Metal-doped hollow mesoporous silica nanospheres 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 synthesis The process steps are simple, the raw materials are widely available and cheap, and the operability is strong

Active Publication Date: 2017-12-15
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing preparation method [Nano Lett.2003,3,609; CN200310107904] utilizes double surfactant (tetrapropylamine hydroxide and cetyltrimethylammonium bromide) as the soft film plate, and ethyl orthosilicate It is a silicon source, aluminum sulfate is an aluminum source, and hydrolyzed under the action of sodium hydroxide to obtain mesoporous aluminosilicate hollow spheres with an MCM-48 structure, but the size of the synthesized hollow spheres is about 600nm and the uniformity is difficult to be effective Regulation; another method [ACS Nano 2012,5,4434; CN201110069212] firstly prepare silica balls as dura, and aluminum source (sodium metaaluminate) and sodium carbonate are added to the silica ball dispersion, After 3 hours of stirring reaction etching, the precipitate was collected, and then prepared into a dispersion liquid for hydrothermal reaction for 48 hours. Ordered mesoporous aluminosilicate hollow spheres were obtained by sacrificing the template, but the preparation process was cumbersome, and aluminum The average particle size of doped mesoporous silica hollow spheres is 270nm

Method used

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  • Metal-doped hollow mesoporous silica nanospheres and preparation method thereof
  • Metal-doped hollow mesoporous silica nanospheres and preparation method thereof
  • Metal-doped hollow mesoporous silica nanospheres 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, which is characterized in that the doped metal element is one of the elements of IIIA, IVA, VA, transition metals and rare earth metals in the periodic table or more than two kinds, the ratio of the molar number of silicon atoms to 0.01-0.2; the nanosphere has a uniform two-dimensional hexagonal channel structure, the particle size is 60-200nm, the cavity diameter is 40-180nm, and the wall thickness is 10‑30nm, mesopore diameter 2.0‑4.0nm, specific surface area 600‑1600m2·g‑1, pore volume 2.0‑4.0cm3·g‑1. The present invention adopts the sol-gel method to directly synthesize the metal-doped hollow mesoporous silicon nanosphere material, does not need to use a hard template, avoids post-processing steps such as etching, and has the advantages of simple process, mild conditions, low raw material cost, high reaction efficiency, It has the advantages of strong operability and easy industrial production. The prepared hollow mesoporous nanospheres have a highly ordered mesoporous structure and large pore volume, which is conducive to the internal and external transport and storage of guest molecules, and can be used in processes such as catalysis, adsorption, separation, and controlled release of drugs.

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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Patent Type & Authority Patents(China)
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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