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WO2022179291A1 - Méthode de séparation de ferronickel à partir d'une solution de lixiviation de minerai de nickel latéritique et de préparation de phosphate de fer, et application - Google Patents

Méthode de séparation de ferronickel à partir d'une solution de lixiviation de minerai de nickel latéritique et de préparation de phosphate de fer, et application Download PDF

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Publication number
WO2022179291A1
WO2022179291A1 PCT/CN2021/142313 CN2021142313W WO2022179291A1 WO 2022179291 A1 WO2022179291 A1 WO 2022179291A1 CN 2021142313 W CN2021142313 W CN 2021142313W WO 2022179291 A1 WO2022179291 A1 WO 2022179291A1
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Prior art keywords
sulfide
iron phosphate
solution
reaction
nickel ore
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Ceased
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PCT/CN2021/142313
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English (en)
Chinese (zh)
Inventor
余海军
谢英豪
张学梅
李长东
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.)
Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Hunan Brunp Vehicles Recycling Co Ltd
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Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Hunan Brunp Vehicles Recycling Co Ltd
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Publication of WO2022179291A1 publication Critical patent/WO2022179291A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/37—Phosphates of heavy metals
    • C01B25/375—Phosphates of heavy metals of iron
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/45—Phosphates containing plural metal, or metal and ammonium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/11—Sulfides; Oxysulfides
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • 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 laterite nickel ore hydrometallurgy, and particularly relates to a method and application for separating ferronickel from a laterite nickel ore leaching solution and preparing ferric phosphate.
  • Laterite nickel ore resources are surface weathering crust deposits formed by weathering-leaching-sedimentation of nickel sulfide ore bodies. Aluminum, etc., have high usable value.
  • the world's laterite nickel ore resources are concentrated in the near equatorial regions, and most of them are close to the coast, which is convenient for transportation.
  • the rapid development and progress of acid leaching technology of laterite nickel ore in recent years can further reduce its production cost.
  • Iron phosphate is mainly used to manufacture lithium iron phosphate battery materials, catalysts and ceramics.
  • the present invention aims to solve at least one of the technical problems existing in the above-mentioned prior art. To this end, the present invention proposes a method and application for separating ferronickel from laterite nickel ore leaching solution and preparing ferric phosphate, which can reduce the cost of separation and make the process more efficient and simple.
  • a method for separating ferronickel from laterite nickel ore leaching solution comprising the following steps:
  • the composite sulfide precipitating agent includes sulfide precipitating agent A and sulfide precipitating agent B, and the sulfide precipitating agent A is a mixture of sodium sulfide, potassium sulfide, lithium sulfide, ammonium sulfide, magnesium sulfide or hydrogen sulfide.
  • the sulfide precipitant B is prepared by mixing one or more of sodium hydrosulfide, ammonium hydrosulfide or potassium hydrosulfide.
  • the whole process of the reaction is controlled under the condition of high acidity to inhibit the precipitation of iron sulfide.
  • the thermodynamically unstable ferrous sulfide is quickly dissolved back into the solution and releases hydrogen sulfide gas, thereby realizing the separation of nickel and iron.
  • the ratio of the molar amount of sulfur in the composite sulfide precipitant to the molar amount of nickel in the laterite nickel ore leaching solution is (1-1.3):1
  • the composite sulfide precipitating agent is prepared by mixing the sulfide precipitating agent A and the sulfide precipitating agent B in a mass ratio of 1:(0.2-1.5).
