Hollow titanium dioxide microsphere based on gel sphere precursor and preparation method of hollow titanium dioxide microsphere

A microsphere, hollow technology, applied in the directions of titanium dioxide, chemical instruments and methods, titanium oxide/hydroxide, etc., to achieve the effects of low preparation cost, improved photocatalytic efficiency, and improved photocatalytic degradation effect

Active Publication Date: 2015-01-28
佛山市卓尔特电器有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to overcome the problem that the template agent needs to be removed by calcination in the process of preparing hollow microsphere materials in the prior art, the present invention provides a hollow TiO 2 Microsphere and its synthesis method, the synthesized TiO 2 Substantial part of the microspheres have carbon and anatase TiO 2 The composite structure has a large specific surface area; after decarburization by high-temperature heat treatment, the hollow TiO 2 The substantial part of the microspheres becomes composed of nano-sized grains and nano-sized channels in the microstructure, TiO with a spatial network structure 2 porous material

Method used

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  • Hollow titanium dioxide microsphere based on gel sphere precursor and preparation method of hollow titanium dioxide microsphere
  • Hollow titanium dioxide microsphere based on gel sphere precursor and preparation method of hollow titanium dioxide microsphere
  • Hollow titanium dioxide microsphere based on gel sphere precursor and preparation method of hollow titanium dioxide microsphere

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Experimental program
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Effect test

Embodiment 1

[0031] 1. Preparation of starch solution

[0032] Dissolve 1.18g of starch in 40mL of deionized water at 90°C, and then naturally cool to room temperature;

[0033] 2. Complexation of tetra-n-butyl titanate

[0034]Add 1 mL of acetylacetone to 2.5 mL of tetra-n-butyl titanate, stir and react for 0.5 h to obtain a complex of tetra-n-butyl titanate;

[0035] 3. Preparation of dispersed system

[0036] In the case of stirring, the tetra-n-butyl titanate complex obtained in step 2 is added to the starch solution obtained in step 1, and stirred evenly to obtain a milky yellow dispersion system;

[0037] 4. Hydrothermal treatment

[0038] Transfer the milky yellow dispersion system obtained in step 3 into a high-pressure reaction kettle with a polytetrafluoroethylene inner cup, and conduct a hydrothermal reaction at 150°C for 10 hours. After the reaction product is sequentially washed with deionized water and ethanol, the Dry at 100°C for 2h to obtain hollow TiO 2 Microspheres....

Embodiment 2

[0041] 1. Preparation of starch solution

[0042] Dissolve 1.18g of starch in 40mL of 90°C deionized water, then cool naturally to room temperature (25°C) to obtain a starch solution, then add 3.6mg of dodecylbenzenesulfonic acid to the starch solution, and stir evenly;

[0043] 2. Complexation of tetra-n-butyl titanate

[0044] Add 1 mL of acetylacetone to 2.5 mL of tetra-n-butyl titanate, stir and react for 0.5 h to obtain a complex of tetra-n-butyl titanate;

[0045] 3. Preparation of dispersed system

[0046] In the case of stirring, the tetra-n-butyl titanate complex obtained in step 2 is added to the starch solution obtained in step 1, and stirred evenly to obtain a milky yellow dispersion system;

[0047] 4. Hydrothermal treatment

[0048] Transfer the milky yellow dispersion system obtained in step 3 into a high-pressure reaction kettle with a polytetrafluoroethylene inner cup, and conduct a hydrothermal reaction at 150°C for 10 hours. After the reaction product is ...

Embodiment 3

[0053] 1. Preparation of starch solution

[0054] Dissolve 7.1g of starch in 40mL of 90°C deionized water, then cool naturally to room temperature (25°C) to obtain a starch solution, then add 3.6mg of dodecylbenzenesulfonic acid to the starch solution, and stir evenly;

[0055] 2. Complexation of tetra-n-butyl titanate

[0056] Add 1 mL of acetylacetone to 2.5 mL of tetra-n-butyl titanate, stir and react for 0.5 h to obtain a complex of tetra-n-butyl titanate;

[0057] 3. Preparation of dispersed system

[0058] In the case of stirring, the tetra-n-butyl titanate complex obtained in step 2 is added to the starch solution obtained in step 1, and stirred evenly to obtain a milky yellow dispersion system;

[0059] 4. Hydrothermal treatment

[0060] Transfer the milky yellow dispersion system obtained in step 3 into a high-pressure reaction kettle with a polytetrafluoroethylene inner cup, and conduct a hydrothermal reaction at 150°C for 10 hours. After the reaction product is s...

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Abstract

The invention belongs to the technical field of inorganic functional material preparation, and particularly relates to a TiO2 hollow microsphere synthesizing technology by using gel spherulite as precursor. A hydrolyzing agent complexed tetra-n-butyl titanate is dispersed into a water solution of starch, and is subjected to hydrothermal treatment at 150 DEG C, the starch reacts with tetra-n-butyl titanate to form a gel sphere with a three-dimensional network structure; a hollow structure is formed in the gel sphere in the mineralizing and carbonizing processes due to volume shrinkage, and the carbon ingredient remained in the gel sphere is removed by a thermal treatment; and the substantial part of the hollow TiO2 microsphere is made of a porous material formed by nano-crystalline grains (8-10nm) and nano-scale passages. According to the synthesized TiO2 spheres, the specific surface area is 230m<2>/g, the porous volume is 0.34cm<3>/g, and the average pore diameter is 6.6nm. By adopting the synthesizing process, water is used as a dispersing medium, and starch participates in the reaction to form the gel spheres, and the process is environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic functional materials, in particular to a kind of TiO with gel ball as precursor 2 Synthesis technology of hollow microspheres. Background technique [0002] TiO 2 Because of its stable chemical and physical properties, non-toxicity, and sufficient material sources, it is widely used as a photocatalyst for the research of degrading harmful gases in the air and organic pollutants in water, as an electrode material for the research of dye-sensitized solar cells, as a surface Coatings are used in the study of self-cleaning materials. TiO 2 Under the irradiation of ultraviolet light, the electrons in the valence band of the semiconductor absorb the energy of photons and jump to the conduction band, thereby forming photogenerated electron-hole pairs. This characteristic is the theory of its application as a photocatalyst and dye-sensitized solar cells. Base. Semiconductor TiO 2 Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053B01J21/06
CPCB01J21/063C01G23/053C01P2002/72C01P2004/03C01P2004/34C01P2006/12C01P2006/14C01P2006/16
Inventor 董如林那驰莫剑臣陈智栋张汉平金长春
Owner 佛山市卓尔特电器有限公司
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