钛白副产物制备电池级磷酸铁及性能研究

Preparation and Properties of Battery Grade FePO₄ from Titanium Dioxide By-Product

摘要: 本文以钛白副产物为铁源，磷酸一铵为磷源，双氧水为氧化剂来合成电池级磷酸铁，并研究陈化时间，反应温度，搅拌速度对磷酸铁性能的影响。利用扫描电子显微镜、X射线衍射分析仪、激光粒度分析仪、电感耦合等离子体发射光谱仪等对制备的磷酸铁形貌、晶体、粒度和杂质元素含量进行表征，采用滴定法测定磷酸铁的铁磷比。实验结果表明，磷酸铁制备过程的最佳实验条件为：反应温度90℃，反应时间2.5 h，搅拌速度35 r/min。在最佳条件下制备的磷酸铁微观形貌均匀，结晶度高，杂质元素含量低，粒度D50 = 5.390，铁磷比 = 0.98。上述性能表征数据均符合HG/T 47041-2014磷酸铁标准。

Abstract: The battery grade iron phosphate was synthesized with titanium dioxide by-product as iron source, monoammonium phosphate as phosphorus source and hydrogen peroxide as oxidant. The effects of aging time, reaction temperature and stirring speed on the performance of iron phosphate were studied. Used SEM, XRD, ICP to study characterizes the morphology, crystal, particle size and impurity element of FePO₄. The iron phosphorus ratio of FePO₄ was determined by titration. The experimental results showed that the best experimental conditions for the preparation of FePO₄ were: reaction temperature 90˚C, reaction time 2.5 h, and stirring speed 35 r/min. The FePO₄ prepared under the optimum conditions has uniform micro morphology, high crystallinity, low impurity element content, particle size D50 = 5.390, and iron phosphorus ratio = 0.98. The above performance characterization data meet the HG/T 47041-2014 iron phosphate standard.