Water-soluble ion liquid synthesizing method

An ionic liquid and water-soluble technology, applied in chemical instruments and methods, dissolution, chemical/physical processes, etc., can solve the problems of process environment toxicity, shortened reaction time, high process cost, etc., and achieve low process cost and cost reduction effect

Inactive Publication Date: 2005-02-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (2) process cost is high if the second step reaction carries out displacement reaction with silver salt in alcoholic water, and reaction time is short, and residual halide ion removal effect is good, but expense is higher;
[0005] (3) The safety of the process is poor. If the second-step reaction is to carry out the displacement reaction with lead salt in alcoholic water, or directly carry out the displacement reaction with acid, the reaction time can also be shortened, but the process is difficult to control the poisoning of the environment.

Method used

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  • Water-soluble ion liquid synthesizing method
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  • Water-soluble ion liquid synthesizing method

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Example 1 1-butyl 3-methylimidazolium bromide

[0019] Take 1mol each of methylimidazole and bromo-n-butane and add it to a 250ml beaker. The 250ml beaker is covered with a 500ml beaker, and an appropriate amount of water is added inside to make a water bath. The temperature of the water bath is not higher than 80°C. Ultrasonic treatment was performed under the ultrasonic condition of 750W, 99 times per round, each working time was 4 seconds, and the rest time was 5 seconds. After 5 rounds, the liquid in the beaker became clear and transparent, slightly pale yellow. After the liquid was cooled, 200 ml of ethyl acetate was added to extract twice to remove unreacted products. The reaction product was vacuum-dried at 80° C. for 6 hours to obtain about 180 ml of product.

Embodiment 2

[0020] Example two 1-butyl 3-methylimidazolium bromide

[0021] Take 0.2 mol of methylimidazole and 0.2 mol of n-bromobutane and put them into a 100ml beaker. The 100ml beaker is covered with a 250ml large beaker, and an appropriate amount of water is added inside as a water bath. The temperature of the water bath is controlled at 20°C to 60°C. Ultrasonic treatment was performed under the ultrasonic condition of 750W, 99 times per round, each working time was 4 seconds, and the rest time was 5 seconds. After 4 rounds, the liquid in the beaker became clear and transparent. After the liquid was cooled, 70 ml of ethyl acetate was added to extract twice to remove unreacted products. The reaction product was vacuum-dried at 80° C. for 6 hours to obtain about 35 ml of product.

Embodiment 3

[0022] Example three 1-butyl 3-methylimidazolium bromide

[0023] Take 0.3 mol of methylimidazole and 0.33 mol of n-bromobutane and put them into a 100ml beaker. The 100ml beaker is covered with a 250ml large beaker, and an appropriate amount of water is added inside as a water bath. The temperature of the water bath is controlled at 30°C to 80°C. Ultrasonic treatment was performed under the ultrasonic condition of 750W, 99 times per round, each working time was 4 seconds, and the rest time was 5 seconds. After 4 rounds, the liquid in the beaker became clear and transparent. After the liquid was cooled, 100 ml of ethyl acetate was added for extraction three times to remove unreacted products. The reaction product was vacuum-dried at 80° C. for 8 hours to obtain about 50 ml of product.

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Abstract

The invention discloses an approach of composing a kind of water soluble ion liquor. Using ultrasonic wave cell smash instrument of 740-760W to process mixed liquor of methylimidazole and bromo carbons whose mol ratio is 1:1.0-1:1.1. The whole reaction is conducted in water bath of 20-80deg.C. Cool after 0.5-1 hour. Use ethyl acetate in same volume to extract for 2-3 times. Obtain water soluble ion liquor after vacuum drying under 60-80deg.C for 6-8 hours. Molecular formula of the production is [RCH3IM] X, thereinto, R for paraffin base of C4, X for Br. The invention has a simple operation and low cost with a short process time. There are little poisonous matters produced at process of producing. Impurities in production are effectively controlled. The production also can serve as medium in catalytic reaction.

Description

technical field [0001] The invention relates to a method for synthesizing a water-soluble ionic liquid. In the method, the ionic liquid is synthesized by means of ultrasonic heating, and the required ionic liquid is purified by dichloromethane and water extraction and stripping. The invention belongs to the technical field of new chemical materials and their preparation. Background technique [0002] In recent years, ionic liquids have attracted widespread attention as green solvents. In addition to being able to replace conventional organic solvents as reaction media in chemical reactions, many enzymes have recently been found to have good catalytic properties in ionic liquids. The steps of the traditional two-step synthesis of ionic liquids are: mixing the raw materials methylimidazole or alkylpyridine with haloalkanes, and heating under reflux to generate ionic liquids such as alkylimidazolium salts or alkylpyridinium salts with halide ions as anions. Then add the metal ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K23/32
Inventor 梅乐和王永泽姚善泾
Owner ZHEJIANG UNIV
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