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Preparation method of mesoporous titanium dioxide microballoons with controllable particle size

A mesoporous titanium dioxide, titanium dioxide technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, nanotechnology, etc., can solve the problems of large specific surface energy of particles, limited application range, wide particle size distribution, etc., to achieve good dispersion, The effect of simple process route and narrow particle size distribution range

Inactive Publication Date: 2014-07-02
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Generally, nano-TiO is prepared industrially 2 The particles are made by dissolving ilmenite in concentrated sulfuric acid, and then dehydrating the obtained titanium oxide hydrate. The nano-TiO obtained by this method 2 The specific surface energy of the particles is large, the particles are easy to agglomerate, the particles are mostly irregular shapes, and the particle size distribution is wide, thus limiting their application range

Method used

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  • Preparation method of mesoporous titanium dioxide microballoons with controllable particle size
  • Preparation method of mesoporous titanium dioxide microballoons with controllable particle size
  • Preparation method of mesoporous titanium dioxide microballoons with controllable particle size

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) Under the condition of magnetic stirring, add titanium tetrachloride dropwise to the mixed solution of n-propanol and deionized water in an ice-water bath (volume ratio is 3:1), control the titanium tetrachloride The concentration is 0.1 mol / liter, and the precursor solution is obtained by continuous stirring at low temperature for 8 hours;

[0030] (2) Transfer the precursor solution in step (1) to a water (oil) bath and heat it to 70°C. White precipitates are formed. Continue to age for 30 minutes to completely hydrolyze the titanium tetrachloride precursor solution. The amount of precipitate no longer increase;

[0031] (3) Add NH with an ammonia concentration of 0.5 mol / liter to the precipitation solution in step (2). 3 A mixed solution of ammonia water and n-propanol with a mass fraction of 27%, the solution is adjusted to neutrality, and the obtained precipitate is successively washed with deionized water and n-propanol by centrifugation;

[0032] (4) Disper...

Embodiment 2

[0036] (1) Under the condition of magnetic stirring, add titanium tetrachloride dropwise to the mixed solution of n-propanol and deionized water in an ice-water bath (volume ratio is 3:1), control the titanium tetrachloride The concentration is 0.1 mol / L, add 0.6 g / L hydroxypropyl cellulose, and continue stirring at low temperature for 6 hours to obtain a precursor solution;

[0037] (2) Transfer the precursor solution in step (1) to a water (oil) bath and heat it to 80°C. White precipitates of titanium dioxide are formed. Continue to age for 20 minutes to completely hydrolyze the titanium tetrachloride precursor solution. The precipitated no longer increase in volume;

[0038](3) Add NH with an ammonia concentration of 0.5 mol / liter to the precipitation solution in step (2). 3 A mixed solution of ammonia water and n-propanol with a mass fraction of 27%, the solution is adjusted to neutrality, and the obtained precipitate is successively washed with deionized water and n-prop...

Embodiment 3

[0043] (1) Under the condition of magnetic stirring, add titanium tetrachloride dropwise to the mixed solution of n-propanol and deionized water in an ice-water bath (volume ratio is 5:1), control the titanium tetrachloride The concentration is 0.05 mol / liter, add 0 g / liter of hydroxypropyl cellulose, and continue stirring at low temperature for 4 hours to obtain a precursor solution;

[0044] (2) Transfer the precursor solution in step (1) to a water (oil) bath and heat it to 60°C. White precipitates are formed. Continue to age for 10 minutes to completely hydrolyze the titanium tetrachloride precursor solution. The amount of precipitate no longer increase;

[0045] (3) Add NH with an ammonia concentration of 2.5 mol / liter to the precipitation solution in step (2). 3 A mixed solution of ammonia water and n-propanol with a mass fraction of 27%, the solution is adjusted to neutrality, and the obtained precipitate is successively washed with deionized water and n-propanol by ce...

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Abstract

The invention relates to a preparation method of mesoporous titanium dioxide microballoons with controllable particle size, which comprises the steps that 1) adding titanium tetrachloride drop by drop in a mixed mixing of n-propanol and deionized water, continuously stirring for 4-10 hours at low temperature to obtain a precursor solution; 2) heating the precursor solution to the temperature of 60-90 DEG C to completely hydrolyzing titanium tetrachloride; 3) adjusting a deposition solution to neutrality and then removing the impurity ions; 4) dispersing the obtained sediment in a mixed solution of ethanol and deionized water, adding ammonia water, performing a solvothermal reaction; and 5) washing and drying the sediment obtained in the step 4) to obtain the mesoporous titanium dioxide microballoons with controllable particle size. According to the invention, the mesoporous titanium dioxide microballoons with controllable particle size can be prepared by a thermal hydrolysis-solvothermal two-step method, the process route is simple, a template is not required, the prepared mesoporous titanium dioxide microballoons have the advantages of good dispersibility, high crystallization degree and large specific surface area, and can be used in the fields of photocatalysis, paints, cosmetics, new energy and the like.

Description

technical field [0001] The invention belongs to the field of preparation of nano titanium dioxide, in particular to a preparation method of mesoporous titanium dioxide microspheres with controllable particle size. Background technique [0002] Since 1972, Japanese scientists Fujishima and Honda published in Nature magazine about TiO 2 Since the paper on the photo-splitting of water on electrodes, TiO 2 Powders have attracted widespread attention from scientists in the fields of international chemistry, physics and materials science. Nano-TiO 2 The powder is non-toxic, cheap, and chemically stable, and is widely used in energy materials, photocatalysts, and gas sensors for sensors. [0003] Generally, nano-TiO is prepared industrially 2 The particles are made by dissolving ilmenite in concentrated sulfuric acid, and then dehydrating the obtained titanium oxide hydrate. The nano-TiO obtained by this method 2 The specific surface energy of the particles is large, the parti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053B82Y40/00
Inventor 张青红芮一川李耀刚王宏志
Owner DONGHUA UNIV
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