A monodisperse nanometer mesoporous silica-titanium dioxide composite sphere and a synthetic method thereof

A nano-mesoporous and silicon dioxide technology, applied in the direction of silicon dioxide, titanium dioxide, silicon oxide, etc., can solve the problems of complex steps, uneven distribution of silicon dioxide and titanium dioxide, long synthesis time, etc., and achieve simple process and high efficiency. Theoretical research and practical application value, the effect of short preparation time

Active Publication Date: 2016-07-06
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Both of the above two technical solutions are carried out under acidic conditions, and the main reaction is self-polymerization, which leads to uneven distribution of titanium and silicon elements in the formed products, which are all six-coordinated amorphous states
[0008] Moreover, the steps of these two methods are relatively complicated. The result of these two methods is that the distribution of silicon dioxide and titanium dioxide in the spherical material itself is uneven. Such titanium is hexa-coordinated titanium, which does not have any catalytic properties. As Catalysts and supports have certain limitations, and the synthesis time is relatively long

Method used

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  • A monodisperse nanometer mesoporous silica-titanium dioxide composite sphere and a synthetic method thereof
  • A monodisperse nanometer mesoporous silica-titanium dioxide composite sphere and a synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Add 73ml of water, 3.0g of CTAB and 12ml of ethanol into the flask and stir vigorously;

[0046] (2) Add 0.4ml triethanolamine to the solution of step (1), and stir for 30min;

[0047] (3) Stir the solution in step (2) and heat up to 60°C, and stir for 30min;

[0048] (4) Add a mixture of 0.385ml tetrabutyl titanate and 7.85ml tetrabutyl orthosilicate dropwise to (3) (tetrabutyl titanate accounts for 5%), stir at the above temperature for 2 hours, and the solution Turned milky white; the obtained product was centrifuged, washed repeatedly with ultrasonic water and alcohol three times; the obtained sample was dried at 25°C for 24 hours to obtain the original powder of nano-mesoporous silica / titanium dioxide balls; the obtained The raw sample powder was burned at 550°C for 5 hours (the heating rate was 1°C / min), and the template agent was removed to obtain a monodisperse nanometer mesoporous silica / titania composite sphere sample. The morphology of the obtained samp...

Embodiment 2

[0050] (1) Add 73ml of water, 6.4gCTAB and 23ml of ethanol into the flask and stir vigorously;

[0051] (2) Add 37.2ml triethanolamine to the solution of step (1), and stir for 10min;

[0052] (3) Stir the solution in step (2) and heat up to 80°C, and stir for 60min;

[0053] (4) Add dropwise a mixture of 0.071ml tetrabutyl titanate and 7.85ml tetrabutyl orthosilicate to (3) (tetrabutyl titanate accounts for 1%), stir at the above temperature for 1 hour, and the solution Turned milky white; the obtained product was centrifuged, washed with ultrasonic water and alcohol three times repeatedly; the obtained sample was dried at 60°C for 10 hours to obtain the original powder of nano-mesoporous silica / titanium dioxide balls; the obtained The raw sample powder was burned at 500°C for 10 hours (the heating rate was 3°C / min), and the template agent was removed to obtain a monodisperse nanometer mesoporous silica / titania composite sphere sample. The morphology of the obtained sample ...

Embodiment 3

[0055] (1) Add 73ml of water and 3.0g of CTAB into the flask and stir vigorously;

[0056] (2) Add 0.14ml triethanolamine to the solution of step (1), and stir for 60min;

[0057] (3) Stir the solution in step (2) and heat up to 60°C, and stir for 60min;

[0058] (4) Add dropwise a mixture of 0.84ml tetrabutyl titanate and 7.85ml tetrabutyl orthosilicate (tetrabutyl titanate accounts for 10%) to (3), stir at the above temperature for 3 hours, and the solution Turned into milky white; the obtained product was centrifuged, washed repeatedly with ultrasonic water and alcohol three times; the obtained sample was dried at 40°C for 24 hours to obtain the original powder of nano-mesoporous silica / titanium dioxide balls; the above obtained The raw sample powder was burned at 600°C for 3 hours (the heating rate was 1°C / min), and the template agent was removed to obtain a monodisperse nanometer mesoporous silica / titania composite sphere sample. The morphology of the obtained sample is...

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Abstract

A synthetic method of a monodisperse nanometer mesoporous silica/titanium dioxide composite sphere is provided. A mole ratio of ethanol, water, a template, an alkali and a silicon source which are raw materials is (0-11.0):115:(0.05-0.5):(0.03-8.0):1. The mass of a titanium source is 1-10% of the mass of a liquid mixture of the titanium source and the silicon source. The composite sphere is synthesized rapidly through the method. The method is simple in process and short in preparation time. The particle size of a product synthesized through the method is controllable in a range from 20 nm to 200 nm. The inside and the surface of the composite sphere can be functionalized, so that the composite sphere has high theoretical research and practical application value in the fields of adsorption separation, catalysis, environment protection, microreactors, synthesis of sensing and nanometer materials, and the like.

Description

technical field [0001] The invention belongs to the technical field of inorganic nanometer materials, and in particular relates to a monodisperse nano mesoporous silicon dioxide and titanium dioxide composite ball and a synthesis method thereof. Background technique [0002] Mesoporous materials have uniform pore diameters due to their high specific surface area and pore volume. The periodically arranged pore structure and the functionalization of the interior and surface of the pore have high theoretical research and practical application value in the fields of adsorption separation, catalysis, environmental protection, microreactor, sensing and synthesis of nanomaterials. In 1992, Mobil Corporation of the United States reported the synthesis method of M41S series mesoporous materials in Nature for the first time. Among them, MCM-41 has uniform hexagonal mesoporous channels, high specific surface area and high thermal stability, has potential application value, and has att...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12C01G23/053B82Y30/00
Inventor 崔亮王仪森王润伟张宗弢义建军蒋尚崔伟松王科峰王永刚
Owner PETROCHINA CO LTD
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