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
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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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