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WO2025124600A1 - Procédé de traitement de résidus de lixiviation acide de minerai de nickel latéritique, et matériau actif - Google Patents

Procédé de traitement de résidus de lixiviation acide de minerai de nickel latéritique, et matériau actif Download PDF

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Publication number
WO2025124600A1
WO2025124600A1 PCT/CN2024/139731 CN2024139731W WO2025124600A1 WO 2025124600 A1 WO2025124600 A1 WO 2025124600A1 CN 2024139731 W CN2024139731 W CN 2024139731W WO 2025124600 A1 WO2025124600 A1 WO 2025124600A1
Authority
WO
WIPO (PCT)
Prior art keywords
slag
acid leaching
nickel ore
leaching residue
laterite nickel
Prior art date
Legal status (The legal status 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 status listed.)
Pending
Application number
PCT/CN2024/139731
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English (en)
Chinese (zh)
Inventor
代文彬
陈奎元
陈曦
祁永峰
王书晓
陈学刚
裴忠冶
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.)
China Enfi Engineering Co Ltd
China ENFI Engineering Corp
Original Assignee
China Enfi Engineering Co Ltd
China ENFI Engineering Corp
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 China Enfi Engineering Co Ltd, China ENFI Engineering Corp filed Critical China Enfi Engineering Co Ltd
Priority to AU2024354211A priority Critical patent/AU2024354211B1/en
Publication of WO2025124600A1 publication Critical patent/WO2025124600A1/fr
Priority to CONC2025/0010007A priority patent/CO2025010007A2/es
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • 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
    • B03C1/02—Magnetic separation acting directly on the substance being separated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028—Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039—Premixtures of ingredients
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/14—Cements containing slag
    • C04B7/147—Metallurgical slag
    • C04B7/153—Mixtures thereof with other inorganic cementitious materials or other activators
    • C04B7/17—Mixtures thereof with other inorganic cementitious materials or other activators with calcium oxide containing activators
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/14—Cements containing slag
    • C04B7/147—Metallurgical slag
    • C04B7/153—Mixtures thereof with other inorganic cementitious materials or other activators
    • C04B7/21—Mixtures thereof with other inorganic cementitious materials or other activators with calcium sulfate containing activators
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/24—Cements from oil shales, residues or waste other than slag
    • C04B7/243—Mixtures thereof with activators or composition-correcting additives, e.g. mixtures of fly ash and alkali activators
    • 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
    • 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
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
    • 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, and in particular to a method for treating laterite nickel ore acid leaching residue and an active material.
  • nickel ores are mainly divided into two categories worldwide: nickel sulfide ores and laterite nickel ores. According to the proven reserves, the reserves of the two nickel ores are approximately 1:3. In the past, nickel sulfide ores were mainly used worldwide, but as its reserves gradually decreased, laterite nickel ores are now gradually used as the main source of nickel sulfide ores, and the proportion is gradually exceeding that of nickel sulfide ores.
  • the largest amount of laterite nickel ore is mainly used to produce stainless steel raw materials - nickel-iron alloys using the RKEF pyrometallurgical process.
  • the waste slag produced is mainly nickel-iron slag.
  • Most of the Ni and Fe elements in the laterite nickel ore are reduced into nickel-iron, and the main components of the solid slag are MgO and SiO 2.
  • this smelting process has the problems of high power consumption and high production cost. Since components such as MgO and SiO 2 in laterite nickel ore are easy to form high melting point phases during the smelting process, a higher furnace temperature is often required to ensure the separation of slag and iron.
  • the amount of slag produced is also large, and the resource utilization rate is low.
  • the main purpose of the present invention is to provide a method for treating laterite nickel ore acid leaching residue and an active material to solve the problem that the prior art cannot effectively utilize laterite nickel ore acid leaching residue.
  • step S2 the calcination temperature is 900-1250°C, and the calcination time is 1-2h.
  • the volume concentration of O2 in the hot flue gas is ⁇ 5%, and the temperature of the hot flue gas is ⁇ 300°C.
