农药氟虫腈与钛白粉副产盐资源化生产电池用磷酸铁工艺  

Production of iron phosphate for batteries using by-product salts from pesticide fipronil and titanium dioxide

作　　者：周哲[1,3] 崔咪芬 陈献[1,3] 于瑞兵 徐希化[1,3] 齐敏 汤吉海 乔旭 ZHOU Zhe;CUI Mifen;CHEN Xian;YU Ruibing;XU Xihua;QI Min;TANG Jihai;QIAO Xu(College of Chemistry Engineering,Nanjing Tech University,Nanjing 211816,China;State Key Laboratory of Materials-Oriented Chemical Engineering,Nanjing Tech University,Nanjing 211816,China;Nanjing Resources and Environment Engineering Technology Research Institute Co.Ltd.,Nanjing 211599,China)

机构地区：[1]南京工业大学化工学院,江苏南京211816 [2]南京工业大学材料化学工程国家重点实验室,江苏南京211816 [3]南京资环工程技术研究院有限公司,江苏南京211599

出　　处：《高校化学工程学报》2024年第5期762-769,共8页Journal of Chemical Engineering of Chinese Universities

基　　金：国家重点研发计划(2019YFC1905804);江苏省重点研发计划重大科技示范项目(BE2021710);南京工业大学“揭榜挂帅”项目。

摘　　要：针对农药氟虫腈与钛白粉生产过程中副产盐的处置难题,提出以副产磷酸钠为磷源,以副产硫酸亚铁为铁源,制备电池级磷酸铁的工艺路线。采用连续催化氧化的方法将磷酸钠废盐中的亚硫酸钠氧化为硫酸钠,副产硫酸亚铁经过除杂后,用双氧水将硫酸亚铁氧化为硫酸铁,再与上述的磷酸钠反应得到磷酸铁。结果表明:亚硫酸钠的氧化率接近100%;副产硫酸亚铁经化学除杂和水解除杂后,杂质镁、锰、钛的质量分数分别降低至80 mg·kg^(-1)以下,杂质铝则被完全去除;除杂后的硫酸亚铁溶液经双氧水氧化后,硫酸亚铁的氧化率达到100%;制备得到的二水合磷酸铁的各项指标均满足标准HG/T 4701-2021《电池用磷酸铁》的要求。In response to the challenge of disposing by-product salts during pesticide fipronil and titanium dioxide production processes,a process to synthesis battery grade iron phosphate was proposed utilizing by-product sodium phosphate as the phosphorus source and by-product ferrous sulfate as the iron source.Sodium sulfite in sodium phosphate wastes was oxidized to sodium sulfate through a continuous catalytic oxidation method.The purified ferrous sulfate was oxidized to ferric sulfate by hydrogen peroxide,and then reacted with the aforementioned sodium phosphate to yield iron phosphate.The results show that the oxidation rate of sodium sulfite is close to 100%.After chemical purification and hydrolytic purification,the mass fraction of impurities such as magnesium,manganese,and titanium in the by-product ferrous sulfate was reduced to below 80 mg·kg^(-1),and the impurity aluminum was completely removed.Various indicators of the prepared dihydrate iron phosphate meet the requirements outlined in the standard HG/T 4701-2021"Iron phosphate for batteries".

关 键 词：氟虫腈 废盐 钛白粉 硫酸亚铁 磷酸铁 资源化 

分 类 号：TQ138.11[化学工程—无机化工]