无机盐工业
主管:中海油天津化工研究设计院有限公司
主办:中海油天津化工研究设计院有限公司
   中海油炼油化工科学研究院(北京)有限公司
   中国化工学会无机酸碱盐专业委员会
ISSN 1006-4990 CN 12-1069/TQ
研究与开发

基于铁法工艺制备电池级磷酸铁技术的研究

  • 倪双林 ,
  • 马航 ,
  • 薛河南 ,
  • 万邦隆 ,
  • 闫银贤 ,
  • 张金源 ,
  • 陈章鸿 ,
  • 魏兴 ,
  • 陈云建 ,
  • 杜建波 ,
  • 代金凤
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  • 1.云南云天化以化磷业研究技术有限公司,云南 昆明 650228
    2.云南云天化股份有限公司研发中心,云南 昆明 650228
倪双林(1974— ),男,高级工程师,主要研究方向为湿法磷加工、精细磷化工;E-mail:Shuanglin.ni@yprtec.com
马航(1981— ),男,博士,正高级工程师,主要从事化工新材料方面的研究;E-mail:hang.ma@yprtec.com

收稿日期: 2024-08-14

  网络出版日期: 2025-09-23

基金资助

云南省科技厅重大专项(202302AF080003)

Study on iron-based process for preparing battery-grade ferric phosphate

  • NI Shuanglin ,
  • MA Hang ,
  • XUE He′nan ,
  • WAN Banglong ,
  • YAN Yinxian ,
  • ZHANG Jinyuan ,
  • CHEN Zhanghong ,
  • WEI Xing ,
  • CHEN Yunjian ,
  • DU Jianbo ,
  • DAI Jinfeng
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  • 1. Yunnan Yuntianhua Phosphorus Industry Research Technology Co. ,Ltd. ,Kunming 650228,China
    2. Yunnan Yuntianhua Co. ,Ltd. ,R&D Center,Kunming 650228,China

Received date: 2024-08-14

  Online published: 2025-09-23

摘要

为获得纯铁法磷酸铁产业化生产工艺技术条件,在完成小试探索试验、公斤级放大试验的基础上,建成1 000 t/a磷酸铁中试装置,以99.9%高纯铁锭、85.0%净化磷酸、27.5%双氧水为原料(均为质量分数),采用磷酸溶铁、双氧水氧化沉淀磷酸二氢亚铁生产磷酸铁的工艺。该工艺实施过程需要以磷酸二氢亚铁液Fe2+质量分数为目标控制磷酸溶铁工艺,实验优化的工艺条件:磷酸质量分数为26%~27%,溶铁温度为88~90 ℃,溶铁时间为13~15 h,并对磷酸二氢亚铁液的存储给出了建议。将磷酸二氢亚铁Fe2+质量浓度控制在44~46 g/L,n(P)∶n(Fe)控制在(2.65~2.75)∶1时,以产品的比表面积为目标的氧化沉淀优化工艺条件:起始氧化温度为62~64 ℃,双氧水加料时间为50~60 min。最终获得的无水磷酸铁产品的P质量分数为20.40%~20.70%、Fe的质量分数为36.18%~36.58%、n(Fe)∶n(P)为(0.970~0.985)∶1、粒径D50为3~5 μm、比表面积为6~9 m2/g、振实密度大于0.60 g/cm3、磁性物含量控制在0.5 mg/kg以下,各项指标达到电池级磷酸铁质的要求。

本文引用格式

倪双林 , 马航 , 薛河南 , 万邦隆 , 闫银贤 , 张金源 , 陈章鸿 , 魏兴 , 陈云建 , 杜建波 , 代金凤 . 基于铁法工艺制备电池级磷酸铁技术的研究[J]. 无机盐工业, 2025 , 57(9) : 73 -81 . DOI: 10.19964/j.issn.1006-4990.2024-0450

Abstract

In order to obtain the industrial production technology conditions for ferric phosphate by using pure iron,Yunnan Yuntianhua Co.,Ltd.,R&D Center after completing the small-scale exploratory experiment and model verification experiment,built a 1 000 t/a pilot plant for ferric phosphate production.The process used high-purity iron ingots(99.9%),purified phosphoric acid(85.0%),and 27.5% hydrogen peroxide as raw materials to produce ferric phosphate by the process of phosphoric acid dissolving iron,hydrogen peroxide oxidizing and precipitating dihydrogen phosphate.The process required the phosphate dihydrogen phosphate solution Fe2+ mass fraction to be controlled as the target during the phosphoric acid dissolving process,and the optimized process conditions were as follows:phosphoric acid mass fraction of 26%~27%,dissolving temperature of 88~90 ℃,and dissolving time of 13~15 h.Suggestions were also given for the storage of phosphate dihydrogen phosphate solution.When the mass fraction of the phosphate dihydrogen phosphate Fe2+ was controlled at 44~46 g/L and the n(P)∶n(Fe) ratio was(2.65~2.75)∶1,the optimized oxidation precipitation process conditions for producing products with specific surface area as the target were as follows:the initial oxidation temperature of 62~64 ℃,and the hydrogen peroxide feeding time of 50~60 min.The final ferric phosphate product had a P mass fraction of 20.40%~20.70%,Fe mass fraction of 36.18%~36.58%,n(Fe)∶n(P) of (0.970~0.985)∶1,particle size D50 of 3~5 μm,specific surface area of 6~9 m2/g,bulk density greater than 0.60 g/cm3,magnetic impurities controlled below 0.5 mg/kg,and all the indicators met the requirements for battery-grade ferric phosphate.

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