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Preparation method of transparent mesoporous silica gel monolith

A mesoporous silica and gel technology, applied in the direction of silica, silica, etc., can solve the problems of industrial production of unfavorable materials, harsh equipment requirements, and complicated operation steps, so as to shorten the preparation cycle, simplify operating conditions, The effect of simplifying compositing procedures

Inactive Publication Date: 2012-05-09
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods generally have harsh requirements on equipment, high energy consumption, very long time (about 8-12 weeks), or complicated operation steps, which are not conducive to the industrial production of such materials.
For example, the patent No.: ZL200310108844.X, the patent No.: ZL200410061428.3 and the patent No.: 2008100550608 invention technical scheme, need to introduce an inert medium as a shape protection agent, and need to adopt complex vacuuming and hydrothermal gelation treatment In the process, it is necessary to introduce short-chain alcohols that have a destructive effect on the order of the mesoporous structure as a co-solvent, and it is necessary to use a slow process of sol-to-gel conversion in a plastic film sealed container with 3-5 pinholes. Harsh operating conditions, long preparation cycle and low preparation efficiency

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0012] 1 g of P123, 0.18 g of water, 0.2 g of 1M hydrochloric acid and 2.08 g of TEOS were mixed and stirred at room temperature for 30 minutes to form a homogeneous sol. Transfer the prepared sol into a container with a certain shape, seal it, and let it stand at a constant temperature at 45° C. for 1 hour, then leave the container open and let it stand at 45° C. for 5.75 hours to make the system gel. Then seal the container again and leave it to age at a constant temperature of 45°C for 1 day, and finally directly dry it in the open at 45°C, and obtain a complete transparent mesoporous silica gel monolith after 48 hours. Then the temperature was raised to 550°C at a rate of 2°C / min and calcined for 6 hours to completely remove the surfactant template to obtain an ordered mesoporous silica monolithic material. XRD, N 2 Analytical tests such as isothermal adsorption show that the obtained material has a high-quality hexagonal phase structure, and its specific surface area is 5...

Embodiment approach 2

[0014] 1 g of P123, 0.18 g of water, 0.2 g of 1M hydrochloric acid and 2.08 g of TEOS were mixed and stirred at room temperature for 30 minutes to form a homogeneous sol. Transfer the prepared sol into a container with a certain shape, seal it, and let it stand at a constant temperature of 60° C. for 1 hour, then leave the container open and let it stand at 60° C. for 3.5 hours to make the system gel. Then seal the container again and leave it to age at a constant temperature of 60°C for 1 day, and finally directly dry it in the open at 60°C, and obtain a complete transparent mesoporous silica gel monolith after 30 hours. Then, the temperature was raised to 550° C. at a rate of 2° C. / min and baked for 6 hours to completely remove the surfactant template. Others were the same as Embodiment 1.

Embodiment approach 3

[0016] 1 g of P123, 0.18 g of water, 0.2 g of 1M hydrochloric acid and 2.08 g of TEOS were mixed and stirred at room temperature for 30 minutes to form a homogeneous sol. Transfer the prepared sol into a container with a certain shape, seal it, and let it stand at a constant temperature of 80°C for 1 hour, then leave the container open and let it stand at 80°C for 1.5 hours to make the system gel. Then seal the container again and leave it to age at a constant temperature of 80°C for 1 day, and finally dry it in the open at 80°C, and obtain a complete transparent mesoporous silica gel monolith after 18 hours. Then the temperature was raised to 550°C at a rate of 2°C / min and calcined for 6 hours to completely remove the surfactant template to obtain an ordered mesoporous silica monolithic material. XRD, N 2 Analytical tests such as isothermal adsorption show that the obtained material has a high-quality hexagonal phase structure, and its specific surface area is 614.75m 2 / g, ...

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Abstract

The invention relates to a rapid preparation method of a transparent mesoporous silica gel monolith, which belongs to the technical field of the inorganic porous material, in particular to a technical scheme of a simple, efficient, rapid and convenient preparation method of a large-sized, crack-free and optically transparent ordered mesoporous silica gel monolith. The preparation method is characterized in that the direction conversion of gel melting, condensation, aging and drying can be realized at a high temperature through adjusting a synthesis ratio without special protection means and complex operating procedures. Moreover, the method has the advantages of short synthesis period, simple operating steps and easy control. The material prepared in the method has an ordered two-dimensional and hexagonal-phase mesoporous structure, the pore size is 2.0-7.0nm, the pore volume is 0.5-0.8 cm3 / g, and the specific surface area is 500-1000m2 / g. Therefore, the material has extensive application value in research and development of optical, electrical and magnetic devices.

Description

technical field [0001] The invention discloses a method for preparing transparent mesoporous silica gel monolith, which belongs to the technical field of inorganic porous materials, and specifically relates to a rapid method for realizing direct open conversion between sol-wet gel-xerogel at a constant temperature Method for preparing large-sized, crack-free and optically transparent mesoporous silica gel monoliths. Background technique [0002] At present, the synthesis of transparent mesoporous silica gel monoliths is usually prepared by the solvent evaporation method or microemulsion method induced by different template agents. In order to avoid the cracking of the synthetic gel during the drying process, a multi-step operation of controlling the slow evaporation of the solvent, supercritical extraction, vacuum drying, introducing an inert medium as a shape protection agent, and combining vacuum and hydrothermal treatment is generally used. A method such as a slow gelati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/16
Inventor 王晓钟陈德贵畅通谢克昌
Owner TAIYUAN UNIV OF TECH
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