  • the magnetic field strength of the first magnetic separation process is higher than that of the second magnetic separation process, and the first magnetic separation strength is 150-250 kA/m, and the second magnetic separation strength is 80-150 kA/m.
  • the present application can further effectively recover the Fe element in the laterite nickel acid leaching residue by adjusting the material, the flux material and the reducing agent to cooperate with each other.
  • the treatment method of the laterite nickel acid leaching residue of the present invention realizes the comprehensive utilization of the laterite nickel acid leaching residue, has a high recovery rate of residual valuable Fe metal, realizes the full utilization of valuable metals (such as Fe, Ni), sulfur and other components, not only realizes the recycling of valuable metals, but also realizes the recycling of sulfur resources, and reduces the procurement cost of sulfuric acid.
  • this application provides a method for treating laterite nickel ore acid leaching residue, as shown in Figure 1, which includes the following steps: step S1, mixing and pressing laterite nickel ore acid leaching residue, adjustment material, fluxing material and reducing agent to obtain a preform; step S2, roasting the preform to obtain hot slag and hot flue gas, and the hot flue gas is used to make acid; step S3, magnetically separating the hot slag to obtain refined iron material and tailings; step S4, mixing and grinding the tailings, active material and stimulating material to obtain active materials; wherein the adjustment material is iron-containing waste slag; the fluxing material is an alkaline substance containing one or more of CaO, MgO and Na2O; the active material is selected from one or more of nickel iron slag, fly ash, blast furnace slag, bottom slag or coal slag; the stimulating material is
  • the tailings can be mixed with active materials and exciting materials for grinding to obtain active materials, which are used in the field of building materials, thereby effectively realizing the recycling of calcium elements in the laterite nickel ore acid leaching residue.
  • the flux is an alkaline substance containing one or more of CaO, MgO, and Na2O , which can react with acidic oxides such as SiO2 in the laterite nickel ore acid leaching residue, and release Fe2O3 originally combined with SiO2 , thereby improving the reduction reaction activity of iron oxides and increasing the yield of metallic iron.
  • the present application can further effectively recover the Fe element in the laterite nickel acid leaching residue by adjusting the material, the flux and the reducing agent.
  • the treatment method of the laterite nickel acid leaching residue of the present invention realizes the comprehensive resource utilization of the laterite nickel acid leaching residue, has a high recovery rate of residual valuable Fe metal, realizes the full utilization of valuable metals (such as Fe, Ni), sulfur and other components, not only realizes the recycling of valuable metals, but also realizes the recycling of sulfur resources, and reduces the procurement cost of sulfuric acid.
  • the treatment method of the laterite nickel acid leaching residue of the present invention can achieve the purpose of coordinated treatment and utilization of various iron-containing waste slags produced in other nickel metallurgy (including hydrometallurgy and pyrometallurgy), steel metallurgy, thermal power and other surrounding supporting industrial production.
  • the treatment method of the present invention has the characteristics of large solid waste consumption, many types of generated products, high product output value, low comprehensive production cost, high resource utilization rate, etc., and provides a more effective solution for the full recovery of valuable components and resource utilization of all components of the laterite nickel acid leaching residue.
  • the laterite nickel ore acid leaching residue of the present invention refers to the waste residue produced after the laterite nickel ore is treated by a wet acid leaching process, which includes the following components: 38-52wt% of Fe, 4-13wt% of FeO, 8-22wt% of SiO 2 , 5-23wt% of CaO, 1-6wt% of Al 2 O 3 and 1-4wt% of MgO.
  • the hot slag includes the following components: 48-68wt% of Fe 2 O 3 , 8-17wt% of SO 3 , 1-5wt% of CaO, 6-25wt% of SiO 2 , 1-4wt% of MgO and 3-8wt% of Al 2 O 3 .
  • the hot flue gas includes SO 2 , and the volume concentration of SO 2 is 4-10%.
  • the laterite nickel ore acid leaching residue is 100 parts
  • the adjusting material is 3-28 parts
  • the flux is 0.5-22 parts
  • the reducing agent is 5-20 parts.
  • the synergistic effect of the laterite nickel ore acid leaching residue and the adjusting material, the flux, and the reducing agent is more significant, so that the Fe element of the laterite nickel ore acid leaching residue can be fully reduced, and more laterite nickel ore acid leaching residue can be effectively treated, so that the iron content of the subsequent refined iron material is higher, and the performance of the tailings active material is better.
