A kind of synthetic method of mesoporous silica-alumina molecular sieve

A technology of mesoporous silica-alumina and synthesis methods, applied in molecular sieve compounds, molecular sieves and alkali exchange compounds, chemical instruments and methods, etc., can solve problems such as narrow pore size distribution, achieve concentrated pore size distribution, large pore volume, and avoid mass use Effect

Active Publication Date: 2011-12-28
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Yu et al. [Ceramics International.2000, 26, 359-362] and Li Yonghuan et al. [Aging and Application of Synthetic Materials, 2006, 35(2): 1-3] using tetraethyl orthosilicate (TEOS) as silicon source, 16 Alkyltrimethylammonium bromide (CTABr) was used as a template, and aluminum trichloride was used as an aluminum source. Mesoporous silica-alumina molecular sieve A1-MCM-41 was synthesized at room temperature, but its pore size distribution was narrow (3.5-4.5nm )

Method used

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  • A kind of synthetic method of mesoporous silica-alumina molecular sieve
  • A kind of synthetic method of mesoporous silica-alumina molecular sieve

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Embodiment 1

[0025] Mesoporous silica-alumina molecular sieves were prepared using tetraethyl orthosilicate as silicon source, aluminum nitrate as aluminum source and sucrose as template.

[0026] With 8.59g ethyl orthosilicate (Beijing Chemical Reagent Company, analytically pure), 3.79g aluminum nitrate (Al(NO 3 ) 3 9H 2 O, Shanghai Zhenxin Reagent Factory, mass content 99.0%), 3.96g sucrose (Sinopharm Chemical Reagent Co., Ltd., analytically pure) was added in 45ml water (deionized water, the same below), at room temperature (26 ° C, the same below) , stirred for 2 hours, adjusted the pH value to 5.0 with a dilute hydrochloric acid solution with a concentration of 10% by weight, stirred for another 5 hours, and then stood and aged at 40 ° C for 96 hours, filtered the resulting mixture, and washed with deionized water , dried at 150°C for 8 hours, and then calcined at 500°C for 12 hours to obtain a mesoporous silica-alumina molecular sieve. The physical and chemical properties of the ob...

Embodiment 2

[0028] Mesoporous silica-alumina molecular sieves were prepared using methyl orthosilicate as silicon source, aluminum isopropoxide as aluminum source and dextran as template.

[0029] 6.15g methyl orthosilicate (Beijing Chemical Reagent Company, analytically pure), 8.21g aluminum isopropoxide (Sinopharm Chemical Reagent Co., Ltd., Al mass content 24.7%), 6.84g dextran (Sinopharm Chemical Reagent Co., Ltd. Company, analytically pure, molecular weight is 80,000) join in 72ml water, stir 4 hours at room temperature, add concentration and be 10% by weight dilute nitric acid solution and adjust pH value to be 4.0, stir 6 hours, leave standstill aging at 60 ℃ then for 72 hour, filtered, washed with deionized water, then dried at 120°C for 15 hours, and calcined at 600°C for 9 hours to obtain a mesoporous silica-alumina molecular sieve. The physical and chemical properties of the obtained products are shown in Table 1. The feeding ratio is shown in Table 2.

Embodiment 3

[0031] Mesoporous silica-alumina molecular sieves were prepared using sodium silicate as silicon source, aluminum isopropoxide as aluminum source and starch as template.

[0032] 28.7g sodium silicate (Na 2 SiO 3 9H 2O, Sinopharm Chemical Reagent Co., Ltd., analytically pure), 1.03g aluminum isopropoxide (Sinopharm Chemical Reagent Co., Ltd., Al mass content 24.7%), 12.8g starch (Sinopharm Chemical Reagent Co., Ltd., analytically pure, average molecular weight 300,000) into 360ml of water, stirred at room temperature for 3 hours, adjusted the pH value to 10.0 with a concentration of 10% dilute sulfuric acid solution by weight, stirred for another 6 hours, then left to age at 80°C for 48 hours, filtered, filtered The cake was washed with deionized water, dried at 110°C for 24 hours, and calcined at 650°C for 6 hours to obtain a mesoporous silica-alumina molecular sieve. The physical and chemical properties of the obtained products are shown in Table 1. The feeding ratio is ...

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Abstract

The invention provides a method for synthesizing a mesoporous aluminosilicate molecular sieve. The method comprises the following steps: mixing silicon sources, aluminium sources, sugar template agents and water, adjusting the pH value of the mixture to 4-13 to prepare a precursor sol, then aging the precursor sol, filtering, washing and drying the precursor sol and roasting the precursor powder to obtain the mesoporous aluminosilicate molecular sieve. The method is simple in process, safe to operate and easy to realize industrial large-scale production. The prepared mesoporous aluminosilicate molecular sieve has the advantages of concentrated pore size distribution and good heat stability, has specific surface area of 300-950m<2> / g and can be used in the adsorption and catalysis processes.

Description

technical field [0001] The invention relates to a method for synthesizing mesoporous silicon-aluminum molecular sieves. Background technique [0002] In 1992, researchers from Mobil Corporation [J.Amer.Chem.Soc.1992, 114, 10834] used alkyl quaternary ammonium salt cationic surfactants as templates for the first time and successfully synthesized M41S (MCM-41, MCM-48 , MCM-50) series of silica-based ordered mesoporous molecular sieves, thereby extending the regular pore size of molecular sieves from the micropore range to the mesoporous field. Mesoporous materials have very broad application prospects in many fields such as biomedicine, environmental protection, host-guest chemistry, and functional materials. It breaks through the pore size limitation of microporous molecular sieves and provides the possibility for catalytic reactions of macromolecules. The synthesis of mesoporous silica-alumina molecular sieves is usually based on surfactants as templates, using sol-gel, pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/00C01B37/00
Inventor 许本静田辉平朱玉霞陆友保
Owner CHINA PETROLEUM & CHEM CORP
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