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WO2020073411A1 - Procédé d'extraction de nickel, de cobalt et de fer à partir de minerai de nickel latéritique de qualité inférieure - Google Patents

Procédé d'extraction de nickel, de cobalt et de fer à partir de minerai de nickel latéritique de qualité inférieure Download PDF

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Publication number
WO2020073411A1
WO2020073411A1 PCT/CN2018/114823 CN2018114823W WO2020073411A1 WO 2020073411 A1 WO2020073411 A1 WO 2020073411A1 CN 2018114823 W CN2018114823 W CN 2018114823W WO 2020073411 A1 WO2020073411 A1 WO 2020073411A1
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WIPO (PCT)
Prior art keywords
slurry
iron
nickel
ore
mixture
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Ceased
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PCT/CN2018/114823
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English (en)
Chinese (zh)
Inventor
刘玉强
沙滨
李维舟
田忠元
王少华
黄海丽
贺来荣
马永刚
杜昊
马海青
陈小林
魏建周
王多江
朱慧
马旻锐
姚菲
张飞
杨松林
秦为涛
李博文
刘世和
马俊
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Jinchuan Group Co Ltd
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Jinchuan Group Co Ltd
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Filing date
Publication date
Application filed by Jinchuan Group Co Ltd filed Critical Jinchuan Group Co Ltd
Publication of WO2020073411A1 publication Critical patent/WO2020073411A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/01—Preparation or separation involving a liquid-liquid extraction, an adsorption or an ion-exchange
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/10—Sulfates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/01—Preparation or separation involving a liquid-liquid extraction, an adsorption or an ion-exchange
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/10—Sulfates
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • 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
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
    • 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 relates to the technical field of hydrometallurgy technology, in particular to a method for extracting nickel, cobalt and iron from low-grade laterite nickel ore.
  • laterite nickel ore With the continuous reduction of nickel sulfide ore resources, laterite nickel ore will be used as the main raw material for the production of nickel products.
  • laterite nickel ore according to the chemical composition and mineral properties of laterite nickel ore, it can be divided into three types: limonite layer, transition layer and humus layer.
  • the laterite nickel ore in the humus layer is high in nickel content and low in iron content. It can be produced by pyrometallurgical reduction technology. At present, the technology is relatively mature and has good economic benefits.
  • the laterite nickel ore in the limonite layer has low nickel content and high iron content. If the fire method is used, the amount of reducing agent is large and the amount of valuable metals obtained is small, which is not economical.
  • the shortcomings of fire process and wet process have been described in the invention patent CN104611558A.
  • the invention patent CN104611558A discloses a method for recovering nickel, cobalt, iron and silicon in laterite nickel ore through a combined leaching process.
  • HPAL high pressure acid leaching
  • the invention patent CN104611558A discloses a method for recovering nickel, cobalt, iron and silicon in laterite nickel ore through a combined leaching process.
  • the limonite pulp and the leaching solution are heated separately and then pumped into the pressurized pipeline reactor by the booster pump. Since the leaching solution is an acidic medium, the booster pump transports the heated leaching solution at 95-100 ° C for a long time. Causes equipment corrosion.
  • the pressure leaching slag is washed with soda ash solution. This method can be used in the test stage. However, considering the industrial production of laterite nickel ore, the amount of iron slag produced is 100-110% of the original ore. If soda ash washing method is used, Due to the high cost of soda ash and the large amount of consumption, it will result in poor economic operation of the system.
  • the present invention provides a hydrometallurgical method for extracting nickel, cobalt, and iron from low-grade laterite nickel ore by sulfuric acid leaching with short process, small equipment volume, simple operation, high product quality and good economic benefit .
