Preparation method of three-dimensional ordered macroporous carrier loaded heteropoly compound catalyst and application thereof

A technology of heteropoly compounds and macroporous carriers, which is applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., and can solve the problem of low activity of methacrolein oxidation reaction problem, to achieve the effect of improving redox, high activity and selectivity, and large pore structure

Active Publication Date: 2017-08-15
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation method of a supported heteropoly compound catalyst to solve the problem of low activity of existing catalysts to methacrolein oxidation reaction

Method used

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  • Preparation method of three-dimensional ordered macroporous carrier loaded heteropoly compound catalyst and application thereof
  • Preparation method of three-dimensional ordered macroporous carrier loaded heteropoly compound catalyst and application thereof

Examples

Experimental program
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Embodiment 1

[0019] A preparation method for a three-dimensional ordered macroporous carrier loaded heteropoly compound catalyst, comprising the following steps:

[0020] (1) Take by weighing 30 grams of monodisperse polystyrene microspheres with a diameter of 150 nanometers, add it to 200 milliliters of water, after stirring evenly, centrifuge at a speed of 10,000 rpm for 30 minutes, discard the upper layer liquid, and Dry at ℃ for 72 hours to obtain a polystyrene colloidal crystal template; configure 100 milliliters of ethanol aqueous solution with a volume concentration of 85%, add 75 grams of ethyl orthosilicate, 4.68 grams of ammonium metavanadate, and 21 milliliters of hydrochloric acid, and stir evenly. Use the obtained solution to impregnate the polystyrene colloidal crystal template for 30 minutes, then take it out and dry it for 2 hours, then repeat the impregnation and drying 3 times, and the obtained solid is subjected to multi-stage temperature-programmed roasting at a heating ...

Embodiment 2

[0025] A preparation method for a three-dimensional ordered macroporous carrier loaded heteropoly compound catalyst, comprising the following steps:

[0026] (1) Take by weighing 30 grams of monodisperse polystyrene microspheres with a diameter of 150 nanometers, add it to 200 milliliters of water, after stirring evenly, centrifuge at a speed of 10,000 rpm for 30 minutes, discard the upper layer liquid, and Dry at ℃ for 72 hours to obtain a polystyrene colloidal crystal template; configure 100 milliliters of ethanol aqueous solution with a volume concentration of 85%, add 75 grams of ethyl orthosilicate, 4.68 grams of ammonium metavanadate, and 21 milliliters of hydrochloric acid, and stir evenly. Use the obtained solution to impregnate the polystyrene colloidal crystal template for 30 minutes, then take it out and dry it for 2 hours, then repeat the impregnation and drying 3 times, and the obtained solid is subjected to multi-stage temperature-programmed roasting at a heating ...

Embodiment 3

[0036] A preparation method for a three-dimensional ordered macroporous carrier loaded heteropoly compound catalyst, comprising the following steps:

[0037] (1) Take by weighing 30 grams of monodisperse polystyrene microspheres with a diameter of 150 nanometers, add it to 200 milliliters of water, after stirring evenly, centrifuge at a speed of 10,000 rpm for 30 minutes, discard the upper layer liquid, and Dry at ℃ for 72 hours to obtain a polystyrene colloidal crystal template; configure 100 milliliters of ethanol aqueous solution with a volume concentration of 75%, add 75 grams of ethyl orthosilicate, 4.68 grams of ammonium metavanadate, and 21 milliliters of hydrochloric acid, and stir evenly. Use the obtained solution to impregnate the polystyrene colloidal crystal template for 30 minutes, then take it out and dry it for 2 hours, and then repeat the impregnation and drying 4 times. The obtained solid is subjected to multi-stage temperature-programmed roasting at a heating ...

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Abstract

The invention discloses a preparation method of a three-dimensional ordered macroporous carrier loaded heteropoly compound catalyst and belongs to the technical field of preparation of catalysts. The preparation method comprises the following steps of: adding tetraethoxysilane, a vanadium-containing compound and hydrochloric acid into a polystyrene colloidal crystal template; immersing and calcining the template to obtain a VOx-SiO2 three-dimensional ordered macroporous carrier; modifying the carrier; and finally, introducing a heteropoly compound to obtain the three-dimensional ordered macroporous carrier loaded heteropoly compound catalyst. According to the preparation method of the three-dimensional ordered macroporous carrier loaded heteropoly compound catalyst, disclosed by the invention, the catalyst has a proper duct structure and a relatively large specific surface area, so that the diffusing process of reactants and products is facilitated; and the oxidation-reduction quality of the catalyst can be improved by doping vanadium in the carrier, so that the catalyst shows high activity and high selectivity in catalyzing the oxidizing reaction of methylacrolein.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and in particular relates to a preparation method and application of a heteropoly compound catalyst loaded on a three-dimensional ordered macroporous carrier. Background technique [0002] The oxidation of methacrolein to methacrylic acid is a key step in the production process of methyl methacrylate with C4 as raw material. This reaction mainly uses heteropoly compounds with Keggin structure as catalysts. There are a large number of patent reports, such as US4803302, WO2005039760, WO2006001360, using phosphorus, molybdenum, vanadium and alkali metal as the main component of heteropolyacid salts as catalysts for the reaction of methacrolein oxidation to methacrylic acid, by adding various auxiliary Agents and optimized preparation methods to improve catalytic activity. However, heteropolyacid catalysts generally have the defect of low specific surface area, which leads to fewer acti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18B01J27/199C07C51/25C07C57/055
CPCB01J27/199C07C51/252C07C57/04
Inventor 张恒王婷婷马鑫鑫朱万诚
Owner QUFU NORMAL UNIV
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