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Method for preparing titanium dioxide microspheres with adjustable particle sizes under anhydrous solvothermal condition

A technology of anhydrous solvent and titanium dioxide, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., to achieve the effect of easy large-scale synthesis, low cost and simple process

Inactive Publication Date: 2014-01-01
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Typically, non-aqueous sol-gel process synthesis requires the introduction of long-chain organic molecules as templating agents, but this results in the need for post-processing to remove these molecules

Method used

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  • Method for preparing titanium dioxide microspheres with adjustable particle sizes under anhydrous solvothermal condition
  • Method for preparing titanium dioxide microspheres with adjustable particle sizes under anhydrous solvothermal condition
  • Method for preparing titanium dioxide microspheres with adjustable particle sizes under anhydrous solvothermal condition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1) Dissolve 1.3 ml of isopropyl titanate in 30 ml of ethanol, then add 0.35 ml of formic acid, stir until uniform to obtain a clear solution.

[0019] 2) Transfer the solution prepared in step 1) to a solvothermal device, perform a solvothermal reaction at 150 °C for 6 h, then centrifuge the obtained material, and then dry it at 60 °C to obtain titanium dioxide microspheres.

[0020] The X-ray diffraction pattern of the prepared titanium dioxide microspheres is shown in Figure 1, and its diffraction peaks are consistent with the standard spectrum of anatase phase titanium dioxide, indicating that the obtained product is anatase phase titanium dioxide. Calculated by the Scherrer formula, the titanium dioxide microspheres are composed of 5 nm titanium dioxide grains. Figure 2 is a scanning electron micrograph of the titanium dioxide microspheres prepared in this example. It can be seen from the figure that the average particle size of the microspheres is about 3 μm. ...

Embodiment 2

[0022] 1) Dissolve 1.5 ml of butyl titanate in 30 ml of methanol, then add 0.35 ml of formic acid, stir until uniform to obtain a clear solution.

[0023] 2) Transfer the solution prepared in step 1) to a solvothermal device, perform a solvothermal reaction at 170 °C for 3 h, then centrifuge the obtained material, and then dry it at 60 °C to obtain titanium dioxide microspheres.

[0024] The transmission electron micrographs of the prepared TiO microspheres are shown in Figure 3. It can be seen from the figure that the average particle size of the microspheres is about 300 nm.

Embodiment 3

[0026] 1) Dissolve 1.3 ml of isopropyl titanate in a mixed solution of 15 ml of methanol and 15 ml of ethanol, then add 0.5m of acetic acid, stir until uniform to obtain a clear solution.

[0027] 2) Transfer the solution prepared in step 1) to a solvothermal device, perform a solvothermal reaction at 150 °C for 6 h, then centrifuge the obtained material, and then dry it at 80 °C to obtain titanium dioxide microspheres.

[0028] The scanning electron micrographs of the prepared TiO microspheres are shown in Figure 4. It can be seen from the figure that the average particle size of the microspheres is about 400 nm.

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Abstract

The invention discloses a method for preparing titanium dioxide microspheres with adjustable particle sizes under an anhydrous solvothermal condition. The method comprises the following steps of dissolving titanium alkoxide in a solvent, adding a carboxylic acid to obtain a clear solution, transferring the solution into a solvothermal device for solvothermal reaction, and performing centrifugation and drying. The particle sizes of the titanium dioxide microspheres can be adjusted by changing compositions of the solvent in which the titanium alkoxide is dissolved. The method for preparing the titanium dioxide microspheres is implemented under an anhydrous condition, and is low in cost, simple equipment is required, a template is not required, the prepared titanium dioxide microspheres are easy to synthesize in a large scale, and have good crystallinity, and the particle sizes can be adjusted within a range of 200nm to 3mu m.

Description

technical field [0001] The invention relates to a method for preparing titanium dioxide microspheres, in particular to a method for preparing titanium dioxide microspheres with adjustable particle diameters under anhydrous solvothermal conditions. Background technique [0002] Titanium dioxide is an environmentally friendly wide bandgap semiconductor, which is widely used in water pollution control, solar cells, lithium-ion batteries, fine chemicals and other fields. Although nanomaterials have many advantages, such as quantum size effect, large specific surface area and so on. However, in practical applications, nanomaterials may cause secondary environmental pollution and biological toxicity due to their small size. Therefore, it is necessary to prepare micro-nano-scale titanium dioxide materials. However, due to technical reasons, the commonly synthesized titanium dioxide microspheres are often unable to independently regulate the particle size of the microspheres, whic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053
Inventor 赵高凌何凯韩高荣
Owner ZHEJIANG UNIV
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