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Preparation method of titanous auto-doping anatase titanium dioxide monocrystalline

A technology of titanium dioxide and trivalent titanium, applied in chemical instruments and methods, nanotechnology, nanotechnology, etc., can solve problems such as difficult to obtain form distribution, expensive equipment, harsh synthesis conditions, etc.

Inactive Publication Date: 2015-07-01
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process, high energy consumption, multi-steps, harsh synthesis conditions, and expensive equipment, and the reduction of these synthesis methods mainly occur in the surface area. Since the surface oxygen vacancies are usually unstable in the air, trivalent titanium is easily oxidized by dissolved oxygen in water, and it is very difficult to It is difficult to obtain stable and uniform trivalent titanium self-doped anatase titanium dioxide nanocrystals, which limits the practical application of these methods

Method used

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  • Preparation method of titanous auto-doping anatase titanium dioxide monocrystalline
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  • Preparation method of titanous auto-doping anatase titanium dioxide monocrystalline

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] a. Dissolve 0.3g of divalent titanium source titanium hydride in 2mL of deionized water, add 30mL of hydrogen peroxide with a mass fraction of 30% dropwise under constant stirring, and keep stirring the mixed reaction solution rapidly at room temperature for 12h to obtain a gel-like shape mixture;

[0019] b. Under uniform stirring, add 40 mL of absolute ethanol to the mixture obtained in step a, adjust the pH of the mixed solution to 8 with 1.0 M sodium hydroxide solution, then add 0.4 g of sodium borohydride to obtain a transparent yellow mixed solution;

[0020] c. Place the mixed solution obtained in step b in an autoclave at a temperature of 180° C. and react for 24 hours;

[0021] d. Remove the mixed solution obtained in step c from the autoclave, wash it in 50.0mL of 1.0M hydrochloric acid solution for 10h, and then centrifuge to obtain the precipitate, wash it twice with absolute ethanol, wash it three times with deionized water, and place it in Dry in a vacuum...

Embodiment 2

[0024] a. Dissolve 0.3g of divalent titanium source titanium hydride in 2mL of deionized water, add 30mL of hydrogen peroxide with a mass fraction of 30% dropwise under constant stirring, and keep stirring the mixed reaction solution rapidly at room temperature for 12h to obtain a gel-like shape mixture;

[0025] b. Under uniform stirring, add 40 mL of absolute ethanol to the mixture obtained in step a, adjust the pH of the mixed solution to 9 with 1.0 M sodium hydroxide solution, then add 0.4 g of sodium borohydride to obtain a transparent yellow mixed solution;

[0026] c. Place the mixed solution obtained in step b in an autoclave at a temperature of 180° C. and react for 24 hours;

[0027] d. Remove the mixed solution obtained in step c from the autoclave, wash it in 50.0mL of 1.0M hydrochloric acid solution for 10h, and then centrifuge to obtain the precipitate, wash it twice with absolute ethanol, wash it three times with deionized water, and place it in Dry in a vacuum...

Embodiment 3

[0030] a. Dissolve 0.3g of divalent titanium source titanium hydride in 2mL of deionized water, add 30mL of hydrogen peroxide with a mass fraction of 30% dropwise under constant stirring, and keep stirring the mixed reaction solution rapidly at room temperature for 12h to obtain a gel-like shape mixture;

[0031] b. Under uniform stirring, add 40 mL of absolute ethanol to the mixture obtained in step a, adjust the pH of the mixed solution to 9 with 1.0 M sodium hydroxide solution, then add 0.4 g of sodium borohydride to obtain a transparent yellow mixed solution;

[0032] c. Place the mixed solution obtained in step b in an autoclave at a temperature of 180° C. and react for 24 hours;

[0033] d. Remove the mixed solution obtained in step c from the autoclave, wash it in 50.0mL of 1.0M hydrochloric acid solution for 10h, and then centrifuge to obtain the precipitate, wash it twice with absolute ethanol, wash it three times with deionized water, and place it in Dry in a vacuum...

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Abstract

The invention relates to a preparation method of titanous auto-doping anatase titanium dioxide monocrystalline. The method comprises the following steps of oxidation gelatinization and solvothermal of a bivalent titanium source so as to form nano-crystalline, product washing and drying based on a principle of forming nano monocrystalline by solvothermal reaction. Compared with the traditional titanous auto-doping anatase titanium dioxide monocrystalline, the titanous auto-doping anatase titanium dioxide monocrystalline obtained by the method provided by the invention is even in size distribution and does not contain other foreign elements, and the introduction of titanous defect endows a material with an excellent visible light catalytic performance. The method has the advantages of operation simplicity, mild conditions, simple technology, high titanous concentration, controllable doped concentration, high visible light absorbance and the like; the prepared titanous auto-doping anatase titanium dioxide monocrystalline has the efficiency of degrading industrial organic dye methylthionine chloride under visible light better than that of P25, and has a wide application prospect in the fields of industrial waste water treatment by inorganic catalysts and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation of photocatalytic nanomaterials, and in particular relates to a preparation method and application of trivalent titanium self-doped anatase titanium dioxide nanocrystals. Background technique [0002] With the continuous development of the global industrialization process, the problem of environmental pollution is becoming more and more serious. Titanium dioxide is most commonly used for its non-toxicity, high catalytic activity, strong oxidation ability, and good stability. However, titanium dioxide has a wide band gap (about 3.2eV), and only ultraviolet Light (<5% of total solar energy) can be used to generate electron-hole pairs and carry out photoelectrochemical processes. Thus, it is particularly important to increase the light absorption of titanium dioxide in the visible region (43% of total solar energy). Among them, an important way is doping (such as: metal doping and non-metal d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/06B82Y30/00B82Y40/00C02F1/30
CPCY02W10/37
Inventor 王传义辛晓烨王兰
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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