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Preparation method of silicon-based dual mesoporous material

A dual-mesoporous, silicon-based technology, applied in the direction of silicon oxide, can solve the problems of sensitive preparation conditions, complicated operation process, and difficult control, and achieve the effects of strong controllability, improved synthesis efficiency, and easy operation

Inactive Publication Date: 2015-07-01
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The research on silicon-based dual-mesoporous materials is still in the initial stage of exploration. The most researched is the sol-gel method, including single-template method and double-template method. The single-template method is similar to the synthesis process of single-mesoporous materials, but requires Add additives, and the preparation conditions are usually sensitive and difficult to control
The double-template method uses two templates to synthesize double-mesoporous silicon in two steps. First, the single-mesoporous silicon-based material is prepared by the traditional method, and then the template is added to hydrothermally synthesize large mesoporous pores. Solvent evaporation can also be used to guide the formation of double-mesoporous silicon. These methods There are disadvantages such as complicated operation process and difficult control

Method used

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  • Preparation method of silicon-based dual mesoporous material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] ① Take 1 g of template agent P123 and 24.5 g of deionized water, put it into a crystallization bottle, stir it in a constant temperature water bath at 45 ℃ until it is completely dissolved (about 4 hours), then add 6.3 g of it with a mass concentration of 36% Concentrated hydrochloric acid, adjust the pH value to <1, continue to stir for 0.5 hours, dropwise add 2.12 g of tetraethyl orthosilicate (TEOS), and continue to stir for 20 hours to obtain a milky white suspension.

[0019] ②Take 1g of template agent F127 and 22.5g of deionized water, put them into a crystallization bottle, stir in a constant temperature water bath at 40 ℃ until completely dissolved (about 1 hour), and then add 7.5g of 36% Concentrated hydrochloric acid, continue to stir for 0.5 hours, add 4.85g Na 2 SO 4 10H 2 O. After another 2 hours, add 4.2 g tetraethyl orthosilicate (TEOS) dropwise, and continue stirring for 20 hours to obtain a milky white suspension.

[0020] ③Mix the above two suspensi...

Embodiment 2

[0022] ①Take 0.5 g of template agent P123 and 12.3 g of deionized water, put them into a crystallization bottle, stir in a constant temperature water bath at 45 ℃ until completely dissolved (about 4 hours), then add 3.15 g of Concentrated hydrochloric acid, adjust the P hour value <1, continue to stir for 0.5 hours, dropwise add 1.06 g tetraethyl orthosilicate (TEOS), and continue to stir for 16 hours to obtain a milky white suspension.

[0023] ②Take 1.5g of template agent F127 and 33.7g of deionized water, put them into a crystallization bottle, stir in a constant temperature water bath at 40 ℃ until completely dissolved (about 1 hour), and then add 11.25g to this solution with a mass concentration of 36% Concentrated hydrochloric acid, continue to stir for 0.5 hours, add 7.3g Na 2 SO 4 10H 2 O. After another 2 hours, add 6.3 g of tetraethyl orthosilicate (TEOS) dropwise, and continue stirring for 16 hours to obtain a milky white suspension.

[0024] ③Mix the above two su...

Embodiment 3

[0026] ① Take 1 g of template agent P123 and 28.0 g of deionized water, put them into a crystallization bottle, stir in a constant temperature water bath at 45 ℃ until completely dissolved (about 4 hours), then add 0.2 g of Concentrated hydrochloric acid, adjust the pH value to <3, continue to stir for 0.5 hours, dropwise add 2.12 g tetraethyl orthosilicate (TEOS), and continue to stir for 16 hours to obtain a milky white suspension.

[0027] ②Take 1g of template agent F127 and 24.0g of deionized water, put them into a crystallization bottle, stir in a constant temperature water bath at 40 ℃ until completely dissolved (about 1 hour), and then add 6.0g of 36% Concentrated hydrochloric acid, continue to stir for 0.5 hours, add 4.85g Na 2 SO 4 10H 2 O. After another 2 hours, 4.2 g of tetraethyl orthosilicate (TEOS) was added dropwise, and stirring was continued for 16 hours to obtain a milky white suspension.

[0028] ③Mix the above two suspensions into the same crystallizatio...

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Abstract

The invention discloses a preparation method of a silicon-based dual mesoporous material. The silicon-based dual mesoporous material is prepared by taking P123 and F127 as template agents through a respective reaction and common crystallization method. Compared with a colloidal sol-gel dual template method, the method provided by the invention has the advantages of being simple and convenient, strong in controllability and easy to operate, nearly one half of work hours is saved, and the combined efficiency is greatly improved; the silicon-based dual mesoporous material has double-peak pore size distribution, the pore diameter of a small mesoporous is about 5nm, the pore diameter of a large mesoporous is about 10-15nm, the silicon-based dual mesoporous material has great potential application values when being taken as a catalyst in the heavy oil processing and taken as an adsorbent in oil product rectification.

Description

1. Technical field [0001] The invention belongs to the technical field of material synthesis, and in particular relates to a preparation method of a silicon-based double mesoporous material. 2. Background technology [0002] Silicon-based dual-mesoporous materials have special pore structures with different grades and independent pore size distribution. Both sets of pores are mesoporous. Larger mesopores are conducive to guiding adsorbates, and reactants can more easily enter small mesopores for adsorption or reaction. (This is beyond the reach of small mesoporous materials), and the smaller mesopores provide a larger specific surface area (this is beyond the reach of large mesoporous and macroporous materials). This structure is conducive to improving the diffusion rate and the carrier metal of dispersion. It has been reported that silicon-based double mesoporous materials loaded with Co active metals can not only significantly increase the dispersion of Co, but also effec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/113
Inventor 李剑杨丽娜董家丽
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY