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, 2

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

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0031] Example 1.

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

[0033] Pour the obtained clear solution into a sealed autoclave, and solvothermally preprocess it at 100° C. for 24 h to prepare a sol.

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

[0035] figure 1 The XRD spectra of the samples prepared above are 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 corresponding to each diffraction peak, it is proved t...

Example Embodiment

[0038] Example 2.

[0039] Under strong stirring at 25℃, add 3.2g EO to 30mL absolute ethanol solution containing 0.64g glacial acetic acid and 1.0g deionized water. 20 PO 70 EO 20 And 3.26g methyl orthosilicate, completely dissolved to obtain a clear solution.

[0040] Pour the obtained clear solution into a sealed autoclave, and solvothermally preprocess it at 80° C. for 24 hours to prepare a sol.

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

[0042] XRD, TEM and N 2 The adsorption-desorption characterization results show that the prepared samples have a highly regular and orderly two-dimensional hexagonal mesoporous pore structure, and there are a large number of micropores in the mesoporous pore wall. Calculate the average mesop...

Example Embodiment

[0043] Example 3.

[0044] Under strong stirring at 25℃, add 3.5g EO to 25mL absolute ethanol solution containing 0.54g oxalic acid and 1.2g deionized water. 20 PO 70 EO 20 And 3.86g of ethyl orthosilicate, completely dissolved to obtain a clear solution.

[0045] Pour the obtained clear solution into a sealed autoclave, and solvothermally preprocess it at 100° C. for 12 hours to prepare a sol.

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

[0047] XRD, TEM and N 2 The adsorption-desorption characterization results show that the prepared samples have a highly regular and orderly two-dimensional hexagonal mesoporous pore structure, and there are a large number of micropores in the mesoporous pore wall. Calculate the average mesoporous ...

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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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