Preparation method of nitrogen-doped titanium dioxide mesoporous visible light photocatalyst

A technology of titanium dioxide and photocatalyst, which is applied in the field of photocatalyst preparation, can solve the problems of high nitriding temperature, difficulty in obtaining high specific surface area, long reaction time, etc., and achieve the effect of high absorption coefficient and high visible light spectrum absorption range

Inactive Publication Date: 2014-04-02
ZHENJIANG DONGYI MACHINERY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, due to the high nitriding temperature and long reaction time, titanium dioxide will inevitably grow up, and it is difficult to obtain a nitrogen-doped titanium dioxide visible light catalyst with a high specific surface area and ultrafine grains by gas-solid reaction of nano-titanium dioxide.

Method used

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  • Preparation method of nitrogen-doped titanium dioxide mesoporous visible light photocatalyst
  • Preparation method of nitrogen-doped titanium dioxide mesoporous visible light photocatalyst
  • Preparation method of nitrogen-doped titanium dioxide mesoporous visible light photocatalyst

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Embodiment 1

[0038] Add 0.1M hydrochloric acid ethanol solution to the ethanol solution of ethyl tetrasilicate with a volume ratio of 1:1, so that the ratio of silicon to water is 1:1, reflux at 70 degrees Celsius for 1 hour, and cool to room temperature. Then add an ethanol solution of butyl titanate with a volume ratio of 1:1, so that the ratio of the amount of Ti / Si material is 1:3. Then gradually add 0.1M ethanol solution of hydrochloric acid, so that the amount of water is twice the sum of the amounts of titanium and silicon. A gel formed after 12 hours. Dried, crushed, sieved, and calcined at 600 degrees Celsius for two hours. Weigh 2 grams after cooling, place in a tube furnace, flow rate is 1000 ml / min in flowing ammonia, nitriding at 900 degrees Celsius for 5 hours, and cool to room temperature in nitrogen protection. Weigh 2 grams, wash in 5.0M sodium hydroxide solution at 60°C for 12 hours, and dry at 110°C after washing with water. Its transmission electron microscope pictur...

Embodiment 2

[0041] Add 0.1M hydrochloric acid ethanol solution to the ethanol solution of tetraethyl orthosilicate with a volume ratio of 1:2, so that the mass ratio of silicon to water is 1:1, reflux at 70°C for 1 hour, and cool to room temperature. Then add an ethanol solution of butyl titanate with a volume ratio of 1:2, so that the ratio of the amount of Ti / Si material is 1:1. Then gradually add 0.1M ethanol solution of hydrochloric acid, so that the amount of water is twice the sum of the amounts of titanium and silicon. A gel formed after 24 hours. Dried, crushed, sieved, and calcined at 600 degrees Celsius for two hours. Weigh 2 grams after cooling, place in a tube furnace, flow rate is 1000 ml / min in flowing ammonia, nitriding at 900 degrees Celsius for 5 hours, and cool to room temperature in nitrogen protection. Weigh 2 grams, wash in 5.0M sodium hydroxide solution at 60°C for 24 hours, and dry at 110°C after washing. The absorption spectrum of the diffuse reflectance mode is...

Embodiment 3

[0044] Add 0.1M hydrochloric acid ethanol solution to the ethanol solution of tetraethyl orthosilicate with a volume ratio of 1:2, so that the mass ratio of silicon to water is 1:1, reflux at 70°C for 1 hour, and cool to room temperature. Then add an ethanol solution of butyl titanate with a volume ratio of 1:2, so that the ratio of the amount of Ti / Si material is 1:4. Then gradually add 0.1M ethanol solution of hydrochloric acid, so that the amount of water is twice the sum of the amounts of titanium and silicon. A gel formed after 24 hours. Dried, crushed, sieved, and calcined at 600 degrees Celsius for two hours. Weigh 2 grams after cooling, place in a tube furnace, flow rate is 1000 ml / min in flowing ammonia, nitriding at 900 degrees Celsius for 2 hours, and cool to room temperature in nitrogen protection. Weigh 2 grams, wash in 5.0M sodium hydroxide solution at 60°C for 24 hours, and dry at 110°C after washing. Raman spectrum such as image 3 Shown, 152.1 degrees Cels...

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Abstract

The invention discloses a preparation method of a nitrogen-doped titanium dioxide mesoporous visible light photocatalyst, and belongs to the field of novel materials. The preparation method is mainly characterized by comprising the following steps: preparing a compound titanium silicon oxide by taking titanium alkoxide and tetraethoxysilane as main raw materials and inorganic acid as a hydrolysis catalyst according to a sol-gel method, drying, grinding and sieving the compound oxide, and performing high-temperature calcinations to remove organic matters from gel; nitriding calcined powder in flowing ammonia gas at 850-950 DEG C, cooling to room temperature, washing through an alkaline solution, and dissolving silicon dioxide and excess nitrogen to obtain the nitrogen-doped titanium dioxide mesoporous visible light photocatalyst. The nitrogen-doped titanium dioxide mesoporous visible light photocatalyst is an agglomerate formed by nitrogen-doped titanium dioxide with the mesoporous and crystal particle sizes less than 10 nm, the specific surface area is more than 150 m<2>/g, and the spectral response range is expanded to the wavelength of 600 nm.

Description

technical field [0001] The invention relates to a preparation method of a nitrogen-doped titanium dioxide mesoporous visible light-responsive photocatalyst, which belongs to the field of new materials. technical background [0002] Nano-titanium dioxide is a very effective photocatalyst, but it also has the disadvantages that it can only absorb ultraviolet light and cannot use visible light, which accounts for 40% of sunlight. After nitrogen and other non-metallic elements replace the oxygen in titanium dioxide, the photoresponse range of titanium dioxide can be extended from ultraviolet light to visible light region, and show visible light catalytic activity. The currently reported nitrogen doping methods mainly include titanium oxide surface nitriding treatment (Asahi R, Morikawa T, Ohwaki T, et al. S degrees Celsius ien degrees Celsius e , 2001, 293, 269-271), using ammonia gas and nano titanium dioxide gas-solid reaction at 500-600 degrees Celsius, nitrogen doped titani...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24
Inventor 张青红陈立军郭冬雪陆最美
Owner ZHENJIANG DONGYI MACHINERY
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