  • the laterite nickel ore acid leaching residue within the above-mentioned ratio range and the adjusting material, the flux, and the reducing agent can improve the roasting metal reduction efficiency and reduce energy consumption and cost.
  • the tailings are 20 to 40 parts, the active material is 50 to 70 parts, and the stimulating material is 3 to 10 parts.
  • the roasting temperature is 900-1250°C and the roasting time is 1-2h.
  • the roasting temperature is too high, it will lead to increased liquid content and over-sintering, which is not conducive to the stable operation of the roasting furnace and the energy consumption will also increase.
  • the roasting temperature is too low, the iron element cannot be fully reduced.
  • the mixture of laterite nickel ore acid leaching residue, adjustment material, flux material and reducing agent is pressed into blocks or spheres for roasting;
  • the fuel used in the roasting process is selected from natural gas and/or coal powder;
  • the preform roasting process can be roasted and reduced in a rotary kiln, a rotary hearth furnace, a sintering car, a belt roasting machine or a tunnel kiln.
  • the volume concentration of O2 in the combustion-supporting gas used in the roasting process is 40-60%.
  • the present invention controls the volume concentration of O2 in the combustion-supporting gas within the above range, which can achieve oxygen-enriched combustion and further reduce energy consumption.
  • the volume concentration of O2 in the hot flue gas is ⁇ 5%, and the temperature of the hot flue gas is ⁇ 300°C.
  • the hot flue gas of the present invention can be recycled as a raw material for acid production, realizing the recycling of sulfur resources of laterite nickel ore acid leaching slag and reducing the procurement cost of sulfuric acid in the laterite nickel ore wet acid leaching process.
  • the present invention controls the volume concentration and temperature of O2 in the hot flue gas discharged from the furnace, which can fully ensure the reducing atmosphere required for the reduction of metal oxides in the slag, while reducing the increase in production energy consumption caused by excessive CO generation and excessive flue gas temperature.
  • the volume concentration of O2 in the hot flue gas is 2-4%, and the temperature of the hot flue gas is 300-350°C.
  • the iron-containing waste slag is selected from one or more of steel slag, wet iron-aluminum slag or nickel smelting slag.
  • the alkaline substance can be raw materials processed from natural ore resources, such as limestone, dolomite, quicklime, etc. From the perspective of turning waste into treasure, metallurgical and chemical waste slag can also be used, such as gypsum slag, carbide slag, magnesium slag, etc.
  • the reducing agent is selected from a solid reducing agent with a carbon content of 40-90% and a calorific value of ⁇ 3000kcal/kg.
  • the solid reducing agent selected from the above can promote the reduction of iron in the laterite nickel ore acid leaching residue on the one hand, and can also be used as a fuel to improve the roasting efficiency and further improve the recovery rate of iron in the laterite nickel ore acid leaching residue on the other hand.
  • the reducing agent can be selected from mineral fuels such as anthracite, lignite, coke, etc., and can also be selected from waste graphite electrodes and biomass waste (for example, straw, carbonized rice husk, etc.).
  • the particle size of the reducing agent is controlled to be ⁇ 10mm.
  • the processing method before pressing, further includes subjecting the laterite nickel ore acid leaching residue, the adjustment material, and the flux material to a first crushing process to control the particle size of the material to be ⁇ 10 mm.
  • the present invention crushes the above materials to control the particle size of the materials to be ⁇ 10 mm so that the materials can be fully mixed and contacted with each other to improve the reaction efficiency.
  • the particle size of the material is 3 to 7 mm.
  • the processing method further includes the step of air cooling the hot slag to obtain the slag.
  • the present invention can not only recover the waste heat of the hot slag to form cooling hot air, and continue to use it as combustion-supporting air, but also promote the formation of the glass phase of the slag tailings, and improve the potential hydration and gelling activity of the tailings.
  • the hot slag is cooled with air, the waste heat of the hot slag converts the cold air into hot air.
  • the present invention then returns the hot air to the preform roasting process as part of the combustion-supporting gas, making full use of the waste heat of the flue gas and saving energy.
