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Preparation method and application of porous silicon sphere supported H3PW6Mo6O40 catalyst

A multi-level porous, heteropolyacid technology, applied in catalyst activation/preparation, organic compound preparation, chemical instruments and methods, etc. and other problems, to achieve the effect of improving product selectivity, increasing pore volume, and increasing specific surface area

Active Publication Date: 2019-08-02
WANHUA CHEM GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of a multi-level porous silicon sphere-supported phosphorus molybdenum tungsten heteropoly acid catalyst. The multi-level porous silicon sphere is loaded with phosphorus molybdenum tungsten heteropoly acid, which solves the problem that the specific surface area of ​​the heteropoly acid is small and the catalytic efficiency is low. The problem is that the synthesis of porous silicon spheres by ion thermal method provides a new method for the synthesis of porous materials. The porous silicon spheres obtained by this method have a smaller particle size and a larger specific surface area
[0006] Another object of the present invention is to provide the application of the above-mentioned catalyst in the synthesis of monoalkylphenols, especially the application of the synthesis of monoalkylphenols in the continuous kettle process. The continuous kettle process solves the problems that the intermittent kettle requires a large amount of manpower and low efficiency; The phenol-ene ratio of this process ensures the conversion rate of olefins > 99.9%, preventing the polymerization of olefins from reducing the activity of the catalyst; the selectivity of the product is > 94%

Method used

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  • Preparation method and application of porous silicon sphere supported H3PW6Mo6O40 catalyst
  • Preparation method and application of porous silicon sphere supported H3PW6Mo6O40 catalyst
  • Preparation method and application of porous silicon sphere supported H3PW6Mo6O40 catalyst

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Experimental program
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Effect test

Embodiment 1

[0038] With 1-ethyl-3-methylimidazolium bromide, tetramethylammonium chloride, ethyl orthosilicate, polyhexadiene dimethyl ammonium chloride, tetraethylammonium hydroxide according to mass ratio 18: 6:1:1:2 Synthesis of Hierarchical Porous Silicon Spheres: Stir 90g of 1-ethyl-3-methylimidazolium sodium bromide at 80°C, and then add 30g of tetramethylammonium chloride dropwise to it , then add 5g of polyhexadiene dimethyl ammonium chloride and 5g of tetraethylammonium hydroxide to the above system, after stirring for 1h, slowly add 10g of tetraethyl orthosilicate into the mixed solution, and continue to stir 4h, put the obtained white emulsion into a high-pressure hydrothermal kettle for crystallization at 180°C for 24h, the crystallized product was centrifuged, washed, and dried at 60°C for 6h to obtain a white solid powder, and then placed in a muffle furnace at 550°C Calcined at high temperature for 6h to obtain hierarchical porous silicon spheres.

[0039] 3g phosphomolybd...

Embodiment 2

[0045] With 1-ethyl-3-methylimidazolium bromide, tetramethylammonium chloride, ethyl orthosilicate, polyhexadiene dimethylammonium chloride, tetraethylammonium hydroxide according to mass ratio 19: 8:2:2:3 Synthesis of hierarchically porous silicon spheres: Stir 95g of 1-ethyl-3-methylimidazolium sodium bromide at 70°C, and then add 40g of tetramethylammonium chloride dropwise to it , then add 10g of polyhexadiene dimethyl ammonium chloride and 10g of tetraethylammonium hydroxide to the above system, after stirring for 1.5h, slowly add 15g of tetraethyl orthosilicate into the mixed solution, continue Stir for 3 hours, put the obtained white emulsion into a high-pressure hydrothermal kettle for crystallization at 200°C for 18 hours, centrifuge, wash, and dry at 70°C for 5 hours to obtain a white solid powder after drying, and then place it in a muffle furnace Calcined at 540°C for 2 hours to obtain hierarchical porous silicon spheres, the electron micrographs of which are shown...

Embodiment 3

[0051] With 1-ethyl-3-methylimidazolium bromide, tetramethylammonium chloride, ethyl orthosilicate, polyhexadiene dimethyl ammonium chloride, tetraethylammonium hydroxide according to mass ratio 20: 9:3:3:4 Synthesis of Hierarchical Porous Silicon Spheres: Stir 100g of 1-ethyl-3-methylimidazolium sodium bromide at 100°C, and then add 45g of tetramethylammonium chloride dropwise to it , then add 15g of polyhexadiene dimethyl ammonium chloride and 15g of tetraethylammonium hydroxide to the above system, after stirring for 2h, slowly add 20g of tetraethyl orthosilicate into the mixed solution, and continue to stir 2h, the obtained white emulsion was put into a high-pressure hydrothermal kettle for crystallization at 120°C for 12h, the crystallized product was centrifuged, washed, and dried at 80°C for 4h to obtain a white solid powder, and then placed in a muffle furnace at a temperature of 450°C Calcined for 10 hours to obtain hierarchical porous silicon spheres.

[0052] 9g ph...

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Abstract

The invention relates to a preparation method and an application of a porous silicon sphere supported H3PW6Mo6O40 catalyst. According to preparation and application of porous silicon sphere supportedH3PW6Mo6O40 in synthesis of monoalkylphenol by a continuous kettle, porous microspheres are prepared firstly, and then, H3PW6Mo6O40 is supported on porous silicon spheres to form the catalyst to be applied to synthesis of monoalkylphenol by the continuous kettle. The catalyst can be reused without treatment, has characteristics of energy saving and high efficiency as compared with a traditional intermittent kettle type process and is suitable for industrial production, and the traditional intermittent kettle type process is upgraded.

Description

technical field [0001] The invention relates to a preparation method of a multi-level porous silicon sphere-loaded phosphorus molybdenum tungsten heteropolyacid catalyst and its application in continuous reactor synthesis of monoalkylphenol. Background technique [0002] Alkylphenol is an important synthetic intermediate in organic synthesis. It has important applications in the fields of medicine, spices, and resins. It is widely used as an additive in plastics, rubber, and other products. The catalysts for the synthesis of alkylphenols mainly include inorganic acids, ion exchange resins, and molecular sieves. Inorganic acid catalysts are cheap and easy to obtain, but they are highly corrosive, corrode equipment, produce a large amount of three wastes, and cause great pressure on the environment; ion exchange resins have good catalytic performance for phenol alkylation, but ion exchange resins are prone to Deactivation and easy swelling have obvious disadvantages; molecula...

Claims

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Application Information

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IPC IPC(8): B01J31/18B01J35/10B01J37/08B01J37/10C07C37/14C07C37/74C07C39/06
CPCB01J27/188B01J37/082B01J37/10C07C37/14C07C37/74B01J35/638B01J35/615C07C39/06Y02P20/52Y02P20/584
Inventor 赵欣王明永王磊曾伟杨恒东丁可胡江林靳少华刘运海王坤宋延方杨洋陈永黎源
Owner WANHUA CHEM GRP CO LTD
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