobalt (nickel) salt raw materials.
  • the slurry is subjected to gravity separation and magnetic separation to obtain heavy crude cobalt (nickel)
  • the powder uses sulfuric acid to prepare cobalt sulfate (nickel) solution.
  • the magnesium content in the raw material is 4.99%, the manganese content is 3.51%, the magnesium content in the solid phase is reduced to 0.048% after the reaction, the slag demagnesia rate is 99.03%, the manganese content is reduced to 0.038%, the slag demanganese The rate is 98.9%.
  • Example 2 A method for efficiently separating cobalt/nickel magnesium manganese from crude cobalt (nickel) salt raw materials.
  • Example 3 A method for efficiently separating cobalt (nickel) magnesium and manganese from crude cobalt (nickel) salt raw materials.
  • the slurry is subjected to gravity separation and magnetic separation to obtain heavy crude cobalt (nickel) powder Hydrochloric acid is used to prepare cobalt (nickel) hydrochloride solution.
  • high-purity cobalt chloride product solution is obtained after extraction of nickel (cobalt) and resin to remove calcium and magnesium.
  • the raw material contains 4.99% magnesium and manganese. 3.51%, after the completion of the reaction, the magnesium content in the solid phase is reduced to 0.039%, the slag removal rate is 99.22%, the manganese content is decreased to 0.03%, and the slag removal rate is 99.1%.

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

Abstract

L'invention concerne un procédé de séparation efficace de cobalt/nickel magnésium manganèse à partir d'une matière première de sel de cobalt/nickel brut. À l'aide d'un sel de cobalt/nickel brut en tant que matière première, un catalyseur est ajouté après mise en suspension; un procédé de réduction à l'hydrogène à haute température et haute pression est utilisé, c'est-à-dire que des points clés tels que le pH, le catalyseur, la pression partielle d'hydrogène, la température, le temps de réaction et similaires sont contrôlés; une fois la réaction terminée, une séparation initiale du cobalt/nickel magnésium manganèse est obtenue au moyen d'une nouvelle séparation; le laitier pauvre en manganèse obtenu est soumis à une séparation magnétique pour récupérer la poudre de cobalt/nickel en grains fins entraînée et pour l'utiliser en tant que catalyseur; la poudre de cobalt/nickel brute obtenue est lixiviée par un acide pour préparer un lixiviat de cobalt/nickel; du P204 est utilisé pour extraire et éliminer les impuretés, puis le magnésium est éliminé par l'intermédiaire d'une résine pour produire une solution de cobalt/nickel exempte de magnésium, ou, lors de l'extraction et de l'élimination supplémentaires d'impuretés et de l'élimination poussée du magnésium à l'aide de résine, une solution de produit de cobalt/nickel de haute pureté est obtenue. Le taux d'élimination du magnésium du procédé de la présente invention peut atteindre 99 % ou plus, le taux d'élimination du manganèse peut atteindre 99 % ou plus, et l'invention présente comme caractéristiques un procédé simple, un faible coût, un flux de traitement court et des taux élevés d'élimination du magnésium et du manganèse.
PCT/CN2019/104293 2019-03-12 2019-09-04 Procédé de séparation efficace de cobalt/nickel magnésium manganèse à partir d'une matière première de sel de cobalt/nickel brut WO2020181745A1 (fr)

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CN201910185841.7A CN109943733A (zh) 2019-03-12 2019-03-12 一种粗制钴/镍盐原料高效分离钴/镍镁锰的方法
CN201910185841.7 2019-03-12

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CN115074540A (zh) * 2022-08-16 2022-09-20 矿冶科技集团有限公司 一种废动力电池有价组分综合回收方法
CN115432724A (zh) * 2022-10-27 2022-12-06 绵阳师范学院 一种铵镁废盐的资源化处理方法

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* Cited by examiner, † Cited by third party
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CN109943733A (zh) * 2019-03-12 2019-06-28 衢州华友钴新材料有限公司 一种粗制钴/镍盐原料高效分离钴/镍镁锰的方法

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CN108977652A (zh) * 2018-09-12 2018-12-11 郑忆依 一种钴镍冶金的废水渣的资源化利用方法
CN109943733A (zh) * 2019-03-12 2019-06-28 衢州华友钴新材料有限公司 一种粗制钴/镍盐原料高效分离钴/镍镁锰的方法

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CN102952954A (zh) * 2011-08-26 2013-03-06 深圳市格林美高新技术股份有限公司 一种三价钴镍氧化物废料与废旧钴、镍合金的处理方法
CN108977652A (zh) * 2018-09-12 2018-12-11 郑忆依 一种钴镍冶金的废水渣的资源化利用方法
CN109943733A (zh) * 2019-03-12 2019-06-28 衢州华友钴新材料有限公司 一种粗制钴/镍盐原料高效分离钴/镍镁锰的方法

Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN115074540A (zh) * 2022-08-16 2022-09-20 矿冶科技集团有限公司 一种废动力电池有价组分综合回收方法
CN115074540B (zh) * 2022-08-16 2022-11-25 矿冶科技集团有限公司 一种废动力电池有价组分综合回收方法
CN115432724A (zh) * 2022-10-27 2022-12-06 绵阳师范学院 一种铵镁废盐的资源化处理方法
CN115432724B (zh) * 2022-10-27 2023-11-21 绵阳师范学院 一种铵镁废盐的资源化处理方法

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