WO2020093365A1 - Procédé métallurgique en voie humide pour le traitement de minerai de nickel latéritique de faible qualité à l'aide d'une lixiviation acide combinée à pression atmosphérique et à haute pression - Google Patents

Procédé métallurgique en voie humide pour le traitement de minerai de nickel latéritique de faible qualité à l'aide d'une lixiviation acide combinée à pression atmosphérique et à haute pression Download PDF

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WO2020093365A1
WO2020093365A1 PCT/CN2018/114816 CN2018114816W WO2020093365A1 WO 2020093365 A1 WO2020093365 A1 WO 2020093365A1 CN 2018114816 W CN2018114816 W CN 2018114816W WO 2020093365 A1 WO2020093365 A1 WO 2020093365A1
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Prior art keywords
leaching
pressure
acid
ore
iron
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PCT/CN2018/114816
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English (en)
Chinese (zh)
Inventor
刘玉强
王少华
沙滨
李维舟
田忠元
黄海丽
贺来荣
马永刚
杜昊
马海青
秦为涛
陈小林
魏建周
王多江
朱慧
马旻锐
姚菲
张飞
杨松林
李博文
唐金
刘世和
马俊
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金川集团股份有限公司
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Publication of WO2020093365A1 publication Critical patent/WO2020093365A1/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
    • C22B3/04—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
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24—Binding; Briquetting ; Granulating
    • 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
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24—Binding; Briquetting ; Granulating
    • C22B1/2406—Binding; Briquetting ; Granulating pelletizing
    • 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
    • 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
    • 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
    • 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 invention relates to the technical field of hydrometallurgical technology of laterite nickel ore, in particular to a hydrometallurgical technology of normal pressure and pressurized combined acid leaching to treat low-grade laterite nickel ore.
  • Laterite mines are not the same in all parts of the world due to differences in geographic location, climatic conditions and degree of weathering.
  • a highly weathered layer usually distributes most of the nickel it contains finely in finely divided goethite particles. This layer is usually called limonite, and it generally contains a high proportion of iron and a low proportion of silicon and magnesium.
  • the nickel contained in the lighter weathered layer is generally more contained in various magnesium silicate minerals, such as serpentine. There may be many other nickel-containing silicate minerals in the incompletely weathered zone.
  • the partially weathered high-magnesium zone is usually called saprolite or silicon-magnesium-nickel ore, and it generally contains a low proportion of iron and a high proportion of silicon and magnesium.
  • transitional ore In some deposits there is another zone, which is usually between limonite and saprolitic soil and mainly contains chlorite clay, called transitional ore.
  • Low-grade laterite ore refers to laterite ore without rot mud, that is, laterite ore composed of limonite and transition ore.
  • limonite is the main component of laterite nickel ore, accounting for 65% -75% of the total laterite; rot soil 15% -25%; transitional mine 10%.
  • the difficulty in recovering nickel and cobalt from laterite nickel ore is that, before chemical treatment to separate metal useful components (such as nickel and cobalt), the useful components of nickel cannot usually be fully enriched by physical means, that is, it cannot be carried out with mineral processing technology.
  • the processing technology of laterite nickel ore can generally be divided into two categories: fire process and wet process.
  • the pyrometallurgical process is suitable for processing saprolite. This process usually only produces ferronickel and cannot recover cobalt, and its application is limited.
  • the hydrometallurgical process is suitable for processing limonite.
  • the hydrometallurgical technology includes high-pressure acid leaching and reduction roasting_ammonia leaching as well as recent atmospheric pressure leaching and heap leaching processes.
  • the heap leaching technology has a low leaching rate and is only suitable for processing high-magnesium laterite ore; the reduction roasting-ammonia leaching process is less used due to the higher energy consumption and long process flow; the atmospheric pressure acid leaching technology is simple and does not require An expensive autoclave is used, but the acid consumption is large to completely dissolve the minerals, and the leaching solution contains various metal ions, which complicates the subsequent leaching and separation process.
  • the high-pressure acid leaching (HPAL) process uses sulfuric acid to leach the laterite nickel ore under high temperature (250 ° C) and high pressure (50 MPa). Under high temperature and high pressure conditions, the metal minerals in the ore are almost completely dissolved.
  • Dissolved iron rapidly hydrolyzes to hematite (Fe 2 0 3 ) precipitates at the high temperature used, nickel, cobalt, etc. remain in solution, and after cooling, the leaching residues containing iron and silicon are concentrated by a series of washings, ie The so-called countercurrent decantation (CCD) circuit is concentrated and separated from the solution containing nickel and cobalt. Therefore, the main purpose of the leaching process is achieved-separating nickel from iron.
