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Ordered mesoporous silica material with pore wall being rich in micropore structures and preparation thereof

A mesoporous silica and microporous structure technology, applied in the direction of silica, silica, etc., can solve the problems of reduced silanol content, reduced intercalation, and less micropore content, and achieve high porosity, mesoporous The effect of concentrated pore size distribution and large specific surface area

Active Publication Date: 2019-10-22
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, as the hydrothermal treatment temperature increased, the hydrophilicity of the polyethylene oxide block in the triblock copolymer nonionic surfactant gradually weakened (Chem. Commun., 2001, 2726–2727), accompanied by The silanol content in the pore wall is significantly reduced due to the rapid polymerization of silicon species (J. Mater. Res. 2011, 26, 804-814), so that in the high-temperature strong acidic hydrothermal synthesis system, polyethylene oxide in the surfactant The embedding amount of alkane block in the silica mesoporous pore wall is significantly reduced, resulting in a relatively small amount of micropores in the pore wall of the prepared SBA-15 material, and it is difficult to effectively control

Method used

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  • Ordered mesoporous silica material with pore wall being rich in micropore structures and preparation thereof
  • Ordered mesoporous silica material with pore wall being rich in micropore structures and preparation thereof
  • Ordered mesoporous silica material with pore wall being rich in micropore structures and preparation thereof

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Experimental program
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Effect test

Embodiment 1

[0032] Under vigorous stirring at 25°C, add 2.5 g of organic template agent EO to 20 mL of absolute ethanol solution containing 0.35 g of citric acid and 0.5 g of deionized water 106 PO 70 EO 106 and 3.35 g of ethyl orthosilicate, completely dissolved to obtain a clear solution.

[0033] The obtained clear solution was poured into a sealed autoclave, and solvothermally pretreated at 100° C. for 24 hours to prepare a sol.

[0034] The obtained sol was transferred to a rotary evaporator, and the solvent was volatilized at 90°C to obtain a solid sample, and then roasted at 500°C for 5 hours to remove the organic template agent, and an ordered mesoporous silica material sample with pore walls rich in microporous structures was prepared.

[0035] figure 1 The XRD spectrum of the sample prepared above is given. It can be seen from the figure that the sample shows three obvious Bragg diffraction peaks at 2θ=1.03, 1.99 and 2.65°. By calculating the interplanar spacing correspondi...

Embodiment 2

[0039] Under vigorous stirring at 25°C, 3.2 g of EO was sequentially added to 30 mL of absolute ethanol solution containing 0.64 g of glacial acetic acid and 1.0 g of deionized water. 20 PO 70 EO 20 and 3.26 g of methyl orthosilicate, completely dissolved to give a clear solution.

[0040] The obtained clear solution was poured into a sealed autoclave, and subjected to solvothermal pretreatment at 80° C. for 24 hours to prepare a sol.

[0041] The obtained sol was transferred to a rotary evaporator, and the solvent was volatilized at 100°C to obtain a solid sample, and then roasted at 550°C for 5 hours to remove the organic template agent, and an ordered mesoporous silica material sample with pore walls rich in microporous structures was prepared.

[0042] XRD, TEM and N 2 The adsorption-desorption characterization results show that the prepared sample has a highly regular and ordered two-dimensional hexagonal mesoporous channel structure, and contains a large number of mic...

Embodiment 3

[0044] Under vigorous stirring at 25 °C, 3.5 g of EO was sequentially added to 25 mL of absolute ethanol solution containing 0.54 g of oxalic acid and 1.2 g of deionized water 20 PO 70 EO 20 and 3.86 g of ethyl orthosilicate, completely dissolved to obtain a clear solution.

[0045] The obtained clear solution was poured into a sealed autoclave, and solvothermally pretreated at 100° C. for 12 hours to prepare a sol.

[0046] The obtained sol was transferred to a rotary evaporator, and the solvent was volatilized at 80°C to obtain a solid sample, and then roasted at 500°C for 5 hours to remove the organic template agent, and an ordered mesoporous silica material sample with pore walls rich in microporous structures was prepared.

[0047] XRD, TEM and N 2 The adsorption-desorption characterization results show that the prepared sample has a highly regular and ordered two-dimensional hexagonal mesoporous channel structure, and contains a large number of micropores in the mesop...

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Abstract

The invention relates to an ordered mesoporous silica material with a pore wall being rich in micropore structures. The material is formed by sequentially dissolving a triblock copolymer nonionic surfactant, organic carboxylic acid and a silicon source in anhydrous ethanol containing a small amount of deionized water, and then sequentially performing solvent thermal treatment, solvent removal andcalcination treatment. The ordered mesoporous silica material has a highly orderly two-dimensional hexagonal mesoporous structure, high porosity, large specific surface area and uniform and adjustablemesoporous aperture, contains a large quantity of micropores, with adjustable contents, in the mesoporous wall, and shows a broader application prospect compared with the traditional microporous materials and mesoporous material in the fields of adsorption, separation and catalysis.

Description

technical field [0001] The invention belongs to the technical field of preparation of microporous-mesoporous composite porous materials, and relates to a microporous-mesoporous composite porous silicon oxide material, in particular to a kind of silicon oxide material with high specific surface area and pore volume, highly regular and orderly mesoporous structure, mesoporous A silicon oxide material with uniform and adjustable pore diameter, rich in micropores in the mesoporous pore wall, and a controllable content thereof, and a preparation method thereof. Background technique [0002] Microporous-mesoporous composite porous silica materials have well-developed pore structure, small bulk density, large specific surface area and pore volume, and stable chemical properties, which can effectively avoid the limitation of single-stage pore structure, and are conducive to integrating the structural advantages of micropores and mesoporous pores. Improve the physical and chemical pr...

Claims

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Application Information

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IPC IPC(8): C01B33/12
CPCC01B33/12C01P2006/16C01P2006/12C01P2006/14Y02C20/40
Inventor 潘大海王永杰于峰陈树伟闫晓亮范彬彬李瑞丰
Owner TAIYUAN UNIV OF TECH
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