Method for preparing rutile type titanium dioxide nanorod microsphere

A titanium dioxide, rutile type technology, applied in titanium dioxide, titanium oxide/hydroxide, nanotechnology and other directions, can solve problems such as unfavorable large-scale production, rare titanium oxide microspheres, wide titanium oxide microspheres, etc., and achieve particle size distribution. The effect of narrow range, short period and high crystallinity

Inactive Publication Date: 2014-07-02
DONGHUA UNIV
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, there have been many studies on the preparation of titanium oxide microspheres by self-assembly of nano-sized grains, but titanium oxide microspheres prepared by self-assembly of nanorods are relatively rare.
Lu Liu et al. used titanium trichloride and surfactant Span 80 to prepare rutile phase titanium oxide nanorod microspheres, but the particle size range of the titanium oxide microspheres they prepared was too wide and the morphology was not uniform (Lu Liu et al. al.Nanotechnology, 2006, 175046-5050)
Sha Tian et al. used titanium trichloride, sodium oxalate and ethylene glycol to synthesize titanium oxide nanorod microspheres through solvothermal, but the microspheres they prepared had a mixed crystal structure, the reaction temperature of the system was high, and the holding time was long. Therefore, the energy consumption is large, which is not conducive to large-scale production (Sha Tian et al. Applied Physics A: Materials Science & Processing, 2011, 104, 149–158)

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing rutile type titanium dioxide nanorod microsphere
  • Method for preparing rutile type titanium dioxide nanorod microsphere
  • Method for preparing rutile type titanium dioxide nanorod microsphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Mix 2ml of concentrated hydrochloric acid, 1ml of deionized water and 20ml of n-hexane, then add 4ml of n-butyl titanate drop by drop under the condition of magnetic stirring, and continue to stir for 60 minutes to make n-butyl titanate The ester is completely hydrolyzed to form a layered mixed solution;

[0027] (2) Transfer the mixed solution to an autoclave with a volume of 70 ml for solvothermal reaction, control the reaction temperature to 180°C, and hold the temperature for 6 hours. After the reaction is completed, place the autoclave at room temperature to cool naturally. The precipitate was poured out, washed successively with deionized water and ethanol, and centrifuged three times to obtain rutile titanium dioxide nanorod microspheres.

[0028] The field emission scanning electron microscope image of the prepared rutile titanium dioxide nanorod microspheres ( figure 1 ), it can be seen that the diameter of the obtained microspheres is 3-5 microns, and th...

Embodiment 2

[0030] (1) Mix 2 ml of concentrated hydrochloric acid, 2 ml of deionized water and 20 ml of n-hexane, then add 4 ml of n-butyl titanate drop by drop under the condition of magnetic stirring, and continue to stir for 40 minutes to make the n-butyl titanate The butyl ester is completely hydrolyzed to form a layered mixed solution;

[0031] (2) Transfer the mixed solution to an autoclave with a volume of 70 ml for solvothermal reaction, control the reaction temperature to 180°C, and hold the temperature for 6 hours. After the reaction is completed, place the autoclave at room temperature to cool naturally. The precipitate was poured out, washed successively with deionized water and ethanol, and centrifuged three times to obtain rutile titanium dioxide nanorod microspheres.

[0032] The field emission scanning electron microscope image of the prepared rutile titanium dioxide nanorod microspheres ( figure 2 ), it can be seen that the diameter of the obtained microspheres is 2~3 m...

Embodiment 3

[0034] (1) Mix 2 ml of concentrated hydrochloric acid, 3 ml of deionized water and 20 ml of n-hexane, then add 4 ml of n-butyl titanate dropwise under the condition of magnetic stirring, and continue to stir for 30 minutes after the dripping to make the n-butyl titanate The butyl ester is completely hydrolyzed to form a layered mixed solution;

[0035] (2) Transfer the mixed solution to a 70 ml autoclave for solvothermal reaction, control the reaction temperature to 180°C, and keep the temperature for 6 hours. After the reaction is completed, place the autoclave at room temperature to cool naturally , poured out the precipitate, washed with deionized water and ethanol, and centrifuged three times to obtain rutile titanium dioxide nanorod microspheres.

[0036] The field emission scanning electron microscope image of the prepared rutile titanium dioxide nanorod microspheres ( image 3 ), it can be seen that the diameter of the obtained microspheres is about 1 micron, and the s...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
diameteraaaaaaaaaa
diameteraaaaaaaaaa
diameteraaaaaaaaaa
Login to view more

Abstract

The invention relates to a method for preparing a rutile type titanium dioxide nanorod microsphere. The method comprises the following steps of (1) mixing concentrated hydrochloric acid, deionized water and non-polar solvent, adding titanium alkoxide in the mixed solvent drop by drop under a magnetic stirring condition, after the titanium alkoxide is added, continuously stirring the mixture for 30-60 minutes, so that the titanium alkoxide can be fully hydrolyzed to form layered mixed solution; and (2) transferring the mixed solution to a high pressure reaction kettle to perform solvothermal reaction, after the reaction is finished, naturally cooling the high pressure kettle by placing the reaction kettle at a room temperature, and repeatedly washing and centrifugally separating the obtained precipitate to obtain the titanium dioxide nanorod microsphere. According to the method provided by the invention, the solvothermal reaction is carried out in the interface of polar / non-polar solution by adopting the titanium alkoxide, the process route is simple and convenient, no surfactant is required; the prepared titanium dioxide nanorod microsphere is good in dispersion, high in degree of crystallinity, large in specific area, and can be used in various fields of photochemical catalyst, paints, cosmetics, new energy and the like.

Description

technical field [0001] The invention belongs to the field of titanium dioxide preparation, in particular to a preparation method of rutile titanium dioxide nanorod microspheres. 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. TiO 2 There are three crystal forms in nature: Rutile, Anatase and Brookite. Although anatase titanium dioxide has been widely used in recent years, rutile titanium dioxide also has its own advantages: higher refractive index, dielectric constant and electrical resistance, lower production cost, and more chemically stable. [0...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053B82Y40/00
Inventor 张青红芮一川杨俊杰孟楠许明洁王宏志李耀刚
Owner DONGHUA UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap