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Preparation method of 4, 5-dicyano-2-trifluoromethyl-imidazolium salt

A technology of trifluoromethyl and dicyano, which is applied in the field of battery materials, can solve problems such as affecting use, affecting subsequent use, and water residue, and achieves the effects of high yield, reduced corrosion, and low water content

Pending Publication Date: 2021-11-02
如鲲(山东)新材料科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of carbonate is likely to cause water residue, which affects its use
[0007] Due to the current preparation method of 4,5-dicyano-2-trifluoromethyl-imidazolium salt is easy to affect its subsequent use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] This embodiment provides a preparation method of 4,5-dicyano-2-trifluoromethyl-imidazolium salt, the specific steps are as follows:

[0039] Add 186.09 g (1 mol ), lithium sulfate 120.9 g (1.1 mol), dimethyl carbonate 400 mL, under the protection of nitrogen, start stirring reaction for 12 h, until the system PH=7, the reaction is complete, filter at 25 °C, remove dimethyl carbonate from the filtrate, add dropwise 600 mL of toluene was crystallized, the wet product was obtained by filtration, and vacuum-dried at 100 °C for 10 h to obtain 181.6 g of dry high-purity 4,5-dicyano-2-trifluoromethyl-imidazole lithium salt with a yield of 94.57% and a purity of 99.95 %, water content 65 ppm, chloride ion content <1 ppm.

Embodiment 2

[0041] This embodiment provides a preparation method of 4,5-dicyano-2-trifluoromethyl-imidazolium salt, the specific steps are as follows:

[0042] 186.09 g (1 mol) of 4,5-dicyano-2-trifluoromethyl-imidazole, Sodium oxalate 268.0 g (2.0 mol), diethylene glycol dimethyl ether 600 mL, start stirring reaction for 4 h under nitrogen protection, until the system pH = 7, the reaction is complete, filter at 25 ° C, the filtrate removes diethylene glycol di Methyl ether, 700 mL of chlorobenzene was added dropwise to crystallize, the wet product was obtained by filtration, and vacuum-dried at 100°C for 10 h to obtain 190.5 g of dry high-purity 4,5-dicyano-2-trifluoromethyl-imidazole sodium salt, which was collected as The yield is 91.55%, the purity is 99.89%, the water content is 56ppm, and the chloride ion content is <1 ppm.

Embodiment 3

[0044] This embodiment provides a preparation method of 4,5-dicyano-2-trifluoromethyl-imidazolium salt, the specific steps are as follows:

[0045] Put 186.09 g (1mol) of 4,5-dicyano-2-trifluoromethyl-imidazole and potassium borate into a 1000ml four-necked round-bottomed flask equipped with an electric stirrer, reflux condenser, thermometer, and airway 264 g (1.5 mol), 800 mL of diethyl carbonate, under nitrogen protection at 100 °C, start stirring reaction for 2 h, until the system pH = 7, the reaction is complete, filter at 25 °C, remove dimethyl carbonate from the filtrate, add 600 mL of diethyl carbonate dropwise Chloromethane was crystallized, and the wet product was obtained by filtration, and vacuum-dried at 100°C for 10 h to obtain 204.7 g of dry high-purity 4,5-dicyano-2-trifluoromethyl-imidazole potassium salt, with a yield of 91.3% and a purity of 99.96% , water content 80 ppm, chloride ion content <1 ppm.

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Abstract

The invention provides a preparation method of 4, 5-dicyano-2-trifluoromethyl-imidazolium salt, and the preparation method comprises the following steps: mixing 4, 5-dicyano-2-trifluoromethyl-imidazole with polybasic acid salt, and carrying out a reaction, so as to obtain the 4, 5-dicyano-2-trifluoromethyl-imidazolium salt. The 4, 5-dicyano-2-trifluoromethyl-imidazolium salt prepared by the preparation method provided by the invention is high in yield and low in water content.

Description

technical field [0001] The invention belongs to the field of battery materials, in particular to a preparation method of 4,5-dicyano-2-trifluoromethyl-imidazolium salt, in particular to a 4,5-dicyano-2- Preparation method of trifluoromethyl-imidazolium salt. Background technique [0002] In recent years, small electronic devices such as mobile power banks, mobile phones, and tablets have been widely used in daily life, and large electric tools such as electric vehicles are also developing rapidly under the promotion of national policies. The demand for secondary batteries will increase. [0003] At present, the lithium secondary battery using lithium reaction as the charge-discharge reaction is the most common and has a wide application prospect. A series of new lithium salts have been synthesized and applied to lithium-ion battery electrolytes in order to solve the above problems. Among them, lithium 4,5-dicyano-2-trifluoromethyl-imidazolium contains less fluorine atoms a...

Claims

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Application Information

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IPC IPC(8): C07D233/90
CPCC07D233/90
Inventor 王广强魏范杰
Owner 如鲲(山东)新材料科技有限公司