  • the slag is subjected to a second crushing treatment and a grinding treatment in sequence, and more than 35% of the slag by mass after the grinding treatment has a particle size of ⁇ 0.074 mm.
  • the magnetic separation includes two magnetic separation processes performed in sequence, and the magnetic field strength of the two magnetic separation processes is independently 80-250 kA/m.
  • the magnetic field strength of the first magnetic separation process is higher than the magnetic field strength of the second magnetic separation process, and the first magnetic separation strength is 150-250 kA/m and the second magnetic separation strength is 80-150 kA/m.
  • the present invention also provides an active material, which is obtained by the aforementioned method for treating laterite nickel ore acid leaching residue, and the specific surface area of the active material is ⁇ 350m 2 /kg.
  • the active material obtained by the above treatment method has potential hydration activity and better activity.
  • the better hydration activity allows the material to be used as an active admixture and can be directly sold as an active admixture to concrete, cement products and other production enterprises.
  • the composition of the laterite nickel ore acid leaching residue is: Fe2O3 is 57wt%, SiO2 is 15wt%, CaO is 4wt%, Al2O3 is 3.7wt %, MgO is 1.7wt%, SO3 is 11wt% and other impurities.
  • the laterite nickel ore acid leaching residue, adjusting material (steel slag) and flux (quicklime) are crushed to a particle size of less than 10 mm, and then mixed with a reducing agent (anthracite) and pressed into balls to obtain a preform; wherein, based on the weight of the dry ore, the laterite nickel ore acid leaching residue is 100 parts, the adjusting material is 15 parts, the flux is 2 parts, and the reducing agent is 15 parts.
  • the preformed product is sent to a rotary kiln for roasting, and the roasting temperature is controlled within the range of 1100-1150°C, and the roasting time is 2 hours.
  • natural gas is used as fuel, and oxygen-enriched combustion air with an oxygen volume concentration of 50% is blown in (wherein the volume concentration of each gas is: O2 is 50%, N2 is 49%, and H2O is 1%), and hot slag (Fe is 43wt%, FeO is 6wt%, CaO is 8.1wt%, SiO2 is 12.3wt%, Al2O3 is 2.3wt %, and MgO is 1.4wt%) and hot flue gas are obtained.
  • the hot flue gas is the flue gas from the roasting furnace, and the SO2 component content is 7%, the flue gas temperature is 340°C, and the O2 concentration is 5%.
  • the recovered hot flue gas is used as a raw material for preparing concentrated sulfuric acid after cooling and dust removal.
  • the hot slag after being discharged from the furnace is air-cooled to 300°C to obtain slag, which is then crushed and ground.
  • the particle size distribution of the slag after grinding is as follows: the weight of the residue after the slag passes through a 0.074 mm sieve is 25%.
  • the ground slag is then subjected to two magnetic separations, with the magnetic field strength of the first magnetic separation being 240 kA/m to obtain middlings and tailings.
  • the middlings are then subjected to secondary magnetic separation, with the magnetic field strength being 100 kA/m to obtain fine iron (TFe content being 78%, Fe recovery rate being 92%) and tailings.
  • tailings According to the weight of dry ore, 30 parts of tailings, 65 parts of active material (fly ash) and 5 parts of stimulating material (desulfurized gypsum) are mixed and ground until the specific surface area reaches 400-450m2 /kg, and the active material is obtained.
  • Example 2 The difference from Example 1 is that the laterite nickel ore acid leaching residue is 100 parts, the adjustment material is 28 parts, the flux material is 22 parts, and the reducing agent is 20 parts.
  • Example 2 The difference from Example 1 is that the laterite nickel ore acid leaching residue is 100 parts, the adjustment material is 15 parts, the flux is 2 parts, and the reducing agent is 2 parts.
  • Example 1 The difference from Example 1 is that the volume concentration of O 2 in the combustion-supporting gas is 20%.
  • Example 1 The difference from Example 1 is that, based on the weight of dry ore, 20 parts of tailings, 70 parts of active materials and 10 parts of exciting materials are mixed and ground.
  • Example 1 The difference from Example 1 is that, based on the weight of dry ore, 37 parts of tailings, 50 parts of active materials and 3 parts of exciting materials are mixed and ground.
  • Example 1 The difference from Example 1 is that, based on the weight of dry ore, 50 parts of tailings, 30 parts of active materials and 20 parts of exciting materials are mixed and ground.
  • Fe recovery rate weight of iron ore concentrate ⁇ Fe content of iron ore concentrate/( ⁇ amount of each input material ⁇ Fe content of each input material) ⁇ 100%.

