阅读说明：本技术 一种新型室温离子液体及其制备方法和应用 (Novel room-temperature ionic liquid and preparation method and application thereof ) 是由 张辉 王志鹏 于姗姗 段海宝 于 2019-10-29 设计创作，主要内容包括：本发明公开了一种新型室温离子液体及制备方法和应用,属于新材料领域。该离子液体是将2-甲基苯甲醛和1-氨基吡啶碘进行反应,得到碘化N-(2-甲基-亚苄基氨基)吡啶,之后将碘化N-(2-甲基-亚苄基氨基)吡啶与双三氟甲基磺酰亚胺锂进行反应,即可得到油状液体的新型室温离子液体。本发明制备方法简单,容易工业化应用。(The invention discloses a novel room-temperature ionic liquid, a preparation method and application thereof, and belongs to the field of novel materials. The ionic liquid is novel room-temperature ionic liquid which is oily liquid and is prepared by reacting 2-methylbenzaldehyde with 1-aminopyridine iodine to obtain N- (2-methyl-benzylidene amino) pyridine iodide and then reacting the N- (2-methyl-benzylidene amino) pyridine iodide with bis (trifluoromethyl) sulfonyl imide lithium. The preparation method is simple and easy for industrial application.)

1. A preparation method of novel room temperature ionic liquid is characterized by comprising the following steps: the preparation method comprises the following steps:

the first step is as follows: synthesis of N- (2-methyl-benzylideneamino) pyridine iodide:

dissolving 2-methylbenzaldehyde in a solvent, adding 1-aminopyridine iodine while stirring, and refluxing for reacting for 3-8 hours; after the reaction is finished, cooling to room temperature, carrying out suction filtration, washing and vacuum drying to obtain N- (2-methyl-benzylidene amino) pyridine iodide;

the second step is that: synthesis of ionic liquid:

dissolving N- (2-methyl-benzylideneamino) pyridine iodide and lithium bis (trifluoromethyl) sulfimide in a solvent a by ultrasonic, reacting for 30-60 h under the condition of stirring, performing rotary evaporation on the obtained solution, and removing the solvent a to obtain oil drops; dissolving the oil drops by using a solvent b, and adding distilled water with the same volume for extraction to obtain an oily liquid product, namely the novel room-temperature ionic liquid.

2. The method for preparing a novel room temperature ionic liquid according to claim 1, characterized in that: in the first step, the molar ratio of 2-methylbenzaldehyde to 1-aminopyridine iodine is 1: 1-3; preferably: the molar ratio of the 2-methylbenzaldehyde to the 1-aminopyridine iodine is 1: 1.

3. the method for preparing a novel room temperature ionic liquid according to claim 2, characterized in that: the reaction time of the first step is 4-6 h.

4. The method for preparing a novel room temperature ionic liquid according to claim 1, characterized in that: the solvent used in the first step of reaction is alcohol, preferably alcohol containing 1-3 carbon atoms or acetonitrile.

5. The method for preparing a novel room temperature ionic liquid according to claim 1, characterized in that: the molar ratio of N- (2-methyl-benzylideneamino) pyridine iodide to lithium bis (trifluoromethyl) sulfonyl imide iodide in the second step is 1: 1-3; preferably: the molar ratio of N- (2-methyl-benzylideneamino) pyridine iodide to lithium bis (trifluoromethyl) sulfonimide iodide was 1: 1.

6. the method for preparing a novel room temperature ionic liquid according to claim 1, characterized in that: the time of the second step reaction is 45-50 h.

7. The method for preparing a novel room temperature ionic liquid according to claim 1, characterized in that: the solvent a used in the second step is alcohol or acetonitrile containing 1-3 carbon atoms; the solvent b is dichloromethane or chloroform.

8. A novel room temperature ionic liquid is characterized in that: the ionic liquid is prepared by the following method:

the first step is as follows: synthesis of N- (2-methyl-benzylideneamino) pyridine iodide:

dissolving 2-methylbenzaldehyde in a solvent, adding 1-aminopyridine iodine while stirring, and refluxing for reacting for 3-8 hours; after the reaction is finished, cooling to room temperature, carrying out suction filtration, washing and vacuum drying to obtain N- (2-methyl-benzylidene amino) pyridine iodide;

the second step is that: synthesis of ionic liquid:

dissolving N- (2-methyl-benzylideneamino) pyridine iodide and lithium bis (trifluoromethyl) sulfimide in a solvent a by ultrasonic, reacting for 30-60 h under the condition of stirring, performing rotary evaporation on the obtained solution, and removing the solvent a; dissolving the oil drops by using a solvent b, and adding distilled water with the same volume for extraction to obtain an oily liquid product, namely the novel room-temperature ionic liquid.

9. The use of the novel room temperature ionic liquid of claim 8 in drug separation assays, fuel cell electrolytes, chemical sensors, and chemical catalysts and green solvents.

