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Preparation method of nitrogen-doped TiO2 microspheres with hollow core-shell structure

A technology of core-shell structure and microspheres, which is applied in the field of preparation of nitrogen-doped TiO2 microspheres, can solve the problems of enhancement, cumbersome process, and affecting product stability, and achieve the goals of enhancing contact, increasing application range, and improving visible light catalytic ability Effect

Inactive Publication Date: 2019-12-24
浙江迈实科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] To sum up, it is of great significance to improve the photocatalytic activity of titanium dioxide by modifying titanium dioxide with the structure of the silicon dioxide protective layer and at the same time doping it with non-metallic N elements. structure of titanium dioxide microspheres, and then use modification technology to dope nitrogen into titanium dioxide particles to enhance its response to visible light. The process is cumbersome and affects product stability, which needs to be improved urgently

Method used

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  • Preparation method of nitrogen-doped TiO2 microspheres with hollow core-shell structure

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Experimental program
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Embodiment 1

[0027] Step 1: To prepare titanium dioxide sol, mix butyl titanate and absolute ethanol at a ratio of 1:5, and shake well to obtain a mixed solution. Take 10ml of the mixed solution and add it dropwise to 35ml. The concentration of the substance is 1 mol / L of nitric acid solution, stirring continuously during the process to prevent coagulation until a colorless and transparent titanium dioxide sol is formed;

[0028] Step 2: Preparation of PAM@TiO 2 For single-shell core-shell microspheres, mix the titanium dioxide sol prepared in step 1 with an aqueous polyacrylamide solution with a concentration of 0.15%, add the initiator ammonium persulfate to cause a polymerization reaction, and wash the polymerization product with anhydrous formaldehyde, Nitrogen drying, anhydrous acetone cleaning and nitrogen drying to obtain single-shell core-shell microspheres wrapped with polyacrylamide on the surface of titanium dioxide;

[0029] Step 3: Preparation of SiO 2 @PAM @TiO 2 Double-s...

Embodiment 2

[0032] Step 1: Prepare titanium dioxide sol, mix butyl titanate and absolute ethanol according to the amount of substance at 1:3, shake well to obtain a mixed solution, take 10ml of the mixed solution and add it dropwise to 20ml with a concentration of 0.8mol / L of nitric acid solution, stirring continuously during the process to prevent coagulation until a colorless and transparent titanium dioxide sol is formed;

[0033] Step 2: Preparation of PAM@TiO 2For single-shell core-shell microspheres, mix the titanium dioxide sol prepared in step 1 with an aqueous polyacrylamide solution with a concentration of 0.1%, add an initiator potassium persulfate to cause a polymerization reaction, and wash the polymerization product with anhydrous formaldehyde, Nitrogen drying, anhydrous acetone cleaning and nitrogen drying to obtain single-shell core-shell microspheres wrapped with polyacrylamide on the surface of titanium dioxide;

[0034] Step 3: Preparation of SiO 2 @PAM @TiO 2 Doubl...

Embodiment 3

[0037] Step 1: Prepare titanium dioxide sol, mix butyl titanate and absolute ethanol according to the amount of the substance at 1:8, shake well to obtain the mixed solution, take 10ml of the mixed solution and add it dropwise to 50ml of the substance with a concentration of 1.5mol / L of nitric acid solution, stirring continuously during the process to prevent coagulation until a colorless and transparent titanium dioxide sol is formed;

[0038] Step 2: Preparation of PAM@TiO 2 For single-shell core-shell microspheres, mix the titanium dioxide sol prepared in step 1 with an aqueous solution of polyacrylamide with a concentration of 0.25%, add the initiator sodium bisulfite to cause polymerization, and wash the polymerization product with anhydrous formaldehyde , nitrogen drying, anhydrous acetone cleaning and nitrogen drying to obtain single-shell core-shell microspheres wrapped with polyacrylamide on the surface of titanium dioxide;

[0039] Step 3: Preparation of SiO 2 @PA...

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Abstract

The invention belongs to the field of photocatalytic nano materials. The invention provides a preparation method of nitrogen-doped TiO2 microspheres with a hollow core-shell structure. The preparationmethod comprises the following steps: (1) preparing titanium dioxide sol; (2) preparing PAM@TiO2 single-shell core-shell microspheres; (3) preparing SiO2@PAM@TiO2 double-shell core-shell microspheres; and (4) preparing SiO2@@TiO<2-x>Nx hollow core-shell structure microspheres. The preparation method comprises the following steps: mixing polyacrylamide for providing an N element with titanium dioxide to form the single-shell core-shell microspheres; coating a silicon dioxide shell with a film to form the double-shell core-shell microspheres; performing high temperature calcination so that polyacrylamide serving as a middle shell layer is subjected to thermal decomposition and removed to form a cavity and an N element is provided for thermal diffusion and doping into titanium dioxide afterthermal decomposition to obtain the nitrogen-doped TiO2 microspheres with the hollow core-shell structure. The preparation method is simple, titanium dioxide modification, core-shell structure titanium dioxide modification and core-shell structure integral forming are realized, the cost is reduced, and the photocatalysis efficiency and stability of a photocatalysis product are improved.

Description

technical field [0001] The invention belongs to the field of photocatalytic nanomaterials, in particular to nitrogen-doped TiO with a hollow core-shell structure 2 Preparation method of microspheres. Background technique [0002] Titanium dioxide (chemical formula: TiO 2 ) has the advantages of good photocatalysis, non-toxic, cheap and easy to obtain, easy preparation, stable performance, no photocorrosion, etc., so it is considered to be one of the best performance and most promising photocatalysts. After excitation, electrons and holes are separated, and the strong redox ability can even break the C-H bond, so it can be used to decompose most organic substances, and has been widely used in environmental catalysis, energy storage, sterilization, photovoltaic cells , sensor devices and many other fields. [0003] Because titanium dioxide has a strong redox ability, it will corrode the surface of the organic carrier while decomposing organic matter. A common practice is to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C02F1/30C02F101/38C02F101/34C02F101/36
CPCB01J27/24B01J37/0018C02F1/30C02F2305/10C02F2101/38C02F2101/34C02F2101/36B01J35/39
Inventor 杨晟尧孔洋波林路云张捷
Owner 浙江迈实科技有限公司
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