Green preparation method of transparent mesoporous sial gel monolith

A mesoporous silica-alumina and gel technology, applied in the field of inorganic porous materials, can solve the problems of increased preparation cost, unfavorable gel skeleton, harsh equipment requirements, etc., and achieves rich adjustable range, wide adjustable range, and reduced preparation. cost effect

Inactive Publication Date: 2013-03-20
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Obviously, the use of such dangerous and corrosive inorganic strong acids as catalysts for the hydrolysis of organosilicon sources not only increases the preparation cost, but also easily causes environmental pollution, and the highly acidic synthesis medium is also not conducive to the embedding of high aluminum content in the gel skeleton. At the same time, there are strict requirements on equipment during industrial batch preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0016] Stir and mix 0.75 g of P123, 0.375 g of aluminum nitrate, 0.098 g of water and 1.12 ml of TEOS at room temperature, and continue to stir for 60 minutes after the system is completely homogeneous. The system will be gelled by standing at constant temperature for 1 hour, and then continue to age in a sealed state at 60°C for 1 day, and finally dry it directly at 60°C. After 48 hours, a complete transparent medium with the shape of a container is obtained. Porous silica-alumina gel monolith, then heated up to 600°C at a rate of 2°C / min and calcined for 6 hours to completely remove the surfactant template agent, and the specific surface area of ​​the mesoporous silica-alumina gel monolith was 397.1m 2 / g, the pore volume is 0.31cm 3 / g, the pore size is 3.6nm.

Embodiment approach 2

[0018]Stir and mix 0.5 g of P123, 0.094 g of aluminum nitrate, 0.188 g of water and 1.12 ml of TEOS at room temperature, and continue to stir for 60 minutes after the system is completely homogeneous. Stand at constant temperature for 1 hour at 60°C, then leave the container open at 60°C for 30 minutes to gel the system, then seal the container again and leave it at 60°C for aging for 1 day, and finally place it directly at 60°C Drying in the open, after 48 hours, a complete transparent mesoporous silica-alumina gel monolith with a container shape was obtained, and then the temperature was raised to 600°C at a rate of 2°C / min and calcined for 6 hours to completely remove the surfactant template agent to obtain a mesoporous silica-alumina gel monolith. Porous silica-alumina gel monolith has a specific surface area of ​​565.4m 2 / g, the pore volume is 0.41cm 3 / g, the pore size is 3.5nm.

Embodiment approach 3

[0020] Stir and mix 0.75 g of F127, 0.375 g of aluminum nitrate, 0.098 g of water, 1.5 ml of n-propanol and 1.12 ml of TEOS at room temperature, and continue stirring for 30 minutes after the system is completely homogeneous, and then transfer the prepared sol into a container with a certain shape After sealing, let it stand at a constant temperature at 60°C for 1 hour, then leave the container at 60°C for 3.5 hours to make the system gel, then seal the container again and leave it at a constant temperature at 60°C for 1 day, and finally directly Open-dried at 60°C, after 48 hours, a complete transparent mesoporous silica-alumina gel monolith with a container shape was obtained, and then heated to 600°C at a rate of 2°C / min and baked for 6 hours to completely remove the surfactant template agent, the specific surface area of ​​the mesoporous silica-alumina gel monolith is 447.9m 2 / g, the pore volume is 0.34cm 3 / g, the pore size is 3.5nm.

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Abstract

The invention provides a green preparation method of transparent mesoporous sial gel monolith, belongs to the technical field of inorganic porous materials, and particularly relates to a quick preparation method of large-sized, crack-free and optically-transparent mesoporous sial gel monolith with a mole ratio of Si to Al being not less than 3. According to the method, inorganic strong acid which has dangerousness and corrosivity is not added to be served as a catalyst, the added aluminium salt is hydrated to generate mild acid condition to introduce the silicon source to be hydrated; the scope of the mole ratio of Si to H2O in the synthesis system is strictly controlled, and the method of gelation of the system is relatively carried out, thus the wet sial gel is directly transferred into dry gel at 45 to 75 DEG C in an open way. The method is simple, efficient and environment-friendly; the prepared transparent mesoporous sial gel monolith is regular in shape, controllable in dimension, high in transparence, and high in application value in the field of development of novel optical devices; and the mesoporous sial gel monolith with a template agent removed in roasting has the specific surface area of 390 to 800m<2> / g, pore volume of 0.3 to 0.5cm<3> / g, and aperture of 1.9 to 4nm, and has a wide application prospect in the fields of catalysis and separation.

Description

technical field [0001] The invention relates to a green preparation method of transparent mesoporous silica-alumina gel monolith, which belongs to the technical field of inorganic porous materials, and specifically relates to a large-sized, crack-free, optically transparent mesoporous silicon with a component Si / Al molar ratio ≥ 3 Green preparation method of aluminum gel monolith. Background technique [0002] The transparent mesoporous gel monolith formed by surfactant as a template has high light transmittance, low external area and adjustable pore structure, which can make dye molecules, photosensitive molecules, semiconductor particles or Guest molecules such as conductive nanowires can be intercalated at a high concentration without mutual aggregation between molecules, so they have broad application prospects in the development of new optical devices. [0003] The synthesis of transparent mesoporous silica-alumina gel monolith, due to the introduction of Al atoms in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B38/00
Inventor 王晓钟白亚东李祥珍谢克昌
Owner TAIYUAN UNIV OF TECH
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