Technical Field

The invention relates to the field of new materials, and particularly relates to a novel room-temperature ionic liquid, and a preparation method and application thereof.

Background

With the development of science and technology and the deepening of research, the continuous improvement of an ionic liquid system leads people to realize that the ionic liquid is not only a novel green solvent, but also an idea for developing a green medium and a new functional material. Due to the characteristics of low volatility, good thermal stability, large liquid range and the like, the ionic liquid has wide application prospects in the fields of catalysis and synthesis, aerospace, ionic batteries, life science and the like.

The currently reported room-temperature ionic liquids all contain alkyl chains in the structure, and the preparation method is complex.

Disclosure of Invention

The invention provides a novel room temperature ionic liquid and a preparation method and application thereof aiming at the technical problems existing last time.

The purpose of the invention can be realized by the following technical scheme:

a preparation method of a novel room temperature ionic liquid comprises the following preparation steps:

the first step is as follows: synthesis of N- (2-methyl-benzylideneamino) pyridine iodide:

dissolving 2-methylbenzaldehyde in a solvent, adding 1-aminopyridine iodine while stirring, and refluxing for reacting for 3-8 hours; after the reaction is finished, cooling to room temperature, carrying out suction filtration, washing and vacuum drying to obtain N- (2-methyl-benzylidene amino) pyridine iodide;

the second step is that: synthesis of ionic liquid:

dissolving N- (2-methyl-benzylideneamino) pyridine iodide and lithium bis (trifluoromethyl) sulfimide in a solvent a by ultrasonic, reacting for 30-60 h under the condition of stirring, performing rotary evaporation on the obtained solution, and removing the solvent a to obtain oil drops; dissolving the oil drops by using a solvent b, and adding distilled water with the same volume for extraction to obtain an oily liquid product, namely the novel room-temperature ionic liquid.

A novel room-temperature ionic liquid is prepared by the following method:

the first step is as follows: synthesis of N- (2-methyl-benzylideneamino) pyridine iodide:

dissolving 2-methylbenzaldehyde in a solvent, adding 1-aminopyridine iodine while stirring, and refluxing for reacting for 3-8 hours; after the reaction is finished, cooling to room temperature, carrying out suction filtration, washing and vacuum drying to obtain N- (2-methyl-benzylidene amino) pyridine iodide;

the second step is that: synthesis of ionic liquid:

dissolving N- (2-methyl-benzylideneamino) pyridine iodide and lithium bis (trifluoromethyl) sulfimide in a solvent a by ultrasonic, reacting for 30-60 h under the condition of stirring, performing rotary evaporation on the obtained solution, and removing the solvent a; dissolving the oil drops by using a solvent b, and adding distilled water with the same volume for extraction to obtain an oily liquid product, namely the novel room-temperature ionic liquid.

The technical scheme of the invention is as follows: in the first step, the molar ratio of 2-methylbenzaldehyde to 1-aminopyridine iodine is 1: 1-3; preferably: the molar ratio of the 2-methylbenzaldehyde to the 1-aminopyridine iodine is 1: 1.

the technical scheme of the invention is as follows: the reaction time of the first step is 4-6 h.

The technical scheme of the invention is as follows: the solvent used in the first step of reaction is alcohol, preferably alcohol containing 1-3 carbon atoms or acetonitrile.

The technical scheme of the invention is as follows: the molar ratio of N- (2-methyl-benzylideneamino) pyridine iodide to lithium bis (trifluoromethyl) sulfonyl imide iodide in the second step is 1: 1-3; preferably: the molar ratio of N- (2-methyl-benzylideneamino) pyridine iodide to lithium bis (trifluoromethyl) sulfonimide iodide was 1: 1.

the technical scheme of the invention is as follows: the time of the second step reaction is 45-50 h.

The technical scheme of the invention is as follows: the solvent a used in the second step is alcohol or acetonitrile containing 1-3 carbon atoms; the solvent b is dichloromethane or chloroform.

The technical scheme of the invention is as follows: the prepared novel room-temperature ionic liquid is applied to medicine separation and analysis, electrolyte of a fuel cell, a chemical sensor, a chemical catalyst and a green solvent.

The invention has the beneficial effects that:

in view of the fact that in the prior art, room-temperature ionic liquids all contain alkyl chains in the structure and the preparation method is complex. The preparation method of the novel room-temperature ionic liquid provided by the invention is simple and easy to realize industrial application.

Drawings

FIG. 1 nuclear magnetic hydrogen spectrum of the compound prepared in example 1.

FIG. 2 nuclear magnetic carbon spectrum of the compound prepared in example 1.

FIG. 3 thermogravimetric mapping of the compound prepared in example 1.

Figure 4 differential scanning calorimetry traces of the compound prepared in example 1.

Detailed Description

The invention is further illustrated by the following examples, without limiting the scope of the invention: