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Imidazole ionic liquid with dual functions of oxidation and temperature control and synthetic method of ionic liquid

A technology of ionic liquids and synthesis methods, applied in chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, organic chemistry, etc., can solve problems that are not involved in specific properties, and achieve the effect of a large adjustment range

Inactive Publication Date: 2013-10-02
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, although the PEG chain is introduced into the cation, its specific properties are not involved

Method used

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  • Imidazole ionic liquid with dual functions of oxidation and temperature control and synthetic method of ionic liquid
  • Imidazole ionic liquid with dual functions of oxidation and temperature control and synthetic method of ionic liquid
  • Imidazole ionic liquid with dual functions of oxidation and temperature control and synthetic method of ionic liquid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] ionic liquid 1 The synthesis steps are as follows. The structural formula is shown in the following formula:

[0048]

[0049] 1. Synthesis of intermediate (I): Accurately weigh 1.7 g of imidazole and 10 mL of n-hexane, add it to a 100 mL autoclave, and refrigerate it in the refrigerator for at least 2 h; then add 20 mL of Ethylene oxide, sealed, with N 2 The air in the kettle was replaced 4 times. After stirring at room temperature for 2 h, the reaction was carried out at 60 °C for 4 h. Cool down, deflate, and open the kettle, transfer the reaction mixture into a 250 mL three-necked flask, wash the kettle wall with absolute ethanol, and transfer the washing solution into the three-necked flask together. The n-hexane and absolute ethanol were evaporated under reduced pressure to constant weight to obtain 17.95 g of intermediate (I). According to the product weight gain method, the average degree of polymerization of the intermediate (I) is calculated to be n=15....

Embodiment 2

[0053] ionic liquid 2 The synthesis steps are as follows. The structural formula is shown in the following formula:

[0054]

[0055] 1. Synthesis of intermediate (I): Accurately weigh 1.7 g of imidazole and 10 mL of n-hexane, add it to a 100 mL autoclave, and refrigerate it in the refrigerator for at least 2 h; then add 25 mL of Ethylene oxide, N for sealing 2 The air in the kettle was replaced 4 times. Stir at room temperature for 2 h, then react at a constant temperature of 60 °C for 4 h, lower the temperature, release gas, and open the kettle, transfer the reaction mixture into a 250 mL three-necked flask, wash the kettle wall with absolute ethanol, and transfer the washing solution into a three-necked flask. Under reduced pressure, n-hexane and absolute ethanol were distilled off to constant weight to obtain 23.30 g of intermediate (I). According to the product weight gain method, the average polymerization degree n=20 of the intermediate (I) was calculated.

[00...

Embodiment 3

[0059] ionic liquid 3 The synthesis steps are as follows. The structural formula is shown in the following formula:

[0060]

[0061] 1. Synthesis of intermediate (I): Accurately weigh 1.7 g of imidazole and 10 mL of n-hexane, add it to a 100 mL autoclave, and place it in the refrigerator for at least 2 h; then add 60 mL of Ethylene oxide, N for sealing 2 The air in the kettle was replaced 4 times. Stir at room temperature for 2 h, then react at a constant temperature of 60 °C for 4 h, lower the temperature, release gas, and open the kettle, transfer the reaction mixture into a 250 mL three-necked flask, wash the kettle wall with absolute ethanol, and transfer the washing solution into a three-necked flask. The n-hexane and absolute ethanol were evaporated under reduced pressure to constant weight to obtain 39.58 g of intermediate (I). According to the product weight gain method, the average polymerization degree n=34 of the intermediate (I) was calculated.

[0062] 2....

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Abstract

The invention provides a novel ionic liquid with dual functions of oxidation and temperature control, and a preparation method of the ionic liquid. The designed synthesis of the imidazole ionic liquid with the dual functions of oxidation and temperature control is completed by introducing a temperature control unit (PEG chain) to an imidazole group positive ion structure of the ionic liquid and taking a heteropoly acid root, which is composed of high-valence tungsten, molybdenum and vanadium with catalytic oxidation active centers, as negative ions of the ionic liquid. The synthesis steps are as follows: imidazole and ethylene oxide are subjected to polymerization reaction to prepare an intermediate I; the intermediate I and alkyl halide are subjected to quaterisation reaction to prepare an intermediate II; the intermediate II and different heteropoly acids are subjected to anion exchange reaction to prepare a target product III. The invention prepares the ionic liquid with the dual functions of oxidation and temperature control for the first time, and the catalytic oxidation reaction system of the ionic liquid has the characteristics of homogeneous reaction at high temperature and two-dimensional separation at low temperature and can realize integration of reaction and separation.

Description

technical field [0001] The invention relates to a functionalized ionic liquid and a synthesis method thereof, in particular to an imidazole oxidation-temperature-controlled dual-functional ionic liquid and a synthesis method thereof, belonging to the field of new chemical materials and their preparation. Background technique [0002] Ionic liquids are salts composed of organic cations and inorganic or organic anions. They have the characteristics of low vapor pressure, designable structure, adjustable properties, good solubility, high thermal stability and no deactivation of catalysts. They are regarded as a class of Environmentally friendly solvents are used in many chemical reactions. Recently, it is the frontier of ionic liquid research to assemble some groups with catalytic active centers or various functional groups into the structure of ionic liquids through chemical reactions to functionalize ionic liquids to meet specific needs. Currently synthesized functionalized ...

Claims

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Application Information

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IPC IPC(8): C07D233/60C08G65/08B01J31/34B01J31/36
Inventor 于凤丽解从霞袁冰柳春玉于世涛
Owner QINGDAO UNIV OF SCI & TECH
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