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Ion liquid based on heteropoly acid and synthesis thereof

An ionic liquid and heteropolyanion technology, applied in the field of new materials and their preparation, to achieve the effect of low cost

Inactive Publication Date: 2008-07-16
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, the ionic liquids based on imidazolium cations-heteropolyanions based on PEG chains have not been reported in domestic and foreign literature.

Method used

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  • Ion liquid based on heteropoly acid and synthesis thereof
  • Ion liquid based on heteropoly acid and synthesis thereof
  • Ion liquid based on heteropoly acid and synthesis thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The chemical formula of ionic liquid 1:

[0037]

[0038](1) At room temperature, 2.38 g of thionyl chloride (20 mmol) dissolved in 10 ml was slowly added dropwise within 30 minutes to a solution containing 2 g of dry PEG 400 (5 mmol), 0.79 g of pyridine (10 mmol) and 15 ml of benzene in the two-neck flask. Thereafter, it was refluxed for 8 hours. After the reaction was completed, the volatile substances were removed under reduced pressure. And it was dissolved in benzene again, and the pyridinium salt was removed by filtration. After the benzene was sucked dry under reduced pressure, it was washed three times with ether to obtain the chlorinated PEG.

[0039] (2) Put 0.6 g (1.5 mmol) of the chlorinated PEG obtained in (1) and 0.74 g (6 mmol) of purified butylimidazole into the reactor, and put them in the reactor at 100 ° C under 10 standard atmospheric pressure N 2 React under protection for 24 hours. After that, it was washed 4 times with diethyl ether, and t...

Embodiment 2

[0042] Ionic liquid 2 chemical formula:

[0043]

[0044] (1) At room temperature, 2.38 g of thionyl chloride (20 mmol) dissolved in 10 ml was slowly added dropwise within 30 minutes to PEG 800 (5 mmol) containing 4 g of dryness, 0.79 g of pyridine (10 mmol) and 15 ml of benzene in the two-neck flask. Thereafter, it was refluxed for 8 hours. After the reaction was completed, the volatile substances were removed under reduced pressure. And it was dissolved in benzene again, and the pyridinium salt was removed by filtration. After the benzene was sucked dry under reduced pressure, it was washed three times with ether to obtain the chlorinated PEG.

[0045] (2) Put 1.2 grams (1.5 mmol) of the chlorinated PEG obtained in (1) and 0.74 grams (6 mmol) of purified butylimidazole into the reactor, and put them in the reactor at 100 ° C under 10 standard atmospheric pressure N 2 React under protection for 24 hours. After that, it was washed 4 times with diethyl ether, and the vo...

Embodiment 3

[0048] The chemical formula of ionic liquid 3:

[0049]

[0050] (1) At room temperature, 2.38 g of thionyl chloride (20 mmol) dissolved in 10 ml of benzene was slowly added dropwise within 30 minutes to a solution containing 4 g of dry PEG 2000 (5 mmol), 0.79 g of pyridine (10 mmol) and 15 ml of Benzene in a two-necked flask. Thereafter, it was refluxed for 8 hours. After the reaction was completed, the volatile substances were removed under reduced pressure. And it was dissolved in benzene again, and the pyridinium salt was removed by filtration. After the benzene was sucked dry under reduced pressure, it was washed three times with ether to obtain the chlorinated PEG.

[0051] (2) Put 1.2 grams (1.5 mmol) of the chlorinated PEG product obtained in (1) and 1.1 grams (6 mmol) of purified octyl imidazole into the reactor, at 100 ° C, under 10 standard atmospheric pressure N 2 React under protection for 24 hours. Afterwards, it was washed 4 times with ether, and the vol...

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Abstract

The invention provides a novel heteropoly acid anion based on an ionic liquid and a synthetic method thereof, which belongs to the technical field of novel chemical material and the preparation thereof. The synthetic steps are as follows: (1) synthesizing a chloride polyethylene glycol; adopting the polyethylene glycol (PEG) with a molecular weight in the scope between 200 to 2000, and taking benzene as a solvent to reflux to acquire chloride PEG under the function of a thionyl chloride and a pyridine; (2) utilizing the reaction of the chloride PEG and alkyl imidazole to acquire the alkyl imidazole hydrochloride provided with PEG macromolecular chains; (3) utilizing the alkyl imidazole hydrochloride provided with PEG macromolecular chains to implement a disproportionation reaction with heteropoly acid (phosphomolybdic acid, phosphotungstic acid and silicotungstic acid) under certain conditions, thereby eventually acquiring a heteropoly acid anions structured functionalized ionic liquid material. The novel heteropoly acid anion based on an ionic liquid and the synthetic method thereof combine the PEG chains to imidazole cations for the first time, and match with heteropoly acid anions to form novel ionic liquid, thereby providing a foundation for researching and developing the novel ionic liquid. In addition, the novel heteropoly acid anion based on an ionic liquid and the synthetic method thereof have the advantages of ready availability of raw materials and simple preparation; therefore, the novel heteropoly acid anion based on an ionic liquid is a great novel material of green chemical industry.

Description

technical field [0001] The invention relates to an ionic liquid and a preparation method thereof, in particular to a novel heteropolyanion-based ionic liquid and a preparation method thereof, belonging to the technical field of new materials and preparation thereof. Background technique [0002] Ionic liquids are molten salt systems composed of large cations and anions that are liquid at or near room temperature. The initial research was to react ethylamine with 20% nitric acid, remove water under reduced pressure, and obtain an oily liquid. After analysis, it was found that it was a liquid salt. Later, people obtained the ionic liquid of alkylpyridine / aluminum trichloride , and used it as an electrolyte to study the electrolytic behavior of organic substances. By the 1980s, people had developed 1-alkyl-3 methyl-imidazolium tetrafluoroborate (hexafluorophosphate), which was more stable to air and water, and then it was found that these ionic liquids were a kind of Good sol...

Claims

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Application Information

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IPC IPC(8): C07D233/60
Inventor 侯震山李欢胡玉冯博
Owner EAST CHINA UNIV OF SCI & TECH
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