Triazole ionic liquid and its preparation method and application
A technology of ionic liquid and triazole, which is applied in the field of triazole ionic liquid, can solve problems such as easy decomposition, increased internal resistance of capacitors, and reduced capacitance
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[0034] The preparation method of the triazole ionic liquid of one embodiment, comprises the following steps:
[0035] Step S11, under the protection of an atmosphere formed by nitrogen or argon, mix methyltriazole and haloalkane in a molar ratio of 1:1 to 1:1.2, heat to 60°C to 80°C, stir and react for 48 to 72 hours, and react After the liquid was cooled, it was washed three times with ethyl acetate, and the washed product was vacuum-dried to obtain a purified alkyl triazole halide.
[0036] Among them, haloalkane is methoxyethoxychloromethane or methoxyethoxymethyl bromide The washed product was vacuum-dried at 80° C. for 48 h to obtain alkyl triazole halides.
[0037] It can be understood that the reaction time is not limited to 48 to 72 hours, as long as the reaction between the methyltriazole and the alkyl halide is complete; the reaction between the methyltriazole and the alkyl halide is not limited to being carried out under the protection of an atmosphere formed by...
Embodiment 1
[0063] This example prepares 4-methoxyethoxymethyl-1-methyltriazole tetrafluoroborate:
[0064] Into a 250mL flask were added (83g, 1mol) N-methyltriazole and (136.4g, 1.1mol) methoxyethoxychloromethane. in N 2 Under the protection of atmosphere, the temperature was raised to 60-80°C, and the reaction was stirred for 48-72h. Let stand to cool, and wash three times with ethyl acetate. Drying in vacuo at 80°C gave a pale yellow solid with a yield of 83%.
[0065] Add (103.5g, 0.5mol) 4-methoxyethoxymethyl-1-methyltriazole chloride, (55g, 0.5mol) NaBF in the 500mL flask 4 And 100mL deionized water, stirred at room temperature for 8-24h. After the reaction was completed, the mixture was extracted three times with 250 mL of dichloromethane, and the extracts were combined. Then back-extract with 60 mL of deionized water each time until saturated with AgNO 3 The aqueous solution was titrated until no precipitation occurred in the aqueous phase. After the dichloromethane phase ...
Embodiment 2
[0069] This example prepares 4-methoxyethoxymethyl-1-methyltriazole hexafluorophosphate:
[0070] Into a 250mL flask were added (83g, 1mol) N-methyltriazole and (184.8g, 1.1mol) methoxyethoxybromethane. in Ar 2 Under the protection of atmosphere, the temperature was raised to 60-80°C, and the reaction was stirred for 48-72h. Let stand to cool, and wash three times with ethyl acetate. Drying in vacuo at 80°C gave a light yellow solid with a yield of 87%.
[0071] In the 500mL flask, add (0.5mol) 4-methoxyethoxymethyl-1-methyltriazole bromide, (92g, 0.5mol) KPF 6 And 150mL deionized water, stirred at room temperature for 8-24h. After the reaction was completed, the mixture was extracted three times with 250 mL of dichloromethane, and the extracts were combined. Then back-extract with 60 mL of deionized water each time until saturated with AgNO 3 The aqueous solution was titrated until no precipitation occurred in the aqueous phase. After the dichloromethane phase was conc...
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