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Application of supported heteropoly acid catalyst in preparation of fluorenyl acrylic ester

A technology of fluorenyl acrylate and immobilized heteropolyacid, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, and catalysts for physical/chemical processes, etc. It can solve the problems of non-recyclable use, low catalytic efficiency, and environmental pollution. , to achieve the effects of high yield, simple reaction operation, and strong temperature controllability

Active Publication Date: 2018-11-23
WUHAN POLYTECHNIC UNIVERSITY +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention provides an application of a solid-loaded heteropolyacid catalyst aimed at the technical defects of the prior art that the environment of the toluenesulfonic acid catalyst is polluted, the catalytic efficiency is on the low side, it cannot be reused, and resources are wasted.

Method used

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  • Application of supported heteropoly acid catalyst in preparation of fluorenyl acrylic ester
  • Application of supported heteropoly acid catalyst in preparation of fluorenyl acrylic ester
  • Application of supported heteropoly acid catalyst in preparation of fluorenyl acrylic ester

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Preparation of solid-supported phosphotungstic acid catalyst: use diatomaceous earth as a carrier, load phosphotungstic acid, and the mass percentage of phosphotungstic acid is 20%;

[0031] Add 100.0 grams of bisether fluorene, 25.0 grams of immobilized phosphotungstic acid catalyst, 0.15 grams of p-hydroxyanisole and 0.15 grams of sodium hypophosphite into a 500 ml four-necked round bottom flask with mechanical stirring, and then add 300 ml of toluene Solvent, start stirring, heating and dissolving, after slowly adding 41.0 g of acrylic acid dropwise, raise the temperature to 110°C for reflux and water separation, and react for 4 hours. Cool down to 55°C and filter, and collect the immobilized phosphotungstic acid for next use. Add 60 ml of deionized water and wash 5 times until neutral. Add 10 grams of anhydrous sodium sulfate, stir and dry for 2 hours and then membrane filter, add 0.02 gram of p-hydroxyanisole in the filtrate and carry out distillation under reduce...

Embodiment 2

[0033] Preparation of solid-supported silicotungstic acid catalyst: use white clay as a carrier to load silicotungstic acid, and the mass percentage of silicotungstic acid is 25%;

[0034] Add 400 grams of bis-ether fluorene, 90 grams of solid-supported silicotungstic acid catalyst, 0.5 grams of p-hydroxyanisole and 0.5 grams of sodium hypophosphite into a 2000 ml three-necked round bottom flask with mechanical stirring, and then add 1100 ml of methyl Cyclohexane solvent, start stirring and heating, raise the temperature to 80°C and stir for 20 minutes, after slowly adding 160 g of acrylic acid dropwise, quickly raise the temperature to reflux and water separation, and react for 4.5 hours. Cool down to about 60°C, filter, and collect solid-supported silicotungstic acid for reuse next time. Add 500 ml of deionized water to wash 7 times until neutral. Add 25 grams of anhydrous sodium sulfate, stir for 15 minutes, let stand for 5 hours, filter the membrane, add 0.1 grams of p-hy...

Embodiment 3

[0036] Preparation of solid silicomomolybdic acid catalyst: using white clay as a carrier, silicomomolybdic acid is loaded, and the mass percentage of silicomomolybdic acid is 30%;

[0037]Add 150 kg of bis-ether fluorene, 6 kg of immobilized silicomolybdic acid catalyst, 100 g of p-hydroxyanisole and 150 g of sodium hypophosphite into a 1000-liter enamel kettle with stirring, then add 450 kg of toluene solvent, and start stirring And heating, slowly add 24.2 kg of acrylic acid, after the addition is completed, the temperature is rapidly raised to 110 ° C for reflux, water is separated, and the reaction is carried out for 6 hours. Cool down to about 55°C, filter, and collect solid-supported silicomomolybdic acid for reuse next time. Add 60 kg of deionized water, stir for 5 minutes, let stand for 25 minutes, separate the water, and wash with water 6 times until neutral. Add 15 kilograms of anhydrous sodium sulfate, stir membrane filtration after 3 hours, add 40 grams of p-hydr...

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Abstract

The invention provides application of a supported heteropoly acid catalyst in preparation of fluorenyl acrylic ester. The application is characterized in that the supported heteropoly acid catalyst isprepared from solid heteropoly acid and a load carrier, wherein the solid heteropoly acid is one or two kinds of materials from heteropoly acid such as phosphotungstic acid, phosphomolybdic acid, silicotungstic acid, silicomolybdic acid, germanotungtic acid or germanium molybdic acid; the load carrier is one or two kinds of materials from carriers such as white clay, bentonite, kieselguhr, natural clay, silicon dioxide, titanium dioxide, aluminum oxide, molecular sieves, kaolin or active carbon. The supported heteropoly acid catalyst is used for replacing paratoluenesulfonic acid used by theoriginal process. The application has the advantages that the catalyst can be repeatedly used for many times; the reaction operation is simple and convenient; the temperature controllability is high;the yield reaches 90 percent or higher; the production cost is reduced; the production efficiency is improved; the environment pollution is reduced; the green chemical production requirements are met.

Description

technical field [0001] The invention relates to the field of chemistry and chemical engineering, in particular to the application of a solid-supported heteropolyacid catalyst in the preparation of fluorenyl acrylate. Background technique [0002] Polyacrylic resin, epoxy acrylic resin and other optical resin polymer materials with fluorene structure as the skeleton, because of their super toughness and excellent insulation, chemical resistance, wear resistance, heat resistance (glass It has become a new high-performance optical Thin-film functional materials have been widely used in modern optical and optoelectronic technology fields including laser systems, high-performance optical communications, optical displays, optical storage, optical switches, and optical waveguides. They are used to manufacture various high-end optical lenses, optical lenses and lenses, Precision optical instruments, cutting-edge electronic devices, automotive engineering plastics and paint coatings...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/54C07C67/26B01J31/18B01J27/188
CPCB01J27/188C07C67/08C07C67/26C07C69/54
Inventor 张智勇李小勇向陆军关金涛周小野
Owner WUHAN POLYTECHNIC UNIVERSITY
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