  • CCD countercurrent decantation
  • HPAL high-pressure acid leaching
  • the latter proton (acid) is not fully used for leaching, and it causes excessive sulfuric acid to be neutralized in the subsequent treatment and consumes the neutralizing agent;
  • the HPAL process is limited to processing mainly raw materials of limonite, because The presence of transition mines will lead to a substantial increase in sulfuric acid consumption. This is caused by the high content of magnesium in the saprolite.
  • the autoclave is easy to scale during the operation of the HPAL process. It needs to be shut down and cleaned regularly, and the operating rate is low. Fifth, the amount of leaching slag is large, and it is silicon and Iron mixed slag cannot be developed and utilized cost-effectively.
  • the purpose of the present invention is to solve the technical problems existing in the prior art, and to provide a hydrometallurgical technology for treating low-grade laterite nickel ore by combining normal pressure and pressurization with acid leaching to carry out sulfuric acid on the transition ore components in laterite nickel ore Method for recovering nickel, cobalt and iron by normal pressure leaching and pressure leaching of limonite components with normal pressure leaching solution.
  • the present invention adopts the following technical solution: a hydrometallurgical method for treating low-grade laterite nickel ore by combining normal pressure and pressurization with acid leaching, characterized in that it includes the following steps:
  • transition ore pulp with a concentration of 30-60% and heat it to 60 °C -80 °C; heat concentrated sulfuric acid at 120 °C -180 °C at the same time.
  • the transitional slurry and concentrated sulfuric acid after heating shall be (2.0-2.3): 1 Proportionally added to the acid leaching reactor, leaching reaction occurs, nickel, cobalt, iron and other metal elements in the transition ore are dissolved in the form of metal ions, silicon and other insoluble materials are produced in the form of solid slag; The material enters into the acid leaching reverse tank, and under the stirring condition of the acid leaching reaction tank, the acid leaching reaction of nickel, cobalt, iron and other metal elements is continued to be fully carried out, the reaction time is 10-30 min; Slag and normal pressure leaching solution; (b) Preparation of 30-60% limonite ore slurry, mixing the limonite slurry and normal pressure leaching solution, and using the high temperature reaction produced by the iron removal reactor in
  • the high-temperature iron removal liquid produced by the iron removal reactor is cooled to below 100 ° C in the iron removal heat exchanger, and solid-liquid separation is performed to obtain pressurized leaching slag and pressurized leaching liquid; the iron removal reactor rotates 360 degrees and is hot and cold
  • the materials are heated inversely and indirectly, the heat exchange efficiency is high, and the flow rate of the hot and cold materials is stable, which solves the problems of local scaling and realizes the recovery and utilization of the system's waste heat.
  • iron powder pellets are made by pressing balls and roasting technology, and exported to iron and steel plants.
  • the concentrated sulfuric acid in the step (a) can be adjusted to strong acids such as nitric acid and hydrochloric acid.
  • the mass ratio of the transition ore pulp and limonite ore pulp in the steps (a) and (b) is 1: 2-1: 3.
  • the atmospheric pressure leaching slag produced in the step (a) is silicon slag, which realizes the separation of silicon and iron compared with the traditional process, and increases the content of the pressure leaching slag iron.
  • the acid leaching reactor realizes the efficient and rapid leaching reaction of laterite nickel ore and sulfuric acid;
  • the iron removal reactor realizes the rapid generation of iron slag in laterite nickel ore;
  • the iron removal heat exchanger realizes the cold and hot materials in the iron removal process Reverse heat energy exchange, heat recovery and utilization;
  • horizontal heater realizes further increase of material temperature before entering the reactor.
  • the pressure leaching slag obtained in the step (c) is iron slag
  • the iron content of the iron ore concentrate can be achieved from 61% to 65% through the briquetting and roasting technology, which satisfies the raw material of iron concentrate powder in the steel plant The requirement solves the problem that the existing process iron slag cannot be recycled.
  • the transition ore slurry and a sufficient amount of concentrated sulfuric acid are quickly and fully mixed, and the metals (nickel, cobalt, iron, magnesium, chromium, aluminum, etc.) in the transition ore and the sulfuric acid react quickly This produces metal sulfates.
  • the reaction time is 10-30min, a large amount of reaction heat makes the reaction of the material completely complete, Silica and very small amounts of unreacted iron and non-ferrous metals form leaching residues.
  • the atmospheric pressure leaching solution and the limonite slurry are added to the iron removal reactor for pressure leaching, and Fe 3+ is hydrolyzed to Fe 2 O 3 hematite precipitation and the acid is released and the brown Iron ore, the reaction pressure is 2MPa-4.0Mpa, the reaction temperature is 220 °C -240 °C, not only can ensure that the hydrolysate of iron ions is hematite, but also has a fast hydrolysis rate and a high nickel and cobalt leaching rate and leaching rate .
