详细介绍了一种锂离子电池电解质盐双草酸硼酸锂（LiBOB）的新制备方法——乙腈溶剂法. 制备过程采用硼酸、碳酸锂、草酸等作为原料, 首先采用P204萃淋树脂预处理锂源, 后将反应物置于乙腈溶剂中直接反应, 所得产品经过乙二醇二甲醚提纯后即得到产物. 产物通过红外光谱和X射线衍射检测手段定性, 用原子吸收和离子色谱检测手段定量, 证明所制备的LiBOB杂质含量少, 纯度达到99.95%. 并通过热分析证实其热稳定性优于一般商品用LiBOB, 整套实验方法优势明显.
A novel preparation method of lithium bis(oxalato)borate (LiBOB) called acetonitrile solution method was introduced. Lithium source was firstly pretreated by P204 extraction resin. Then Li2CO3 was reacted with H3BO3 and H2C2O4 directly in acetonitrile solution. As-prepared LiBOB was finally purified in ethylene glycol di-methyl ether (C4H10O2). The synthesized LiBOB was characterized by infrared spectrum, X-ray diffraction (XRD) pattern, atomic absorption and ion chromatography. Thermal stability capability of as-synthesized LiBOB was analyzed by differential thermal analysis and thermogravimetry. The results indicate that the as-synthesized LiBOB has higher purity, lower impurity contents and better thermal stability than commercialized LiBOB, the purity of the as-synthesized LiBOB reaches 99.95%.
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