摘要
以六甲基二硅氮烷(HMDS)和硼酸为原料合成了锂离子电池电解液新型添加剂三(三甲基硅烷)硼酸酯(TMSB),采用气相色谱、气质联用等测试手段对合成反应机理与最优化工艺条件进行了研究。研究中发现硼酸脱水以及HMDS水解是最主要的副反应,对产品收率有重要影响。在优化的反应条件下,n(HMDS)∶n(硼酸)=5∶4,于80℃反应6h得到粗产品,过滤后滤液经减压蒸馏可得到高纯度产品。与传统方法相比,在优化条件下价高的HMDS得到更充分利用,产品产率(以HMDS计)可提高到70%以上。
Tris(trimethylsilyl) borate(TMSB), a new additive for lithium ion battery electrolyte, was synthesized from hexamethyldisilazane(HMDS)and boric acid. Reaction mechanism and the optimal process conditions were studied by GC and GC-MS. The research revealed that boric acid dehydration and HMDS hydrolysis were the main side reactions which greatly affected the yield. The optimal condition was n(HMDS) : n(boric acid)=5 : 4,80℃ as reaction temperature for 6h,then the filtrate was easily distilled under reduced pressure to obtain high purity product. Expensive HMDS was fully used and the yield was increased to more than 70% (according to HMDS)as compared to traditional method.
出处
《化工新型材料》
CAS
CSCD
北大核心
2014年第10期48-49,56,共3页
New Chemical Materials
基金
高等学校博士学科点专项科研基金(20120171110043)
2014年黄埔区科技计划项目(201423)