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Yolk-eggshell-structured zeolite molecular sieve-mesoporous titanium oxide composite material 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: 2014-07-02
元颉新材料科技(浙江)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

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

Method used

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  • Yolk-eggshell-structured zeolite molecular sieve-mesoporous titanium oxide composite material and preparation method thereof
  • Yolk-eggshell-structured zeolite molecular sieve-mesoporous titanium oxide composite material and preparation method thereof
  • Yolk-eggshell-structured zeolite molecular sieve-mesoporous titanium oxide composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (I) Add 0.5 g ZSM-5 zeolite (Si / Al=100) into 280 mL deionized water, add 0.3 mL ammonia water, then add 0.4 g resorcinol and 0.6 mL formaldehyde, stir at 30 ℃ for 24 h , and then stirred at 80 °C for 5 h, the reaction solution turned into brick red, 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;

[0044] (II) Disperse the ZSM-5PF obtained in step (I) into 600 mL of ethanol, sonicate for 1 h, then add 1.8 mL of concentrated ammonia water, and then slowly add 12 mL of tetrabutyl titanate with a syringe (the dropwise addition is completed in 1 hour) ), stirred at 25 °C for 24 h, the color of the reaction solution changed from brick red to lighter, and centrifuged, the obtained solid product was washed with ethanol and deionized water three times, dried at 80 °C for 12 h, and finally calcined at 500 °C in air atmosphere for 2 h. h, ZSM-5TiO with high specific sur...

Embodiment 2

[0047] (I) Add 0.5 g ZSM-5 zeolite (Si / Al = 40) to 280 mL deionized water, add 0.3 mL ammonia water, then add 0.4 g phenol and 0.6 mL formaldehyde, stir at 30 °C for 24 h, and then Stirring at 80 °C for 24 h, the reaction solution turned yellow, 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 600 mL of ethanol, sonicate for 1 h, then add 1.8 mL of concentrated ammonia water, and then slowly add 6 mL of tetrabutyl titanate (0.5 hours) ), stirred at 25 °C for 24 h, the color of the reaction solution changed from yellow to light, centrifuged, the obtained solid product was washed three times with ethanol and deionized water, dried at 80 °C for 12 h, and finally calcined at 450 °C for 3 h in air atmosphere , to obtain ZSM-5TiO with a high specific surface area egg yolk-eggshell structure 2 Composite material, ...

Embodiment 3

[0051] (I) Add 0.5 g ZSM-5 zeolite (Si / Al = 200) into 280 mL deionized water, add 0.3 mL ammonia water, then add 0.4 g resorcinol and 0.6 mL formaldehyde, stir at 30 ℃ for 24 h , and then stirred at 80 °C for 24 h, the reaction solution turned into brick red, 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;

[0052] (II) Disperse the ZSM-5PF obtained in step (I) into 600 mL of ethanol, sonicate for 1 h, then add 1.8 mL of concentrated ammonia water, and then slowly add 18 mL of tetrabutyl titanate (1.5 hours) ), stirred at 25 °C for 24 h, the color of the reaction solution changed from brick red to light, and centrifuged, the obtained solid product was washed three times with ethanol and deionized water, dried at 80 °C for 12 h, and finally calcined at 450 °C in air atmosphere for 3 h, ZSM-5TiO with high specific surface area egg yolk-eggshell structure 2 Composite m...

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Abstract

The invention belongs to the technical fields of inorganic porous materials and catalysts and patricianly relates to a yolk-eggshell-structured zeolite molecular sieve-mesoporous titanium oxide composite material and a preparation method thereof. The composite material is characterized in that a yolk is made of zeolite molecular sieve materials, an eggshell is made of a mesoporous titanium oxide nanocrystal aggregate, and a size-adjustable cavity is formed between a zeolite molecular sieve and the mesoporous titanium oxide. The preparation method comprises the steps of wrapping a phenolic resin macromolecule layer or amorphous silicon dioxide on the outer surface of the zeolite molecular sieve, then wrapping a layer of amorphous silicon dioxide, forging to transform the titanium dioxide into crystallized titanium dioxide nanocrystals, and finally removing the phenolic resin macromolecule layer or the amorphous silicon dioxide, so as to obtain the targeted composite material. The method is simple and is easy to control. The composite material has a hierarchical pore structure and can be taken as a catalyst or a catalyst carrier for continuous reaction as well 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 (< 2 nm), 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(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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