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Method for preparing ion liquid in halogenated alkyl imidazole type

A halogenated alkylimidazole-type ionic liquid technology, which is applied in the new preparation field of ionic liquids, can solve the problems of low utilization rate of raw material halogenated hydrocarbons, complex process, etc., and achieve the effect of eliminating environmental problems, simple operation, and improving utilization rate

Inactive Publication Date: 2005-11-16
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the deficiencies and defects of the prior art, the purpose of the present invention is to provide a new preparation method of a halogenated alkylimidazole type ionic liquid, to overcome the complex process of the existing preparation method, the use of a large amount of volatile organic solvents, and the fact that the raw materials are halogenated The shortcomings of low utilization of hydrocarbons, thus providing an efficient and environmentally friendly preparation method for ionic liquids

Method used

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  • Method for preparing ion liquid in halogenated alkyl imidazole type
  • Method for preparing ion liquid in halogenated alkyl imidazole type
  • Method for preparing ion liquid in halogenated alkyl imidazole type

Examples

Experimental program
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Effect test

Embodiment 1

[0021] In a 200ml sealable reactor, 8.212g (0.100mol) of N-methylimidazole and 9.720g (0.105mol) of 1-chlorobutane were sequentially added, and the reaction was stirred at 40°C for 24 hours. After the reaction, the supercritical CO 2 , at a pressure of 7.0 MPa and a temperature of 40 °C, CO 2 Flow rate 1.0L / min, continuous extraction for 4 hours, the product N,N-butylmethylimidazolium chloride salt 14.796g and unreacted reactant 3.136g (containing chlorobutane 1.875g and N-methylimidazole 1.261g) were isolated; The yield based on chlorobutane was 80.7%.

Embodiment 2

[0023] In a 200ml sealable reactor, 12.318g (0.150mol) of N-methylimidazole and 15.135g (0.163mol) of 1-chlorobutane were sequentially added, and the reaction was stirred at 80°C for 12 hours. After the reaction is over, supercritical CO 2 , at a pressure of 20.0 MPa and a temperature of 80 °C, CO 2 Flow rate 1.0L / min, continuous extraction for 4 hours, the product N,N-butylmethylimidazolium chloride salt 24.249g and unreacted reactant 3.204g (containing chlorobutane 2.285g and N-methylimidazole 0.919g) were isolated; The yield calculated by chlorobutane is 84.9%.

Embodiment 3

[0025] In a 200ml sealable reactor, 16.424g (0.200mol) of N-methylimidazole and 19.440g (0.210mol) of 1-chlorobutane were sequentially added, and the reaction was stirred at 150°C for 8 hours. After the reaction is over, supercritical CO 2 , at a pressure of 15.0 MPa and a temperature of 150 °C, CO 2 Flow rate 1.0L / min, continuous extraction for 3 hours, the product N,N-butylmethylimidazolium chloride salt 33.568g and unreacted reactant 2.296g (containing chlorobutane 1.652g and N-methylimidazole 0.644g) were separated; The yield based on chlorobutane is 91.5%.

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Abstract

A process for preparing the haloalkyl imidazole type ionic liquid includes addition reaction between halohydrocarbon and N-alkylimidazole in sealed reactor to generate the ionic liquid composed of the cations of N,N-dimethylimidazole and the anions of halogen, and supercritical Co2 extracting to separate said ionic liquid from unreacted raw material.

Description

technical field [0001] The invention belongs to the technical field of chemical material preparation and relates to a new preparation method of ionic liquid. The method is applicable to the occasion of synthesizing an ionic liquid composed of N, N-dialkylimidazolium cations and halogen anions by using N-alkylimidazoles and halogenated hydrocarbons as raw materials. Background technique [0002] The ionic liquid refers to a substance composed of ions that is liquid at a temperature around room temperature. Due to the unique properties of ionic liquids such as wide liquid range, wide dissolution range, low volatility, high stability, wide electrochemical window, adjustable chemical properties and easy recycling, they are widely used in separation processes, chemical reactions (especially catalytic reactions) and Many satisfactory results have been obtained in the application research of electrochemistry and so on. Therefore, it is considered to be a new environment-friendly g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/06
CPCY02P20/54
Inventor 周震寰王涛邢华斌
Owner TSINGHUA UNIV
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