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Novel method for controlling aperture and hole pitch of mesoporous materials

A mesoporous material and pore spacing technology, applied in the direction of silica, silicon oxide, etc., can solve the problems of high cost, complicated preparation, long reaction time, etc., and achieve high production efficiency, short reaction time and low cost.

Active Publication Date: 2010-06-09
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above methods can adjust the pore size of mesoporous materials to a certain extent, but they use a new type of template or add an auxiliary solvent to the reaction system, which has the disadvantages of complex preparation, high cost, and long reaction time.

Method used

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  • Novel method for controlling aperture and hole pitch of mesoporous materials
  • Novel method for controlling aperture and hole pitch of mesoporous materials
  • Novel method for controlling aperture and hole pitch of mesoporous materials

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Prepared with the following raw materials, the molar ratio is: ethyl orthosilicate (0.9): cetyltrimethylammonium bromide (0.09): absolute ethanol (9.1): deionized water (6): 37.5% concentrated Hydrochloric acid (0.0015).

[0028] a. Add 1.79g of cetyltrimethylammonium bromide to 27.2ml of absolute ethanol, then add 4.2ml of deionized water to the solution, stir for 10 minutes to make the solution uniform, then add 9.5ml of orthosilicic acid Ethyl ester, stirring was continued for 5 minutes. Finally, 0.8ml of 0.083mol / L hydrochloric acid solution was added to the solution, and the stirring was continued for 10 minutes to obtain the precursor.

[0029] b. Drop 6ml of the precursor solution prepared in step a on the silicon substrate, place the substrate loaded with the precursor in a vacuum oven, control the vacuum at 0.03, 0.05, 0.07 respectively, and set the temperature When the temperature is 40°C, the rate of solvent volatilization increases successively. After the...

Embodiment 2

[0036]Prepared with the following raw materials, the molar ratio is: ethyl orthosilicate (1.1): hexadecyltrimethylammonium bromide (0.11): absolute ethanol (10.8): deionized water (6.5): 37.5% concentrated Hydrochloric acid (0.0019).

[0037] a. Add 1.88g of cetyltrimethylammonium bromide to 30.2ml of absolute ethanol, then add 5.1ml of deionized water to the solution, stir for 10 minutes to make the solution uniform, then add 11.2ml of orthosilicic acid Ethyl ester, stirring was continued for 5 minutes. Finally, 1.2 ml of 0.083 mol / L hydrochloric acid solution was added to the solution, and the stirring was continued for 10 minutes to obtain a precursor.

[0038] b. Drop 6ml of the precursor solution prepared in step a on the silicon substrate, and place the substrate loaded with the precursor in a vacuum oven and a laboratory open system (air conditioner) respectively, set the temperature to 30°C, and solvent The volatilization rate of the former is lower than that of the ...

Embodiment 3

[0045] Prepared with the following raw materials, the molar ratio is: ethyl orthosilicate (1.0): cetyltrimethylammonium bromide (0.1): absolute ethanol (10): deionized water (6.3): 37.5% concentrated Hydrochloric acid (0.0017).

[0046] a. Add 1.82g of cetyltrimethylammonium bromide to 29.2ml of absolute ethanol, then add 4.8ml of deionized water to the solution, stir for 10 minutes to make the solution uniform, then add 10.8ml of orthosilicic acid Ethyl ester, stirring was continued for 5 minutes. Finally, 1 ml of 0.083 mol / L hydrochloric acid solution was added to the solution, and the stirring was continued for 10 minutes to obtain the precursor.

[0047] b. Drop 6ml of the precursor solution prepared in step a on the silicon substrate, and place the substrate loaded with the precursor in a blast oven with the temperature set at 30°C. Under this condition, the volatilization rate is fast, and after the solvent volatilizes, the silica mesoporous material containing the tem...

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Abstract

The invention discloses a novel method for controlling aperture and hole pitch of mesoporous materials, and belongs to the technical field of methods for preparing massive mesoporous materials. In the method, gelation time length in the process of synthesizing the massive mesoporous materials is adjusted for controlling the aperture and the hole pitch of the synthesized materials. The method comprises the following steps: preparing tetraethoxysilane, hexadecyl trimethyl ammonium bromide, absolute ethyl alcohol, deionized water and 37.5 percent concentrated hydrochloric acid in a molar ratio of 0.9-1.1: 0.09-0.11: 9.1-10.8: 6-6.5: 0.0015-0.0019 into sol-gel precursors; and dispersing the precursors on a silicon substrate and placing in different environments. The volatilization velocity is adjusted through environmental differences to further change gelation time. The method has the advantages of simple and fast operation, low cost without impurity, and no adverse effect on the mesoporous order degree of the materials.

Description

technical field [0001] The invention relates to a novel method for adjusting the pore diameter and pore spacing of a mesoporous material, belonging to the technical field of mesoporous material preparation. Background technique [0002] With the rapid development of the global petrochemical industry, porous materials as the carrier of its catalytic cracking have attracted more and more attention. As a new member of the porous material family, mesoporous materials have attracted worldwide attention as soon as they appeared. Because mesoporous materials have nanometer-sized pores, high specific surface area and single ordered mesoscopic structure, it has been widely used in the fields of catalysis, adsorption, chromatographic separation and microelectronics, and its ordered microscopic pore structure is also Mesoporous materials are widely used as sensors and carriers for some special microscopic reactions. [0003] As one of the key factors of mesoporous materials, mesoporo...

Claims

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Application Information

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IPC IPC(8): C01B33/12
Inventor 蔡强俞义轩
Owner TSINGHUA UNIV
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