Method for preparing sulfur and nitrogen co-doped titanium dioxide with visible light catalytic activity

A technology of titanium dioxide and catalytic activity, applied in the field of preparation of titanium dioxide photocatalyst, can solve the problems of high risk and pollution, and achieve the effects of less consumption of raw materials, improved absorption range, and high sintering activity

Inactive Publication Date: 2010-06-09
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

[0004] Chinese patent CN1562461A discloses the name: sulfur and nitrogen anion doped nano-titanium oxide catalyst and its synthesis method. This patent uses hydrothermal synthesis and ammonia nitriding to prepare sulfur and nitrogen co-doped titanium dioxide powder. Due to Use of dangerous and polluting NH 3 , there is a safety problem in the process; Chinese patent CN1850618A (publication number) proposes a kind of: "nitrogen and sulfur two-component doped nano-titanium dioxide with long-wave absorption function and its preparation method", the method adopts sol-gel method , by introducing nitrogen and sulfur sources into titanate hydrolysis process to prepare sulfur and nitrogen co-doped titanium dioxide, wherein the nitrogen source comes from urea, and the sulfur source comes from thiocyanate amine

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  • Method for preparing sulfur and nitrogen co-doped titanium dioxide with visible light catalytic activity
  • Method for preparing sulfur and nitrogen co-doped titanium dioxide with visible light catalytic activity

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Embodiment 1

[0019] Embodiment 1: Sol-gel method prepares sulfur-nitrogen co-doped titanium dioxide: the raw material ratio (percentage by weight, total weight is 50 grams) of synthetic titanium dioxide sol: butyl titanate (analytical pure) 5%, dehydrated alcohol (analytical Pure) 88%, acetic acid (analytical pure) 5%, thiourea (analytical pure) 2%, put butyl titanate, absolute ethanol, acetic acid in the reaction flask according to the above ratio, and stir at a temperature of 15°C for 30 Minutes, then thiourea aqueous solution was added to the reaction solution, and the reaction was continued for 2 hours to obtain a titanium dioxide sol. The solvent was evaporated to obtain a gel, and the gel was dried in an air atmosphere at 100° C. for 2 hours to obtain a dried solid. Grind the dried solid, put it into a muffle furnace after grinding, heat up to 450°C at a rate of 2°C / min at room temperature, calcinate at 450°C for 2 hours, and cool down to room temperature to obtain the target product...

Embodiment 2

[0021]Embodiment 2: Sol-gel method prepares sulfur and nitrogen co-doped titanium dioxide, the raw material ratio (percentage by weight, total weight is 50 grams) of synthetic titanium dioxide sol: butyl titanate (analytical pure) 5%, dehydrated alcohol (analytical pure) 88%, acetic acid (analytical pure) 5%, thiourea (analytical pure) 1%, butyl titanate, dehydrated alcohol, acetic acid are placed in the reaction flask according to the above ratio, and stirred at a temperature of 15°C for 30 Minutes, then thiourea aqueous solution was added to the reaction solution, and the reaction was continued for 2 hours to obtain a titanium dioxide sol. The solvent was evaporated to obtain a gel, and the gel was dried in an air atmosphere at 100° C. for 2 hours to obtain a dried solid. Grind the dried solid, put it into a muffle furnace after grinding, heat up to 450°C at a rate of 2°C / min at room temperature, calcinate for 2 hours, and cool down to room temperature to obtain a sample of ...

Embodiment 3

[0022] Embodiment 3: Sol-gel method prepares sulfur and nitrogen co-doped titanium dioxide, the raw material ratio (percentage by weight, total weight is 50 grams) of synthetic titanium dioxide sol: butyl titanate (analytical pure) 5%, dehydrated alcohol (analytical Pure) 88%, acetic acid (analytical pure) 5%, thiourea (analytical pure) 3%, put butyl titanate, absolute ethanol, acetic acid in the reaction flask according to the above ratio, and stir at a temperature of 15°C for 30 Minutes, then thiourea aqueous solution was added to the reaction solution, and the reaction was continued for 2 hours to obtain a titanium dioxide sol. The solvent was evaporated to obtain a gel, and the gel was dried in an air atmosphere at 100° C. for 2 hours to obtain a dried solid. Grind the dried solid, put it into a muffle furnace after grinding, raise the temperature to 450°C at a rate of 2°C / min at room temperature, calcinate for 2 hours, and cool down to room temperature to obtain the targe...

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Abstract

The invention provides a method for preparing sulfur and nitrogen co-doped titanium dioxide with visible light catalytic activity, which adopts a sol-gel method and comprises the following steps: hydrolyzing titanium ester and introducing sulfur and nitrogen sources to obtain a titanium dioxide sol, wherein the sulfur and nitrogen sources are from thiourea solution; in a sol system, dropwise adding 1 to 5 percent saturated aqueous solution of thiourea to perform the hydrolysis reaction to obtain the sol; then performing aging and volatilizing a diluent to obtain a titanium dioxide gel; drying the titanium dioxide gel and grinding into powders; performing heat treatment on the solid powder; and calcinating to obtain sulfur and nitrogen co-doped titanium dioxide nano powder. In the method, the thiourea is used as the raw materials of the nitrogen and sulfur sources, the sulfur and the nitrogen are simultaneously introduced in the process of the hydrolysis reaction of the sol to achieve synergistic effect and improve the reaction efficiency, raw material consumption is less, the process is simplified, the absorption range of visible light is effectively improved, the wavelength of the visible light is expanded to about 650nm, and the sulfur and nitrogen co-doped titanium dioxide has obvious visible light activity in the photocatalytic degradation reaction of organic pollutant molecules.

Description

Technical field: [0001] The present invention relates to a kind of titanium dioxide (TiO 2 ) A method for preparing a photocatalyst, especially a method for preparing sulfur and nitrogen co-doped titanium dioxide with visible light catalytic activity. Background technique: [0002] The problem of environmental pollution has also become a focal issue that threatens human existence, and the use of semiconductor photocatalyst photocatalytic technology to solve environmental pollution, due to its high photochemical conversion efficiency, high stability and non-selectivity to various organic pollutants , especially the unique advantage of directly using solar energy for photochemical conversion, has been highly valued by scientists. At present, semiconductor photocatalysts have been successfully applied and eliminated various organic pollutants, such as: alkanes, fuels, olefins, fatty alcohols, aliphatic carboxylic acids, simple aromatic compounds and pesticide residues. In the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/06
Inventor 魏刚李翔熊蓉春
Owner BEIJING UNIV OF CHEM TECH
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