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Zeolite molecular sieve-mesoporous titanium oxide composite material with egg yolk-eggshell structure and preparation method thereof

A technology of zeolite molecular sieve and mesoporous titanium oxide, which can be used in molecular sieve catalysts, chemical instruments and methods, silicon compounds, etc., and can solve problems such as limitations

Active Publication Date: 2016-01-13
元颉新材料科技(浙江)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the limitation of its pore size (<2nm), its wide application in modern chemical industry, petrochemical and other fields is limited to a certain extent.

Method used

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  • Zeolite molecular sieve-mesoporous titanium oxide composite material with egg yolk-eggshell structure and preparation method thereof
  • Zeolite molecular sieve-mesoporous titanium oxide composite material with egg yolk-eggshell structure and preparation method thereof
  • Zeolite molecular sieve-mesoporous titanium oxide composite material with egg yolk-eggshell structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (I) Add 0.5g of ZSM-5 zeolite (Si / Al=100) into 280mL of deionized water, add 0.3mL of ammonia water, then add 0.4g of resorcinol and 0.6mL of formaldehyde, stir at 30°C for 24h, and then Stir at 80°C for 5 hours, the reaction solution turns brick red, centrifuge, and the solid product obtained is washed three times with ethanol and deionized water respectively, to obtain ZSM-5PF with a core-shell structure;

[0044] (II) Disperse the ZSM-5PF obtained in step (I) into 600mL of ethanol, sonicate for 1h, then add 1.8mL of concentrated ammonia water, and then slowly add 12mL of tetrabutyl titanate dropwise with a syringe (the dropwise addition is completed in 1 hour), 25 Stir at ℃ for 24 hours, the color of the reaction solution turns from brick red to light, centrifuge, and the solid product obtained is washed 3 times with ethanol and deionized water, dried at 80℃ for 12h, and finally calcined at 500℃ for 2 hours in an air atmosphere to obtain a high specific surface area ...

Embodiment 2

[0047] (I) Add 0.5g of ZSM-5 zeolite (Si / Al=40) into 280mL of deionized water, add 0.3mL of ammonia water, then add 0.4g of phenol and 0.6mL of formaldehyde, stir at 30°C for 24h, then stir at 80°C After 24 hours, the reaction solution turned yellow and was centrifuged, and the obtained solid product was washed three times with ethanol and deionized water respectively to obtain ZSM-5PF with a core-shell structure;

[0048] (II) Disperse the ZSM-5PF obtained in step (I) into 600mL of ethanol, sonicate for 1h, then add 1.8mL of concentrated ammonia water, then slowly add 6mL of tetrabutyl titanate dropwise with a syringe (0.5 hours to complete), 25 Stir at ℃ for 24 hours, the color of the reaction solution turns from yellow to lighter, and centrifuge to separate the obtained solid product, which is washed three times with ethanol and deionized water, dried at 80℃ for 12 hours, and finally roasted at 450℃ for 3 hours in an air atmosphere to obtain egg yolk with high specific surfa...

Embodiment 3

[0051] (I) Add 0.5g of ZSM-5 zeolite (Si / Al=200) into 280mL of deionized water, add 0.3mL of ammonia water, then add 0.4g of resorcinol and 0.6mL of formaldehyde, stir at 30°C for 24h, and then Stir at 80°C for 24 hours, the reaction solution turns brick red, centrifuge, and the obtained solid product is washed three times with ethanol and deionized water respectively, to obtain ZSM-5PF with a core-shell structure;

[0052] (II) Disperse the ZSM-5PF obtained in step (I) into 600mL ethanol, sonicate for 1h, then add 1.8mL concentrated ammonia water, and then slowly add 18mL tetrabutyl titanate dropwise with a syringe (1.5 hours to complete), 25 Stir at ℃ for 24 hours, the color of the reaction solution turns from brick red to lighter, and centrifuge to separate the obtained solid product, which is washed three times with ethanol and deionized water, dried at 80℃ for 12 hours, and finally calcined at 450℃ for 3 hours in an air atmosphere to obtain a high specific surface area ZS...

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Abstract

The invention belongs to the technical field of inorganic porous materials and catalysts, in particular to a zeolite molecular sieve-mesoporous titanium oxide composite material with a high specific surface area egg yolk-eggshell structure and a preparation method thereof. The composite material uses zeolite molecular sieve materials as egg yolk, and mesoporous titanium dioxide nano crystal grain aggregates as eggshell, and there is a cavity with adjustable size between the zeolite molecular sieve and mesoporous titanium dioxide. The preparation method is to wrap a layer of phenolic resin macromolecule or amorphous silica on the surface of zeolite molecular sieve, and then wrap a layer of amorphous titanium dioxide, convert the titanium dioxide into crystalline titanium dioxide nanocrystals by calcining, and finally remove the phenolic resin polymer layer or amorphous silica to obtain the target composite material; the method is simple and the control is easy. The composite material has a multi-level porous structure and can be used as a catalyst or catalyst carrier for continuous reactions, and can also be used as an adsorption-catalysis composite material.

Description

technical field [0001] The invention belongs to the technical field of inorganic porous materials and catalysts, and specifically relates to a zeolite molecular sieve-mesoporous titanium oxide composite material with a high specific surface area egg yolk-eggshell structure and a preparation method thereof. Background technique [0002] Zeolite molecular sieves are widely used in the fields of adsorption, separation and catalysis. However, due to the limitation of its pore size (<2nm), its wide application in modern chemical industry, petrochemical and other fields is limited. In recent years, core-shell materials with zeolite molecular sieve as the core and mesoporous silica and mesoporous carbon materials as the shell have been intensively studied. A mesoporous silica or mesoporous carbon layer is wrapped on the surface of the zeolite molecular sieve, which not only introduces a multi-level pore structure and a gradient distribution of acid centers, but also performs di...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/40B01J29/035B01J29/08B01J32/00B01J35/10B01J20/18B01J20/10B01J20/28B01J20/30
Inventor 薛招腾冯珊珊高文君李伟李彬赵东元
Owner 元颉新材料科技(浙江)有限公司
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