Synthesis method of disubstituted-fluoride imidazole ionic liquid

A technology of imidazole fluoride and ionic liquid, which is applied in the field of ionic liquid synthesis, can solve problems such as complicated operation, difficult to remove impurities, and strict equipment requirements, and achieve the effect of simple operation and fast reaction speed

Inactive Publication Date: 2014-03-05
NORTHEASTERN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method of fluorination with HF gas and disubstituted imidazole chloride is complicated in operation due to the high toxicity and corrosiveness of HF gas, and the equipment requirements are very strict; the purity of disubstituted imidazole fluoride obtained by electrochemical method is not high, Low purity is difficult to meet the requirements of room temperature molten salt electrolysis; the conventional method of using chemical replacement reaction is also difficult to remove impurities in the post-treatment process

Method used

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  • Synthesis method of disubstituted-fluoride imidazole ionic liquid
  • Synthesis method of disubstituted-fluoride imidazole ionic liquid
  • Synthesis method of disubstituted-fluoride imidazole ionic liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0034] 1, the synthetic method of 3-dimethyl imidazole fluoride, its steps are:

[0035] 1) Take 10g of 1,3-dimethyl imidazole chloride (purity 90%) and 10.44g AgF (purity 90%) respectively, and dissolve them in 25ml and 20ml of distilled water respectively. After the solution is mixed, a metathesis reaction occurs rapidly to produce a white precipitate. Stir until Fully react; after the stirring is stopped, the precipitate settles rapidly, and the supernatant is a clear liquid;

[0036]2) Prepare 0.01ml / L 1,3-dimethylimidazolium chloride solution, add it into the supernatant by titration method, there will be a white precipitate, and there will be no precipitate after adding a total of 5.5ml solution;

[0037] 3) Filtrate to obtain the filtrate and filter residue; the filtrate was left to stand for 6 hours, and the filter residue was fully dried and weighed, the weight was 11.67g, number 1;

[0038] 4) Take a small glass bottle, take 1 drop of standing solution, add a small ...

Embodiment 2

[0042] 1, the synthetic method of 3-dimethyl imidazole fluoride, its steps are:

[0043] 1) Dissolve 7.63g of AgF (purity 95%) in 12ml of distilled water and mix it with 10g of 1,3-dimethylimidazole bromide (purity 99%) dissolved in 12.5ml. After the solution is mixed, metathesis reaction occurs rapidly to produce yellow precipitate. Stir until fully reacted; after the stirring stops, the precipitate settles rapidly, and the supernatant is a clear liquid;

[0044] 2) Prepare 0.01ml / L 1,3-dimethylimidazole bromide solution, add it to the supernatant by titration method, there will be a light yellow precipitate, and there will be no precipitate after adding 1ml of the solution in total;

[0045] 3) Filtrate to obtain filtrate and filter residue. Weigh the filter residue after fully drying, the weight is 11.01g, number 1;

[0046] 4) Take a small glass bottle, take 1 drop of filtrate, add a small amount of distilled water to dilute, add KCl, and check whether there is still Ag ...

Embodiment 3

[0050] 1-ethyl-3-methyl imidazole fluoride synthetic method, its steps are:

[0051] 1) Take 10g of 1-ethyl-3-methylimidazole chloride (purity 99%) and 8.8gAgF (purity 98%), respectively, and dissolve them in 25ml and 20ml of distilled water respectively. After the solutions are mixed, metathesis reaction occurs rapidly to produce white precipitate. Stir with a magnetic stirrer for 24 hours to fully react; after the stirring stops, the precipitate settles rapidly, and the supernatant is a clear liquid;

[0052] 2) Prepare 0.01ml / L of 1-ethyl-3-methylimidazole chloride solution, add it to the supernatant by titration method, there will be a white precipitate, and there will be no precipitate after adding a total of 32ml of the solution;

[0053] 3) Filtrate to obtain filtrate and filter residue. The filtrate was left to stand for 24 hours, and the filter residue was fully dried and weighed, the weight was 9.97g, and the number 1;

[0054] 4) Take a small glass bottle, take 1 ...

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Abstract

The invention discloses a synthesis method of a disubstituted-fluoride imidazole ionic liquid. The method comprises the following steps; taking equal molar ratio of halogenated imidazole and silver fluoride, completely dissolving halogenated imidazole and silver fluoride into water, and mixing water solutions; carrying out replacement reaction so as to generate disubstituted-fluoride imidazole and a silver halide precipitate; fully and completely reacting with silver ions in a reaction solution for twice; filtering, precipitating and drying in vacuum, so as to obtain a pure final product. An AlCl3 electrochemical experiment proves that the disubstituted-fluoride imidazole ionic liquid obtained by the method can carry out electrolytic deposition on an aluminum coating, and no silver is separated out. The synthesis method of the disubstituted-fluoride imidazole ionic liquid is simple in technology, free of organic solvent, environment-friendly, high in final product quality, and free of waste.

Description

technical field [0001] The invention relates to a synthesis method of an ionic liquid, in particular to a synthesis method of a fluorinated imidazole ionic liquid. Background technique [0002] Ionic liquids refer to material systems composed entirely of ions that appear liquid within a certain temperature range. As ionic compounds, ionic liquids are widely used in electrochemistry, It is widely used in organic synthesis, catalysis, separation and other fields. The advantages of ionic liquids in hydrogenation reactions are: the reaction rate is several times faster than in ordinary solvents; the mixture of ionic liquids and catalysts can be reused, and research shows that ionic liquids play a dual role as solvents and catalysts. In electrochemical applications, ionic liquids can reduce discharge, and the temperature used as battery electrolytes is much lower than that of molten salts. Ionic liquids have been used as electrolytes to manufacture new high-performance batterie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/58C25C3/18
CPCC07D233/56
Inventor 石忠宁钟熊伟熊婷高炳亮王兆文胡宪伟于江玉徐君莉
Owner NORTHEASTERN UNIV
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