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Process for preparing anatase type nano-titanium dioxide

A nano-titanium dioxide, anatase type technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of low equipment material requirements, low operating temperature, expensive raw materials, etc., and achieve low cost and uniform particle size distribution. , the effect of less raw material components

Inactive Publication Date: 2009-08-19
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Titanium alkoxide vapor phase hydrolysis has low operating temperature, low energy consumption, low requirements on equipment materials, and sustainable production. The disadvantage is that the raw materials are more expensive
At the same time, in order to improve the photocatalytic activity of nano-titanium dioxide powder, it is necessary to ensure the source of sufficient hydroxyl radicals, while patents CN1686823 and CN1478725 do not guarantee
[0008] P.Billik et al. (Scripta Mater.56 (2007) 979-982) with TiCl 4 As raw materials, anatase nano-titanium dioxide powder is obtained by mechanochemical reaction and heat treatment. Due to the need for high-temperature heat treatment, hard agglomeration of the powder will inevitably occur, which will affect the activity of the powder.

Method used

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  • Process for preparing anatase type nano-titanium dioxide
  • Process for preparing anatase type nano-titanium dioxide
  • Process for preparing anatase type nano-titanium dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] like figure 1 So, 1) Get 50ml of absolute ethanol and put it into an ice-water bath, add 10ml of TiCl dropwise 4 , a pale yellow solution was obtained. The light yellow solution was vigorously stirred in an ice-water bath for 10 minutes, then 50 ml of deionized water was added to form a colorless transparent solution, and the vigorous stirring was continued for 120 minutes. 2) Then add ρ=0.91×10 3 kg / m 3 ammonia solution to pH = 8 to obtain a white solid; then filtered and washed with deionized water to pH = 7 to obtain an anatase nano-titanium dioxide precursor (white solid). 3) Add 50ml of ρ=1.11×10 to the anatase nano-titanium dioxide precursor 3 kg / m 3 H 2 o 2 , Stirring at 60°C for 2h, a yellow sol was obtained. Transfer the yellow sol into a polytetrafluoroethylene-lined reactor for hydrothermal treatment at 140°C for 2 hours, and vacuum-dry at 60°C to obtain white anatase-type nano-titanium dioxide powder with high activity and controllable particle size...

Embodiment 2

[0031] 1) Take 200ml of absolute ethanol and put it in an ice water bath, add 10ml of TiCl dropwise 4 , a pale yellow solution was obtained. The light yellow solution was vigorously stirred in an ice-water bath for 60 minutes, then 300 ml of deionized water was added to form a colorless transparent solution, and the vigorous stirring was continued for 10 minutes. 2) Then add ρ=0.91×10 3 kg / m 3 ammonia solution to pH = 8 to obtain a white solid, which was then filtered and washed with deionized water until pH = 7 to obtain an anatase-type nano-titanium dioxide precursor (white solid). 3) Add 200ml of ρ=1.11×10 to the anatase nano-titanium dioxide precursor 3 kg / m 3 H 2 o 2 , Stirring at 60°C for 2h, a yellow sol was obtained. Transfer the yellow sol into a polytetrafluoroethylene-lined reactor for hydrothermal treatment at 180°C for 8 hours, and vacuum-dry at 60°C to obtain white anatase-type nano-titanium dioxide powder with high activity and controllable particle size....

Embodiment 3

[0033] 1) Take 100ml of absolute ethanol and put it in an ice-water bath, add 10ml of TiCl dropwise 4 , a pale yellow solution was obtained. The light yellow solution was vigorously stirred in an ice-water bath for 40 minutes, then 150 ml of deionized water was added to form a colorless transparent solution, and the vigorous stirring was continued for 90 minutes. 2) Then add ρ=0.91×10 3 kg / m 3 ammonia solution to pH = 8 to obtain a white solid, which was then filtered and washed with deionized water until pH = 7 to obtain an anatase-type nano-titanium dioxide precursor (white solid). 3) Add 100ml of ρ=1.11×10 to the anatase nano-titanium dioxide precursor 3 kg / m 3 H 2 o 2 , Stirring at 60°C for 2h, a yellow sol was obtained. Transfer the yellow sol into a polytetrafluoroethylene-lined reactor for hydrothermal treatment at 160°C for 4 hours, and vacuum-dry at 60°C to obtain white anatase-type nano-titanium dioxide powder with high activity and controllable particle size....

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Abstract

The invention relates to a method for preparing anatase type nanometer titanium dioxide. The method is characterized by comprising the following steps: 1) TiCl4 hydrolyzation, in which, selecting the TiCl4, absolute ethyl alcohol and deionized water according to a ratio of 10 ml:50-200 ml:50-300 ml; placing the absolute ethyl alcohol into ice-water bath to be dripped with the TiCl4; and adding the deionized water into the solution to keep on violent stirring for 10 to 120 minutes so as to obtain an achromatic transparent solution; 2) precursor preparation; and 3) hydro-thermal treatment, in which, adding H2O2 with rho of 1.11*10kg / m into the precursor to be stirred for 2 hours at 60 DEG C so as to obtain yellow sol; then, transferring the yellow sol into a reaction kettle with a polyfluortetraethylene lining at a temperature of hydro-thermal treatment of between 140 and 180 DEG C for 2 to 8 hours; and directly drying the product subjected to the hydro-thermal treatment in vacuum at 60 DEG C to obtain anatase type nanometer titanium dioxide powder. The method has the characteristics of low cost, high purity, simple process, high activity and controllable granularity.

Description

technical field [0001] The invention relates to a preparation method of anatase nano-titanium dioxide. Background technique [0002] With the development of the economy, the environmental pollution is becoming more and more serious, especially the pollution of water resources has seriously threatened the health of human beings, and also restricted the development of the economy. There are many ways to treat sewage, common ones are: filtration, sedimentation, air flotation, chemical coagulation, physical and chemical adsorption, etc., but these technologies exist to varying degrees or have low efficiency and cannot be completely removed. Pollutants, easy to produce secondary pollution; or narrow range of use, only suitable for specific pollutants; or high energy consumption, not suitable for large-scale promotion and other defects. [0003] In 1972, Fujishima et al. found that in TiO 2 Photolysis of water on a single crystal electrode, TiO 2 Due to its stable structure, ex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053
Inventor 史晓亮王盛杨行勇王书伟章桥新
Owner WUHAN UNIV OF TECH
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