  • step (1) the specific steps of step (1) are: adjusting the pH of the laterite nickel ore leaching solution to 0.5-1.5, and then adding the composite sulfide precipitant dropwise to react for 4-6 hours, and continuously adding during the period Compound sulfide precipitating agent and coagulant, and adding acid during the reaction to maintain the pH of the solution at 0.5-1.5.
  • the coagulant in step (1), is prepared by using alum and sodium polyacrylate in a molar ratio of (1-2):(1-2). Coagulants can further promote the formation of sulfide precipitates.
  • step (1) the process of adjusting the pH of the laterite nickel ore leachate is: placing the laterite nickel ore leachate in a beaker, placing the beaker on a magnetic stirrer, adding a stirring magnet, Adjust the rotation speed to 100rpm ⁇ 300rpm, and keep stirring, at the same time, add sodium bicarbonate solution dropwise to the laterite nickel ore leaching solution, and use a pH meter to monitor and control the pH of the solution in real time under constant stirring until the pH of the solution remains at within the range of 0.5 to 1.5.
  • step (1) the filtration adopts Buchner funnel suction filtration.
  • the oxidant in step (2), is one of hydrogen peroxide, nitric acid, hypochlorous acid, oxygen or ozone; when the oxidant is hydrogen peroxide, the oxidant is The concentration of hydrogen oxide is 30% to 60%.
  • the concentration of the phosphoric acid solution is 50% to 80%.
  • the pH adjustment is to use at least one of concentrated ammonia water, ferric hydroxide or ferrous hydroxide to adjust the pH to 2-4.
  • step (2) the reaction time is 3-5 h.
  • step (2) the heating is heated to 85-110° C. at a heating rate of 3-5° C./min.
  • step (2) after the concentrated crystallization, the process of washing the iron phosphate with deionized water is further included.
  • the present invention also provides an iron phosphate prepared by the above method.
  • the present invention also proposes a lithium iron phosphate, which is prepared from the raw materials including the above-mentioned iron phosphate.
  • the present invention also provides a method for preparing lithium iron phosphate, which includes the following steps: preparing a lithium carbonate solution and an ascorbic acid solution, dispersing the iron phosphate in water to obtain an iron phosphate suspension, and dispersing the iron phosphate suspension, The lithium carbonate solution and the ascorbic acid solution are evenly mixed, stirred, and then heated for reaction to obtain the lithium iron phosphate.
  • the stirring time is 2-4 hours.
  • the temperature of the heating reaction is 150-250° C., and the time is 20-30 h.
  • the sulfide solubility products of nickel and iron are not much different, so the separation coefficient of the two sulfide precipitations is not large, but the present invention controls the reaction process under high acidity conditions, ingeniously.
  • the reaction kinetics process is controlled, so as to realize one-step high-efficiency and low-cost separation of nickel and iron, with good separation effect and low impurity content of iron phosphate.
  • the sulfide precipitation method adopted in the present invention can not only be applied to the sulfuric acid system, but also can be applied to other systems such as hydrochloric acid, and has a wide range of applicability, so it has practical significance for the improvement of the enrichment process for the sulfide separation research of ferronickel.
  • the present invention prepares the precursor iron phosphate of lithium iron phosphate through a simple separation and preparation method, and finally prepares lithium iron phosphate, and its first charge-discharge specific capacity can reach more than 164mAh/g.
  • FIG. 1 is a SEM image of the iron phosphate prepared in Example 1 of the present invention.
  • the present embodiment utilizes the sulfidation method to separate ferronickel from the leaching solution of laterite nickel ore and prepares iron phosphate and lithium iron phosphate, and the specific process is:
  • Preparation of composite sulfide precipitant get sodium sulfide and potassium sulfide to mix and prepare sulfide precipitant A, get sodium hydrosulfide and ammonium hydrosulfide to mix and prepare sulfide precipitant B, mix sulfide precipitant A with sulfur
  • the precipitant B is mixed and prepared into a composite sulfide precipitant, which is ready for use; at the same time, the solid alum and the solid sodium polyacrylate are prepared according to the molar ratio of 2:1 to prepare a coagulant to promote the precipitation process of the sulfide;
