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Macropore-mesopore ordered magnesium-aluminum composite oxide material and preparation method thereof

A technology of mesoporous ordering and aluminum compounding, which is applied in the preparation of alumina/hydroxide, preparation of liquid hydrocarbon mixtures, aluminum compounds, etc., can solve the problems of collapse of alumina mesoporous skeleton structure, few catalytic active sites, poor Alkali catalytic conversion activity and other issues, to achieve high catalytic activity, process is simple and easy, high thermal stability

Active Publication Date: 2017-08-01
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the pore walls of the ordered alumina mesoporous materials prepared by the EISA method are still mainly composed of amorphous hydroxyl aluminum, which makes the aluminum species on the pore walls very vulnerable to the attack of water molecules during the post-treatment process of impregnating alkaline active species. The hydrolysis reaction of the skeleton Al-O-Al bond occurs, resulting in the collapse of the alumina mesoporous skeleton structure (Angew. Chem.-Int. Edit. 2008,47, 3418.)
[0006] In addition, when mesoporous alumina-supported solid base catalytic materials are prepared by traditional methods, the obtained materials are often a mixture of alumina and alkali metal or alkaline earth metal oxides, and it is difficult to achieve highly uniform dispersion of basic active species (such as magnesium oxide) , resulting in relatively few catalytically active sites (Micropor. Mesopor. Mater. 2010, 128, 41.)
In addition, the single mesoporous channel structure is not conducive to the rapid diffusion of organic macromolecules such as biodiesel, resulting in poor alkali catalytic conversion activity of organic macromolecules supported by alumina mesoporous materials (Micropor. Mesopor. Mater. 2010, 128, 41.)

Method used

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  • Macropore-mesopore ordered magnesium-aluminum composite oxide material and preparation method thereof
  • Macropore-mesopore ordered magnesium-aluminum composite oxide material and preparation method thereof
  • Macropore-mesopore ordered magnesium-aluminum composite oxide material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0038] Under strong stirring at 30°C, add 0.4g citric acid and 3.2g EO to 20mL absolute ethanol solution containing 1.5g 6M nitric acid 106 PO 70 EO 106 , 0.51g of magnesium nitrate hexahydrate and 3.27g of aluminum isopropoxide were completely dissolved to obtain a clear solution; the resulting clear solution was poured into a sealed autoclave for solvothermal pretreatment at 80°C for 24 hours; subsequently, the resulting reaction solution was poured 0.7 g of polystyrene microspheres with a particle diameter of 200 nm were added to a petri dish, and after ultrasonication at 25 °C for 1 h, the solvent was volatilized at 60 °C for 24 h in an open state; finally, the obtained solid sample was roasted at 550 °C for 5 h, In addition to organic templates existing in mesoporous channels and polystyrene microspheres with macroporous structures, magnesium-aluminum composite oxides with highly ordered two-dimensional hexagonal mesoporous structures and network-like three-dimensional o...

Embodiment 2

[0047] Under vigorous stirring at 35°C, add 0.6 g of glacial acetic acid and 3.5 g of EO to 20 mL of absolute ethanol solution containing 1.8 g of 6M hydrochloric acid 106 PO 70 EO 106 , 1.0g magnesium nitrate hexahydrate and 3.95g aluminum tert-butoxide were completely dissolved to obtain a clear solution; the resulting clear solution was poured into a sealed high-pressure reactor, and solvothermal pretreatment was performed at 100°C for 24 hours; subsequently, the resulting reaction solution was poured into 0.7 g of polystyrene microspheres with a particle size of 200 nm were added to a petri dish, and after ultrasonication at 35 °C for 1 h, the solvent was volatilized at 60 °C for 24 h in an open state; finally, the obtained solid sample was roasted at 650 °C for 5 h, The magnesium-aluminum composite oxide sample is obtained by removing the organic template agent existing in the mesoporous channel and the polystyrene microspheres that produce a macroporous structure.

[0...

Embodiment 3

[0052] Under strong stirring at 40°C, add 0.4g oxalic acid and 2.0g EO to 20mL absolute ethanol solution containing 1.0g 6M nitric acid 20 PO 70 EO 20 , 0.1g of magnesium oxide and 6.0g of aluminum nitrate were completely dissolved to obtain a clear solution; the resulting clear solution was poured into a sealed autoclave, and solvothermal pretreatment was performed at 120°C for 24 hours; then, the resulting reaction solution was poured into a petri dish , adding 0.7g of polystyrene microspheres with a particle size of 300nm, ultrasonication at 40°C for 1h, and solvent volatilization at 80°C for 24h in an open state; finally, the obtained solid sample was roasted at 650°C for 5h to remove the The organic template agent in the pore channel and the polystyrene microspheres with macroporous structure were used to obtain the magnesium-aluminum composite oxide sample.

[0053] The XRD, SEM and nitrogen adsorption characterization results confirmed that the obtained magnesium-alum...

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Abstract

The invention relates to a macropore-mesopore ordered magnesium-aluminum composite oxide material and a preparation method thereof. The preparation method comprises the following steps of dissolving inorganic acid, organic carboxylic acid, a block copolymer non-ionic surfactant, a magnesium source and an aluminum source into absolute ethyl alcohol, preheating in solvent under the sealing condition at high pressure, adding organic high polymer microspheres, volatilizing the solvent under the opening condition, and calcining at the temperature of 450 to 750 DEG C, so as to obtain the macropore-mesopore ordered magnesium-aluminum composite oxide material. The prepared macropore-mesopore ordered magnesium-aluminum composite oxide material has the advantages that the lattice three-dimensional ordered macroporous structure, the highly regular ordered two-dimensional hexagonal mesoporous structure and the larger specific surface area and pore volume are realized; the diameters of macropore and mesopore can be adjusted; the alkaline matter can be highly and uniformly dispersed in the wall of mesopore at atom level; the heat stability is higher, and the alkaline catalytic conversion property on organic macromolecules is effectively improved.

Description

technical field [0001] The invention relates to a magnesium-aluminum composite oxide material, especially a material with high specific surface area and pore volume, highly ordered mesopore structure, uniform and adjustable macropore diameter, and highly uniformly dispersed magnesium and aluminum species on the pore wall at the atomic level. A highly thermally stable and ordered macroporous-mesoporous magnesium-aluminum composite oxide alkaline material and a preparation method thereof. Background technique [0002] Ordered alumina mesoporous materials are beneficial to strong alkaline species due to their highly regular pore structure, large specific surface area and pore volume, concentrated and adjustable mesoporous pore size, and no reaction with strong alkaline species. A large amount of introduction and stabilization in its mesoporous channels brings hope for the preparation of high-performance supported solid base catalytic materials, and has become a research hotspot...

Claims

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Application Information

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IPC IPC(8): C01F7/30C01F7/32B01J21/10C10G3/00C11C3/00
CPCY02P30/20C01F7/30B01J21/10B01J23/002C01F7/308C01F7/32C01P2002/72C01P2004/03C01P2006/10C01P2006/14C01P2006/16C01P2006/17C01P2006/90C10G3/44C11C3/003
Inventor 潘大海朱淑英陈树伟于峰崔杏雨陈伟李瑞丰
Owner TAIYUAN UNIV OF TECH
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