Inorganic Chemicals Industry >
Study on preparation and properties of high⁃purity lithium 2-trifluoromethyl-4，5-dicyanoimidazole
Received date: 2023-03-15
Online published: 2024-02-06
Lithium 2-trifluoromethyl-4，5-dicyanoimidazole（LiTDI） with high purity was synthesized by the raw materials of 2-trifluoromethyl-4，5-dicyanoimidazole（TDI） and lithium chloride.The effects of volume ratio of reactants，reaction temperature，reaction time on the crude product yield were investigated，and the effects of recrystallization solvent，amount of solvent，cooling rate，recrystallization time on the product purity and yield were studied.The experimental results showed that after filtration⁃concentration⁃cooling crystallization of the reaction liquid，the crude product yield was 78% at m（DMC）/m（TDI）=2，n（LiCl）/n（TDI）=1，reaction temperature of 45 ℃，reaction time of 5 h，and the product purity was greater than or equal to 99.95% and the yield was 88%，when the recrystallization solvent was dimethoxyethane，m（dimethoxyethane）/m（crude LiTDI）=2，the cooling rate was 3 ℃/h，the recrystallization time was 10 h.In addition，adding LiTDI in electrolyte could significantly improve the performance of battery at room temperature and high temperature.
Key words： LiTDI; TDI; lithium chloride; lithium battery
YANG Shuiyan , YANG Mingxia , XIN Wanwan . Study on preparation and properties of high⁃purity lithium 2-trifluoromethyl-4，5-dicyanoimidazole[J]. Inorganic Chemicals Industry, 2024 , 56(2) : 74 -79 . DOI: 10.19964/j.issn.1006-4990.2023-0144
| 1 | 薛旭金.国内外高性能六氟磷酸锂性能分析［J］.无机盐工业，2014，46（3）：1-4. |
| XUE Xujin.Analysis on performances of high quality lithium hexafluorophosphate in China and abroad［J］.Inorganic Chemicals Industry，2014，46（3）：1-4. | |
| 2 | PAILLET S， SCHMIDT G， LADOUCEUR S，et al.Power capability of LiTDI-based electrolytes for lithium?ion batteries［J］.Journal of Power Sources，2015，294：507-515. |
| 3 | NIEDZICKI L， ?UKOWSKA G Z， BUKOWSKA M，et al.New type of imidazole based salts designed specifically for lithium ion batteries［J］.Electrochimica Acta，2010，55（4）：1450-1454. |
| 4 | WEN Zhipeng， LI Hang， LI Huiyang，et al.Highly stable and robust bi?electrodes interfacial protective films for practical lithium metal batteries［J］.Journal of Power Sources，2021，509：230370. |
| 5 | NOJABAEE M， KüSTER K， STARKE U，et al.Solid electrolyte interphase evolution on lithium metal in contact with glyme?based electrolytes［J］.Small，2020，16（23）：2000756. |
| 6 | SHKROB I A， PUPEK K Z， GILBERT J A，et al.Chemical stability of lithium 2-trifluoromethyl-4，5-dicyanoimidazolide，an electrolyte salt for Li-ion cells［J］.The Journal of Physical Chemistry C，2016，120（50）：28463-28471. |
| 7 | 周旺鹰，陶哲，冯娜娜.一种连续制备 2-三氟甲基-4，5-二氰基咪唑锂盐的方法及反应装置：中国，113277982A［P］.2022-07-05. |
| 8 | 周旺鹰，冯娜娜，陶哲.一种咪唑基含氟锂盐的干燥方法：中国，113354587B［P］.2022-07-05. |
| 9 | 周永妍，周宜海，杨光，等.4，5-二氰基-2-三氟甲基咪唑、其制备中间体及其盐的制备方法：中国，106008262A［P］.2016-10-12. |
| 10 | 陈晓军，张利萍，徐三善.高纯度4，5-二氰基-2-三氟甲基咪唑及其盐的制备方法：中国，104447564A［P］.2016-08-31. |
| 11 | 王广强，魏范杰.一种4，5-二氰基-2-三氟甲基-咪唑盐的制备方法：中国，113582930A［P］.2021-11-02. |
| 12 | 时二波，刘磊，印李达，等.4，5-二氰基-2-三氟甲基咪唑盐的合成方法：中国，113683568A［P］.2021-11-23. |
| 13 | XU Chao， RENAULT S， EBADI M，et al.LiTDI：A highly efficient additive for electrolyte stabilization in lithium?ion batteries［J］.Chemistry of Materials，2017，29（5）：2254-2263. |
| 14 | JANKOWSKI P， ?UKOWSKA G Z， DRANKA M，et al.Understanding of lithium 4，5-dicyanoimidazolate?poly（ethylene oxide） system：Effect of the architecture of the solid phase on the conductivity［J］.The Journal of Physical Chemistry C，2016，120（41）：23358-23367. |
| 15 | RUSHING J C， LEONIK F M， KURODA D G.Effect of solvation shell structure and composition on ion pair formation：The case study of LiTDI in organic carbonates［J］.The Journal of Physical Chemistry C，2019，123（41）：25102-25112. |
| 16 | DRANKA M， JANKOWSKI P， ?UKOWSKA G Z.Snapshots of the hydrolysis of lithium 4，5-dicyanoimidazolate?glyme solvates.impact of water molecules on aggregation processes in lithium?ion battery electrolytes［J］.The Journal of Physical Chemistry C，2018，122（6）：3201-3210. |
/
| 〈 |
|
〉 |