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Phosphoric acid modified montmorillonite loaded tungsten oxide catalyst, preparation method and application

A technology of tungsten oxide and montmorillonite, which is applied in the preparation of carbon-based compounds, organic compounds, physical/chemical process catalysts, etc., can solve the problems of poor thermal stability, unfavorable catalyst regeneration, catalyst deactivation, etc., and achieve stable Good performance, good development prospects, and high catalytic activity

Inactive Publication Date: 2016-07-13
ZHEJIANG COLLEGE OF ZHEJIANG UNIV OF TECHOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the solid acid catalyst supported by tungstophosphopolyacid shows strong Brnsted acid sites, its thermal stability is poor, which is not conducive to the regeneration of the catalyst. When the regeneration temperature exceeds 500 °C, the supported tungstophosphopolyacid decomposes into phosphorus-containing Oxide and bulky 3D WO 3 crystal grains, leading to severe deactivation of the catalyst, therefore, the calcination temperature of the solid acid catalyst supported by tungstophosphoheteropolyacid is generally lower, which is 250-400 °C
[0005] So far, there are no domestic and foreign literature reports on solid acid catalysts loaded with tungsten oxide after phosphoric acid activated montmorillonite

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In this example, 5g of montmorillonite was dispersed in 25ml of phosphoric acid aqueous solution with a concentration of 15% by mass (the mass ratio of solute phosphoric acid, water, and montmorillonite was 0.8:4.3:1). After stirring and reacting at 60°C for 4 hours, After cooling, centrifugation, precipitation, washing with deionized water to neutrality, and drying at 80°C for 10 hours, phosphoric acid modified montmorillonite is obtained. 0.43 g of ammonium metatungstate tetrahydrate, 0.08 g of oxalic acid dihydrate, 1 ml of ethanol and 5 g of deionized water were mixed to prepare a transparent immersion liquid. Disperse 4g of phosphoric acid-modified montmorillonite in the impregnating solution (the mass of tungsten accounts for 8% of the mass of phosphoric acid-modified montmorillonite). After standing at room temperature for 10 hours, dry at 80°C for 12 hours, and then at 400°C in air atmosphere Medium roasting for 3 hours, natural cooling to room temperature, table...

Embodiment 2

[0028] In this example, 5g of montmorillonite was dispersed in 25ml of phosphoric acid aqueous solution with a concentration of 15% by mass (the mass ratio of solute phosphoric acid, water, and montmorillonite was 0.8:4.3:1), and after stirring and reacting at 65°C for 6 hours, After cooling, centrifugation, precipitation, washing with deionized water to neutrality, and drying at 80°C for 10 hours, phosphoric acid modified montmorillonite is obtained. 0.68 g of ammonium paratungstate tetrahydrate, 0.12 g of oxalic acid dihydrate, 2 ml of ethanol and 7 g of deionized water were mixed to prepare a transparent immersion liquid. Disperse 4g of phosphoric acid-modified montmorillonite in the impregnating solution (the mass of tungsten accounts for 12% of the mass of phosphoric acid-modified montmorillonite). After standing at 45°C for 6h, drying at 80°C for 10h, and then air at 350°C It is calcined in an atmosphere for 4 hours, naturally cooled to room temperature, tableted, granula...

Embodiment 3

[0031] In this example, 5g of montmorillonite was dispersed in 25ml of phosphoric acid aqueous solution with a concentration of 20% by mass (the mass ratio of solute phosphoric acid, water, and montmorillonite was 1:4:1). After stirring and reacting at 80°C for 6 hours, After cooling, centrifugation, precipitation, washing with deionized water to neutrality, and drying at 80°C for 10 hours, phosphoric acid modified montmorillonite is obtained. Mix 0.91 g of ammonium paratungstate tetrahydrate, 0.12 g of oxalic acid dihydrate, 2 ml of ethanol and 8 g of deionized water to prepare a transparent immersion liquid. Disperse 4g of phosphoric acid-modified montmorillonite in the impregnating solution (the mass of tungsten accounts for 16% of the mass of phosphoric acid-modified montmorillonite). After standing at 45℃ for 8h, drying at 80℃ for 8h, then air at 350℃ It is calcined in an atmosphere for 4 hours, naturally cooled to room temperature, tableted, granulated, and passed through...

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PUM

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Abstract

The invention discloses a phosphoric acid modified montmorillonite loaded tungsten oxide catalyst, a preparation method and application.The preparation method includes: using a phosphoric acid solution to modify montmorillonite, and adopting a soaking method to load tungsten oxide on phosphoric acid modified montmorillonite, wherein active species are H+ among montmorillonite layers, Al3+ outside a montmorillonite framework and WOx with different tungsten-oxygen atom coordination structures, and x is greater than or equal to 2.7 and less than or equal to 3; soaking phosphoric acid modified montmorillonite in a water solution of ammonium tungstate hydrate, oxalate dihydrate and low carbon, drying, and baking to obtain the phosphoric acid modified montmorillonite loaded tungsten oxide catalyst.The catalyst can be used for catalyzing glycerol gas-phase selective dehydration to produce acrylic aldehyde, glycerol conversion rate is 70-100%, acrylic aldehyde selectivity is 75-95%, and the catalyst is simple in preparation process, high in catalytic performance and long in service life.

Description

Technical field [0001] The invention relates to a phosphoric acid modified montmorillonite supported tungsten oxide catalyst, a preparation method, and application in the production of acrolein by the selective dehydration of glycerin in the gas phase. Background technique [0002] Montmorillonite is a natural mineral, rich in resources, cheap, and environmentally friendly. Its main component is aluminosilicate, which has a layered structure. The layers are composed of a "sandwich" of silicon-oxygen tetrahedrons with aluminum-oxygen octahedrons, and a certain amount of Na is absorbed between the layers. + , Ca 2+ Such as hydrated cations, the cations between the layers are exchangeable. After montmorillonite is modified by acid activation, interlayer pillaring, surface loading, grafting and other methods, the specific surface area increases, showing multi-mesoporous, strong adsorption and acidity, so that it can meet different uses and requirements. Therefore, modified montmoril...

Claims

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Application Information

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IPC IPC(8): B01J27/188C07C47/22C07C45/52
CPCB01J27/188C07C45/52C07C47/22
Inventor 俞卫华周春晖童东绅
Owner ZHEJIANG COLLEGE OF ZHEJIANG UNIV OF TECHOLOGY
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