以硝酸铁为原料水热合成电池级磷酸铁的研究  

Hydrothermal Synthesis of Battery Grade Iron Phosphate with Iron Nitrate as Raw Materials

作　　者：谢彦宇 李立平 黄司平 XIE Yanyu;LI Liping;HUANG Siping(Guangdong Guanghua Sci-Tech Co.,Ltd.,Shantou 515000,China)

机构地区：[1]广东光华科技股份有限公司,广东汕头515000

出　　处：《化工技术与开发》2024年第7期1-6,共6页Technology & Development of Chemical Industry

基　　金：广东重点领域研发计划项目(2020B090919003)。

摘　　要：作为合成锂离子电池正极材料磷酸铁锂的一种重要前驱体,电池级磷酸铁的品质受到诸多限制。本研究以硝酸铁为原料,磷酸二氢铵为沉淀剂,通过水热反应与脱水热处理相结合的合成路线,省去氧化过程的同时,引入的杂质离子易分解除去,从而提高了产品纯度。在磷酸浓度为3.0mol·L^(-1)、磷酸二氢铵浓度为0.6 mol·L^(-1)、反应温度80℃、反应时间4h的条件下,合成了D_(50)值为6.243μm的无水磷酸铁颗粒,产率可稳定控制在95%以上。产品的铁磷比为0.970,其中铁含量的平均值为36.20wt.%,磷含量的平均值为20.69wt.%,其他金属杂质的含量均很低,达到了电池级磷酸铁的要求。本方法具有产物纯度高、工艺路线短等优点,对于电池级磷酸铁的工业化生产有一定的参考价值。As an important precursor for the synthesis of lithium iron phosphate for lithium ion batteries cathode,battery-grade iron phosphate were limited by many quality requirements.A synthetic route combining hydrothermal reaction with ferric nitrate as raw material and ammonium dihydrogen phosphate as precipitant with subsequent calcination was proposed in this research.The oxidation process was eliminating while the easily decomposed and removed impurity ions were introducing skillfully,thus improved the purity of the product.Under the experimental conditions of phosphoric acid concentration of 3.0 mol/L,ammonium dihydrogen phosphate concentration of 0.6 mol/L,reaction temperature of 80℃and reaction time of 4h,anhydrous iron phosphate particles with D_(50) value of 6.243μm were synthesized,and the yield was stably controlled above 95%.The iron-phosphorus ratio was 0.970 with the average iron content of 36.20wt%,the average phosphorus content of 20.69 wt%,and a very low content of other metal impurities,which met the requirements of battery-grade iron phosphate.This method showed a merits of high product purity and short process route,which had certain reference significance for industrial production of battery grade iron phosphate.

关 键 词：锂离子电池 正极材料 磷酸铁 电池级 水热合成 

分 类 号：TQ138.11[化学工程—无机化工]