Metal-doped hollow mesoporous silicon oxide nanosphere and preparation method thereof

A mesoporous silicon oxide and metal doping technology, which is applied in the direction of silicon oxide, silicon dioxide, nanotechnology for materials and surface science, etc., can solve the problems of cumbersome steps and difficult to effectively control the size of hollow spheres, and achieve the synthesis The process steps are simple, the raw materials are widely available and cheap, and the operability is strong

Active Publication Date: 2016-07-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Existing preparation method [NanoLett.2003,3,609; CN200310107904] utilize double surfactant (tetrapropylamine hydroxide and hexadecyltrimethylammonium bromide) as the soft film plate, with ethyl orthosilicate as Silicon source and aluminum sulfate are the aluminum source, and they are hydrolyzed under the action of sodium hydroxide to obtain mesoporous aluminosilicate hollow spheres with MCM-48 structure, but the size of the synthesized hollow spheres is about 600nm and the uniformity is difficult to effectively control ; Another method [ACSNano2012,5,4434;...

Method used

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  • Metal-doped hollow mesoporous silicon oxide nanosphere and preparation method thereof
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  • Metal-doped hollow mesoporous silicon oxide nanosphere and preparation method thereof

Examples

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Embodiment 1

[0031] Example 1 Synthesis of aluminum-doped hollow mesoporous silica nanospheres

[0032] Ethyl orthosilicate is used as the silicon source, and aluminum isopropoxide is used as the aluminum source. The surfactant CTAB was added into deionized water, adjusted to pH = 11.4 with concentrated ammonia water (25 wt%), stirred and dissolved in a water bath at 50°C. Prepare dilute ethanol solution A of tetraethyl orthosilicate, the concentration is 0.2mol L -1 ; Concentrated ethanol solution B of tetraethyl orthosilicate, the concentration is 1.1mol L -1 ; The ethanol solution of aluminum isopropoxide, the concentration is 0.065mol L -1 or 0.0325mol L -1 (Correspondingly, Al / Si=0.025, 0.05). Quickly add solution A to the above mixture under stirring, seal the reactor, stir for 5 hours, open the reactor, add solution B drop by drop, after vigorous stirring for 1 hour, add the ethanol solution of aluminum isopropoxide dropwise, and stir for 1 hour , 50 ° C water bath for 20 hours...

Embodiment 2

[0033] Example 2 Synthesis of tin-doped hollow mesoporous silica nanospheres

[0034] Ethyl orthosilicate is used as the silicon source, and tin tetrachloride is used as the tin source. The surfactant CTAB was added into deionized water, adjusted to pH = 11.4 with concentrated ammonia water (25 wt%), stirred and dissolved in a water bath at 50°C. Prepare dilute ethanol solution A of tetraethyl orthosilicate, the concentration is 0.2mol L -1 ; Concentrated ethanol solution B of tetraethyl orthosilicate, the concentration is 1.1mol L -1 ; Ethanol solution of tin tetrachloride, the concentration is 0.065mol L -1 (Correspondingly, Sn / Si=0.025). Quickly add solution A to the above mixture under stirring, seal the reactor, stir for 5 hours, open the reactor, add solution B drop by drop, after vigorous stirring for 1 hour, add the ethanol solution of tin tetrachloride drop by drop, and stir for 1 hour , standing in a 60°C water bath for 20 hours. The molar ratio of the raw mater...

Embodiment 3

[0035] Example 3 Synthesis of Niobium-doped Hollow Mesoporous SiO Nanospheres

[0036] Ethyl orthosilicate is used as the silicon source, and niobium pentachloride is used as the niobium source. The surfactant CTAB was added into deionized water, adjusted to pH = 11.4 with concentrated ammonia water (25 wt%), stirred and dissolved in a water bath at 50°C. Prepare dilute ethanol solution A of tetraethyl orthosilicate, the concentration is 0.2mol L -1 ; Concentrated ethanol solution B of tetraethyl orthosilicate, the concentration is 1.1mol L -1 ; Ethanol solution of niobium pentachloride, the concentration is 0.065mol L -1 (Correspondingly, Nb / Si=0.025). Quickly add solution A to the above mixture under stirring, seal the reactor, stir for 5 hours, open the reactor, add solution B drop by drop, after vigorously stirring for 2 hours, add niobium pentachloride ethanol solution drop by drop, stir for 1 hour , standing in a water bath at 130°C for 20 hours. The molar ratio of ...

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Abstract

The invention discloses a metal-doped hollow mesoporous silicon oxide nanosphere and a preparation method thereof. The nanosphere is characterized in that a doped metal element is one or two or more of group IIIA elements, group IVA elements, group VA elements, transition metals and rare earth metals in the periodical table, and a molar ratio of the doped metal element to silicon atoms is 0.01-0.2; and the nanosphere has a uniform two-dimensional hexagonal porous structure, the particle size is 60-200nm, the cavity diameter is 40-180nm, the spherical wall thickness is 10-30nm, the aperture of mesopores is 2.0-4.0nm, the specific surface area is 600-1600m<2>.g<-1>, and the pore volume is 2.0-4.0cm<3>.g<-1>. The metal doped hollow mesoporous silicon oxide nanosphere material can be directly synthesized through a sol-gel technology without a hard template, so etching and other post-treatment steps are avoided, thereby the preparation method has the advantages of simple process, mild conditions, cheap raw materials, high reaction efficiency, strong operability and easy industrial production. The hollow mesoporous nanosphere prepared in the invention has a highly ordered mesoporous structure and a large pore volume, so internal and external transportation and storage of guest molecules are facilitated, and the nanosphere can be used in catalysis, adsorption, separation an drug controlled release processes.

Description

technical field [0001] The invention relates to the field of inorganic porous materials, in particular to mesoporous silicon-based nanomaterials, more specifically to a metal-doped hollow mesoporous silicon oxide nanosphere and a preparation method thereof. Background technique [0002] In 1992, Mobil Corporation publicly reported the ordered mesoporous silicon oxide material represented by MCM-41 for the first time [J.Am.Chem.Soc.1992, 114, 10834], setting off an upsurge in research on mesoporous materials. However, the pure silicon M41s molecular sieve has a neutral framework, few defects, small ion exchange capacity, low acid content and low reactivity, which limits its application in catalysis, adsorption, separation and environmental protection. Studies have shown that the introduction of metal heteroatoms (such as Al, Ti, Fe, Ce, etc.) And improve the hydrothermal stability of mesoporous molecular sieves, so metal-doped mesoporous silica molecular sieves have attracte...

Claims

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Application Information

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IPC IPC(8): C01B33/12B82Y30/00B82Y40/00
Inventor 徐杰陈佳志路芳张俊杰于维强高进苗虹
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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