  • a method for extracting nickel, cobalt and iron from low-grade laterite nickel ore characterized in that the method includes the following steps:
  • step (3) Pre-neutralization, impurity removal, resin adsorption, and sulfuric acid analysis of the resin in step (2) to obtain nickel sulfate solution and cobalt sulfate solution.
  • the nickel sulfate solution and cobalt sulfate solution are evaporated and concentrated. Crystallization yields nickel sulfate products and cobalt sulfate products.
  • step (1) the first slurry and the concentrated sulfuric acid are heated separately to perform the mixing reaction under the following conditions: the first slurry is heated to 60 °C -80 °C, concentrated sulfuric acid is heated to 100 °C -150 °C 1.
  • the mixing reaction time is 1h-2h.
  • the process of obtaining the first slurry in step (2) is as follows: after pressurizing the mixture of the leaching liquid and the second ore slurry in step (1), a heat exchange is performed through the heat exchanger, and The mixture after the first heat exchange is heated, and the heated mixture is reacted through an iron removal autoclave to obtain a second slurry;
  • the heat exchanger includes a shell and a pipe body, and the heat exchanger shell is The mixture and the second slurry in the heat exchanger tube body exchange heat with the second slurry, and the second slurry undergoes secondary heat exchange through the heat exchanger to obtain the first slurry.
  • the mixture and the second slurry adopt countercurrent heat exchange; after the mixture undergoes a heat exchange, the temperature rises from 30 ° C-50 ° C to 180 ° C-210 ° C; the second slurry passes After the heat exchanger performs secondary heat exchange, the temperature decreases from 230 ° C-250 ° C to 60 ° C-80 ° C.
  • the method is characterized in that the process of removing impurities in the step (3) is divided into one stage of impurity removal and two stages of impurity removal.
  • the slag removal returns to the pre-neutralization stage of step (3).
  • the present invention uses transition layer laterite nickel ore and brown iron layer laterite nickel ore as raw materials, combined with inorganic resin adsorption nickel and cobalt technology to directly produce nickel cobalt sulfate that can be used as a battery raw material
  • the crystalline product has high product quality and good economic benefits
  • the present invention uses the nickel-containing iron solution leached at normal pressure as a leaching agent to react with the laterite nickel ore of the limonite layer, not only to supplement
  • the iron grade in the iron slag is also improved.
  • the iron grade of the iron slag can reach 53-60%.
  • the present invention uses a heat exchanger to realize the conversion of reaction heat, the temperature of the material in the heat exchanger shell is increased from 30-50 ° C to 180-210 ° C, and the temperature of the material in the heat exchanger tube is from 230 -250 °C reduced to 60-80 °C, compared with the traditional flash evaporation process, has the characteristics of short process, small equipment size, simple operation and so on.
  • Figure 1 is a schematic diagram of the process of the present invention.
  • a method for extracting nickel, cobalt and iron from low-grade laterite nickel ore according to the present invention includes the following steps: (1) The transition layer laterite nickel ore is added with water to prepare a first slurry, and the mass percentage of the first slurry is 30 % -50%, the first slurry is heated to 60 °C -80 °C, concentrated sulfuric acid is heated to 100 °C -150 °C and mixed to obtain a mixed slurry, mixing reaction time is 1h-2h, the mixed slurry is diluted with water to dilute, dilute
  • the conditions are: the mass ratio of the mixed slurry to water is 1: (1.5-2), the dilution and stirring time is 0.5h-1h, after dilution, solid-liquid separation is carried out to obtain leaching residue and leaching liquid, and the leaching liquid contains iron 80g / L 120g / L; (2) The brown iron layer laterite nickel ore is added into water to make a second slurry, the mass percentage of the second s
  • the specific process is: Pressurize the mixture of the leaching liquid and the second ore pulp in step (1), heat exchange through the heat exchanger for one time
  • the temperature of the heated mixture rises from 30 ° C-50 ° C to 180 ° C-210 ° C.
  • the mixture after primary heat exchange is heated to increase the temperature of the mixture from 180 ° C-210 ° C to 230 ° C-250 ° C and keep it for 1h- 2h, preferably, the heating source is high-pressure steam, and the heated mixture is subjected to iron removal autoclave reaction to obtain a second slurry.
