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Preparation method of composite ZnO-mesoporous silica nanomaterial

A technology of mesoporous silica and nanomaterials, applied in the preparation of organic compounds, chemical instruments and methods, luminescent materials, etc., can solve the problems of poor uniformity of nano-zinc oxide, excessive particle size of ZnO, and unstable performance. Achieve the advantages of production cost, uniform ZnO, and stable properties

Active Publication Date: 2011-11-23
SOUTH CHINA NORMAL UNIVERSITY
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Problems solved by technology

In these two methods, there are problems that the ZnO particle size is too large and uniform and non-distributed.
The existence of these problems makes the existing mesoporous silica-loaded nano-zinc oxide have poor uniformity and unstable performance, so they cannot be well used in actual production.

Method used

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  • Preparation method of composite ZnO-mesoporous silica nanomaterial
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preparation example Construction

[0032] A preparation method of composite ZnO mesoporous silicon dioxide nanomaterial, comprising the following steps:

[0033] 1) Solvothermal in-situ substitution: mix silicon-based molecular sieve powder, ZnO precursor, dopant elements, and organic solvent evenly, put them in an autoclave, pass in protective gas, and react at 140-200°C for at least 12 hours; filter the reaction solution , washed and dried to obtain dry powder;

[0034] 2) Calcination and crystallization: heat up the dry powder to 550-700°C, and calcine at a constant temperature for 6-10 hours to obtain a composite ZnO mesoporous silica nanomaterial.

[0035] During solvothermal in-situ substitution, the reaction time can be adjusted according to the actual situation. In order to ensure that the substitution reaction is more complete, the reaction time can be extended appropriately. However, as known to those skilled in the art, if the reaction time is too long, the energy consumed Also more, for the conside...

Embodiment 1

[0049] (1) Preparation of the original molecular sieve

[0050] Mix OP1-10 (nonylphenol polyoxyethylene (10) ether), TEOS (tetraethyl silicate), HCl (concentrated hydrochloric acid), H 2 O (water), TBAB (tetrabutylammonium bromide), and petroleum ether are mixed evenly in a molar ratio of 0.2:1:32:200:0.2:2.0, stirred and reacted at room temperature for 3 hours, and left for 24 hours; ultrasonic for 10 minutes Afterwards, it was suction filtered and dried at 90°C for 12 hours to obtain a white original molecular sieve powder.

[0051] (2) Calcination crystallization:

[0052] The temperature of the product obtained in step (1) was raised to 550°C and calcined at a constant temperature for 6 hours to obtain the final product as a white powder nano-mesoporous material SiO 2 .

Embodiment 2

[0054] (1) Preparation of the original molecular sieve

[0055] Mix OP-10 (nonylphenol polyoxyethylene (10) ether), TEOS (tetraethyl silicate), HCl (concentrated hydrochloric acid), H 2 O (water), TBAB (tetrabutylammonium bromide), and petroleum ether are mixed evenly in a molar ratio of 0.4:1:32:200:0.2:2.0, stirred and reacted at room temperature for 3 hours, and left standing for 24 hours; 10 minutes of ultrasound After that, it was suction filtered and dried at 90° C. for 12 hours to obtain a white original molecular sieve powder.

[0056] (2) Solvothermal in situ substitution

[0057] Take 0.5g of the white original molecular sieve powder obtained in step (1) and place it in a 50ml hydrothermal reaction kettle, add 0.1g of zinc acetate doped with 1% aluminum (molar percentage), 10ml of acetone and 10ml of absolute ethanol, and pass nitrogen gas for 3 minutes, React at a constant temperature of 140°C for 24 hours.

[0058] (3) filter and dry

[0059] Suction filter the...

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Abstract

The invention discloses a preparation method of a composite ZnO-mesoporous silica nanomaterial, namely a solvothermal in situ substitution method. The preparation method comprises the following steps of: uniformly mixing silicon-based molecular sieve powder, a ZnO precursor, a doping element and an organic solvent, adding the mixture into a high-pressure reaction kettle, and introducing a shielding gas to the reaction kettle for reaction; filtering the reaction mixture, washing, and drying to obtain dry powder; and heating and calcining the dry powder to obtain the composite ZnO-mesoporous silica nanomaterial. The composite ZnO-mesoporous silica nanomaterial prepared by the preparation method disclosed by the invention has the advantages of uniform ZnO loading, stable properties, excellent optical properties and catalytic properties and strong SHG (second harmonic generation) and TPL (two-photon luminescence) optical properties when used as an excellent catalyst for organic ester synthesis or as a laser nonlinear optical material, and is suitable for being prepared into a purple light-emitting material or a functional polymer additive. The preparation method disclosed by the invention has the advantages of wide and available raw materials, simplicity of operation and advantageous production cost.

Description

technical field [0001] The invention relates to a preparation method of a composite silicon-based nanometer material, in particular to a preparation method of a composite ZnO mesoporous silicon dioxide nanometer material. Background technique [0002] "Composite nanostructure material" refers to a composite material composed of two or more substances combined in a certain way at the nanometer scale. The result of compounding can not only effectively tune the material properties, but compound nanostructured materials often produce many novel properties. Research on composite nanostructured materials has aroused people's strong interest and has become the frontier of scientific research on nanomaterials. [0003] Silica-based mesoporous molecular sieves refer to a series of molecular sieves with a pore size ranging from 2 to 50 nm and a pore wall composed of silica. Due to the advantages of large specific surface area, adjustable pore size, and controllable morphology, mesop...

Claims

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Application Information

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IPC IPC(8): C09K11/54B01J29/70C07C69/704C07C67/08C09F1/04C02F1/30C08L67/06C08K9/06C08K3/22C08K3/36C09D167/06C09D5/03
Inventor 铁绍龙林海燕兰胜符志成
Owner SOUTH CHINA NORMAL UNIVERSITY
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