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Method for preparing ionic liquid with anion being as ion in halogen family

A technology of ionic liquid and anion, applied in the field of ionic liquid preparation, can solve the problems of long reaction time, low conversion rate, affecting product quality, etc., achieve the effect of reducing the amount of solvent used, reducing recycling costs, and improving reaction efficiency

Inactive Publication Date: 2007-12-26
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] (1) The reaction time is long, and the reaction often requires reflux heating for more than 24 hours, and the conversion rate is low
[0008] (2) The method of excessive halogenated hydrocarbons is used to increase the reaction conversion rate, which increases the amount of solvent used for product washing and purification and the number of washings, and the cost rises
Due to the use of high-power ultrasonic treatment in this method, the reaction is too violent, which affects the quality of the product and increases the cost of product purification.

Method used

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  • Method for preparing ionic liquid with anion being as ion in halogen family
  • Method for preparing ionic liquid with anion being as ion in halogen family
  • Method for preparing ionic liquid with anion being as ion in halogen family

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Add 41.055g (0.500mol) of N-methylimidazole and 46.300g (0.500mol) of n-chlorobutane successively in a 250ml pressurized and airtight reaction kettle, stir at room temperature to mix them uniformly and pass into N 2 After 5 minutes, heat the reaction kettle containing the reaction mixture to 85°C, control the pressure in the kettle to 0.12MPa, stop stirring after 8 hours of reaction, release the pressure in the kettle to normal pressure, and take out the reaction after the reactants are cooled to room temperature. The product was extracted 3 times with 20ml of ethyl acetate, and then distilled under reduced pressure at 80°C for 0.5h to obtain 85.695g of ionic liquid of 1-butyl 3-methylimidazolium chloride salt, the product calculated by N-methylimidazole The rate is 98.1%.

Embodiment 2

[0036] Add 41.055g (0.500mol) of N-methylimidazole and 38.648g (0.505mol) of allyl chloride successively in a 250ml pressurized and airtight reaction kettle, stir and add dropwise at room temperature to make it mix uniformly and pass into N 2 After 25 minutes, heat the reaction kettle containing the reaction mixture to 70°C, control the pressure inside the kettle to 0.16MPa, stop stirring after 0.5 hours of reaction, release the pressure inside the kettle to normal pressure, and take out the reaction after the reactants are cooled to room temperature. The product was extracted 3 times with 25ml of ethyl acetate, and then distilled under reduced pressure at 40°C for 0.8h to obtain 74.164g of ionic liquid of 1-allyl 3-methylimidazolium chloride salt, calculated as N-methylimidazole The yield was 93.5%.

Embodiment 3

[0038] Add 41.055g (0.500mol) N-methylimidazole and 68.515g (0.500mol) n-butane bromide successively in a 250ml pressurized and airtight reactor, stir at room temperature to make it evenly mixed and pass into N 2After 5 minutes, heat the reaction kettle containing the reaction mixture to 110°C, control the pressure in the kettle to 0.2MPa, stop stirring after 2 hours of reaction, release the pressure in the kettle to normal pressure, and take out the reaction after the reactants are cooled to room temperature. The product was extracted 3 times with 56ml of ethyl acetate, and then distilled under reduced pressure at 75°C for 1.2h to obtain 103.763g of ionic liquid of 1-butyl 3-methylimidazolium bromide. The rate is 94.7%.

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Abstract

This invention relates to a method for preparing an ionic liquid with halogen anions. The method comprises: (1) uniformly mixing compound (I) and halogenated hydrocarbon (II) at a mol. ratio of 1:(1.0-1.05) at normal temperature; (2) adding into a reaction kettle, reacting at room temperature to 150 deg.C under 0.105-0.25 MPa for 0.5-20 h, recovering the pressure to normal pressure after the reaction, cooling, extracting with 1 / 5-4 / 5 volume ethyl acetate for 2-3 times, and vacuum-distilling at 40-80 deg.C for purification. The method has such advantages as rapid reaction, short time and low cost, and is environmentally friendly. The prepared ionic liquid can be used as the solvent for organic reactions and polymerizations, and in chemical separation and electrochemical field.

Description

technical field [0001] The invention belongs to the technical field of ionic liquid preparation, in particular to a preparation method of an ionic liquid whose anions are halogen ions. Background technique [0002] Compared with traditional solvents, room temperature ionic liquids have low melting point, high boiling point, non-volatile, exist in liquid state in a wide temperature range, and have good thermal stability; they can be changed by selecting the appropriate combination of anions and cations Its physical and chemical properties are good solvents for many organic, inorganic and polymer materials. As a green solvent, ionic liquids are widely used in the fields of electrochemistry, organic synthesis, catalysis and separation, and are also good solvents for many polymer polymerization reactions and processing. Therefore, it is considered as a new environment-friendly solvent with broad prospects in green synthesis and clean production. [0003] The preparation method...

Claims

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Application Information

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IPC IPC(8): C07D233/58C07D231/12C07D213/20C07C211/63C07C215/40C07F9/54
Inventor 张玉梅王华平张红燕刘崴崴王强华
Owner DONGHUA UNIV
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