A kind of graded mixed crystal tio2 micro-nano material, preparation method and application thereof

A micro-nano and nano-sheet technology, applied in the field of photocatalysis, can solve problems such as limiting catalytic activity and structural stability, and achieve the effects of excellent catalytic activity, simple process flow, and easy popularization and use.

Active Publication Date: 2015-09-23
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The micro-nano materials disclosed in the above-mentioned prior art are all hierarchical flower-like structures assembled by one-dimensional nanowires, which limit the TiO 2 Catalytic Activity and Structural Stability of Micro-nanomaterials as Catalysts

Method used

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  • A kind of graded mixed crystal tio2 micro-nano material, preparation method and application thereof
  • A kind of graded mixed crystal tio2 micro-nano material, preparation method and application thereof
  • A kind of graded mixed crystal tio2 micro-nano material, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] (1) Put 0.67 mol / L metal Ti powder into a mixed solution of 9 mol / L hydrogen peroxide and 0.8 mol / L nitric acid (the total volume is kept at 150 mL), condense and reflux in an oil bath at 80°C for 2 hours to obtain orange Yellow solution, hydrothermal reaction with 10mol / L NaOH solution at 150°C for 5 hours, after natural cooling to room temperature, centrifuge the product, wash once with 0.1mol / L nitric acid and wash with water until the pH value is 7 , dried and calcined at 450°C to obtain anatase graded TiO 2 ;

[0064] (2) Add 0.2mol / L tetrabutyl titanate dropwise to a mixed solution of 1.36mol / L concentrated hydrochloric acid and 3mL absolute ethanol, stir evenly in a polytetrafluoroethylene liner, remove 31mL Ionized water was mixed with the above solution, and after stirring for 30 minutes, the liner was sealed and placed in a stainless steel reaction kettle, and the hydrothermal reaction was carried out at 120°C, and the reaction time was 24 hours. After natural...

Embodiment 2

[0073] (1) Put 0.67 mol / L metallic Ti powder into a mixed solution of 9 mol / L hydrogen peroxide and 0.6 mol / L nitric acid (the total volume is kept at 150 mL), condense and reflux in an oil bath at 90°C for 2 hours to obtain orange Yellow solution, hydrothermal reaction with 10mol / L NaOH solution at 150°C for 5 hours, after natural cooling to room temperature, centrifuge the product, wash with 0.05mol / L nitric acid for 5 times, then wash with water until the pH value is 7 , dried and calcined at 350°C to obtain anatase graded TiO 2 ;

[0074] (2) Add 0.3mol / L tetrabutyl titanate dropwise to a mixed solution of 4mol / L concentrated hydrochloric acid and 3mL ethanol, stir well in a polytetrafluoroethylene liner, mix 31mL deionized water with The above solutions were mixed and stirred for 30 minutes, then the inner tank was sealed and placed in a stainless steel reaction kettle, and the hydrothermal reaction was carried out at 120° C., and the reaction time was 24 hours. After n...

Embodiment 3

[0078] (1) Put 0.067 mol / L metallic Ti powder into a mixed solution of 5 mol / L hydrogen peroxide and 0.1 mol / L nitric acid (the total volume is kept at 150 mL), condense and reflux in an oil bath at 80°C for 1 hour to obtain orange Yellow solution, hydrothermal reaction with 5mol / L NaOH solution at 120°C for 1 hour, after natural cooling to room temperature, centrifuge the product, wash twice with 0.5mol / L nitric acid, then wash with water until the pH value is 6.5 , dried and calcined at 450°C to obtain anatase graded TiO 2 ;

[0079] (2) Add 0.02mol / L tetrabutyl titanate dropwise to a mixed solution of 0.1mol / L concentrated hydrochloric acid and 3mL ethanol, stir evenly in a polytetrafluoroethylene liner, add 90mL deionized water Mix with the above solution, stir for 10 minutes, seal the liner and put it into a stainless steel reaction kettle, carry out hydrothermal reaction at 100°C, and the reaction time is 12 hours. After naturally cooling to room temperature, the produ...

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Abstract

The invention belongs to the field of preparation of inorganic micro / nano materials and relates to a fractionated mixed-crystalline TiO2 micro / nano material prepared by a physical mixing method. The method comprises the following steps: preparing anatase type fractionated TiO2 particles and rutile TiO2 particles both composed of two-dimensional nanosheets as base structures by a hydrothermal method, respectively, then enabling rutile particles to be evenly attached on the surface of the anatase by use of a solvent, and enabling the rutile particles and the anatase to be closely bonded with each other by virtue of low-temperature calcination without destroying the morphology, thus obtaining the fractionated mixed-crystalline TiO2 micro / nano material. The diameter of the fractionated mixed-crystalline TiO2 micro / nano material ranges from 0.8 to 2 microns, the width of the nanosheets ranges from 50 to 100nm, the diameter of the rutile particles ranges from 5 to 15nm, and the mass percent of the rutile particles ranges from 1 to 40%. The fractionated mixed-crystalline TiO2 micro / nano material is applicable to the photocatalysis field, and better than Degussa P25 in adsorption property and photocatalysis property while degrading a methylene blue dye.

Description

technical field [0001] The invention relates to a physical mixing method for preparing graded mixed crystal TiO 2 Micro-nano materials and their applications, especially related to an anatase-type hierarchical TiO assembled by two-dimensional nanosheets 2 Graded mixed crystal TiO composed of small particles of rutile 2 Micro-nano materials, preparation methods, and their applications in the field of photocatalysis. Background technique [0002] TiO 2 Nanomaterials have become one of the most deeply researched semiconductor materials in the field of photocatalysis because of their good stability, high photocatalytic efficiency, environmental friendliness and low price. TiO 2 The physical and chemical properties such as photocatalytic activity and refractive index are related to factors such as crystal form, morphology, size, specific surface area and exposed crystal plane. Therefore, how to effectively control the TiO 2 It has been a hot spot in the field of photocataly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053B01J21/06
Inventor 朴玲钰解英娟吴志娇张晓马佩军
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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