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Process for preparing room temperature ionic liquid

A technology of room temperature ionic liquid and ions, applied in the direction of organic chemistry, etc., to achieve mild reaction conditions, good product quality, and environmental friendliness

Inactive Publication Date: 2004-08-18
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcoming of existing synthetic method, provide a kind of preparation method of room temperature ionic liquid that does not need to use volatile organic solvent in the reaction process, easy to operate, environment friendly

Method used

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  • Process for preparing room temperature ionic liquid
  • Process for preparing room temperature ionic liquid
  • Process for preparing room temperature ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] In a 50mL three-necked flask, add 18.4g potassium hexafluorophosphate, 17.5g 1-n-butyl-3-methylimidazole ammonium chloride and 20.0g 1-n-butyl-3-methylimidazole hexafluorophosphate. Ionic liquid, stirred and reacted at 80°C for 10 hours. At the end of the reaction, the reaction solution was washed three times with 20 mL×3 water, and then the residual water was removed under reduced pressure to obtain 46.0 g of colorless 1-n-butyl-3-methylhexafluorophosphate ionic liquid. The actual reaction 26.0 g of ionic liquid was newly produced, with a yield of 91.5%.

Embodiment 2

[0014] In a 150mL three-necked flask, 11.0g of ammonium fluoroborate, 21.6g of N-butylpyridinium ammonium bromide and 30.0g of N-butylpyridine tetrafluoroborate ionic liquid were added in sequence, and the reaction was stirred at 50°C for 12 hours. . After the reaction is over, add 30 mL of water and stir well. Then, the ionic liquid in the water phase is extracted three times with 40 mL×3 dichloromethane, the dichloromethane extracts are combined, and the solvent is removed by distillation to obtain 50.7 g of almost colorless N-butylpyridine tetrafluoroborate ionic liquid, 20.7g of ionic liquid was newly produced by actual reaction, and the yield was 92.8%.

Embodiment 3

[0016] In a 150mL three-necked flask, add 22.1g silver trifluoroacetate, 19.1g 1-ethyl-3-methylimidazole ammonium bromide and 40.0g 1-ethyl-3-methylimidazole trifluoroacetate ion in sequence Liquid, stir and react at 25°C for 1 hour. After the reaction is over, add 30 mL of dichloromethane, stir well, filter to remove the silver bromide, wash the filter cake with 10 mL×3 dichloromethane three times, then combine the dichloromethane solutions, and remove the solvent under reduced pressure to obtain 62.2 g Colorless 1-ethyl-3-methylimidazole trifluoroacetate ionic liquid, 22.2g of ionic liquid was newly produced by actual reaction, and the yield was 99.1%.

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Abstract

The present invention relates to the preparation process of room temperature ionic liquid. The present invention features that the room temperature ionic liquid comprising alkyl pyridine cation or alkyl imidazole cation and fluoride anion is prepared with the object product or room temperature ionic liquid as reaction medium and with alkyl pyridine-ammonium halide or alkyl imidazole-ammonium halide and fluoride salt as material. The process is simple in operation, mild in reaction, high in product quality and environment friendly.

Description

Technical field [0001] The invention relates to a preparation method of room temperature ionic liquid. The method is suitable for preparing room temperature ionic liquids composed of alkylpyridine cations or alkylimidazole cations and fluorine-containing anions by using alkylpyridine ammonium halide or alkylimidazole ammonium halide and fluorine-containing salt as raw materials. Background technique [0002] Room temperature ionic liquid, also known as "designer solvent", refers to a substance composed of ions that is liquid at or near room temperature. Room temperature ionic liquids are another class of green solvent systems after water and supercritical carbon dioxide, and have broad application prospects in separation processes, chemical reactions and electrochemistry. [0003] Room temperature ionic liquids composed of alkyl pyridine cations, alkyl imidazole cations and fluorine-containing anions are the most widely used room temperature ionic liquids currently in research. T...

Claims

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Application Information

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IPC IPC(8): C07D211/00C07D233/00
Inventor 许丹倩刘宝友徐振元
Owner ZHEJIANG UNIV OF TECH