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Polymer supported imidazole ion catalyst as well as preparation method and application thereof

A technology for polymers and imidazoles, applied in the field of organic synthesis, can solve the problems of high catalyst preparation cost, harsh reaction conditions, low catalytic activity, etc., and is suitable for large-scale production, good thermal stability, high catalytic activity and selectivity. Effect

Active Publication Date: 2013-04-10
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of homogeneous catalytic systems are the high cost of catalyst preparation, difficulty in recycling, and the need to add solvents or / and co-catalysts; heterogeneous catalysts have problems such as low catalytic activity, poor selectivity, poor stability, and harsh reaction conditions.

Method used

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  • Polymer supported imidazole ion catalyst as well as preparation method and application thereof
  • Polymer supported imidazole ion catalyst as well as preparation method and application thereof
  • Polymer supported imidazole ion catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] S1: Mix imidazolized polydivinylbenzene and 3-bromopropionic acid in a molar ratio of 1: [1-3], vacuumize, and add 5-10 times the molar amount of imidazolized polydivinylbenzene under the protection of an inert gas 1,1,1,-Trichloroethane is used as a solvent, and the reaction system is heated to reflux for 20-30h.

[0024] S2: After stopping the reaction, cool to room temperature, filter, wash to remove the solvent, and dry in vacuo to obtain a light yellow solid.

[0025] Preparation of cyclic carbonates:

Embodiment 2

[0027] In a 30mL autoclave, add 0.2g of polymer-supported imidazole ion catalyst, 0.2g of biphenyl as an internal standard, 2mL of propylene oxide, and introduce CO at room temperature. 2 2.0MPa, placed in an oil bath reactor with magnetic stirring at 140°C for reaction, after 4 hours of reaction, the reactor was taken out and placed in an ice-water mixture, and the remaining CO was released after the reactants were cooled. 2 , Take out the reactant, take the supernatant after centrifugation and carry out GC analysis: the productive rate of propylene carbonate is 96.5%, and the selectivity is 99.8%.

Embodiment 3

[0029] In a 30mL autoclave, add 0.2g of polymer-supported imidazole ion catalyst, 0.2g of biphenyl as an internal standard, 2mL of propylene oxide, and introduce CO at room temperature. 2 2.5MPa, placed in an oil bath reactor with magnetic stirring at 160°C for reaction, after 6 hours of reaction, the reactor was taken out and placed in an ice-water mixture, and the remaining CO was released after the reactants were cooled. 2 , Take out the reactant, take the supernatant after centrifugation and carry out GC analysis: the productive rate of propylene carbonate is 98.8%, and the selectivity is 99.6%.

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Abstract

The invention provides a polymer supported imidazole ion catalyst as well as a preparation method and application thereof. The preparation method is characterized in that a polymer supported imidazole ion liquid catalyst is prepared by utilizing a chemical method; and cyclic carbonate is prepared at high selectivity through a cycloaddition reaction of CO2 and epoxide under the conditions that initial CO2 pressure is 1-3.5MPa, reaction temperature is 110-170 DEG C and reaction time is 1-8 hours. The catalyst can be simply prepared and has good hydrothermal stability and mild cycloaddition reaction condition in no need of adding any organic solvents and co-catalysts; and the selectivity of obtained cyclic carbonate is high, and the catalyst can be repeatedly utilized. The method is expectedto have wide application prospect in the field of industrial catalysis.

Description

【Technical field】 [0001] The invention relates to the field of organic synthesis, in particular to a polymer-supported imidazole ion catalyst, a preparation method thereof and an application in cycloaddition reactions of epoxides. 【Background technique】 [0002] Carbon dioxide (CO2) produced by burning fossil fuels (coal, oil, natural gas) 2 ) is currently the most important greenhouse gas on Earth. With the process of human industrialization, the greenhouse effect poses a serious challenge to human survival and development. At the same time, CO 2 It is the cheapest and most abundant resource in the C1 family, and its carbon content is 10 times that of coal, oil, and natural gas. Due to the double consideration of environmental protection and energy, CO 2 The preparation of organic chemical products from raw materials has become the focus of global attention. [0003] Cyclic carbonates are good polar aprotic solvents and are widely used in medicine and fine chemicals. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/36B01J31/06C07D317/46
Inventor 尹双凤张媛媛罗胜联周永波邱仁华
Owner HUNAN UNIV