  • the pressure leaching material is cooled and solid-liquid separation is performed to obtain pressure leaching slag and pressure leaching liquid; the main component of the pressure leaching slag after washing is Fe 2 O 3 hematite, and iron concentrate is produced through ball pressing and roasting process. It is exported to steel mills as a raw material for production.
  • the present invention has the following beneficial effects:
  • a hydrometallurgical technology that combines low-grade laterite nickel ore with normal pressure and pressurized acid leaching has been implemented.
  • Sulphuric acid leaching of transition ore components in laterite nickel ore and atmospheric pressure leaching solution for limonite components The method of recovering nickel, cobalt and iron by pressure leaching overcomes the deficiencies of the traditional methods of fire and wet processes.
  • the pressure leaching of the present invention is carried out at 2.0 MPa-4.0 MPa, and the pressure is much lower than the high-pressure acid leaching conditions of 4.5 MPa-5.0 MPa.
  • the normal pressure leaching time of the invention is 1-12 minutes, and the existing normal pressure acid leaching time is usually 240 minutes to 2400 minutes.
  • the corresponding investment of the normal pressure acid leaching equipment of the present invention is much smaller than the investment of the existing normal pressure acid leaching equipment.
  • the sulfuric acid consumption of the present invention is not only much lower than the acid consumption of the existing atmospheric acid leaching, but also lower than the acid consumption of the existing high-pressure acid leaching.
  • the acid consumption of the existing atmospheric acid leaching is 2.57- 3.33 times
  • the acid consumption of the existing high-pressure pickling is 1.39-1.71 times that of the present invention.
  • the sulfuric acid and iron added at one time in the normal pressure leaching stage of the transition mine react to produce ferric sulfate.
  • no additional sulfuric acid is needed, but instead rely on Fe 3+ hydrolysis to precipitate hematite
  • the protons (acids) released to leach limonite can greatly reduce the consumption of subsequent neutralizers.
  • the existing high-pressure acid leaching process and normal pressure acid leaching process have a large amount of leaching slag.
  • the leaching slag is a mixed slag of silicon and iron, which cannot be used to develop and utilize iron ore and a small amount of silicon as leaching residues.
  • the present invention effectively separates the atmospheric leaching slag and the pressure leaching slag, that is, the pressure leaching slag has a high iron content. After pressing and roasting, the iron concentrate containing 61-65% iron can be obtained and directly exported to the iron plant .
  • the nickel leaching rate of the present invention is not only much higher than that of the existing normal pressure acid leaching, but also higher than the existing high pressure acid leaching nickel leaching rate.
  • the nickel leaching rate of the existing normal pressure acid leaching is 70-85%, the nickel leaching rate of the existing high pressure acid leaching is 90-93%, and the leaching rate of the nickel, cobalt and iron of the present invention is above 96%.
  • FIG. 1 is a schematic flowchart of the present invention.
  • transition ore dry and add 500Kg of water to make transition ore slurry, prepare 500Kg of concentrated sulfuric acid with 98% mass fraction, heat the transition ore slurry to 60 °C, concentrated sulfuric acid to 200 °C, then heat it with mortar pump and concentrated sulfuric acid pump The late transition pulp and concentrated sulfuric acid are added to the feed port of the acid leaching reactor simultaneously. After rapid mixing, the transition pulp and concentrated sulfuric acid are forced to flow into the acid leaching reactor for rapid reaction to dissolve the soluble non-ferrous metals and soluble iron. The reaction takes 1 minute Then the reaction materials are pushed out of the acid leaching reactor.
  • Atmospheric pressure leaching solution (B1) makes the final pH value of the reaction material 0.5, and controls the temperature to heat, leaching under pressure at 2 MPa and 240 °C for 50 minutes, Fe 3+ in the atmospheric leaching solution is hydrolyzed to hematite Precipitate and release acid and then leaching limonite; after cooling to 85 °C, remove the reaction slurry from the iron removal reactor for solid-liquid separation and wash the filter residue, to obtain pressure leaching residue 28Kg (dry), pressure leaching solution 76L, add After the non-nickel and cobalt impurities are removed by the pressure leaching solution, nickel and / or cobalt can be recovered by an immediate method.
  • the components of the pressure leaching residue and pressure leaching solution are shown in
  • the leaching rates of normal pressure acid leaching nickel, cobalt, and iron are: 97.8%, 96.1%, and 96.5%, respectively.
  • the leaching rates of nickel and cobalt under pressure leaching are: 97.5% and 96.2%, respectively.
  • Sulfuric acid consumption 250Kg ⁇ sulfuric acid / t ⁇ ore.
  • the iron content of iron concentrate is> 61%.
  • the leaching rates of normal pressure acid leaching nickel, cobalt, and iron are: 97.5%, 96.3%, and 96.3%, respectively.
  • the pressure leaching rates of nickel and cobalt are 98.0% and 96.7%, respectively.
  • Sulfuric acid consumption 280Kg ⁇ sulfuric acid / t ⁇ ore.
  • the iron content of iron concentrate is> 61%.

