摘要
详细介绍了一种锂离子电池电解质盐LiBF4的全新制备方法乙腈溶剂法。制备过程采用氟硼酸钠加热分解产生BF3,BF3和LiF在CH3CN溶剂中反应,经过滤冷却结晶得到产物。其中中间产物BF3的制备过程采用GC-MS-SIM法监测,确定条件为氟硼酸钠在500℃下加热3h。粗品LiBF4经有机溶剂提纯后,通过红外和XRD检测手段定性,用原子吸收和离子色谱检测手段定量,证明产物LiBF4杂质含量少,并通过热分析证实其热稳定性优于LiPF6,整套实验方法优势明显。
A LiBF4 electrolyte was prepared by an acetonitrile solvent method. The preparation process includes the thermal decomposition of NaBF4 to produce BF3, the reaction of BF3 with LiF in acetonitrile solvent, and the product recovery by filtration, cooling and crystallization. The intermediate BF3 for the process was monitored by GC-MS (in Selected Ion Monitoring (SIM) mode) by heat treatment of NaBF4 at 500 ℃ for 3 h. The product after purification in organic solvent was characterized by FTIR, XRD, AAS, Ion ehromatography(IC) and TG-DTG. The results indicate that the product obtained by the present method is with less impurity and better thermal stability than conventional LiPF6.
出处
《无机化学学报》
SCIE
CAS
CSCD
北大核心
2009年第1期31-36,共6页
Chinese Journal of Inorganic Chemistry
基金
国家重点基础研究发展计划(973计划)(No.2007CB613607)资助项目
关键词
LiBF4
乙腈溶剂法
制备
表征
lithium tetra-fluoride borate
acetonitrile organic reagent method
preparation
characterization