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Polymer supported quaternary ammonium salt ion catalyst as well as preparation method and application thereof

A quaternary ammonium salt ion and polymer technology, which is applied to a polymer-supported quaternary ammonium salt ion catalyst and its preparation and application fields, can solve the problems of poor reusability, harsh reaction conditions, and high preparation costs, and achieve reusable performance. Good, low cost and simple preparation method

Inactive Publication Date: 2012-10-03
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of these catalysts have one or more of the following problems: low catalytic activity, poor selectivity, and the need to add solvents or / and co-catalysts; difficult to recycle, poor reusability; harsh reaction conditions, high preparation costs, etc., which limit its use. large scale use

Method used

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  • Polymer supported quaternary ammonium salt ion catalyst as well as preparation method and application thereof
  • Polymer supported quaternary ammonium salt ion catalyst as well as preparation method and application thereof
  • Polymer supported quaternary ammonium salt ion catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] S1: Mix chlorine balls and N,N-dimethylethylamine at a molar ratio of 1:[1-3], vacuumize, add methanol as a solvent at 5-10 times the molar amount of chlorine balls under the protection of an inert gas, The reaction system was heated to reflux at 60-90°C for 24-48h.

[0029] S2: After the reaction, cool to room temperature, filter, wash with methanol to remove unreacted N,N-dimethylglycine, and dry in vacuum to obtain a light yellow solid, which is the heterogeneous catalyst of quaternary ammonium salt ionic liquid supported by chlorine balls , denoted as PS-QNS.

[0030] Preparation of cyclic carbonates:

Embodiment 2

[0032] Add 0.2 g of polymer-loaded quaternary ammonium salt ion catalyst, 0.2 g of internal standard biphenyl, and 2 mL of propylene oxide in sequence in a 30 mL autoclave. 2 2.0MPa, react in an oil bath reactor with magnetic stirring at 150°C for 3h, after the reaction, place the reactor in a mixture of ice and water, and release the remaining CO after the reactants are cooled. 2 , Take out reactant, get supernatant after centrifugation and carry out GC analysis: the productive rate of propylene carbonate is 98.9%, and selectivity is 99.2%.

Embodiment 3

[0034] Add 0.2 g of polymer-loaded quaternary ammonium salt ion catalyst, 0.2 g of internal standard biphenyl, and 2 mL of propylene oxide in sequence in a 30 mL autoclave. 2 2.6MPa, react in an oil bath reactor with magnetic stirring at 150°C for 3h, after the reaction is completed, place the reactor in a mixture of ice and water, and release the remaining CO after the reactants are cooled. 2 , Take out reactant, get supernatant after centrifugation and carry out GC analysis: the productive rate of propylene carbonate is 96.1%, and selectivity is 99.1%.

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Abstract

The invention relates to a polymer supported quaternary ammonium salt ion catalyst as well as a preparation method and an application thereof. The preparation method is characterized in that chloromethylated polystyrene is taken as a carrier and reacts with N, N-dimethylethylamine to obtain polymer supported quaternary ammonium salt ion liquid catalyst; and under the condition that the catalyst dosage is 0.04-0.4 g, the initial pressure of carbon dioxide is 0.5-5.0 MPa, the reaction temperature is 110-180 DEG C, and the reaction time is 1-10 h, cyclic carbamate is prepared with high selectivity through cycloaddition reaction of carbon dioxide and epoxide. The catalyst has higher catalytic activity to the cycloaddition reaction of carbon dioxide and epoxide without adding any organic solvent or catalyst promoter, and the reaction condition is mild, and the obtained cyclic carbamate has a high yield and selectivity. The solid catalyst has the advantages of low price of raw material, simplie preparation method, good hydrothermal stability, convenience in recovery, and reusability.

Description

【Technical field】 [0001] The present invention relates to a kind of polymer loaded quaternary ammonium salt ion catalyst and its preparation method and CO 2 Application in the preparation of cyclic carbonates by cycloaddition reaction with epoxides. 【Background technique】 [0002] carbon dioxide (CO 2 ) is the most important greenhouse gas on the earth, and the content of carbon dioxide in the air is about 0.03%. However, with the gradual improvement of the degree of human industrialization, CO 2 Emissions are increasing year by year, which directly exacerbates the greenhouse effect. In the past 100 years, the global temperature has risen by 0.6°C, the sea level has risen by 14cm, and so on. These changes pose serious challenges to human survival and development. As a greenhouse gas, CO 2 It is also the cheapest and most abundant C1 resource, and its carbon content is 10 times that of oil, coal, and natural gas. Therefore, CO 2 The utilization of resources is imperat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07D317/38C07D317/36
Inventor 尹双凤张媛媛罗胜联周永波邱仁华
Owner HUNAN UNIV
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