  • the heat exchanger includes a shell and a tube body. The second slurry is in the tube body, and the mixture and the second slurry exchange heat.
  • the iron concentrate contains 60% -65% iron, which can be used as iron concentrate for blast furnace ironmaking ; (3) Pre-neutralization, impurity removal, resin adsorption, sulfuric acid analysis of the resin in step (2) in order to obtain nickel sulfate Solution and cobalt sulfate solution, nickel sulfate solution contains nickel 30g / L-35g / L, cobalt sulfate solution contains cobalt 2g / L-3g / L, the nickel sulfate solution and cobalt sulfate solution are evaporated, concentrated and crystallized to obtain nickel sulfate product And cobalt sulfate products, nickel sulfate products contain nickel 20% -23%, cobalt sulfate products contain cobalt 1% -2.2%, of which, the impurity removal process is divided into one stage of impurity removal and two stages of impurity removal, one stage of impurity removal The slag is discharged, and the impurity removal slag obtained by
  • Table 1 shows the composition and mass percentage of the ore used in the examples of the present invention.
  • Example 1 4830L of iron removal liquid was added to lime milk with a mass percentage concentration of 30%, followed by pre-neutralization, one-stage removal of impurities, and two-stage removal of impurities, to obtain 5100L of removal liquid, and then 5100L of removal liquid passed through copper removal resin ⁇ Nickel and cobalt extraction resin and impurity removal resin adsorption and sulfuric acid analysis resin to obtain 520L nickel sulfate and cobalt sulfate enrichment solution. The 520L nickel sulfate and cobalt sulfate enrichment solution is evaporated, concentrated and crystallized. 75kg of nickel sulfate and cobalt sulfate products for batteries. Table 2 shows the components and contents of the materials produced in Example 1. Compared with the existing process, the iron concentrate produced in Example 1 has an iron grade of greater than 60% and can be sold as a by-product, while producing high-grade nickel sulfate and cobalt sulfate products, which has better economic benefits.
  • the mixture was heated to 240 ° C with high-pressure steam at 270 ° C, and the reaction was kept for 1 hour; the heated mixture was reacted through an iron removal autoclave to obtain a second slurry, and the second slurry was subjected to secondary heat exchange to obtain the first Slurry and the temperature was reduced from 240 °C to 80 °C; after the first slurry was depressurized through the pressure relief valve group, solid-liquid separation was carried out to obtain 1150kg iron slag and 4920L iron removal liquid. Take 1000g iron slag for ball pressing before proceeding Iron concentrate is obtained by roasting at 1200 °C for 30min.
  • Table 3 shows the components and contents of the materials produced in Example 2.
  • the iron grade of the iron concentrate produced in Example 2 is greater than 60%, and can be sold as a by-product, while producing high-grade nickel sulfate and cobalt sulfate products, which has better economic benefits.
  • the mixture is heated to 250 ° C with high-pressure steam at 270 ° C, and the reaction is kept for 1 hour; the heated mixture is reacted through an iron-removing autoclave to obtain a second slurry, and the second slurry is subjected to second heat exchange to obtain the first Slurry and the temperature was reduced from 250 °C to 85 °C; after the first slurry was depressurized through the pressure relief valve group, solid-liquid separation was performed to obtain 1310kg iron slag and 5020L iron removal liquid, and then take 1000g iron slag for ball pressing Iron concentrate is obtained by roasting at 1200 °C for 30min.
  • Nickel and cobalt extraction resin and impurity removal resin adsorption and sulfuric acid analysis resin to obtain 540L nickel sulfate and cobalt sulfate enrichment liquid
  • the 540L nickel sulfate and cobalt sulfate enrichment liquid is then evaporated, concentrated and crystallized, the final output can be used as production 78kg of nickel sulfate and cobalt sulfate products for batteries.
  • Table 4 shows the components and contents of the materials produced in Example 3. Compared with the existing process, the iron concentrate produced in Example 1 has an iron grade of greater than 60% and can be sold as a by-product, while producing high-grade nickel sulfate and cobalt sulfate products, which has better economic benefits. Table 4 Example 3 Material composition and content

