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Method for synthesizing ionic liquid

A technology of ionic liquid and synthesis method, which is applied in the direction of organic chemistry, can solve the problems of type limitation, achieve the effects of rapid response, convenient replacement, and environmental protection

Inactive Publication Date: 2013-03-20
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the synthesis of ionic liquids by acid-base neutralization with strong bases is severely limited in the types of ionic liquids that can be synthesized, and it is necessary to develop other convenient and efficient synthetic methods

Method used

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  • Method for synthesizing ionic liquid
  • Method for synthesizing ionic liquid

Examples

Experimental program
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Embodiment 1

[0024] Example 1: Synthesis of ethylmethylimidazolium hydrogen sulfate (1-methyl-3-ethylimidazolium hydrogen sulfate)

[0025] (1) Add 0.1mol 1-methylimidazole into a single-necked flask, and add 0.1mol diethyl sulfate dropwise, and continue stirring for about 3 hours after the addition, to obtain a colorless and transparent ionic liquid 1-methyl-3- Ethyl imidazolium ethyl sulfate ([Emim]EtSO 4 ), is the precursor.

[0026] (2) Dissolve the precursor in propanol, and take an equimolar CH 3 COOK is dissolved in propanol. When the two solutions were mixed, a white precipitate was produced immediately, which was removed by filtration to obtain a colorless transparent liquid.

[0027] (3) Add equimolar sulfuric acid solution in this solution, it can be seen that a small amount of solid is produced, and this body is metal bisulfate, because NaHSO 4 or KHSO 4 The solubility in alcohol is extremely low (insoluble), so it precipitates. The solids are filtered off here and metere...

Embodiment 2

[0029] Embodiment two ethyl methylimidazolium dihydrogen phosphate synthesis

[0030] The steps are basically similar to Example 1, except that the CH 3 COOK with [Emim] EtSO 4 The molar ratio is changed to 1.5:1, sulfuric acid is changed to phosphoric acid, and propanol is changed to ethanol. Yield 98.7%. NMR data: [Emim]H 2 PO 4 : 1 H NMR (D 2 (0, 500MHz): δ=8.66(s, 1H), 7.44(s, 1H), 7.37(s, 1H), 4.19-4.09(m, 2H), 3.78(s, 3H), 1.45(t, J= 7.5Hz, 3H).

Embodiment 3

[0031] Embodiment three ethylmethylimidazolium borofluoride synthesis

[0032] The steps are basically similar to Example 1, KOH and [Emim]EtSO 4 The molar ratio was changed to 1.5:1, methanol was used as solvent, and sulfuric acid was changed to boric acid. Yield 92%. NMR data is: [Emim]BF 4 : 1 H NMR (D 2 (0, 500MHz): δ=8.65(s, 1H), 7.45(s, 1H), 7.38(s, 1H), 4.22-4.18(m, 2H), 3.86(s, 3H), 1.47(t, J= 7.25Hz, 3H).

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Abstract

The invention discloses a method for synthesizing halogen-free imidazole ionic liquid, which comprises the following steps of: slowly dropping dialkyl sulfate in equal molar amount of 1-alkyl imidazole; putting a reactor in an ice bath and continuously stirring because the reaction is severe and is intense in heat discharge; after dropping, continuing to stir until the reaction is completed, to obtain dialkyl imidazole sulfate ionic liquid; separately dissolving the obtained dialkyl imidazole sulfate ionic liquid and potassium carboxylate in alcohol; mixing two solutions, and filtering and removing the generated solid to obtain a colorless clear solution; adding acid of target negative ion to neutralize the obtained colorless clear solution, filtering to obtain a solution of the colorless clear target ionic liquid; evaporating alcohol and water to obtain a target ionic liquid product; and drying in a vacuum environment to obtain pure target ionic liquid. The synthesizing method disclosed by the invention has characteristics of moderate and rapid reaction condition, no need of heating, pressurizing and other conditions, and easiness in implementation; and the solvent used in the synthesizing process can be recycled.

Description

1. Technical field [0001] The present invention relates to ionic liquid synthesis. 2. Background technology [0002] Ionic liquids are a new class of solvents that are receiving much attention. They are salts with melting points close to room temperature (see: Fernicola, A.; Scrosati, B.; Ohno, H., Potentialities of ionic liquids as new electrolyte media in advanced electrochemical devices. Ionics 2006, 12(2), 95-102.). Ionic bodies usually consist of larger, less symmetrical cations and relatively smaller, more symmetrical anions. With the characteristics of high electrical conductivity, low vapor pressure and strong solubility, it is considered to be a green chemical reaction medium that can replace traditional volatile solvents. With the gradual and in-depth exploration of the understanding of ionic liquids, their applications have far exceeded the original scope of green chemistry, and there are huge application prospects in the fields of electrolysis, solar cells, fue...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/58C07D213/20
Inventor 高建谭小耀刘秀军潘璠初园园卢素敏
Owner TIANJIN POLYTECHNIC UNIV