两步法合成锂离子电池用双草酸硼酸锂  

Synthesizing lithium bis( oxalate) borate for Li-ion battery via two-step method

作　　者：陈姚[1] 杨倩韵 于欣伟[1] 陈胜洲[1] CHEN Yao YANG Qian-yun YU Xin-wei CHEN Sheng-zhou(School of Chemistry and Chemical Engineering, Guangzhou University, Guangzhou, Guangdong 510006, China)

机构地区：[1]广州大学化学化工学院,广东广州510006

出　　处：《电池》2016年第5期251-254,共4页Battery Bimonthly

基　　金：广东省科技计划项目(2013B01405015);广州市高校科研项目(1201420606);广州市科技计划项目(20150903005)

摘　　要：以草酸、硼酸和氢氧化锂为原料,采用两步法合成锂离子电池用电解质锂盐双草酸硼酸锂（LiBOB）。通过正交实验确定双草酸硼酸酯（HBOB）的最佳合成条件为：n（草酸）∶n（硼酸）=2.2∶1.0,反应温度90℃,反应时间4 h。由单因素实验确定合成LiBOB的最佳工艺条件为：n（HBOB）∶n（Li OH）=1.0∶0.6、中和反应温度100℃,中和反应时间4 h。在此条件下,LiBOB的转化率为83.61%。用XRD、红外光谱（FT-IR）、核磁共振碳谱（NMR）13C-NMR、1H-NMR和热重（TG-DTG）测试等对合成样品进行分析。合成的LiBOB纯度较高,且热稳定性较好。在50℃下,使用Li PF6＋LiBOB混合电解液的052545型软包装电池以1 C在3.00~4.35 V循环50次,容量衰减率为7.6%,低于使用纯Li PF6电解液的电池。Lithium electrolyte salts double oxalate lithium borate （LiBOB） used for Li-ion battery was synthesized via two-step method with oxalic acid, boric acid and lithium hydroxide as raw materials. By orthogonal experiment, the best synthesizing conditions for bisoxalatoborate ester （HBOB） were as follows ： n （oxalicacid） ： n （ boric acid） = 2. 2： 1.0, reaction temperature 90℃, reaction time 4 h. By single factor experiment,the best synthesis conditions of LiBOB were as follows：n（ HBOB）：n（LiOH） = 1.0： 0. 6, neutralization reaction temperature 100℃, neutralization reaction time 4 h. The conversion rate of LiBOB was 83.61% under the condition. The synthesized samples were characterized by XRD,infrared spectroscopy（ FT-IR）, t3C-nuclear magnetic resonance （NMR）, 1H-NMR and thermogravimetric（TG-DTG） tests. The synthesized LiBOB had higher purity and better thermal stability. At 50 ℃, after 50 cycles with 1 C in 3. 00 -4. 35 V, the capacity fading rate of 052545 type soft pack battery using LiPF6 ＋ LiBOB mixed electrolyte was 7. 6% ,lower than that of pure LiPF6 electrolyte.

关 键 词：锂离子电池 合成 两步法 电解质 双草酸硼酸锂 

分 类 号：TQ261.1[化学工程—有机化工] TM912[电气工程—电力电子与电力传动]