Method of continuously synthesizing ionic liquid at room temperature

A technology of room temperature ionic liquid and synthesis method, applied in the field of continuous synthesis of room temperature ionic liquid, can solve the problems of difficult control of reaction conditions by microwave method, unspecified ionic liquid synthesis method, unfavorable industrialization promotion and application, etc., and is beneficial to large-scale industrialization. Production, elimination of separation and purification steps, and good product quality

Inactive Publication Date: 2007-10-24
NANJING UNIV OF SCI & TECH
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  • Abstract
  • Description
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  • Application Information

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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, TetrahedronLett.2002,43,5381-5383), yet, the reaction condition of microwave m

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  • Method of continuously synthesizing ionic liquid at room temperature
  • Method of continuously synthesizing ionic liquid at room temperature

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Experimental program
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Embodiment 1

[0021] In a 100 mL three-necked flask, add 13.7 g of n-bromobutane and 8.2 g of N-methylimidazole, and stir and react at 70-80° C. for 2 hours. Another 18.4 g of potassium hexafluorophosphate was added and stirring was continued for 2 hours. After the reaction was completed, 20 mL of water was added, and the water phase was left to stand to separate after fully stirring. The ionic liquid phase was washed three times with 20 mL×3 water respectively, and the residual water was removed under reduced pressure to obtain 26.4 g of alkylimidazole hexafluorophosphate ionic liquid. Yield 92.9%

Embodiment 2

[0023] In a 100 mL three-necked flask, 15.1 g of n-pentane bromide and 8.2 g of N-methylimidazole were added, and the reaction was stirred at 80° C. for 2 hours. Another 12.6 g of potassium tetrafluoroborate was added and stirring was continued for 2 hours. After the reaction was completed, 20 mL of acetone was added, stirred thoroughly, filtered, and the solvent was distilled off to obtain 21.6 g of alkylimidazole tetrafluoroborate ionic liquid with a yield of 90.2%.

Embodiment 3

[0025] In a 100 mL three-necked flask, 13.7 g of n-bromobutane and 8.2 g of N-methylimidazole were added, and the mixture was stirred and reacted at 110° C. for 2 hours. Another 11.0 g of sodium tetrafluoroborate was added and stirring was continued for 2 hours. After the reaction was completed, 20 mL of acetone was added, stirred thoroughly, filtered, and the solvent was removed by distillation to obtain 21.5 g of alkylpyridine tetrafluoroborate ionic liquid with a yield of 85.0%.

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Abstract

The invention discloses a continuous synthesizing method of indoor ion liquid, which comprises the following steps: adopting pyridine or N-alkyl imidazole and halogenated hydrocarbon under normal pressure; stirring; making hydrocarbyl pyridine ammonium halides or 1, 3-dialkyl imidazole ammonium halides; adding fluorine salt to stir to react; obtaining the ion liquid under normal temperature; avoiding pollution due to using organic solvent; temperating reacting condition; improving reacting receiving rate and product quality; fitting for large scale of industrial manufacturing.

Description

a technical field [0001] The invention relates to a continuous synthesis method of room temperature ionic liquid, which is suitable for using pyridine or N-alkylimidazoles, halogenated hydrocarbons, and fluorine-containing salts as raw materials to synthesize hydrocarbyl pyridinium cations or 1,3-dihydrocarbyl imidazolium cations and In the case of room temperature ionic liquids composed of fluorine-containing anions. Two background technology [0002] Ionic liquid refers to a material system completely composed of ions in a liquid state at room temperature (generally at 100°C). It is generally composed of organic cations, inorganic anions, and organic anions. Its performance is mainly determined by the composition of cations and anions, and molecular design can be used to adjust it. Ionic liquids have many unique physical and chemical properties. It has been determined that the thermal decomposition temperature of ionic liquids composed of many imidazolium cations is as hi...

Claims

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Application Information

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IPC IPC(8): C07D233/58C07D213/20C07D213/127
Inventor 刘祖亮方东
Owner NANJING UNIV OF SCI & TECH
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