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Double-silicon-source-oriented hollow-sandwich-hollow silicon dioxide mesoporous material and synthesizing method thereof

A technology of silicon dioxide and mesoporous materials, applied in the fields of silicon dioxide, silicon oxide, nanotechnology for materials and surface science, etc., can solve the problems of cumbersome operation, time-consuming and laborious, skeleton collapse, etc., and achieve mild preparation conditions. , Expand the effect of the application

Active Publication Date: 2016-11-23
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although the hard template method has certain advantages in precisely controlling the morphology and structure of such materials, there are inevitably some defects: if a suitable template needs to be prepared in advance, the skeleton collapses easily during the removal of the template, and the operation Complicated, time-consuming and labor-intensive, not conducive to mass production
Although the above research has made some progress, the self-template preparation technology still needs to be further improved to expand its application space

Method used

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  • Double-silicon-source-oriented hollow-sandwich-hollow silicon dioxide mesoporous material and synthesizing method thereof
  • Double-silicon-source-oriented hollow-sandwich-hollow silicon dioxide mesoporous material and synthesizing method thereof
  • Double-silicon-source-oriented hollow-sandwich-hollow silicon dioxide mesoporous material and synthesizing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] a. Mix ethanol and ammonia water at a volume ratio of 3:1, stir for 30 minutes to make it evenly mixed; the total volume of solvent is 40mL;

[0025] b. Mix the organosilicon source 3-(2-aminoethyl)-aminopropyltrimethoxysilane (TSD) and tetraethylorthosilicate (TEOS) at a volume ratio of 1:40 and disperse them in 8 mL of ethanol , the mass ratio of the mixed silicon source and ammonia water is 1:4.5; the mixed silicon source is ultrasonicated for 5 min to make it fully uniform;

[0026] c. At room temperature, add the silicon source mixed in b to the solution in a at a constant speed. After the dropwise addition is completed, continue stirring for 2~3 h; after the reaction is completed, the reactant is centrifuged, washed with ethanol and deionized water, and dried to obtain a white powder;

[0027] d. Disperse 30 mg of the white powder obtained in step c into 10 mL of water, and sonicate for 30 minutes to obtain a white suspension;

[0028] e. Quickly drop 200 μL of ...

Embodiment 2

[0031] The preparation process and steps of this embodiment are basically the same as in Example 1, except that the b step:

[0032] Mix organic silicon source 3-(2-aminoethyl)-aminopropyltrimethoxysilane (TSD) and tetraethylorthosilicate (TEOS) at a volume ratio of 1:10 and disperse them into 8 mL of ethanol;

[0033] The result obtained is quite different from the structure of Example 1. The obtained material is a sandwich hollow mesoporous silica nanosphere. There is an obvious solid silica core in the cavity of the ball. The particle size is about 150 nm, and the overall particle size is about 400 nm. , the outer shell is around 40 nm.

Embodiment 3

[0035] The preparation process and steps of this embodiment are basically the same as in Example 1, except that the b step:

[0036] Mix organic silicon source 3-(2-aminoethyl)-aminopropyltrimethoxysilane (TSD) and tetraethylorthosilicate (TEOS) at a volume ratio of 1:20 and disperse them into 8 mL of ethanol;

[0037] Compared with the results obtained in Examples 1 and 2, part of the obtained material is a hollow mesoporous silica sphere, and a small amount is a sandwich hollow structure. The particle size and shell thickness of the two types of silica nanospheres are similar to those in Example 1.

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Abstract

The invention relates to a double-silicon-source-oriented hollow-sandwich-hollow silicon dioxide mesoporous material and a synthesizing method thereof. The synthesizing method includes the steps that ethyl alcohol serves as a solvent, and under the base catalysis effect of ammonium hydroxide, 3-(2-aminoethyl)-aminopropyl trimethoxy silane (TSD) and tetraethoxysilane (TEOS) are subjected to hydrolytic polymerization to obtain solid hybridization silicon dioxide spheres; the spheres are converted into the hollow or solid sandwich-hollow silicon dioxide mesoporous material under the etching effect of hydrofluoric acid (HF), wherein in the process of preparing the solid hybridization silicon dioxide spheres, the silicon dioxide mesoporous material of different structures can be obtained by simply adjusting the volume ratio of the two silicon sources. According to the hollow silicon dioxide mesoporous material obtained with the method, the particle size ranges from 350 nm to 420 nm, the shell thickness ranges from 30 nm to 50 nm, and the hole diameter ranges from 3 nm to 4 nm; according to the obtained sandwich-hollow silicon dioxide mesoporous material, the particle size ranges from 350 nm to 420 nm, silicon dioxide solid spheres with the particle size of 100 nm to 160 nm serve as cores, the shell thickness ranges from 30 nm to 50 nm, and the hole diameter ranges from 3 nm to 4 nm. According to the silicon dioxide mesoporous material obtained with the method, a certain amount of amino exists for modification, and the application in the fields of catalysis, biological medicine and the like is greatly expanded.

Description

technical field [0001] The invention relates to a double-silicon source-guided hollow and sandwich hollow silicon dioxide mesoporous material and a synthesis method thereof. Background technique [0002] Hollow mesoporous silica nanomaterials are widely used in catalysis, drug delivery, and fluorescent labeling due to their excellent properties such as low density, high specific surface area, tunable pore size, and good biocompatibility. Compared with traditional hollow materials, sandwich hollow silica, as a special kind of mesoporous material, has adjustable core particle size, controllable cavity size, and the core can also be made of functionalized metal or oxide (such as gold or oxide Iron, etc.) and other significant advantages, which greatly enhance the application space of hollow silica mesoporous nanomaterials. To this end, a series of preparation techniques have been developed to synthesize hollow and sandwich hollow silica nanomaterials, such as the hard template...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B33/12C01P2004/34C01P2004/62C01P2004/64
Inventor 张海娇刘兴稳
Owner SHANGHAI UNIV
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