无机盐工业
主管:中海油天津化工研究设计院有限公司
主办:中海油天津化工研究设计院有限公司
   中海油炼油化工科学研究院(北京)有限公司
   中国化工学会无机酸碱盐专业委员会
ISSN 1006-4990 CN 12-1069/TQ
研究与开发

水相法制备双乙二酸硼酸锂的中试工艺研究

  • 刘艳蕊 ,
  • 宋从从 ,
  • 石桂珍 ,
  • 王坤
展开
  • 1.潍坊工程职业学院应用化学与食品药品学院,山东潍坊 262500
    2.中海油天津化工研究设计院有限公司
刘艳蕊(1981— ),女,硕士,讲师,研究方向为精细化工;E-mail: liuyanrui27@163.com

收稿日期: 2020-04-29

  网络出版日期: 2020-11-24

基金资助

潍坊工程职业学院2019年度科研课题资助项目

The study of double oxalate lithium borate preparation technology by aqueous phase method

  • Yanrui Liu ,
  • Congcong Song ,
  • Guizhen Shi ,
  • Kun Wang
Expand
  • 1. Collegel of Applied Chemistry and Food and Drug,Weifang Engineering College,Weifang 262500,China
    2. CenerTech Tianjin Chemical Research and Design Institute Co.,Ltd.

Received date: 2020-04-29

  Online published: 2020-11-24

摘要

以水相法制备双乙二酸硼酸锂(LiBOB)。研究了中试条件下的反应物料比、反应温度、反应时间、析晶溶剂加入量对产品质量的影响,所得产品利用FTIR、TG-DSC和XRD进行了确认,目前中试装置已实现10 t/a的生产规模。实验结果表明,较优工艺条件为:物料比(草酸、硼酸、碳酸锂的物质的量比)为4∶2∶1.1,反应温度为80 ℃,反应时间为8 h,在浓缩析晶过程中浓缩比(蒸发溶剂占总溶剂的质量比)为80%左右,析晶剂加入量为产品质量的4倍。干燥采用动态干燥方式,干燥时间为8 h。经过分析,该工艺制备的产品质量超过市售产品水平。

本文引用格式

刘艳蕊 , 宋从从 , 石桂珍 , 王坤 . 水相法制备双乙二酸硼酸锂的中试工艺研究[J]. 无机盐工业, 2020 , 52(10) : 100 -105 . DOI: 10.11962/1006-4990.2019-0605

Abstract

The double oxalate lithium borate(LiBOB) was prepared by aqueous-phase method.The effect of material ratio,reaction temperature,reaction time and amount of crystallization solvent on the product quality under the condition of pilot test was studied.The result of products was confirmed by FTIR,TG-DSC and XRD.The pilot plant had achieved a production scale of 10 t/a at present.The experimental results showed the optimum operating parameters which were material ratio(the amount-of-substance ratio of oxalic acid to lithium carbonate to boric acid) of 4∶2∶1.1,reaction temperature of 80 ℃,reaction time of 8 h,the concentration amount(the mass ratio of residual solvent to total solvent mass) of about 80% in the process of concentration and crystallization,and the addition amount of crystallization agent of 4 times of the product mass.The dynamic drying was adopted for 8 h.After analysis,the quality of the product prepared by this process exceeded the level of the market products.

参考文献

[1] Fan Lizhen, Xing Taofeng, Rafi Awan. Studies on lithium bis(oxalato)-borate/propylene carbonate-based electrolytes for Li-ion batteries[J]. Ionics, 2011,17(6):491-494.
[2] 王艳菊, 乔庆东, 李琪, 等. 双乙二酸硼酸锂的合成及性能研究[J]. 化工新型材料, 2015,43(10):193-195.
[3] 平平. 锂离子电池热失控与火灾危险性分析及高安全性电池体系研究[D]. 合肥:中国科学技术大学, 2014.
[4] 邓凌峰, 陈洪, 魏银烨. 锂离子电池电解质锂盐双乙二酸硼酸锂的制备与性能[J]. 材料导报, 2009,23(S1):295-298.
[5] 宋洋, 赵连海, 梁子雷, 等. 双乙二酸硼酸锂在液态电解质中的研究进展[J]. 无机盐工业, 2009,41(10):11-14.
[6] 赵本好. 一种应用于电池电解液中环保型添加剂的性能研究[J]. 电池工业, 2017,21(3):9-11.
[7] 李世友, 马培华, 滕祥国, 等. 锂离子电池电解质的新型锂盐——双乙二酸硼酸锂[J]. 化学进展, 2007(5):695-699.
[8] Swiderska-Mocek A, Naparstek D. Physical and electrochemical properties of lithium bis(oxalate)borate-organic mixed electrolytes in Li-ion batteries[J]. Electrochimica Acta, 2016,204:69-77.
[9] Ulrich Wietelmann,Uwe Lischka,Marion Wegner, Lithium bisox alatoborate,the production thereof and its use as a conducting salt:US,6506516B1[P]. 2003-01-14.
[10] 张玥, 袁莉, 刘锦平, 等. 锂离子电池用双草酸硼酸锂的固相合成[J]. 无机盐工业, 2011,43(4):42-44.
[11] 陈姚, 杨倩韵, 于欣伟, 等. 两步法合成锂离子电池用双草酸硼酸锂[J]. 电池, 2016,46(5):251-254.
文章导航

/