In situ crystilization assembling method for heteropolyacid nano particles in mesoporous material

A mesoporous material, in-situ crystallization technology, applied in the in-situ crystallization and assembly of heteropolyacid nanoparticles in mesoporous materials, and the in-situ crystallization of heteropolyacid nanoparticles in mesoporous silica materials In the field of assembly, to achieve the effect of efficient catalysis of organic reactions

Inactive Publication Date: 2006-02-22
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The impregnation method is mostly used in the background technology, and mesoporous SiO such as ZSM and MCM-41 with small pore size (2 Molecular sieves are used as carriers to adsorb heteropolyacids to the pores or surfaces of mesoporous molecular sieves. The heteropolyacids in the pores have always existed in the form of monomolecular or monolayer distributed amorphous forms. The disadvantage is that heteropolyacids will not form in nanometer The particle form is assembled into a mesoporous molecular sieve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The first step carrier preparation and processing

[0018] Prepare SBA-15 silica mesoporous material with relatively large mesoporous pores with a pore size of 10-40nm according to the literature method, take 1g of the material in an autoclave, add water until the material is submerged, and then add diethyl ether on the water surface L, diethyl ether The volume is equal to that of water, hydrothermally treated at 80°C for 24 hours, and filtered with suction to obtain water-saturated SBA-15 silica mesoporous material;

[0019] The second step is to prepare heteropoly acid ether compound

[0020] The ether compound of the heteropolyacid is prepared by the traditional diethyl ether acidification extraction method for later use, wherein the heteropolyacid is 1:12 structure H 3或4 XM 12 o 40 The heteropoly acid, in the molecular formula, X=P, Si or Ge, M=W or Mo;

[0021] The third step is the in-situ crystallization assembly of heteropolyacid nanoparticles in mesoporous ...

Embodiment 2

[0024] The first step carrier preparation and processing

[0025] Prepare SBA-15 silica mesoporous material with relatively large mesoporous pores with a pore size of 10-40 nm according to the literature method, take 1 g of the material in an autoclave, add water until the material is submerged, and then add diethyl ether on the water surface, diethyl ether The volume is equal to that of water, hydrothermally treated at 80°C for 24 hours, and filtered with suction to obtain water-saturated SBA-15 silica mesoporous material;

[0026] The second step is to prepare heteropolyacid etherate

[0027] The ether compound of the heteropolyacid is prepared by the traditional diethyl ether acidification extraction method for later use, wherein the heteropolyacid is 1:12 structure H 3或4 XM 12 o 40 The heteropoly acid, in the molecular formula, X=P, Si or Ge, M=W or Mo;

[0028] The third step is the in-situ crystallization assembly of heteropolyacid nanoparticles in mesoporous materia...

Embodiment 3

[0031] The first step carrier preparation and processing

[0032] Prepare SBA-15 silica mesoporous material with relatively large mesoporous pores with a pore size of 10-40 nm according to the literature method, take 1 g of the material in an autoclave, add water until the material is submerged, and then add diethyl ether on the water surface, diethyl ether The volume is equal to that of water, hydrothermally treated at 80°C for 24 hours, and filtered with suction to obtain water-saturated SBA-15 silica mesoporous material;

[0033] The second step is to prepare heteropolyacid etherate

[0034] The ether compound of the heteropolyacid is prepared by the traditional diethyl ether acidification extraction method for later use, wherein the heteropolyacid is 1:12 structure H 3或4 XM 12 o 40 The heteropoly acid, in the molecular formula, X=P, Si or Ge, M=W or Mo;

[0035] The third step is the in-situ crystallization assembly of heteropolyacid nanoparticles in mesoporous materia...

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Abstract

The present invention relates to in-situ crystallization assembling process of nano heteropolyacid particles in mesoporous material, and belongs to the field of inorganic chemical synthesis technology. SBA-15 SiO2 material with relatively large mesopores of 10-40 nm size is added with ether compound of heteropolyacid for hydrolysis under hydrothermal condition, and through further in-situ crystallization, suction filtering, ether washing and stoving, the mesoporous material with in-situ crystallized and assembled nano heteropolyacid particles is obtained. The present invention has the outstanding effects of SBA-15 SiO2 material as carrier with relatively large mesopores favorable to heteropolyacid to enter into; high pressure hydrothermally produced favorable to the crystallization of heteropolyacid; in-situ crystallization to form nano heteropolyacid particles; and homogeneous dispersion of nano heteropolyacid particles forming excellent nano catalyst.

Description

technical field [0001] The invention relates to an in-situ crystallization assembly method of heteropolyacid nanoparticles in mesoporous materials, more precisely, relates to an in-situ crystallization assembly method of heteropolyacid nanoparticles in mesoporous silica materials , belongs to the technical field of inorganic chemical synthesis. Background technique [0002] Heteropolyacids have catalytic properties such as acidity, oxidation-reduction, "pseudo-liquid phase" behavior, polymerization inhibition, multi-function (acid, oxidation-reduction, photoelectromagnetic), low temperature and high activity, etc. Catalysis holds tantalizing practical prospects. So far, there have been 8 chemical processes that have been industrialized using heteropolyacid catalysts. However, the heteropoly acid itself has problems such as small specific surface area, easy dissolution and separation in homogeneous reaction, difficult separation, corrosion and pollutio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/035
Inventor 单永奎余淑媛孔爱国何鸣元
Owner EAST CHINA NORMAL UNIV
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