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Process for preparing nano mesoporous titanium dioxide at low tempeature

A titanium dioxide, nano-mesoporous technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of small specific surface area and large grain size, and achieve the effect of high photocatalytic activity

Inactive Publication Date: 2006-08-23
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the problems that the nano-mesoporous titanium dioxide prepared by the existing technology has a large grain size and a small specific surface area, and the preparation process needs high-temperature heat treatment, etc., to provide a preparation process that does not require high-temperature calcination. The temperature is lower than 100°C, and the prepared nano-mesoporous titanium dioxide grains are very small, and has the advantages of large specific surface area and crystal phase control. A low-temperature preparation method of nano-mesoporous titanium dioxide

Method used

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  • Process for preparing nano mesoporous titanium dioxide at low tempeature
  • Process for preparing nano mesoporous titanium dioxide at low tempeature

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Example 1: Dissolve 10ml of butyl titanate in 20ml of absolute ethanol solution, stir and mix. In addition, dissolve 3g of P123 in 45ml of absolute ethanol, then add 2.6ml of 2mol / L dilute hydrochloric acid, and stir to mix. Add this solution dropwise to the ethanol solution of butyl titanate, stir at 40°C for 1 hour, let it stand and solidify for 20 hours, then let it dry at room temperature to form a xerogel and grind it into powder. Take 3.5g of finely ground dry powder, put it into 111.4ml of 0.15mol / L hydrochloric acid ethanol solution (1.4ml of concentrated hydrochloric acid + 10ml of water + 100ml of absolute ethanol), heat to 78°C and stir and reflux for 24h. Centrifuge at high speed, wash the precipitate three times with water, and then wash once with absolute ethanol. Dry at 80°C for 12 hours to obtain a specific surface area of ​​234.5m 2 / g, mesopore size is 3.4nm (by figure 1 It can be seen from the pore size distribution diagram), the grain size is abou...

Embodiment 2

[0021] Example 2: 10ml of butyl titanate was dissolved in 20ml of absolute ethanol solution, and stirred and mixed. In addition, dissolve 3gP123 in 45ml of absolute ethanol, then add 2.6ml of 2mol / L dilute hydrochloric acid, stir and mix. Add this solution dropwise to the ethanol solution of butyl titanate, stir at 40°C for 1 hour, let it stand and solidify for 20 hours, then let it dry at room temperature to form a xerogel and grind it into powder. Take 2.5g of finely ground dry powder, put it into 80ml of 0.4mol / L hydrochloric acid ethanol solution (2.6ml of concentrated hydrochloric acid + 7.4ml of water + 70ml of absolute ethanol), heat to 78°C and stir and reflux for 24h. Centrifuge at high speed, wash the precipitate three times with water, and then wash once with absolute ethanol. Dry at 80°C for 12 hours to obtain a specific surface area of ​​202.7m 2 Titanium dioxide mixed crystal powder containing 80% anatase phase and 20% crystal redite phase with a mesopore size ...

Embodiment 3

[0022] Example 3: 10 ml of butyl titanate was dissolved in 20 ml of absolute ethanol solution, and stirred and mixed. In addition, dissolve 3g of P123 in 45ml of absolute ethanol, then add 2.6ml of 2mol / L dilute hydrochloric acid, and stir to mix. Add this solution dropwise to the ethanol solution of butyl titanate, stir at 40°C for 1 hour, let it stand and solidify for 20 hours, then let it dry at room temperature to form a xerogel and grind it into powder. Take 6.0 g of finely ground dry powder, put it into 155 ml of 2.35 mol / L hydrochloric acid ethanol solution (30 ml of concentrated hydrochloric acid + 5 ml of water + 120 ml of absolute ethanol), and heat to 78°C and stir and reflux for 24 hours. Centrifuge at high speed, wash the precipitate three times with water, and then wash once with absolute ethanol. Dry at 80°C for 12 hours to obtain a specific surface area of ​​165.9m 2 / g, titanium dioxide powder in the rutile phase with a mesopore size of 4.0nm and a grain siz...

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Abstract

The present invention relates to one low temperature preparation process of nanometer mesoporous titania with high photocatalytic activity, and the preparation process has reaction temperature lower than 100deg.c and can prepare nanometer mesoporous titania with superfine crystal grain size, great specific surface area and controllable crystal phase. The preparation process includes the following steps: dissolving titanate in absolute ethyl alcohol to obtain solution A, dissolving three block copolymer in alcohol and adding acid to obtain solution B, and dropping the solution B into the solution A under stirring to obtain solution C; stilling solution C to cure, air drying to obtain gel and grinding to obtain powder; setting the powder into alcohol solution of acid, heating, stirring and refluxing, extracting template agent P123 while converting titania from amorphous form into crystalline form; and centrifuging, washing and drying the precipitate.

Description

technical field [0001] The invention relates to a nanometer mesoporous titanium dioxide, in particular to a low-temperature preparation method of the nanometer mesoporous titanium dioxide with relatively high photocatalytic activity. Background technique [0002] Ordered mesoporous materials are one of the international interdisciplinary research hotspots in recent years. Classified by chemical composition, mesoporous materials can generally be divided into two categories: silicon-based and non-silicon-based. The former mainly includes ordered mesoporous SiO 2 , There are many reports on its research, the latter including transition metal oxides, phosphates and sulfides. Since most non-silicon-based mesoporous materials have variable valence states, it is possible to open up new and broader application fields for mesoporous materials. Titanium dioxide is one of the most widely used materials among them. [0003] TiO2 has been one of the most widely studied metal oxides as...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053
Inventor 廖代伟欧延林敬东邹红梅方舒玫
Owner XIAMEN UNIV
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