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  • Ceramic Engineering (AREA)
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  • Structural Engineering (AREA)
  • Mechanical Engineering (AREA)
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  • Metallurgy (AREA)
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Abstract

L'invention concerne un procédé de traitement de résidus de lixiviation acide de minerai de nickel latéritique, et un matériau actif. Le procédé comprend les étapes suivantes consistant à : étape S1, mélanger des résidus de lixiviation acide de minerai de nickel latéritique, un matériau d'ajustement, un matériau fondant et un agent réducteur, et presser le mélange, de façon à obtenir un préfabriqué; étape S2, griller le préfabriqué pour obtenir des scories de grillage et un gaz de combustion chaud, le gaz de combustion chaud étant utilisé pour préparer un acide; étape S3, soumettre les scories de grillage à une séparation magnétique, de façon à obtenir un matériau ferreux raffiné et des résidus; et étape S4, mélanger les résidus, une charge active et un matériau d'excitation, et broyer le mélange, de façon à obtenir un matériau actif. Le procédé de traitement présente les caractéristiques d'une grande consommation de déchets solides, de multiples types de produits générés, d'une valeur de sortie de produit élevée, d'un faible coût de production global, d'un taux d'utilisation des ressources élevé, etc., et fournit une solution plus efficace pour la récupération complète de composants précieux et le recyclage complet de résidus de lixiviation acide de minerai de nickel latéritique.
PCT/CN2024/139731 2023-12-14 2024-12-16 Procédé de traitement de résidus de lixiviation acide de minerai de nickel latéritique, et matériau actif Pending WO2025124600A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU2024354211A AU2024354211B1 (en) 2023-12-14 2024-12-16 Method for Treating Lateritic Nickel Ore Acid Leaching Residue, and Activated Material
CONC2025/0010007A CO2025010007A2 (es) 2023-12-14 2025-07-23 Método para el tratamiento de residuos de lixiviación ácida de minerales lateríticos de níquel y material activado

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN202311717499.3A CN117403057B (zh) 2023-12-14 2023-12-14 红土镍矿酸浸渣的处理方法、活性材料
CN202311717499.3 2023-12-14

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WO2025124600A1 true WO2025124600A1 (fr) 2025-06-19

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CN (1) CN117403057B (fr)
AU (1) AU2024354211B1 (fr)
CO (1) CO2025010007A2 (fr)
WO (1) WO2025124600A1 (fr)

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CN118910404B (zh) * 2024-10-10 2025-01-24 中南大学 一种基于渣高效利用的红土镍矿高压酸浸低耗工艺处理方法

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