Benzothiazole ionic liquid and preparation method as well as application thereof

An ionic liquid and benzothiazole technology, applied in the field of ionic liquid catalysts, can solve the problems such as low price of Bronsted acid functionalized ionic liquid, and achieve the effects of easy recycling, convenient recovery and high catalytic efficiency.

Active Publication Date: 2016-04-06
NANJING FORESTRY UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Bronsted acid functionalized ionic liquid prepared by benzothiazole is cheap and has not been reported

Method used

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  • Benzothiazole ionic liquid and preparation method as well as application thereof
  • Benzothiazole ionic liquid and preparation method as well as application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add a solution of 6.75g (50nmol) of benzothiazole in 25mL of absolute ethanol to the reaction flask, and add H2 dropwise within 30min at 0-5°C under full stirring. 2 SO 4 12.08g (55nmol) of ethanol solution in 10mL, react at room temperature for 3h after dropping. The solvent was evaporated, the residue was washed with ethyl acetate (3×5 mL), and then recrystallized from absolute ethanol to obtain the product as a white crystalline solid, benzothiazole thiohydrogen salt ionic liquid. The yield was 98.4%.

Embodiment 2

[0017] Add 6.75g (50nmol) of benzothiazole in 25mL of absolute ethanol solution in the reaction flask, and add HCLO dropwise at 0-5°C within 30min under full stirring. 4 7.85g (55nmol) of 70% aqueous solution was reacted at room temperature for 3h after dripping. The solvent was evaporated, the residue was washed with ethyl acetate (3×5 mL), and recrystallized from absolute ethanol to obtain a white powder, benzothiazole perchlorate ionic liquid. The calculated yield was 98.6%.

Embodiment 3

[0019] Add 6.75g (50nmol) of benzothiazole in 25mL of absolute ethanol solution in the reaction bottle, add dropwise 12.08g (55nmol) of phosphoric acid in 10mL of ethanol solution at 0-5°C within 30min under full stirring, Reaction 3h. The solvent was evaporated, the residue was washed with ethyl acetate (3×5 mL), and recrystallized from absolute ethanol to obtain the product benzothiazole dihydrogen phosphate ionic liquid. The calculated yield was 96.5%.

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Abstract

The invention discloses benzothiazole ionic liquid and a preparation method as well as application thereof. The preparation method of the benzothiazole ionic liquid comprises the steps of reacting benzothiazole and acid containing target anions, with equal molar weight, under a low temperature condition, and preparing corresponding benzothiazole salt ionic liquid, wherein the acid containing the target anions is one of sulfuric acid, phosphoric acid, perchloric acid and nitric acid. The benzothiazole ionic liquid can serve as a mild, special and efficient catalyst of a specific organic synthesis reaction, and is convenient to recover and reuse circularly and capable of effectively alleviating corrosion to equipment, and the production cost is lowered. In a ricinoleic acid dihydric alcohol ether ester preparation process, by adopting the benzothiazole salt ionic liquid as the catalyst, the catalytic efficiency is high, the catalyst and a product are easy to separate, the synthetic product is high in purity, the posttreatment is simple, the generation of a great amount of wastewater due to catalyst treatment is avoided, and the environmental pollution is reduced.

Description

technical field [0001] The invention belongs to the technical field of ionic liquid catalysts, and in particular relates to a benzothiazole ionic liquid and a preparation method and application thereof. Background technique [0002] Ionic liquids have non-volatility, high thermal stability, selective solubility, good physical and chemical properties, especially their designability, which provides a basis for innovation. According to the requirements of reaction and economy, it can be designed to meet different reaction conditions and ionic liquids for special reaction environments. New ionic liquids are a necessary condition to promote the sustained and rapid development of ionic liquids, so it is of great significance to study the preparation and application of new ionic liquids. [0003] Benzothiazole has similar structural characteristics and physical and chemical properties to the existing imidazole ionic liquid cations, so it is regarded as a potential substance for pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/62B01J31/02C07C67/08C07C69/732
CPCB01J31/0281B01J2231/49C07C67/08C07D277/62C07C69/732
Inventor 朱新宝张海飞刘准朱丰帆刘涌
Owner NANJING FORESTRY UNIV
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