  • a coagulant is added during the reaction to further promote the formation of sulfide precipitation.
  • the whole process of the reaction should be controlled under high acidity conditions to inhibit the precipitation of iron sulfide.
  • the thermodynamically unstable ferrous sulfide will be quickly dissolved back into the solution and release hydrogen sulfide gas, thereby To achieve the separation of nickel and iron;
  • Fig. 1 is the SEM image of the iron phosphate prepared by the present embodiment, as can be seen from the figure, the prepared iron phosphate material has a regular morphology, uniform particle size, no obvious agglomeration, and is relatively fluffy and has pores, which is conducive to the follow-up Preparation of Lithium Iron Phosphate.
  • the present embodiment utilizes the sulfidation method to separate ferronickel from the leaching solution of laterite nickel ore and prepares iron phosphate and lithium iron phosphate, and the specific process is:
  • Preparation of composite sulfide precipitating agent get potassium sulfide, lithium sulfide and ammonium sulfide and mix and prepare sulfide precipitating agent A, get sodium hydrosulfide, ammonium hydrosulfide and potassium hydrosulfide and mix and prepare sulfide precipitating agent B.
  • Sulfide precipitating agent A and sulfide precipitating agent B are mixed to prepare a composite sulfide precipitating agent, which is ready for use; at the same time, solid alum and solid sodium polyacrylate are prepared in a molar ratio of 1:1 to prepare a coagulant to promote sulfide the precipitation process;
  • a coagulant is added during the reaction to further promote the formation of sulfide precipitation.
  • the whole process of the reaction should be controlled under high acidity conditions to inhibit the precipitation of iron sulfide.
  • the thermodynamically unstable ferrous sulfide will be quickly dissolved back into the solution and release hydrogen sulfide gas, thereby To achieve the separation of nickel and iron;
  • the present embodiment utilizes the sulfidation method to separate ferronickel from the leaching solution of laterite nickel ore and prepares iron phosphate and lithium iron phosphate, and the specific process is:
  • Preparation of composite sulfide precipitating agent get ammonium sulfide, magnesium sulfide and hydrogen sulfide to mix and prepare sulfide precipitating agent A, take ammonium hydrosulfide as sulfide precipitating agent B, mix sulfide precipitating agent A and sulfide precipitating agent B is mixed and prepared into a composite sulfide precipitation agent, which is ready for use; at the same time, solid alum and solid sodium polyacrylate are prepared according to the molar ratio of 1:2 to prepare a coagulant to promote the precipitation process of sulfide;
  • a coagulant is added during the reaction to further promote the formation of sulfide precipitation.
  • the whole process of the reaction should be controlled under high acidity conditions to inhibit the precipitation of iron sulfide.
  • the thermodynamically unstable ferrous sulfide will be quickly dissolved back into the solution and release hydrogen sulfide gas, thereby To achieve the separation of nickel and iron;
  • This comparative example adopts the solvent extraction method to separate ferronickel from the leaching solution of laterite nickel ore and prepares iron phosphate and lithium iron phosphate.
  • the difference from Example 1 is that the principle of separating ferronickel is different, and the specific process is:
  • Table 1 is the impurity element content of the iron phosphate products prepared by Examples 1-3 and Comparative Examples, and the specific data are obtained by ICP-AES equipment testing.
  • Table 2 shows the electrochemical properties of lithium iron phosphate batteries prepared in Examples 1-3 and Comparative Examples, and the specific data are obtained by testing equipment such as electrochemical workstations.
  • Electrochemical performance Example 1 Example 2
  • Example 3 Comparative ratio First charge-discharge specific capacity (mAh/g) 164.3 165.2 164.2 135.7 First charge-discharge efficiency (%) 95.8 97.6 96.1 92.3 1C cycle 1000 times discharge capacity retention rate (%) 97.7 98.6 97.9 88.9

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
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  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
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Abstract

La présente invention concerne une méthode de séparation de ferronickel à partir d'une solution de lixiviation de minerai de nickel latéritique et de préparation de phosphate de fer, et une application. La méthode comprend les étapes consistant à : ajuster le pH d'une solution de lixiviation de minerai de nickel latéritique à 0,5 à 1,5, ajouter goutte à goutte un précipitant de sulfure composite pour réaction, ajouter un agent coagulant et filtrer pour obtenir des précipités de sulfure de nickel et un filtrat ; puis ajouter un oxydant et une solution d'acide phosphorique au filtrat, ajuster le pH pour réaction, et réaliser un chauffage, une concentration et une cristallisation pour obtenir du phosphate de fer. Selon la présente invention, un procédé de réaction est contrôlé dans une condition d'acidité élevée, et un procédé de cinétique de réaction est subtilement contrôlé, de telle sorte qu'une séparation en une étape, efficace et à faible coût de ferronickel est mise en œuvre, l'effet de séparation est bon, et la teneur en impuretés du phosphate de fer est faible.
PCT/CN2021/142313 2021-02-26 2021-12-29 Méthode de séparation de ferronickel à partir d'une solution de lixiviation de minerai de nickel latéritique et de préparation de phosphate de fer, et application Ceased WO2022179291A1 (fr)

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CN202110217258.7A CN113023701A (zh) 2021-02-26 2021-02-26 从红土镍矿浸出液中分离镍铁并制备磷酸铁的方法和应用

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Cited By (4)

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CN115448282A (zh) * 2022-09-15 2022-12-09 广东邦普循环科技有限公司 一种镍铁合金制备磷酸铁锂的方法及应用
CN115676789A (zh) * 2022-09-28 2023-02-03 成都盛威兴科新材料研究院合伙企业(有限合伙) 一种采用铁基含镍合金生产电池级磷酸铁的制备方法
CN116411164A (zh) * 2023-01-16 2023-07-11 上海锦源晟新能源材料有限公司 一种红土镍矿与镍锍合金协同浸出的方法
CN119349523A (zh) * 2024-12-24 2025-01-24 四川大学 一种从废旧磷酸铁锂中高效分离回收锂元素的方法

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CN113023701A (zh) * 2021-02-26 2021-06-25 广东邦普循环科技有限公司 从红土镍矿浸出液中分离镍铁并制备磷酸铁的方法和应用
CN113942986B (zh) * 2021-09-27 2023-06-16 荆门市格林美新材料有限公司 一种从镍铁合金中回收镍和铁的方法
CN113979415A (zh) * 2021-11-24 2022-01-28 四川顺应动力电池材料有限公司 一种生产磷酸铁的方法
CN114789994B (zh) * 2022-05-24 2024-04-16 荆门市格林美新材料有限公司 一种由红土镍矿提取制备电池级磷酸铁的方法
CN115196609B (zh) * 2022-09-15 2023-01-13 中国科学院过程工程研究所 一种从磷酸铁锂提锂渣中回收磷酸铁的方法以及其应用

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115448282A (zh) * 2022-09-15 2022-12-09 广东邦普循环科技有限公司 一种镍铁合金制备磷酸铁锂的方法及应用
CN115448282B (zh) * 2022-09-15 2024-01-05 广东邦普循环科技有限公司 一种镍铁合金制备磷酸铁锂的方法及应用
CN115676789A (zh) * 2022-09-28 2023-02-03 成都盛威兴科新材料研究院合伙企业(有限合伙) 一种采用铁基含镍合金生产电池级磷酸铁的制备方法
CN115676789B (zh) * 2022-09-28 2024-01-23 成都盛威兴科新材料研究院合伙企业(有限合伙) 一种采用铁基含镍合金生产电池级磷酸铁的制备方法
CN116411164A (zh) * 2023-01-16 2023-07-11 上海锦源晟新能源材料有限公司 一种红土镍矿与镍锍合金协同浸出的方法
CN119349523A (zh) * 2024-12-24 2025-01-24 四川大学 一种从废旧磷酸铁锂中高效分离回收锂元素的方法

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