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Abstract

L'invention concerne un procédé métallurgique en voie humide pour le traitement de minerai de nickel latéritique de faible qualité à l'aide d'une lixiviation acide combinée à pression atmosphérique et à haute pression, comprenant les étapes suivantes : la formulation d'une pulpe de minerai de métal de transition, le mélange de la pulpe de minerai de métal de transition chauffée et d'acide sulfurique concentré chauffé en une certaine proportion, la mise en œuvre d'une réaction de lixiviation acide et la mise en œuvre d'une séparation solide-liquide après dissolution dans de l'eau pour obtenir un résidu de lixiviation atmosphérique et un liquide de lixiviation atmosphérique ; la formulation d'une pulpe de minerai de limonite, le mélange de la pulpe de minerai de limonite et du liquide de lixiviation atmosphérique, le chauffage de ceux-ci, la mise en œuvre d'une lixiviation sous pression sous une pression de 2,0 MPa à 4,0 MPa et une température de 220 °C à 240 °C, puis la mise en œuvre d'une séparation solide-liquide après refroidissement pour obtenir un résidu de lixiviation sous pression et un liquide de lixiviation sous pression ; et la transformation du résidu de lixiviation sous pression en poudre de fer à l'aide d'un pressage à billes et d'un processus de grillage.
PCT/CN2018/114816 2018-11-08 2018-11-09 Procédé métallurgique en voie humide pour le traitement de minerai de nickel latéritique de faible qualité à l'aide d'une lixiviation acide combinée à pression atmosphérique et à haute pression WO2020093365A1 (fr)

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CN201811322426.3A CN111154974A (zh) 2018-11-08 2018-11-08 一种常压及加压联合酸浸处理低品位红土镍矿的湿法冶金方法

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CN112646973B (zh) * 2020-12-09 2022-11-25 金川集团股份有限公司 一种三段选择性浸出红土矿的方法
CN113604656A (zh) * 2021-07-12 2021-11-05 四川顺应动力电池材料有限公司 常压-高压联合浸出红土镍矿生产高品位铁精矿的方法
CN113957242A (zh) * 2021-10-11 2022-01-21 荆门市格林美新材料有限公司 一种镍铁合金料与含镍原料的联合处理方法

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WO2008019451A1 (fr) * 2006-08-17 2008-02-21 Ab Tall (Holdings) Pty Ltd Collecteurs et procédés de flottation
CN104611580A (zh) * 2014-12-31 2015-05-13 金川集团股份有限公司 一种处理低品位红土镍矿的方法
CN104611579A (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回收镍的方法
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
CN104611548A (zh) * 2014-12-31 2015-05-13 金川集团股份有限公司 一种回收低品位红土镍矿中的镍的方法

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