Prepn process of nanometer crystal titania aerogel with high photocatalysis activity

A catalytic activity, nanocrystalline technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc. Controllable crystal phase, high thermal stability, short preparation cycle, easy separation and recovery

Inactive Publication Date: 2006-08-02
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using titanium alkoxides such as butyl titanate as raw materials, airgel TiO can be obtained by using the traditional sol-gel method combined with supercritical drying technology. 2 , this process not only has a long preparation cycle, but also usually needs to use titanium alkoxide as a precursor which is expensive and difficult to control the hydrolysis process (J Non Cryst Solids, 2004, 350: 314; J Mol CatalA, 2005, 229 (1-2)

Method used

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  • Prepn process of nanometer crystal titania aerogel with high photocatalysis activity
  • Prepn process of nanometer crystal titania aerogel with high photocatalysis activity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Preparation of bulk nanocrystalline airgel TiO with propylene oxide as gelling agent 2 The method of photocatalyst is as follows: take titanium tetrachloride as titanium source, 2 milliliters of titanium tetrachloride (TiCl 4 ) was added dropwise in the mixed solution that 20 milliliters of absolute ethanol and 1 milliliter of distilled water formed, the mol ratio of water and titanium tetrachloride was 3, stirred for 15 minutes; Control the reaction temperature of gel-forming container to be 25 ℃; Quickly add 3.5 milliliters of ring Propylene oxide, the molar ratio of propylene oxide to titanium tetrachloride is 5, after stirring for 3-5 minutes, a block titanium oxide alcohol gel is obtained; aging at room temperature for 2 hours, and then block is obtained under the supercritical condition of carbon dioxide near room temperature TiO 2 Aerogel ( figure 1 ). Finally, the bulk airgel TiO 2 Calcined at 400 °C for 4 hours to obtain bulk nanocrystalline airgel TiO in a...

Embodiment 2

[0022] Titanium source is titanium tetrachloride (TiCl 4 ), the epoxide is epichlorohydrin, and the organic alcohol solvent is isopropanol, water and TiCl 4 The molar ratio is 6, and the reaction temperature of the gel-forming container is controlled to be 0°C. Other conditions such as titanium source concentration, solvent and epichlorohydrin relative to the amount of titanium source, alcohol gel aging time, roasting temperature and time, etc. are all the same as those in the examples. 1 is the same. Blocky Amorphous TiO Prepared by Supercritical Carbon Dioxide Drying at Near Room Temperature 2 airgel. After the sample was pulverized and calcined at 500°C for 6 hours, the specific surface area was 101m 2 g -1 Powdered Anatase Crystalline Nanocrystalline Airgel TiO 2 . The photocatalytic experiment of nitrobenzene was the same as that in Example 1. The photocatalytic degradation experiment results showed that the removal rate of nitrobenzene on the sample synthesized in ...

Embodiment 3

[0024] Titanium source is titanium tetrachloride (TiCl 4 ), the epoxide is epichlorohydrin, and the organic alcohol solvent is methanol, water and TiCl 4 The molar ratio is 6, the reaction temperature of the gel-forming container is controlled at 80°C, and the alcohol gel is aged at room temperature for 12 hours. Other conditions such as the concentration of titanium source, the amount of solvent and epichlorohydrin relative to the titanium source, and the roasting temperature and time are uniform. Same as Example 1. Blocky Amorphous TiO Prepared by Supercritical Carbon Dioxide Drying at Near Room Temperature 2 Airgel, after calcination at 700°C for 6 hours, the nanocrystalline airgel TiO with mixed crystal structure with anatase and rutile ratios of 80 and 20 were obtained 2 , with a specific surface area of ​​71m 2 g -1 . The photocatalytic experiment of nitrobenzene was the same as that in Example 1. The photocatalytic degradation experiment results showed that the rem...

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Abstract

The preparation process of aerogel TiO2 with high photocatalysis activity includes the following steps: dissolving non-titanium alkoxide and titanium source in alcohol-water mixture solution through stirring; adding metered epoxide to obtain translucent lumpy alcohol gel of titanium oxide in minutes; ageing, supercritical drying and roasting to obtain nanometer crystal aerogel TiO2 block or powder with adjustable micro structure and specific surface area greater than 100 sq m/g. Where, the titanium source is titanium tetrachloride, titanium trichloride or titanium sulfate; the epoxide is ethylene oxide, propylene oxide, chloropropylene oxide or butylenes oxide; and the organic alcohol solvent is methanol, ethanol, isopropanol or tert-butyl alcohol. When used in degrading nitrobenzene and other sewage treatment, the aerogel TiO2 has photocatalysis activity as high as three times that of commercial P-25 photocatalyst.

Description

technical field [0001] The invention relates to a method for preparing a highly active nanocrystalline titanium dioxide powder semiconductor photocatalyst, and in particular provides a method for preparing nanocrystalline titanium dioxide airgel through a non-titanium alkoxide sol-gel route. technical background [0002] Titanium dioxide (TiO 2 ) Photocatalytic materials have very broad application prospects in the fields of solar energy storage and utilization, photochemical conversion, organic pollutant treatment, sterilization and disinfection, and ecological building materials, which has aroused extensive interest and enthusiasm from governments, industrial departments and academic circles around the world. focus on. For decades, especially in the past ten years, semiconductor photocatalytic materials have become the research focus and focus of scientists all over the world. There are more and more research papers and patents in this area, and thousands of research work...

Claims

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Application Information

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IPC IPC(8): B01J21/06B01J37/00
Inventor 曹勇陈麟朱建刘永梅范康年
Owner FUDAN UNIV
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