摘要
为了制备高纯二氟磷酸锂产品,以六氟磷酸锂和碳酸锂为原料,研究反应时间、反应温度、六氟磷酸锂与碳酸锂的物质的量比和二氟磷酸锂浓度对产品纯度的影响。实验结果表明,当反应温度为60℃、反应时间为5 h、六氟磷酸锂与碳酸锂的物质的量比为1∶2、二氟磷酸锂浓度为0.95 mol/L时,二氟磷酸锂产品的纯度可达到99.95%,收率可达到55.64%。而且,二氟磷酸锂作为电解液的添加剂,可以有效地改善锂电池的高温、常温循环性能。
In order to prepare LiPO_2F_2 products with high purity,the effects of reaction time,reaction temperature,amountof-substance ratio of lithium hexafluorophosphate to lithium carbonate and concentration of LiPO_2F_2 on the purity of the product were mainly studied by using lithium hexafluorophosphate and lithium carbonate as raw materials.The best conditions were described as following:the reaction temperature was 60 ℃,the reaction time was 5 h,the amount-of-substance ratio of lithium hexafluorophosphate to lithium carbonate was 1 ∶2,and the concentration of LiPO_2F_2 was 0.95 mol/L.Under the best conditions,the purity of LiPO_2F_2 was 99.95% and the recovery was 55.64%. In addition,adding LiPO_2F_2 in electrolyte could effectively improve the performance of battery at high temperature and room temperature.
引文
[1]Tarascon J M,Armand M.Issues and challenges facing rechargeable lithium batteries[J].Nature,2001,414:359-367.
[2]Armand M,Tarascon J M.Building better batteries[J].Nature,2008,451:652-657.
[3]刘海霞.高纯晶体六氟磷酸锂新工艺探讨及市场供需分析[J].无机盐工业,2017,49(7):7-10.
[4]侯红军.中国六氟磷酸锂生产工艺研究及产业化难点剖析[J].无机盐工业,2015,47(12):9-11.
[5]Yang G,Shi J,Shen C,et al.Improving the cyclability performance of lithium-ion batteries by introducing lithium difluorophosphate(Li PO2F2)additive[J].Rsc Advances,2017,7(42):26052-26059.
[6]Hong S,Hong B,Song W,et al.Communication—lithium difluorophosphate as an electrolyte additive to improve the high voltage performance of Li Ni0.5Co0.2Mn0.3O2/graphite cell[J].Journal of the Electrochemical Society,2018,165(2):A368-A370.
[7]Yang B,Zhang H,Yu L,et al.Lithium difluorophosphate as an addi tive to improve the low temperature performance of Li Ni0.5Co0.2Mn0.3O2/graphite cells[J].Electrochimica Acta,2016,221:107-114.
[8]Kim K E,Jang J Y,Park I,et al.A combination of lithium difluorophosphate and vinylene carbonate as reducible additives to improve cycling performance of graphite electrodes at high rates[J].Electrochemistry Communications,2015,61:121-124.
[9]竹原雅裕.二氟磷酸锂、含有二氟磷酸锂的电解液、二氟磷酸锂的制备方法、非水电解液的制备方法、非水电解液以及使用该非水电解液的非水电解质二次电池:中国,101507041[P].2009-08-12.
[10]王海,张品杰,周强.一种二氟磷酸锂的制备方法及其锂离子电池非水电解液:中国,104445133[P].2015-03-25.
[11]贾凤雷,陈效飞,吕蕾,等.一种二氟磷酸锂的制备方法:中国,106829910[P].2017-06-13.