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

Abstract

L'invention concerne un procédé d'extraction de nickel, de cobalt et de fer à partir d'un minerai de nickel latéritique de qualité inférieure, le procédé consistant : à traiter respectivement un minerai de nickel latéritique de couche de transition et un minerai de nickel latéritique de couche de limonite, le degré de fer d'un concentré de minerai de fer produit atteignant 60 % à 65 % ; en même temps, à l'aide d'une technique d'adsorption sur résine et par évaporation, concentration et cristallisation, à produire des produits de sulfate de nickel et de sulfate de cobalt contenant 20 % à 30 % de nickel et contenant 1 % à 2,2 % de cobalt, utilisables en tant que matières premières pour produire une batterie.
PCT/CN2018/114823 2018-10-08 2018-11-09 Procédé d'extraction de nickel, de cobalt et de fer à partir de minerai de nickel latéritique de qualité inférieure Ceased WO2020073411A1 (fr)

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CN201811165423.3 2018-10-08
CN201811165423.3A CN111004915A (zh) 2018-10-08 2018-10-08 一种从低品位红土镍矿中提取镍、钴、铁的方法

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114480877A (zh) * 2021-12-16 2022-05-13 中南大学 一种红土镍矿的资源综合回收方法
CN114789994A (zh) * 2022-05-24 2022-07-26 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
CN116570997A (zh) * 2023-05-10 2023-08-11 荆门市格林美新材料有限公司 提高过滤效率的氢氧化镍酸浸除杂液除杂系统和除杂方法
WO2024221531A1 (fr) * 2023-04-26 2024-10-31 中国科学院过程工程研究所 Procédé de lixiviation pour minerai de latérite de nickel
CN119330416A (zh) * 2024-10-28 2025-01-21 山东美多科技有限公司 一种以镍铁合金为原料分别制备电池级硫酸镍和硫酸亚铁的方法
WO2025107108A1 (fr) * 2023-11-20 2025-05-30 广东邦普循环科技有限公司 Procédé d'élimination de fer ferreux d'un minerai de latérite de nickel par lixiviation acide à haute pression

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CN115161495B (zh) * 2022-08-18 2023-08-18 上海锦源晟新能源材料有限公司 一种从高杂质硫酸钴溶液中分离富集钴的方法
WO2025020123A1 (fr) * 2023-07-26 2025-01-30 青美邦新能源材料有限公司 Méthode de préparation d'une solution de sulfate de nickel-cobalt-manganèse de qualité batterie à partir d'une matte à faible teneur en nickel
CN117191507B (zh) * 2023-07-27 2024-04-12 长沙矿冶院检测技术有限责任公司 红土镍矿中不同物相中镍的分离方法

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US20120204680A1 (en) * 2011-02-11 2012-08-16 Emc Metals Corporation System and Method for Recovery of Nickel Values From Nickel-Containing Ores
CN104611549A (zh) * 2014-12-31 2015-05-13 金川集团股份有限公司 一种用硫酸铁溶液酸浸红土镍矿提取镍、钴的方法
CN104611581A (zh) * 2014-12-31 2015-05-13 金川集团股份有限公司 一种从低品位红土镍矿中提取镍的方法
CN104630464A (zh) * 2014-12-31 2015-05-20 金川集团股份有限公司 一种常压酸浸红土镍矿提取镍、钴的方法
CN104651634A (zh) * 2014-12-31 2015-05-27 金川集团股份有限公司 一种从红土镍矿中回收镍、钴和铁的方法
CN108396157A (zh) * 2018-03-15 2018-08-14 李宾 一种红土镍矿硫酸浸出液和硅胶螯合树脂提纯生产硫酸镍钴的方法

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114480877A (zh) * 2021-12-16 2022-05-13 中南大学 一种红土镍矿的资源综合回收方法
CN114480877B (zh) * 2021-12-16 2023-10-17 中南大学 一种红土镍矿的资源综合回收方法
CN114789994A (zh) * 2022-05-24 2022-07-26 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
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
WO2024221531A1 (fr) * 2023-04-26 2024-10-31 中国科学院过程工程研究所 Procédé de lixiviation pour minerai de latérite de nickel
CN116570997A (zh) * 2023-05-10 2023-08-11 荆门市格林美新材料有限公司 提高过滤效率的氢氧化镍酸浸除杂液除杂系统和除杂方法
WO2025107108A1 (fr) * 2023-11-20 2025-05-30 广东邦普循环科技有限公司 Procédé d'élimination de fer ferreux d'un minerai de latérite de nickel par lixiviation acide à haute pression
CN119330416A (zh) * 2024-10-28 2025-01-21 山东美多科技有限公司 一种以镍铁合金为原料分别制备电池级硫酸镍和硫酸亚铁的方法

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