高纯4，5-二氰基-2-三氟甲基咪唑锂的制备与性能研究

doi:10.19964/j.issn.1006-4990.2023-0144

Abstract

Abstract:

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

CLC Number:

O614.11

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.

Figures/Tables 13

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重结晶溶剂	产品纯度/%	w（不溶物）/10^-6	酸度/ 10^-6	w（水分）/10^-6	w（Cl^-）/10^-6	收率/ %
碳酸二甲酯	99.79	673	208	105	447	78
碳酸甲乙酯	99.76	796	229	114	530	75
碳酸二乙酯	99.81	683	221	102	375	71
乙酸乙酯	99.77	814	151	111	439	65
异丙醚	99.92	278	73	75	41	85
乙醚	99.94	169	93	55	37	83
1，4-二氧六环	99.93	122	245	96	63	80
乙二醇二甲醚	99.96	121	59	27	21	87

m（乙二醇二甲醚）/ m（LiTDI粗品）	产品纯度/ %	产品收率/ %
1.0	99.91	88
1.5	99.95	87
2.0	99.96	87
2.5	99.97	81
3.0	99.98	76

批次	w（主要物质）/%	w（水分）/10^-6	酸度/ 10^-6	w（不溶物）/10^-6	w（Cl）/ 10^-6	w（Na）/ 10^-6	w（K）/ 10^-6	w（Ca）/ 10^-6	w（Mg）/ 10^-6	w（Fe）/ 10^-6
1	99.96	61	55	121	21	3.5	1.4	2.5	0.7	1.8
2	99.95	73	89	133	23	2.2	1.6	2.4	0.6	2.9
3	99.97	47	53	104	15	1.7	0.2	1.2	0.2	0.2
4	99.96	59	79	123	19	2.6	0.9	1.4	0.4	0.7
5	99.98	24	48	101	9	1.1	0.1	1.3	0.1	0.6
6	99.96	62	77	129	20	1.8	0.3	1.5	0.3	0.9

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Study on preparation and properties of high⁃purity lithium 2-trifluoromethyl-4，5-dicyanoimidazole

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