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Synthetic method of imidazole acidic ionic liquid

A technology of acidic ionic liquid and synthesis method, which is applied in the field of chemistry, can solve the problems of easy decomposition, unstable water and air, etc., and achieve the effects of easy separation, pollution avoidance and high catalytic performance

Inactive Publication Date: 2017-07-14
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the 1960s, ionic liquids with better electrochemical stability were gradually used in organic synthesis, but they were very unstable to water and air and easily decomposed

Method used

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Examples

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Embodiment 1

[0023] A kind of synthetic method of imidazole acidic ionic liquid, comprises the following steps:

[0024] (1) Weigh 1-methylimidazole and ethyl bromide at a molar ratio of 1:1.2, then add 1-methylimidazole into a three-necked flask with stirring and condensing and reflux, heat to 75°C, and stir under the condition of ( Add bromoethane dropwise into the three-necked flask at 500~800rpm), keep the temperature at 75°C and stir and reflux for 12h after the dropwise addition is completed for 10~60min to obtain the first mixture, wash the first mixture with ethyl acetate three times, after washing Put it into a vacuum drying oven to dry at 80°C and 0.09MPa for 12 hours to obtain the intermediate;

[0025] (2) Weigh the intermediate obtained in step (1) and 85% phosphoric acid at a molar ratio of 1:1.1, then add the intermediate to a three-necked flask with stirring and reflux, and put it in an ice-water bath to keep the temperature at 0-5 ℃, under the condition of stirring (500-8...

Embodiment 2

[0028] The imidazole-based acidic ionic liquid synthesized in Example 1 has the advantages of good catalytic performance, easy product separation, easy recovery, reusability and environmental friendliness. For example, the ionic liquid can be used in the synthesis of polyaspartic acid. The specific catalytic usage method can be found in patent CN104788674A. The specific operation steps and experimental results are as follows:

[0029] Weigh 10 g of L-aspartic acid and 20 g of the ionic liquid described in Example 1 into a three-neck flask with stirring and cold water separation, wherein the ionic liquid is used as the reaction medium and catalyst, heat up to 180 ° C, and react for 3 hours to obtain Polysuccinimide solution. Quickly add 100ml of ethanol to the polysuccinimide solution to precipitate the polysuccinimide, filter, and rotate the filtrate at 70° C. for 2 hours to obtain the recovered ionic liquid. The polysuccinimide obtained above is hydrolyzed to polyaspartic ...

Embodiment 3

[0033] A kind of synthetic method of imidazole acidic ionic liquid, comprises the following steps:

[0034] (1) Weigh 1-methylimidazole and ethyl bromide at a molar ratio of 1:1.1, then add 1-methylimidazole into a three-necked flask with stirring and condensing and reflux, heat to 65°C, and stir under the condition of ( Add bromoethane dropwise into the three-necked flask at 500rpm), keep the temperature at 65°C and stir and reflux for 9h after the dropwise addition is completed for 60 minutes to obtain the first mixture, wash the first mixture twice with ethyl acetate, and put it into vacuum drying after washing Oven drying at 80°C and vacuum drying at 0.09MPa for 10 hours to obtain the intermediate;

[0035] (2) Weigh the intermediate obtained in step (1) and 85% phosphoric acid at a molar ratio of 1:1.5, then add the intermediate to a three-necked flask with stirring and reflux, and put it in an ice-water bath to keep the temperature at 0-5 ℃, under the condition of stirr...

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Abstract

The invention discloses a synthetic method of an imidazole acidic ionic liquid. The method comprises the following steps: (1) taking 1-methylimidazole, heating the 1-methylimidazole to 65-85 DEG C, dropise adding bromoethane under a stirring condition, carrying out stirring refluxing at 65-85 DEG C for 9-15 h to obtain a first mixture, washing the first mixture, and drying the first mixture in a vacuum drying box to obtain an intermediate; and (2) taking the intermediate obtained in step (1), placing the intermediate in ice water bath, dropwise adding a phosphoric acid solution under a stirring condition at 0-5 DEG C, carrying out stirring refluxing at 20-30 DEG C for 1-4 h after the dropwise addition ends in order to obtain a second mixture, and carrying out washing, rotary evaporation and drying on the second mixture to obtain the imidazole acidic ionic liquid. The method has the advantages of simplicity and easiness in operation, and the imidazole acidic ionic liquid has the advantages of high catalytic performance, repeated use, easiness in separation from reactants, easiness in recycling, and convenience in use.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and in particular relates to a method for synthesizing an imidazole-based acidic ionic liquid. Background technique [0002] Ionic liquids are a class of liquids composed entirely of ions, and are salts with a melting point below 100°C at or below room temperature. The so-called ionic liquid is a room temperature ionic liquid, which is generally composed of relatively large organic cations and relatively small inorganic anions. Compared with traditional ionic compounds, it is liquid at room temperature; compared with traditional liquid substances, it is composed of anions and cations in structure. Therefore, ionic liquids have unique physical and chemical properties and have the prospect of replacing traditional environmentally unfriendly solvents. [0003] The history of ionic liquids dates back to 1914, when Walden reported (EtNH 2 )+HNO 3 - (melting point 12°C), which is the first ionic...

Claims

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Application Information

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IPC IPC(8): C07D233/58C08G69/08
CPCC07D233/58C08G69/08Y02P20/582
Inventor 马江锋陈晓吴若凡吴昊任晓乾姜岷
Owner NANJING UNIV OF TECH
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