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Method for modulating titanium dioxide crystalline phases by using fluoride ions

A technology of titanium dioxide and fluorine ions, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of complex process, high reaction temperature, high energy consumption, etc., and achieve the effect of simple process, mild reaction conditions and low energy consumption

Active Publication Date: 2015-02-11
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, the preparation of composite phase titanium dioxide generally adopts high temperature treatment, high reaction temperature (above 550°C), high energy consumption, complex process and large investment

Method used

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  • Method for modulating titanium dioxide crystalline phases by using fluoride ions
  • Method for modulating titanium dioxide crystalline phases by using fluoride ions
  • Method for modulating titanium dioxide crystalline phases by using fluoride ions

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0038] This embodiment provides a method for adjusting the crystal phase of titanium dioxide using fluoride ions, which includes the following steps:

[0039] Add 0.1g of titanium powder (200 mesh) into 30mL of HCl solution with a concentration of 2mol / L to obtain a suspension solution, and stir for 15min;

[0040] Then, 0 mL (as a comparison), 0.01 mL, 0.05 mL, 0.1 mL, 0.2 mL, 0.3 mL, and 0.4 mL of HF solution with a concentration of 5 mol / L were added to the seven suspension solutions to obtain seven parts of the reaction mixture. Quickly transfer to a 50mL autoclave with a Teflon liner;

[0041] Transfer the high-pressure reactor to an electric oven, heat the reaction mixture to 220°C and keep it for 12 hours for crystallization;

[0042] After the crystallization treatment is completed, the reaction mixture is cooled to room temperature, filtered, washed with water, and dried at 50°C to obtain a solid product;

[0043] Finally, the solid product was treated with NaOH solut...

Embodiment 2

[0047] This embodiment provides a method for adjusting the crystal phase of titanium dioxide using fluoride ions, which includes the following steps:

[0048] Add 0.1g of titanium powder (200 mesh) into 30mL of HCl solution with a concentration of 2mol / L to obtain a suspension solution, and stir for 15min;

[0049] Then, 0.01mL, 0.05mL, 0.1mL, 0.2mL, 0.5mL, 1mL, and 2mL of NH4F solutions with a concentration of 5mol / L were added to the seven suspension solutions to obtain seven reaction mixtures, which were quickly transferred to 50mL autoclave with PTFE lining;

[0050] Transfer the high-pressure reactor to an electric oven, heat the reaction mixture to 220°C and keep it for 12 hours for crystallization;

[0051] After the crystallization treatment is completed, the reaction mixture is cooled to room temperature, filtered, washed with water, and dried at 50°C to obtain a solid product;

[0052] Finally, the solid product was treated with NaOH solution with a concentration o...

Embodiment 3

[0056] This embodiment provides a method for adjusting the crystal phase of titanium dioxide using fluoride ions, which includes the following steps:

[0057] Add 0.1g of titanium powder (200 mesh) into 30mL of HCl solution with a concentration of 2mol / L to obtain a suspension solution, and stir for 15min;

[0058] Then, 0 mL (as a comparison), 0.1 mL, 0.5 mL, 1 mL, 2 mL, and 3 mL of NaF solution with a concentration of 5 mol / L were added to the seven suspension solutions to obtain six reaction mixtures, which were quickly transferred to a volume of 50 mL. In a high-pressure reactor with a PTFE liner;

[0059] Transfer the high-pressure reactor to an electric oven, heat the reaction mixture to 220°C and keep it for 12 hours for crystallization;

[0060] After the crystallization treatment is completed, the reaction mixture is cooled to room temperature, filtered, washed with water, and dried at 50°C to obtain a solid product;

[0061] Finally, the solid product was treated w...

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Abstract

The invention relates to a method for modulating titanium dioxide crystalline phases by using fluoride ions. According to the method, during the preparation of titanium dioxide by using a hydrothermal method or a solvothermal method, the fluoride ions are added to modulate the titanium dioxide crystalline phases, and the modulation is performed among three phases of rutile, brookite and anatase. The method has the following advantages: phase transformation of the titanium dioxide is realized under a mild processing condition, and the transformation trend is from a steady rutile phase to a metastable anatase phase; the prepared compound phase titanium dioxide is high in crystallinity, is a monocrystal titanium dioxide, and is conducive to fast transfer of photoexcited electrons; and the method for preparing the compound phase titanium dioxide is simple in process, mild in processing condition, low in energy consumption and easy to realize large-scale promotion and application.

Description

technical field [0001] The invention relates to a method for modulating the crystal phase of titanium dioxide by using fluorine ions, and belongs to the technical field of titanium dioxide preparation. Background technique [0002] Titanium dioxide is a kind of semiconductor with high photocatalytic activity, good photochemical stability and water stability, which is non-toxic to human body, abundant in reserves, and cheap and easy to obtain. It has always been one of the hot research materials in the field of photochemistry and optoelectronics. [0003] How to further improve its photocatalytic and photoelectrochemical properties has been a research hotspot in this field. There are many factors affecting the properties of titanium dioxide, among which the crystal form is a major factor. Titanium dioxide has three crystal forms: anatase, rutile and brookite. Anatase titanium dioxide is recognized as having the best photocatalytic activity. But there are also controversies...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053
Inventor 姜桂元崔晓峰徐春明赵震段爱军刘坚韦岳长
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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