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One for normal pressure co 2 Mesoporous polyionic liquid catalyst for cycloaddition reaction, preparation method and application

A technology of polyionic liquid and ionic liquid, which is applied in the field of preparation of heterogeneous catalysts in organic chemical industry, can solve problems such as high temperature and high pressure, and achieve the effects of good thermal stability, rich halogen sites, and efficient conversion

Active Publication Date: 2022-01-18
HEFEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved in the present invention is aimed at the current industrial CO 2 The cycloaddition reaction needs defects such as high temperature and high pressure, providing a mesoporous polyionic liquid catalyst with good substrate compatibility, excellent catalytic activity and good recovery stability

Method used

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  • One for normal pressure co <sub>2</sub> Mesoporous polyionic liquid catalyst for cycloaddition reaction, preparation method and application
  • One for normal pressure co <sub>2</sub> Mesoporous polyionic liquid catalyst for cycloaddition reaction, preparation method and application
  • One for normal pressure co <sub>2</sub> Mesoporous polyionic liquid catalyst for cycloaddition reaction, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Dinuclear ionic liquid polymerized monomer bis-(3-vinyl-1-imidazole) methylene dibromide [C 1 Preparation of DVIM]Br

[0029] The preparation route is:

[0030]

[0031] Dissolve N-vinylimidazole (5.00g, 53.2mmol) and dibromomethane (4.62g, 26.6mmol) in 5mL of tetrahydrofuran, stir at room temperature for 1h, put it into a 100°C oven for solvent heat treatment for 24h, and after cooling to room temperature, get The crystalline yellow crude product was washed three times with ether and ethyl acetate respectively, filtered by suction and dried in a 70°C oven to obtain a yellow solid—monomer [C 1 DVIM] Br.

[0032] 2) Preparation of mesoporous polyionic liquids

[0033] The preparation route is:

[0034]

[0035] The monomer [C 1 DVIM] Br (0.3g), PEG-200 (6g) and initiator azobisisobutyronitrile AIBN (0.03g, [C 1 DVIM] 10% of the mass of Br) into the reaction tube, followed by 1 mL of deionized water, stirred at room temperature for 2 h, after the raw materi...

Embodiment 2

[0040] Effect of Different Polyethylene Glycols on Specific Surface Area of ​​Prepared Products

[0041] The preparation process is the same as in Example 1, and the polyethylene glycol is replaced by PEG-400, PEG-600, and PEG-800 respectively from PEG-200, and the specific surface areas of the prepared products are as follows: 185m 2 .g -1 、173m 2 .g -1 、164m 2 .g -1 , by comparison, it can be found that under the same preparation conditions, as the molecular weight of polyethylene glycol gradually increases, the specific surface area of ​​the prepared product gradually decreases.

Embodiment 3

[0043] 1) Dinuclear ionic liquid polymerized monomer bis-(3-vinyl-1-imidazole) methylene dibromide [C 1 Preparation of DVIM]Br

[0044] Dissolve N-vinylimidazole (7.05g, 75.01mmol) and dibromomethane (5.21g, 29.99mmol) in 10mL of tetrahydrofuran, stir at room temperature for 0.5h, put it in a 120°C oven for solvent heat treatment for 30h, and cool to room temperature. A crystalline yellow crude product was obtained, which was washed three times with ether and ethyl acetate, filtered by suction and dried in an oven at 80°C to obtain a yellow solid—monomer [C 1 DVIM] Br.

[0045] 2) Preparation of mesoporous polyionic liquids

[0046] The monomer [C 1 DVIM]Br (0.1g), PEG-400 (5g) and initiator 2,2'-azobis(2-methylpropylamidine) dihydrochloride (0.02g, [C 1 DVIM] 20% of the mass of Br) into the reaction tube, followed by 1 mL of deionized water, stirred at room temperature for 2.5 h, after the raw materials were fully dissolved, heated in an oil bath at 80° C. for 15 h static...

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Abstract

One for atmospheric pressure CO 2 The invention relates to a mesoporous polyionic liquid catalyst for cycloaddition reaction, a preparation method and application, and relates to the technical field of preparation of heterogeneous catalysts in organic chemical industry. Utilize N-vinylimidazole and dibromomethane to obtain dinuclear ionic liquid polymerization monomer [C through solvothermal reaction 1 DVIM] Br, adding initiator in the polyethylene glycol-water solvent system, the polymerization monomer completes free radical self-polymerization. The present invention uses cheap polyethylene glycol as a solvent and a small amount of water as a co-solvent, and the mesoporous polyionic liquid prepared by self-polymerization under the action of an initiator has a typical polycation skeleton, abundant halogen sites and good thermal stability It can be used as a metal-free heterogeneous catalyst to oxidize styrene and other epoxy compounds as substrates of CO under normal pressure. 2 cycloaddition reaction, and exhibits excellent catalytic activity and good recovery stability.

Description

technical field [0001] The invention relates to the technical field of preparation of heterogeneous catalysts in organic chemical industry, in particular to a 2 Mesoporous polyionic liquid catalyst for cycloaddition reaction, preparation method and application. Background technique [0002] CO 2 The cycloaddition reaction is an "atom-economical" CO 2 Green chemical transformation to synthesize five-membered cyclic carbonates with pharmaceutical and fine chemical value. Due to CO 2 Thermodynamically stable and kinetically inert, CO 2 Cycloaddition reactions are currently carried out industrially under conditions of high temperature and high pressure. Explore the realization of CO under extreme temperature conditions (atmospheric pressure and low temperature) 2 High-efficiency conversion catalytic system can reduce the requirements of reaction equipment, reduce the energy consumption required for reaction, and promote CO 2 Development of chemically immobilized green pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02B01J31/06C07D317/36C07D317/50C07D317/44C08F126/06
Inventor 王晓晨刘安求董强高大明吴云徐泽忠蔡威盟陈郑叶超杰
Owner HEFEI UNIV
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