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Method for preparing titanium dioxide mesoporous material

A technology of titanium dioxide and mesoporous materials, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of poor thermal stability, complicated preparation process, inability to generate photo-generated holes and photo-generated electrons, etc. Stability and photocatalytic activity, the effect of broadening the range of applications

Inactive Publication Date: 2005-03-16
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Even if the template agent is completely removed by organic solvent extraction and the pores do not collapse, the amorphous pore walls cannot generate photogenerated holes and photogenerated electrons under photoexcitation, so there is no photocatalytic activity.
For example, as disclosed in Chinese patent CN 1287878A, titanium dioxide with a mesoporous structure and crystalline pore walls is obtained by first preparing a titanium-silicon composite and then removing silicon oxide with alkali, but the preparation process is complicated and requires a large amount of silicon source and base
Report in Chem.Mater.2003,15,3841., use Pluronic series block copolymer as template agent, can obtain the mesoporous titania of bigger aperture, thicker wall, but relevant research concentrates on the preparation of titania thin film, and The thermal stability is not very good. When the temperature reaches 350°C and the crystal transformation occurs, the pore wall collapses and the specific surface area decreases rapidly.

Method used

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  • Method for preparing titanium dioxide mesoporous material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 3.2g template agent series block copolymer EO 20 PO 70 EO 20 Dissolve in 15mL of n-butanol, and then add 7.5mL of tetrabutyl titanate. After stirring for 3 h, 0.04 g of La(NO 3 ) 3 ·nH 2 O, 1.4 mL of hydrochloric acid, 1.9 mL of water in 15 mL of butanol were added dropwise to the above solution. After the dropwise addition was completed, stirring was continued for 3h. The obtained sol was poured into a Petri dish and aged at room temperature for 48 h. Then continue aging at 40°C for 48h, and then aging at 150°C for 12h. The obtained xerogel was ground for use.

[0035] Take 2 g of the obtained xerogel, and program the temperature in the air flow, 1 ° C min -1 , to 400 ℃ and then keep warm for 5h. Then at 10°C min -1 Cool down to room temperature. 0.70 g of white solid powder was obtained.

[0036] Take 0.5g of the obtained catalyst, use a UV lamp with a cooling water jacket and a power of 300 watts as a light source, and degrade 50mL of concentration to 20...

Embodiment 2

[0038] 3.2g template agent series block copolymer EO20 PO 70 EO 20 Dissolve in 12 mL of isopropanol, and then add 6.3 mL of isopropyl titanate. After stirring for 3 h, 0.08 g of La(NO 3 ) 3 ·nH 2 O, 1.4 mL of hydrochloric acid, 1.9 mL of water in 12 mL of isopropanol were added dropwise to the above solution. After the dropwise addition was completed, stirring was continued for 3h. The obtained sol was poured into a petri dish and aged at room temperature for 36 h. Then continue aging at 60°C for 24h, and then aging at 130°C for 24h. The obtained xerogel was ground for use.

[0039] Take 2 g of the obtained xerogel, and program the temperature in the air flow, 1 ° C min -1 , to 450 ℃ and then keep warm for 3h. Then at 10°C min -1 Cool down to room temperature. 0.68 g of white solid powder was obtained.

Embodiment 3

[0041] 1.5g template agent series block copolymer EO 106 PO 70 EO 106 Dissolve in 10mL ethanol, then add 5.0mL tetraethyl titanate. After stirring for 3 h, 0.02 g of La(NO 3 ) 3 ·nH 2 O, 1.4 mL of hydrochloric acid, 1.9 mL of water in 10 mL of ethanol were added dropwise to the above solution. After the dropwise addition was completed, stirring was continued for 3h. The obtained sol was poured into a Petri dish and aged at room temperature for 24 h. Then continue aging at 50°C for 36h, and then aging at 120°C for 36h. The obtained xerogel was ground for use.

[0042] Take 1.5 g of the obtained xerogel, and heat it up in an air stream at 1°C min -1 , to 550 ℃ and then keep warm for 1h. Then at 10°C min -1 Cool down to room temperature. 0.52 g of white solid powder was obtained.

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Abstract

The invention relates to a method for preparing titanium dioxide mesoporous material which consists of, using segmented copolymer as mold plate, employing sol gel method to obtain large-hole diameter, high thermal stability and high optical catalytic activity rare earth doped titanium dioxide mesoporous material. The doped rare-earth salts can substantially improve the thermal stability and optical catalytic activity for the titanium dioxide mesoporous material.

Description

technical field [0001] The invention relates to a method for preparing a titanium dioxide mesoporous material, in particular to a method for preparing a rare earth-doped titanium dioxide mesoporous material with high photocatalytic activity and high thermal stability. Background technique [0002] Porous materials are widely used in catalysis, separation and other fields, and can be divided into microporous materials, mesoporous materials and macroporous materials according to pore size. Mesoporous materials refer to porous materials with a pore size between 2nm and 50nm, which have special properties different from molecular sieves and macroporous materials. Since Mobil first prepared mesoporous silica MCM series in 1992, the preparation of mesoporous materials has become a hot field. [0003] Transition metal oxides have special properties and are widely used in catalysis and other fields. Transition metal oxides with various mesoporous structures have received unpreceden...

Claims

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Application Information

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IPC IPC(8): C01G23/053
Inventor 张金龙袁帅盛巧蓉陈锋田宝柱孙健
Owner EAST CHINA UNIV OF SCI & TECH
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