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Purification method of ion liquid

A technology of ionic liquid and purification method, applied in the field of purification of ionic liquid, can solve the problem of low purity of ionic liquid, etc., and achieve the effect of high-efficiency removal

Inactive Publication Date: 2007-07-25
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a kind of purification method of ionic liquid, to overcome the shortcoming that the purity of ionic liquid is not high in the existing preparation process, thereby provide a kind of efficient, environment-friendly ionic liquid purification method

Method used

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Experimental program
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Effect test

Embodiment 1

[0019] 1-methylimidazole and 1-bromoethane join in the reactor with the ratio of 1: 1.2 (mol / mol), in N2 atmosphere, react 24 hours under 65 ℃, the product that obtains, joins the inlet of molecular distillation unit In the feeder, turn on the vacuum pump to make the pressure reach 30Pa, preheat the raw material ionic liquid to 35°C, start the wiper, open the injection valve, control the feed rate at 1.44g / min, and carry out molecular distillation at 120°C. The collected heavy component is the purified ionic liquid, its mass accounts for 85.77% of the total mass, and the purity is 99.0% through NMR analysis. The light component accounts for 14.23% of the total mass. According to gas chromatography analysis, the content of 1-bromobutane is 87.92%, and the content of methylimidazole is 11.27%.

Embodiment 2

[0021] 1,2-dimethylimidazole and 1-bromopropane were added to the reactor in a ratio of 1:1.2 (mol / mol), and reacted for 24 hours under N2 atmosphere at 65°C, and the obtained product was added to the molecular distillation device In the feeder, turn on the vacuum pump to make the pressure reach 12Pa, preheat the raw material ionic liquid to 30°C, start the wiper, open the injection valve, control the feed rate at 1.32g / min, and carry out molecular distillation at 100°C . The collected heavy component is the purified ionic liquid, and its mass accounts for 86.01% of the total mass. According to NMR analysis, the purity is 99.1%. The light component accounts for 13.99% of the total mass. According to gas chromatography analysis, the content of 1-bromobutane is 84.72%, and the content of methylimidazole is 15.20%.

Embodiment 3

[0023] 1-methylimidazole and 1-bromoisopropane are added in the reactor with the ratio of 1: 1.2 (mol / mol), in N Atmosphere, reacted 24 hours under 65 ℃, the product that obtains, joins the inlet of molecular distillation unit In the feeder, turn on the vacuum pump to make the pressure reach 1Pa, preheat the raw material ionic liquid to 30°C, start the wiper, open the injection valve, control the feed rate at 1.44g / min, and carry out molecular distillation at 100°C. The collected heavy component is the purified ionic liquid, and its mass accounts for 85.49% of the total mass. According to NMR analysis, the purity is 99.3%. The light component accounts for 14.51% of the total mass. According to gas chromatography analysis, the content of 1-bromobutane is 89.23%, and the content of methylimidazole is 10.16%.

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Abstract

This invention discloses a method for purifying ionic liquid by molecular distillation. The method comprises: preheating crude ionic liquid, adding into a molecular distillation apparatus, adjusting the pressure, performing molecular distillation at an appropriate temperature, and collecting the heavy component to obtain purified ionic liquid. The method can efficiently remove residual volatile organic reactants, and the purity of purified ionic liquid is higher than 99%. Since the light component can be recovered for recycling, the method is thus environmentally friendly.

Description

technical field [0001] The invention relates to a method for preparing a high-purity ionic liquid, in particular to a method for purifying the ionic liquid. Background technique [0002] Ionic liquids refer to substances that are liquid at or near room temperature and are composed of organic cations and organic or inorganic anions. Due to the excellent properties of ionic liquids such as low-temperature melting, thermal stability, non-volatility, and wide electrochemical window, they have received great attention in recent years, and the synthesized ionic liquids have also developed at an extremely fast speed. Moreover, the research progress in the application of organic synthesis, catalysis, polymerization and other processes is extremely fast. [0003] Ionic liquids are often restricted by their purity during use. Since ionic liquids have almost no vapor pressure and there are many kinds of raw materials for synthesizing ionic liquids, there is no efficient method for pur...

Claims

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Application Information

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IPC IPC(8): C07D233/58B01D3/12
Inventor 方岩雄任清刚张赛丹周蓓蕾张焜纪红兵赵肃清杜志云黄宝华
Owner GUANGDONG UNIV OF TECH
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