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Ionic liquid based on peroxyheteropolyacid and preparation method thereof

A technology of peroxopolyacid and ionic liquid, applied in organic chemistry and other directions, to achieve strong oxidizing effect

Inactive Publication Date: 2011-12-28
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The anion of the ionic liquid based on peroxoheteropolyacid of the present invention is a peroxoheteropolyanion, and the ionic liquid has stronger oxidizing properties relative to the ionic liquid based on heteropolyacid, and at the same time, a sulfonic acid has been introduced into the imidazole ring of its cation The acid functional group makes the ionic liquid have stronger Brönsted acidity, and its acidity and oxidation can be adjusted in a wide range. There is no literature report on the ionic liquid based on peroxoheteropolyacid

Method used

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  • Ionic liquid based on peroxyheteropolyacid and preparation method thereof
  • Ionic liquid based on peroxyheteropolyacid and preparation method thereof
  • Ionic liquid based on peroxyheteropolyacid and preparation method thereof

Examples

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Effect test

example 1

[0021] a) Add 100mL toluene and 75mL N-propylimidazole to a 250mL four-necked flask respectively, and slowly add 23g of 1,3-propane sultone dropwise into the four-necked flask at 60°C under the protection of nitrogen. After completion, the reaction was continued for 3 h to produce a white solid, cooled, filtered, washed with 50 mL of toluene and acetone, respectively, and dried in vacuum at 60° C. for 24 h to obtain an ionic liquid intermediate.

[0022] b) Take 2.88g of phosphotungstic acid and add it to a 100mL four-necked flask. At room temperature, slowly drop 10mL of 30% hydrogen peroxide into the four-necked flask. After the dripping, continue the reaction at 30°C for 1.5h , to obtain peroxopolyacid solution.

[0023] c) Get 0.55g of the ionic liquid intermediate prepared in a) and add it to a four-necked flask, and slowly add the peroxopolyacid solution prepared in b) dropwise to the four-necked flask at room temperature. After dripping, Continue to react at 60°C for 5...

example 2

[0026] a) Add 100mL toluene and 75mL N-propylimidazole to a 250mL four-necked flask respectively, and slowly drop 25g of 1,4-butane sultone into the four-necked flask at 60°C under the protection of nitrogen. After completion, the reaction was continued for 3 h to produce a white solid, cooled, filtered, washed with 50 mL of toluene and acetone, respectively, and vacuum-dried at 60° C. for 24 h to obtain an ionic liquid intermediate.

[0027] b) Take 2.88g of phosphotungstic acid and add it to a 100mL four-necked flask. At room temperature, slowly drop 10mL of 30% hydrogen peroxide into the four-necked flask. After the dripping, continue the reaction at 30°C for 1.5h , to obtain peroxopolyacid solution.

[0028] c) Get 0.3g of the ionic liquid intermediate prepared in a) and add it to a four-necked flask, and slowly add the peroxopolyacid solution prepared in b) to the four-necked flask at room temperature. After the drop, Continue to react at 60°C for 5h, cool, filter, wash ...

example 3

[0031] a) Add 100mL toluene and 75mL N-octylimidazole to a 250mL four-necked flask respectively, and slowly add 25g of 1,4-butane sultone dropwise into the four-necked flask at 60°C under nitrogen protection. After completion, the reaction was continued for 3 h to produce a white solid, which was cooled and filtered. The white solid was washed with 50 mL of toluene and acetone respectively, and dried in vacuum at 60° C. for 24 h to obtain an ionic liquid intermediate.

[0032] b) Take 2.88g of phosphotungstic acid and add it to a 100mL four-necked flask. At room temperature, slowly drop 10mL of 30% hydrogen peroxide into the four-necked flask. After the dripping, continue the reaction at 30°C for 1.5h , to obtain peroxopolyacid solution.

[0033] c) Get 0.95g of the ionic liquid intermediate prepared in a) and add it to a four-necked flask, and slowly add the peroxopolyacid solution prepared in b) to the four-necked flask at room temperature. After the drop, Continue to react...

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Abstract

The invention provides a novel peroxoheteropolyacid-based ionic liquid and a preparation method of the ionic liquid. The ionic liquid is first reacted with an alkylimidazole and a sultone to generate an ionic liquid intermediate, and then the ionic liquid is The liquid intermediate is reacted with a peroxoheteropolyacid solution, and its general structural formula is: RxH3-x{QO4[MO(O2)2]4} where: Q is a P or As atom, and M is a Mo or W atom , R is, m is 0~8, n is 3 or 4, and x is 1~3. The new ionic liquid has strong Brönsted acidity and oxidation.

Description

Technical field [0001] The present invention provides a ionic liquid and preparation method based on peroxide -based hybrid acids, belongs to the areas of new materials and their preparation technology. Background technique [0002] Ionic liquid is composed of relatively large structure asymmetric organic yang ions and relatively small anion. Organic yang ions mainly include alkyl ammonium yang ions, alkyl-based phosphorus yang ions, 1, 3-alkyl mimazole yang ions and N-N-Instead of pyridine yang ions, etc., the node is mainly [PF 6 ] - , [CF 3 So 3 ] - , [BF 4 ] - CL - , [MESO 4 ] - , [MESO 3 ] - , [OCSO 4 ] - , [CH 3 So 3 ] - , AlCl 4 - , FeCl 4 - , CUCL 2 - wait.As early as 1914, P. Walnden prepared nitrate aceinerine [ETNH 3 ] [NO 3 ] Although the melting point is low, it is easy to explode and does not attract people's attention.Until 1992, Wilkes and others prepared a low melting point, with strong stability 1-ethyl-3-methylimazole tetrafluorosilicate ([Emim] BF 4 ) Later...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/60
Inventor 周钰明葛建华杨勇翁佳佳
Owner SOUTHEAST UNIV
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