Preparation method of hollow oxide microspheres

An oxide and microsphere technology, applied in chemical instruments and methods, titanium oxide/hydroxide, zirconium oxide, etc., can solve the problems of difficult to control the thickness of the shell layer, reduce the number of homogeneous nucleation, etc., to reduce the number of , the effect of good application prospects

Active Publication Date: 2017-09-08
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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Problems solved by technology

[0004] The purpose of the present invention is to: overcome the problems of easy homogeneous nucleation and difficult control of shell thickness in the existing preparation of oxide hollow microspheres, and provide a method for confining water on the surface of carbon spheres, which can greatly reduce homogeneous nucleation The preparation method of oxide hollow microspheres with the quantity and effective control of shell thickness

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  • Preparation method of hollow oxide microspheres

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Effect test

Embodiment 1

[0022] Embodiment 1 Titanium dioxide hollow microspheres——metal alkoxide

[0023] (1) Take 0.1g of carbon spheres with a size of 200nm, add deionized water at a mass ratio of 1:1, make the surface of the carbon spheres absorb water, and disperse the carbon spheres that have absorbed water in 20ml of acetylacetone;

[0024] (2) Take 1.5g of tetrabutyl titanate and add it to the above carbon sphere template suspension under high-speed stirring. The molar ratio of tetrabutyl titanate to carbon spheres is 0.5:1. Add acetylacetone to make titanate The concentration of tetrabutyl ester is 0.05mol / l, stirring and reacting for 2h;

[0025] (3) Transfer the solution obtained in step (2) into an autoclave, and conduct a hydrothermal reaction at 180° C. for 6 hours;

[0026] (4) Washing: absolute ethanol washing / centrifugation, repeated 2 to 4 times, to obtain C / oxide microspheres with a core-shell structure;

[0027] (5) The C / oxide microspheres were dried in air, and then heat-treate...

Embodiment 2

[0029] Embodiment 2 Titanium dioxide hollow microspheres——metal alkoxide

[0030] (1) Take 0.05g of carbon spheres with a size of 500nm, add deionized water at a mass ratio of 1:1, make the surface of the carbon spheres absorb water, and disperse the carbon spheres that have absorbed water in 20ml of ethylene glycol;

[0031] (2) Take 3g of isopropyl titanate and add it to the above carbon sphere template suspension under high-speed stirring. The molar ratio of isopropyl titanate to carbon spheres is 2.5:1, add ethylene glycol to make titanate The concentration of isopropyl ester is 0.25mol / l, stirring and reacting for 2h;

[0032] (3) Transfer the solution obtained in step (2) into an autoclave, and perform a hydrothermal reaction at 200° C. for 12 hours;

[0033] (4) Washing: absolute ethanol washing / centrifugation, repeated 2 to 4 times, to obtain C / oxide microspheres with a core-shell structure;

[0034] (5) The C / oxide microspheres were dried in air, and then heat-treat...

Embodiment 3 2

[0036] Embodiment 3 Tin dioxide hollow microspheres——metal alkoxide

[0037] (1) Take 0.1g of carbon spheres with a size of 400nm, add deionized water at a mass ratio of 1:1, make the surface of the carbon spheres absorb water, and disperse the carbon spheres that have absorbed water in 20ml of acetylacetone;

[0038] (2) Take 1.5g butyl stannate and add it to the above carbon sphere template suspension under high-speed stirring. The molar ratio of butyl stannate to carbon spheres is 0.5:1. Add acetylacetone to make butyl stannate Concentration of 0.05mol / l, stirring reaction 2h;

[0039] (3) Transfer the solution obtained in step (2) into an autoclave, and conduct a hydrothermal reaction at 200° C. for 6 hours;

[0040] (4) Washing: absolute ethanol washing / centrifugation, repeated 2 to 4 times, to obtain C / oxide microspheres with a core-shell structure;

[0041] (5) The C / oxide microspheres were dried in air, and then heat-treated at 450° C. for 2 h to obtain hollow oxide ...

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Abstract

The invention discloses a preparation method of hollow oxide microspheres. The preparation method includes the following steps that 1, carbon spheres serve as templates, the surfaces of the carbon spheres adsorb water, then, the carbon spheres are dispersed in solvent with the coordination effect with metal alkoxide, and carbon sphere template suspension is obtained; 2, metal alkoxide is added into the carbon sphere template suspension, the solvent with the coordination effect with metal alkoxide is added to enable the concentration of metal alkoxide to be 0.05-0.5 mol / L, and stirring reaction is conducted; 3, after a solution obtained in the step 2 is subjected to high-temperature and high-pressure reaction, and through washing and separation, C / oxide microspheres with core-shell structures are obtained; 4, after the C / oxide microspheres obtained in the step 3 are dried and subjected to heat treatment, the hollow oxide microspheres are obtained. According to the preparation method of the hollow oxide microspheres, the solvent with the coordination effect is adopted, the water is limited to the surfaces of the carbon spheres, the quantity of homogeneous nucleation can be greatly reduced, the thicknesses of the shell layers of the hollow oxide microspheres are effectively controlled, and the preparation method of the hollow oxide microspheres has good application prospects.

Description

technical field [0001] The invention belongs to the technical field of preparation of oxide hollow microspheres, more specifically, the invention relates to a preparation method of oxide hollow microspheres with a small amount of homogeneous nucleation and controllable shell thickness. Background technique [0002] Hollow oxide microspheres have the characteristics of low density, large specific surface area, high light scattering index, and low thermal conductivity, and have potential application value in the fields of dye-sensitized solar cells, photocatalysis, lithium-ion batteries, and building thermal insulation coatings. For this reason, researchers have proposed many methods for preparing hollow microspheres, such as template method, hydrothermal / solvothermal method, sol-gel method and so on. [0003] Template method is an effective way to prepare hollow microspheres of inorganic compounds. Usually, the preparation of oxide hollow microspheres using carbon spheres as...

Claims

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Application Information

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IPC IPC(8): C01B13/36C01G23/053C01G19/02C01G9/02C01B33/12C01G25/02C01F7/02C01G30/00B82Y40/00
CPCB82Y40/00C01B13/366C01B33/12C01F7/02C01G9/02C01G19/02C01G23/053C01G25/02C01G30/005C01P2004/34C01P2004/61C01P2004/62C01P2004/64
Inventor 徐雪青徐得华靳虎徐刚
Owner GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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