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Environmental protection Method for synthesizing room temperature ion liquid

A technology of room temperature ionic liquid and synthesis method, which is applied in the field of green synthesis of room temperature ionic liquid, can solve the problems of unsuitable large-scale synthesis of room temperature ionic liquid, difficult control of reaction conditions by microwave method, and a large amount of organic solvents, and achieves environmental friendliness and product quality. Good, high reaction yield effect

Inactive Publication Date: 2004-09-01
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest disadvantage of this method is that it needs to use a large amount of volatile organic solvents, which is easy to cause environmental pollution.
In order to avoid the pollution of organic solvents to the environment, Namboodiri and Varma have successively studied the non-solvent synthesis of 1,3-dialkylammonium halide and 1,3-dialkyltetrafluoroborate room temperature ionic liquids promoted by microwave technology. method (Chem.Commun.2001,643-644; Tetrahedron Lett.2002,43,5381-5383), yet, this method requires special equipment, is not suitable for realizing large-scale synthetic room temperature ionic liquid; In addition, the reaction condition of microwave method is not easy Control, the heating effect of microwave and the action of electric field can easily cause overheating of reaction materials and affect product quality

Method used

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  • Environmental protection Method for synthesizing room temperature ion liquid
  • Environmental protection Method for synthesizing room temperature ion liquid
  • Environmental protection Method for synthesizing room temperature ion liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a 100mL three-necked flask, add 18.4g potassium hexafluorophosphate, 19.3g 1-bromooctane, 8.2g N-methylimidazole and 20.0g 1-n-octyl-3-methylimidazolium hexafluorophosphate ion Liquid, stirred at 135°C for 5 hours. After the reaction was completed, 25 mL of water was added, stirred thoroughly, and left to separate the water phase. The ionic liquid phase was washed with 20 mL×3 water for 3 times, and then the residual water was removed under reduced pressure to obtain 48.4 g of 1-n-octyl-3- Methyl hexafluorophosphate ionic liquid, 28.4g of ionic liquid was newly generated in the actual reaction, and the yield was 83.5%.

Embodiment 2

[0021] In a 50mL three-necked flask, sequentially add 11.0g sodium fluoroborate, 14.0g 1-chlorobutane, 9.6g 1,2-dimethylimidazole and 20.0g 1-n-butyl-2,3-dimethylimidazole Tetrafluoroborate ionic liquid, stirred and reacted at 80°C for 35 hours. After the reaction, transfer the reaction solution to a 150mL flask, add 40mL of water, stir thoroughly, then extract the ionic liquid in the water phase with 30mL×5 dichloromethane for 5 times, combine the dichloromethane extracts, and distill to remove the solvent , 39.5g of 1-n-butyl-2,3-dimethylimidazolium tetrafluoroborate ionic liquid was obtained, and 19.5g of ionic liquid was newly generated by the actual reaction, with a yield of 81.3%.

Embodiment 3

[0023] In a 100mL three-necked flask, add 9.4g lithium fluoroborate, 17.9g 2-bromoheptane, 8.2g N-methylimidazole and 25.0g 1-(1-methylhexyl)-3-methylimidazolium tetrafluoro Borate ionic liquid, stirred and reacted at 100°C for 12 hours. After the reaction was completed, 25 mL of water was added, stirred thoroughly and allowed to stand to separate the water phase. The ionic liquid phase was washed with 20 mL×3 water for 3 times, and then the residual water was removed under reduced pressure to obtain 48.3 g of 1-(1-methylhexyl) - 3-methylimidazolium tetrafluoroborate ionic liquid, 23.3 g of ionic liquid was newly generated in the actual reaction, and the yield was 86.9%.

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Abstract

The invention relates to an environmental friendly method for synthesizing ambient temperature ionic liquid, wherein corresponding destination product is utilized as reaction agent, and pyridine or N-alkyl glyoxaline or 1,2-dialkyl glyoxaline, alkylogen and fluorine containing salt are used as raw material to synthesizing ambient temperature ionic liquid at normal atmosphere by continuation method or one step method, which comprises alkyl pyridine positive ions or 1,3-dialkyl glyoxaline positive ions, or 1,2,3-trialkyl glyoxaline positive ions and negative ions containing fluorine.

Description

technical field [0001] The invention relates to a green synthesis method of room temperature ionic liquid. This method is suitable for using pyridine or N-alkylimidazole or 1,2-dialkylimidazole and halogenated alkanes and fluorine-containing salts as raw materials to synthesize alkylpyridinium cations or 1,3-dialkylimidazolium cations or 1,2 , In the case of a room temperature ionic liquid composed of 3-trialkylimidazolium cations and fluorine-containing anions. Background technique [0002] Room temperature ionic liquids, also known as "designer solvents", refer to substances composed of ions that are liquid at or near room temperature. Due to the unique properties of room temperature ionic liquids such as wide liquid range, wide dissolution range, zero vapor pressure, good stability, adjustable acidity and alkalinity, wide electrochemical window and easy recycling, they are widely used in separation processes, chemical reactions (especially catalytic Reaction) and electr...

Claims

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Application Information

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