Preparation and application method of polyionic liquid solid acid catalyst

A solid acid catalyst, polyionic liquid technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve problems such as unfavorable industrial production, and achieve easy separation , less corrosive, less residual effect

Active Publication Date: 2017-10-27
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although the chloroaluminate-type ionic liquids with high catalytic activity that have been studied more have been used in catalytic reactions in the laboratory, this ionic liquid is very sensitive to water vapor in the air and needs to be processed under absolutely anhydrous conditions. use, and thus is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] After mixing 1.68g of crosslinking agent N,N-methylenebisacrylamide, 0.50g of 2-methyl-1-vinylimidazole and 0.025g of initiator azobisisobutyronitrile (AIBN), the above mixture was dissolved in In 25ml of N,N-dimethylformamide, stirred at 20°C for 3h, hydrothermally reacted at 120°C for 48h, suction filtered, and the precipitate was dried at 120°C for 12h to obtain a pale yellow precursor porous polymer solid. Dissolve the above-mentioned pale yellow precursor porous polymer solid in 30ml of absolute ethanol, stir at 20°C for 3h, continue to add 3ml of propane sultone to continue the reaction for 48h, evaporate to dryness at 60°C, and dry at 80°C for 12h to obtain Polyionic liquids with different cationic chain lengths. The polyionic liquids obtained above with different cationic chain lengths were impregnated with 10 mmol / L toluene sulfate solution at 30°C for 24 hours, then filtered with suction, and the precipitate was washed with a large amount of ether and filtered...

Embodiment 2

[0028] After mixing 1.68g of crosslinking agent N,N-methylenebisacrylamide, 0.68g of 1-vinylimidazole and 0.007g of initiator azobisisobutyronitrile (AIBN), the above mixture was dissolved in 25ml of N,N- Stir in dimethylformamide at 20°C for 3h, hydrothermally react at 120°C for 12h, filter with suction, and dry the precipitate at 120°C for 12h to obtain a pale yellow precursor porous polymer solid. Dissolve the above-mentioned pale yellow precursor porous polymer solid in 30ml of absolute ethanol, stir at 20°C for 3h, continue to add 3ml of n-bromohexane to continue the reaction for 24h, evaporate to dryness at 60°C, and dry at 80°C for 12h to obtain different Polyionic liquids with long cationic chains. The polyionic liquids obtained above with different cationic chain lengths were impregnated with 3mmol / L toluene trifluoromethanesulfonate solution at 30°C for 48h, then suction filtered, and the precipitate was washed with a large amount of ether and filtered for several ti...

Embodiment 3

[0032]After mixing 1.68g of crosslinking agent N,N-methylenebisacrylamide, 0.76g of 2-ethyl-1-vinylimidazole and 0.07g of initiator azobisisobutyronitrile (AIBN), the above mixture was dissolved in In 30ml of N,N-dimethylformamide, stirred at 20°C for 3h, hydrothermally reacted at 120°C for 24h, suction filtered, and the precipitate was dried at 120°C for 12h to obtain a pale yellow precursor porous polymer solid. Dissolve the above-mentioned pale yellow precursor porous polymer solid in 30ml of absolute ethanol, stir at 20°C for 3h, continue to add 3ml of methyl iodide to continue the reaction for 24h, evaporate to dryness at 60°C, and dry at 80°C for 12h to obtain different cationic chains. long polyionic liquids. The polyionic liquids obtained above with different cationic chain lengths were impregnated with 15mmol / L acrylic toluene solution at 30°C for 48h, then filtered with suction, and the precipitate was washed with a large amount of ether and filtered for several time...

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PUM

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Abstract

The invention discloses preparation and an application method of a polyionic liquid solid acid catalyst, and relates to a polyionic liquid solid acid catalyst for preparing diphenylethane via alkylation reaction of ortho xylene and styrene, and a preparation method of the polyionic liquid solid acid catalyst. The catalyst has a higher alkylation conversion rate, diphenylethane yield and reusability at high temperature and atmospheric pressure. The polyionic liquid catalyst is prepared by performing a hydrothermal reaction of a vinyl imidazole monomer, N,N-methylene bisacrylamide cross-linking agent, an initiator and a dispersant to form a precursor porous polymer, and adding the obtained precursor porous polymer into haloalkane and strong acid for reaction.

Description

technical field [0001] The invention relates to a preparation technology of a polyionic liquid solid acid catalyst used for the alkylation reaction of o-xylene and styrene to prepare diaryleethane, and belongs to the technical field of industrial catalysis. Background technique [0002] Diarylethane (1-phenyl-1-xylylethane), referred to as PXE, is a product developed by Japan and the United States in the 1970s that can replace chlorinated biphenyl-type power capacitor impregnants. . 1-phenyl-1-xylylethane (1-pHenyl-1-xylylethane, referred to as PXE) synthesized from styrene and xylene has the characteristics of high boiling point, low viscosity and low freezing point, and is widely used in Solvent for pressure-sensitive dyes of carbonless copy paper. In addition, it can also be used as organic heat carrier, plasticizer and lubricating oil for plastic processing. [0003] Traditionally, the reaction for synthesizing PXE directly uses concentrated sulfuric acid as an acid ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07C2/70C07C15/18
CPCB01J31/06C07C2/70C07C15/18Y02P20/52
Inventor 盛晓莉高华颖周钰明张一卫
Owner SOUTHEAST UNIV
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