高性能电池级磷酸铁制备工艺过程控制研究  

Research on process control of high-performance battery-grade iron phosphate preparation

作　　者：盛国臣 余欣鑫 管庆永 何兵兵 龙小康 SHENG Guochen;YU Xinxin;GUAN Qingyong;HE Bingbing;LONG Xiaokang(Guizhou Phosphate New Energy Technology Co.,Ltd.,Xifeng Guizhou 550000,China)

机构地区：[1]贵州磷化新能源科技有限责任公司,贵州息烽550000

出　　处：《化工矿物与加工》2025年第2期25-34,共10页Industrial Minerals & Processing

基　　金：贵州优势特色矿产资源高效利用研究(黔科合战略找矿〔2022〕ZD006)。

摘　　要：随着全球新能源动力电池产业的快速发展,锂离子电池逐渐成为市场主流,其中磷酸铁锂电池因性能优异而受到广泛关注,作为前驱体的磷酸铁对磷酸铁锂正极材料的性能具有重要影响。本文采用钠法工艺制备磷酸铁,探讨了沉淀温度、搅拌速度、洗涤次数、煅烧温度和时间、沉淀pH以及添加分散剂等因素对磷酸铁产品质量的影响,结果表明:产品的铁磷比随着沉淀pH的降低而升高,阴离子表面活性剂的引入有助于提升产品的铁磷比;产品硫含量随着洗涤次数的增加、沉淀pH的降低以及煅烧温度的升高而降低;比表面积随着煅烧温度的升高而减小,引入阴离子或高分子表面活性剂可增大比表面积。综合分析得到了最佳工艺条件:搅拌速度为800 r/min,沉淀pH为1.6,沉淀温度为80℃,洗涤4次,煅烧温度为500℃,煅烧时间为3 h,添加阴离子表面活性剂及其复配物。在此条件下,制备的高性能电池级磷酸铁产品硫含量≤30×10^(-6),比表面积≥9.5 m^(2)/g,铁磷比为0.970~0.978。With the development of the global new energy power battery industry,lithium-ion batteries have become the mainstream of the market.Among them,lithium iron phosphate batteries have received widespread attention due to their excellent performance.As a precursor,iron phosphate has an important impact on the performance of lithium iron phosphate cathode materials.This article used the sodium method to prepare iron phosphate and explored the effects of precipitation temperature,stirring speed,washing frequency,calcination temperature and time,precipitation pH,and addition of dispersants on the quality of iron phosphate products.The results indicate that the iron phosphorus ratio of the product increases with the decrease of precipitation pH,and the introduction of anionic surfactants helps to improve the iron phosphorus ratio of the product.The sulfur content of the product decreases with the increase of washing times,the decrease of precipitation pH,and the increase of calcination temperature.The specific surface area decreases with the increase of calcination temperature,and the introduction of anionic or polymeric surfactants can increase the specific surface area.The optimal process conditions were obtained through comprehensive analysis:stirring speed of 800 r/min,precipitation pH of 1.6,precipitation temperature of 80℃,washing 4 times,calcination temperature of 500℃,calcination time of 3 hours,and addition of anionic surfactants and their complexes.Under these conditions,the sulfur content of the high-performance battery grade iron phosphate product prepared is less than or equal to 30×10^(-6),and the specific surface area is greater than or equal to 9.5 m^(2)/g,and an iron phosphorus ratio of 0.970~0.978.

关 键 词：磷酸铁 铁磷比 硫含量 比表面积 表面活性剂 锂电池 

分 类 号：TM912[电气工程—电力电子与电力传动]