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Method for synthesizing quaternary ammonium salt ionic liquid by microwave radiation heating

A technology of quaternary ammonium salt ions and microwave radiation, which is applied in the field of synthesis of quaternary ammonium salt ionic liquids, can solve the problems of structure damage, inability to react, imidazole ring breakage, etc. The effect of reaction time

Inactive Publication Date: 2012-02-08
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because imidazole ionic liquids are very sensitive to acid and alkali, the addition of alkali will break the imidazole ring and destroy its structure, resulting in the failure of reactions involving acid and alkali

Method used

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  • Method for synthesizing quaternary ammonium salt ionic liquid by microwave radiation heating
  • Method for synthesizing quaternary ammonium salt ionic liquid by microwave radiation heating

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Microwave Continuous Heating Synthesis of N,N-Dimethylallylethanolammonium Chloride

[0033] Add N,N-dimethylethanolamine (22.3g, 0.25mol) and allyl chloride (21.1g, the molar ratio to N,N-dimethylethanolamine is 1.1:1) into a three-necked flask, and put it into a microwave reaction In the vessel, the temperature was set at 55°C, the power was 300W, and the reaction was heated by microwave continuous radiation for 10 minutes. During the reaction, it was condensed and refluxed. After the reaction, the crude product was rotary evaporated to remove excess allyl chloride. At room temperature, 40.6 g of white solid N,N-dimethylallylethanol ammonium chloride was obtained, with a yield of 96%.

Embodiment 2

[0037] Microwave Continuous Heating Synthesis of N,N-Dimethylbutylethanolammonium Chloride

[0038] Add N,N-dimethylethanolamine (22.3g, 0.25mol) and chlorobutane (25.5g, the molar ratio of N,N-dimethylethanolamine is 1.1:1) into a three-necked flask, and put it in the microwave In the reactor, the temperature was set at 60°C, the power was 300W, and the microwave was continuously irradiated to heat and react for 10 minutes. During the reaction, it was condensed and refluxed. After the reaction, the crude product was rotary evaporated to remove excess chlorobutane. At room temperature, 42.7 g of white solid N,N-dimethylbutylethanolammonium chloride was obtained, with a yield of 94%.

Embodiment 3

[0042] Synthesis of N,N-Dimethyloctadecylethanolammonium Chloride by Microwave Continuous Heating

[0043] Add N,N-dimethylethanolamine (22.3g, 0.25mol) and octadecyl chloride (79.5g, the molar ratio to N,N-dimethylethanolamine is 1.1:1) into a three-necked flask, and put it in the microwave In the reactor, the temperature was set at 60°C, the power was 300W, and the reaction was heated by microwave continuous radiation for 8 minutes. During the reaction, condensation was refluxed. After the reaction, the crude product was rotary evaporated to remove excess octadecyl chloride. At room temperature, 85.1 g of white solid N,N-dimethyloctadecylethanolammonium chloride was obtained, with a yield of 90%.

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Abstract

The invention provides a method for synthesizing quaternary ammonium salt ionic liquid by microwave radiation heating, which comprises the following steps: mixing tertiary amine compounds (N,N-dimethylethanolamine, trimethylamine or triethanolamine) and halohydrocarbon compounds (allyl chloride, n-butyl chloride, n-butyl bromide, octadecyl chloride) with a molar ratio of 1:1.05-1:2 under a microwave radiation heating condition, putting the mixture into a microwave reactor to perform a microwave reaction with an adjusted microwave power of 100 W-400 W, a heating temperature of 30 DEG C-80 DEG C, and reaction time of 1 min-15 min so as to obtain a crude product, removing residual halohydrocarbon compounds in the crude product to obtain quaternary ammonium salt ionic liquid with halogens as anions; the halohydrocarbon compounds are chlorinated hydrocarbon compounds or brominated hydrocarbon compounds. The preparation method of the invention is simple, does not require the addition of any solvent except reaction raw materials, and can prepare high-purity quaternary ammonium salt ionic liquid simply, efficiently, rapidly, and economically.

Description

technical field [0001] The invention relates to a synthesis process of quaternary ammonium salt ionic liquid, in particular to a method for synthesizing quaternary ammonium salt ionic liquid by microwave radiation heating. Background technique [0002] Due to the high cost of solvent separation and recovery of organic solvents commonly used in polymerization reactions, and the disadvantages of causing harm to human health and the environment, the further development of solution polymerization is restricted. Therefore, the search for new solvents with high reaction rate, high solubility (increased monomer concentration and production capacity), small chain transfer constant, and easy recycling has attracted great attention from academia and industry. [0003] Ionic liquids are salts that remain liquid at low temperatures (<100°C). Ionic liquid is a liquid composed entirely of ions. It has many excellent properties: high physical and chemical stability, low vapor pressure,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/08C07C215/40C07C209/12C07C211/63
Inventor 陈威李友明万小芳
Owner SOUTH CHINA UNIV OF TECH
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