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

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

Inactive Publication Date: 2004-12-15
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 a large mesoporous SBA-15 silica mesoporous material with a pore diameter of 10-40nm according to the literature method. Take 1g of this material in an autoclave, add water until the material is submerged, and then add ether and ether on the water surface. The volume of SBA-15 is equal to that of water. The hydrothermal treatment is carried out at 80℃ for 24 hours and then filtered by 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 heteropoly acid is prepared by traditional ether acidification extraction method, and the heteropoly acid is 1:12 structure H 3 or 4 XM 12 O 40 (X=P, Si, Ge, M=W, Mo);

[0021] Step 3: In-situ crystallization assembly of heteropolyacid nanoparticles in mesoporous materials

[0022] Take 1g of water-saturated SBA-15 silica mesoporous material as the carrier in ...

Embodiment 2

[0024] The first step: carrier preparation and processing

[0025] Prepare a large mesoporous SBA-15 silica mesoporous material with a pore diameter of 10-40nm according to the literature method. Take 1g of this material in an autoclave, add water until the material is submerged, and then add ether and ether on the water surface. The volume of SBA-15 is equal to that of water. The hydrothermal treatment is carried out at 80℃ for 24 hours and then filtered by suction to obtain water-saturated SBA-15 silica mesoporous material;

[0026] The second step is to prepare heteropoly acid ether compound

[0027] The ether compound of heteropoly acid is prepared by traditional ether acidification extraction method, and the heteropoly acid is 1:12 structure H 3 or 4 XM 12 O 40 (X=P, Si, Ge, M=W, Mo);

[0028] Step 3: In-situ crystallization assembly of heteropolyacid nanoparticles in mesoporous materials

[0029] Take 1g of water-saturated SBA-15 silica mesoporous material as the carrier in ...

Embodiment 3

[0031] The first step: carrier preparation and processing

[0032] Prepare a large mesoporous SBA-15 silica mesoporous material with a pore diameter of 10-40nm according to the literature method. Take 1g of this material in an autoclave, add water until the material is submerged, and then add ether and ether on the water surface. The volume of SBA-15 is equal to that of water. The hydrothermal treatment is carried out at 80℃ for 24 hours and then filtered by suction to obtain water-saturated SBA-15 silica mesoporous material;

[0033] The second step is to prepare heteropoly acid ether compound

[0034] The ether compound of heteropoly acid is prepared by traditional ether acidification extraction method, and the heteropoly acid is 1:12 structure H 3 or 4 XM 12 O 40 (X=P, Si, Ge, M=W, Mo);

[0035] Step 3: In-situ crystallization assembly of heteropolyacid nanoparticles in mesoporous materials

[0036] Take 1g of water-saturated SBA-15 silica mesoporous material as the carrier in ...

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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 a method for in-situ crystallization assembly of heteropoly acid nanoparticles in mesoporous materials, specifically, to a method for in-situ crystallization assembly of heteropoly acid nanoparticles in mesoporous silica materials , Belongs to the technical field of inorganic chemical synthesis. Background technique [0002] Heteropolyacids also have catalytic properties such as acidity, oxidation-reduction, "pseudo-liquid phase" behavior, polymerization inhibition, multi-functionality (acid, oxidation-reduction, photoelectromagnetic), low temperature and high activity, etc., and are used in atomic economic reactions and environmentally friendly Catalysis has attractive practical prospects. So far, there have been 8 chemical processes using heteropolyacid catalysts to achieve industrial production. However, the heteropoly acid itself has a small specific surface area, easy to dissolve in a homogeneous reaction, ...

Claims

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Application Information

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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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