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红土镍矿硝酸加压浸出渣制备电池级磷酸铁

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近年来,在我国"碳达峰"和"碳中和"目标的引领下,新能源行业发展迅速,新能源汽车的推广与使用促进了锂离子电池行业的蓬勃发展.作为三元锂电池的关键原材料,镍的需求量不断增加.但由于硫化镍矿日益枯竭,红土镍矿逐渐成为了主要的提镍原料,在镍产量中占比超过70%.褐铁型红土镍矿在红土镍矿中占比超过60%,经硝酸加压浸出(NAPL)提取镍钴后产生的浸出渣中含有丰富的有价金属资源(铁含量>60%),浸出渣的综合利用对资源回收和环境保护具有重要意义.以褐铁型红土镍矿硝酸加压浸出渣为原料,在磷酸单一介质中制备电池级磷酸铁材料.以磷酸为介质,通过预浸、溶解实现浸出渣中铁的高效提取.预浸时磷酸溶液浓度较低,可以使含铁相初步转型为FePO4·2H2O,同时除去浸出渣中Cr、Mg、Al等杂质元素.然后采用高浓度磷酸溶液溶解处理预浸渣,实现Fe的完全溶解.最后稀释调节pH值直接沉淀制备磷酸铁,得到FePO4·2H2O产品,该产品不含杂质元素Mg、Si,Cr、Al的含量为0.019%、0.016%.通过XRD、SEM、EDS等技术手段对预浸渣和磷酸铁产品的物相组成和微观形貌进行了研究,明确了预浸过程可实现铁由Fe2O3向FePO4·2H2O的转变,最终产品的晶体结构与标准磷酸铁相匹配.由磷酸铁合成的磷酸铁锂材料也表现出优异的电化学性能.该研究有望实现对褐铁型红土镍矿硝酸加压浸出渣中宏量组元铁的高值化利用,从而优化磷酸铁制备工艺.
Preparation of battery-grade iron phosphate from nitric acid pressure leaching residue of nickel laterite ore
In recent years,under the guidance of"carbon peaking"and"carbon neutrality"goals in China,the new energy industry is developing rapidly.The promotion and use of new energy vehicles have promoted the vigorous development of the lithium-ion battery industry.Nickel is a key raw material for ternary lithium-ion batteries,and its demand is increasing.Due to the depletion of nickel sulfide ores,laterite nickel ores have gradually become the main raw material for yielding nickel,accounting for more than 70%of nickel production.The limonitic laterite nickel ore accounts for more than 60%of the laterite nickel ore.The leach residue produced after the extraction of nickel and cobalt by nitric acid pressure leaching(NAPL)is rich in valuable metal resources(iron content>60%).The comprehensive utilization of leach residue is of great significance to resource recovery and environmental protection.In this paper,the raw material is nitric acid pressure-leaching residue of limonitic laterite nickel ore,which was used to prepare battery-grade iron phosphate in a single phosphoric acid medium.The efficient extraction of iron from leach residue was realized by pre-leaching and dissolving with phosphoric acid as medium.The low concentration of phosphoric acid solution during pre-leaching allowed the initial transformation of the iron-containing phase to FePO4·2H2O,while Cr,Mg,Al and other impurity elements in leach residue were removed.Then,the pre-leaching residue was dissolved by phosphoric acid with high concentration,which achieved complete dissolution of Fe.Finally,the iron phosphate was directly precipitated by diluting and adjusting the pH values,and then the product of FePO4·2H2O was obtained.The product did not contain impurity elements such as Mg,Si,and the content of Cr and Al is only 0.019%and 0.016%,respectively.The phase composition and microstructure of pre-leaching residue and iron phosphate products were investigated by XRD,SEM and EDS.It is clarified that the pre-leaching process could realize the transformation from Fe2O3 to FePO4·2H2 O.The crystal structure of the final product matches the standard iron phosphate well.The lithium iron phosphate materials synthesized from iron phosphate also exhibited excellent electrochemical properties.This study is expected to achieve high-value utilization of macro component iron in the nitric acid pressurized leaching residue of brown iron type laterite nickel ore,thereby optimizing the preparation process of iron phosphate.

limonitic laterite orenitric acid pressure leachingleaching residuephosphoric acidpre-leachingiron phosphateseparation and impurity removalhigh-value utilization

金赐安、马保中、曹志河、陈永强、王成彦

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北京科技大学冶金与生态工程学院,北京 100083

褐铁型红土镍矿 硝酸加压浸出 浸出渣 磷酸 预浸出 磷酸铁 分离除杂 高值利用

国家自然科学基金自资助项目

U2202254

2024

矿冶
北京矿冶研究总院

矿冶

CSTPCD
影响因子:0.78
ISSN:1005-7854
年,卷(期):2024.33(2)
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