Method for catalyzing and preparing annular carbonic ester by supported ionic liquid

A technology of cyclic carbonate and ionic liquid, which is applied in organic chemistry and other fields, and can solve problems such as single function

Active Publication Date: 2012-02-01
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Conventional loaded ionic liquids include imidazoles, pyridines, quaternary

Method used

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  • Method for catalyzing and preparing annular carbonic ester by supported ionic liquid
  • Method for catalyzing and preparing annular carbonic ester by supported ionic liquid
  • Method for catalyzing and preparing annular carbonic ester by supported ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020]

[0021] Implementation method: in a 100ml stainless steel autoclave, add the 4-hydroxyethyl-1,2,4-triazole bromide of SBA-15 load successively (n=2 in the structural formula, R 1 =OH, X=Br) 1.5g (1.7mmol, 1.2mol% based on the content of the ionic liquid, the same below), 10ml propylene oxide (1a) (0.143mol), a closed reactor, filled with 1.0Mpa pressure For carbon dioxide, the temperature was controlled by a temperature controller to slowly rise to 110° C., and then the reaction pressure was controlled to 2.0 MPa, and the reaction was carried out for 2.0 hours. After the reaction, the reactor was cooled to 5° C., and excess carbon dioxide was slowly released. After the catalyst was separated by filtration, the obtained product (2a) was analyzed by gas chromatography. The selectivity was 99.8%, and the yield was 99%.

Embodiment 2

[0023] Same as Example 1, the catalyst used is 4-ethyl-1,2,4-triazole bromide supported by SBA-15 (n=2 in the structural formula, R 1 =H, X=Br) 1.5g (about 2.2mmol), and other conditions remain unchanged, the selectivity of product (2a) is 99.0%, and the yield is 80%.

Embodiment 3

[0025] Same as Example 1, the catalyst used is 4-carboxypropyl-1,2,4-triazole bromide supported by SBA-15 (n=2 in the structural formula, R 1 =COOH, X=Br) 1.5g (about 1.2mmol), other conditions remain unchanged, the product (2a) was obtained with a selectivity of 99.0% and a yield of 99%.

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Abstract

The invention relates to a method for catalyzing and preparing annular carbonic ester by supported ionic liquid, which is characterized in that supported 1,2,4-triazole ionic liquid is taken as a catalyst, the amount of a catalyst accounts for 0.2-5 mol% of that of epoxy compounds (calculated by the content of ionic liquid), the epoxy compounds and carbon dioxide are synthesized into the relevantannular carbonic ester through cycloaddition under the condition that the reaction pressure is 0.1-10.0MPa, the reaction temperature is 50 DEG C-150 DEG C and the reaction time is for 0.5-8 hours. The synthetic method has the characteristics of high catalyst activity, low cost, long usage life, easy products separation, easy catalyst recovery and the like, and a tertiary amino group contained in 1,2,4-triazole is capable of possessing the effect of the synergetic catalysis.

Description

Technical field: [0001] The invention relates to a method for preparing cyclic carbonate by cycloaddition of epoxy compound and carbon dioxide. Background technique: [0002] As the most important greenhouse gas, carbon dioxide is also an important C1 resource, its absorption and utilization has become one of the most challenging issues in this century, and the synthesis of cyclic carbonate is a good way to fix carbon dioxide . Cyclic carbonate is a very good polar solvent, which is widely used in the synthesis of pharmaceutical and fine chemical intermediates. In addition, cyclic carbonates can be hydrolyzed or alcoholyzed to produce bulk chemicals such as glycols and dimethyl carbonate with high selectivity. Compared with the original process, it can effectively reduce production costs and save energy. It has a good application prospect. [0003] At present, most of the methods for producing cyclic carbonates use binary homogeneous catalysts composed of Lewis acid metal...

Claims

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Application Information

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IPC IPC(8): C07D317/36C07D317/38C07D317/46
Inventor 张锁江陈曦孙剑王金泉成卫国张香平
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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