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Load type polymeric acidic ionic liquid catalyst and preparation method and application thereof

An acidic ionic liquid, supported technology, applied in the field of supported polymeric acidic ionic liquid catalyst and its preparation, achieves the effects of easy recovery, mild reaction conditions and good repeatability

Active Publication Date: 2016-06-22
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, polymerized ionic liquids still have the disadvantage of liquid form

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 0.5mol of 2-bromoisobutyryl bromide and 0.5mol of aminopropyltriethoxysilane to the three ports, N 2 Protected, reacted at 0°C for 24h; take 0.5g of synthesized initiator and 1g of silicon dioxide, the solvent is 2% triethylamine in benzene solution, at 25°C, N 2 Protection, reaction 48h; SiO after taking 1g loaded initiator 2 powder, and 60g of vinylpyridine, the reaction system is added with 20ml of benzene solution of dimethylformamide, dimethylaminobisethyl ether and cuprous bromide, the dimethylformamide, dimethylaminobis The mass ratio of ethyl ether, cuprous bromide and benzene is 1:1:1:5, react at 110°C for 24 hours, wash with toluene and ethanol for 5 times each after the reaction is completed, dry at 80°C for 5 hours for later use, and obtain loaded ethylene pyridine polymer. Subsequently, the polymer was reacted with 78g of 1,4-butane sultone at 80°C for 4h, 86g of trifluoromethanesulfonic acid was added, and reacted at 70°C for 10h, followed by repeate...

Embodiment 2

[0028] Add 0.5mol of 2-bromoisobutyryl bromide and 0.75mol of aminopropyltriethoxysilane to the three ports, N 2 Protection, reaction at 10°C for 20h; take 1g of synthesized initiator and 1g of activated carbon, solvent is 10% triethylamine in benzene solution, at 10°C, N 2 protection, reaction for 48h; take 1g of activated carbon loaded with initiator, and 30g of vinylimidazole, and add 50ml of benzene solution with dimethylformamide, dimethylaminodiethyl ether and cuprous bromide to the reaction system, and the The mass ratio of dimethylformamide, dimethylaminodiethyl ether, cuprous bromide and benzene is 1:1:1:10, react at 80°C for 12h, and wash with toluene and ethanol for 5 hours each after the reaction is completed. The second time, it was dried at 80°C for 5 hours for later use, and the loaded vinylimidazole polymer was obtained. Then react the polymer with 80g-1,3-propane sultone at 70°C for 4h, add 58g of phosphoric acid, and react at 80°C for 4h, then wash with tolu...

Embodiment 3

[0030] Add 0.5mol of 2-bromoisobutyryl bromide and 0.6mol of aminopropyltriethoxysilane to the three ports, N 2 Protected, reacted at 0°C for 24h; take 1g of the synthesized initiator and 1g of MCM-41 molecular sieve, the solvent is 5% triethylamine in benzene solution, under nitrogen protection, at 25°C, N 2Protection, reaction for 48h; take 1g of MCM-41 molecular sieve loaded with initiator, and 40g of vinylpyrrolidone, and add benzene solution with dimethylformamide, dimethylaminodiethyl ether and cuprous bromide to the reaction system 30ml, the mass ratio of dimethylformamide, dimethylaminodiethyl ether, cuprous bromide and benzene is 1:1:1:8, react at 90°C for 10h, wash with toluene and ethanol for 5 Once, it was dried at 80°C for 5 hours for later use to obtain a vinylpyridine-loaded polymer. Then react the polymer with 35g of 1,4-propane sultone at 70°C for 4h, add 56g of sulfuric acid, and react at 60°C for 5h, then wash with toluene, ethanol, and ether repeatedly for...

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Abstract

The invention relates to a load type polymeric acidic ionic liquid catalyst and a preparation method and application thereof, and belongs to the technical fields of catalysis, materials and chemical industry. The catalyst comprises granules which are dispersed on the surface of a porous carrier and contain ionic liquid, the loading capacity of the acidic ionic liquid of the catalyst ranges from 2% to 10%, and for the catalyst, the specific surface area measured through a specific surface area and micropore adsorption analysis meter ranges from 250 m<2> / g to 350 m<2> / g. The load type polymeric acidic ionic liquid catalyst and the preparation method and application thereof have the advantages that the loaded ionic liquid content of the catalyst is high, and the catalytic esterification effect is good; under a specific reaction device and reaction condition, the yield of catalytically synthesizing dimethyl succinate can reach 85%.

Description

technical field [0001] The invention belongs to the technical field of polymers and catalysts, and in particular relates to a supported polymeric acidic ionic liquid catalyst and its preparation method and application. Background technique [0002] Dimethyl succinate, also known as dimethyl succinate, can be used in food additives, synthetic light stabilizers, high-grade coatings, fungicides, and pharmaceutical intermediates. The esterification reaction of succinic acid and methanol to generate dimethyl succinate is a reversible reaction like other esterification reactions, and the selection of a suitable catalyst is beneficial to the catalytic reaction. As a catalyst, acidic ionic liquids have made great progress in green synthesis. Ionic liquid catalysts have good reusability, high catalytic activity and easy separation from products. For example, ionic liquids are widely used in esterification reactions, such as the preparation of temperature-sensitive acidic ionic liqui...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07C69/40C07C67/08
CPCB01J31/06B01J2231/49C07C67/08C07C69/40
Inventor 胡颜荟张娟李未康
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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