Method for synthesizing nano titanium dioxide through microwaves

A nano-titanium dioxide and microwave synthesis technology is applied in the nano field to achieve the effects of excellent performance, excellent sensitivity and excellent photoelectric conversion efficiency.

Inactive Publication Date: 2010-04-28
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In summary, no report has been found in the search to use inorganic titanium salts as raw materials wi

Method used

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  • Method for synthesizing nano titanium dioxide through microwaves
  • Method for synthesizing nano titanium dioxide through microwaves
  • Method for synthesizing nano titanium dioxide through microwaves

Examples

Experimental program
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Example Embodiment

[0030] Example 1

[0031] (1) Use titanium sulfate as the titanium source and deionized water as the reaction medium to prepare a 0.05 mol / L titanium sulfate solution. Take 50 ml of the above solution and place it in a polytetrafluoroethylene microwave reactor at 0.1Mpa, 110°C React for 30 minutes under the conditions, and cool to room temperature to obtain a milky white suspension;

[0032] (2) Ultrafiltration, take the solid and wash until there is no SO 4 2- Finally, it is washed with absolute ethanol for 1 to 2 times, and dried under vacuum at 75°C for 1 hour to obtain nano-sized titanium dioxide particles.

[0033] XRD results are as figure 1 As shown, figure 2 Is the TEM image (a) and the TEM fine structure image (b), image 3 It is an electron diffraction pattern. The phases are anatase and brookite, mainly anatase.

[0034] In step (1), ethanol or a mixture of ethanol and deionized water at any ratio can also be used as the reaction medium, and the reaction can be carried ou...

Example Embodiment

[0036] Example 2

[0037] (1) Using titanium tetrachloride as the titanium source, place the mixture of ethanol / deionized water = 1:0.5 (volume ratio) in an ice water bath in a fume hood, and gradually add TiCl while stirring. 4 Prepare a stock solution with a concentration of 0.2mol / L, which is light golden yellow. Dilute 10ml of the stock solution with deionized water (or ethanol, or a mixture of ethanol and deionized water in any ratio, the result is the same) to 50ml, and pour it into a 100ml PTFE microwave reactor, at 1.0Mpa about 180 React for 20 min at ℃, then cool to room temperature to obtain a milky white suspension;

[0038] (2) Centrifuge at high speed, take the solid and wash until there is no Cl - After ionization, wash with absolute ethanol for 1 to 2 times, and vacuum-dry at 80°C for 1.5 hours to obtain nano-sized titanium dioxide particles.

[0039] Characterization results, XRD results such as Figure 5 As shown, Image 6 Is the TEM image (a) and the TEM fine struc...

Example Embodiment

[0040] Example 3

[0041] (1) Use metatitanic acid as the titanium source and deionized water as the reaction medium to prepare a 0.25 mol / L metatitanic acid solution. Take 5 ml and add deionized water (or ethanol, or ethanol and deionized water at any ratio). The composition of the mixture, the results are the same) Dilute to 50ml, pour it into a 100ml polytetrafluoroethylene microwave reactor, react at 2.0Mpa, 210°C for 15min, and cool to room temperature to obtain a milky white suspension;

[0042] (2) Ultrafiltration, take the solid and wash until there is no SO 4 2- So far (neutral at this time), and finally washed with absolute ethanol for 1 to 2 times, and dried under vacuum at 60°C for 2 hours to obtain nanometer titanium dioxide particles.

[0043] Characterization results, XRD results such as Figure 8 As shown, Picture 9 Is the TEM image (a) and the TEM fine structure image (b), Picture 10 It is an electron diffraction pattern. The phases are anatase and brookite, mainl...

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Abstract

The invention relates to a method for synthesizing nano titanium dioxide through microwaves, which comprises the following steps: (1) dissolving inorganic titanium compounds in a reaction medium to prepare a prodromic mixed solution of which the concentration of the element titanium is 0.01-0.50 mol/L; putting the prodromic mixed solution in a microwave reactor, and carrying out the microwave synthetic reaction under high pressure of 0.1-4.0 MPa in the presence of microwaves, wherein the frequency of the microwaves is 2-3 GHz, the reaction time is 5min to 1h, and the temperature is 100-250 DEG C; and (2) separating the obtained solid-liquid mixture, taking the solid, washing and drying. The obtained nano titanium dioxide has the advantages of small particle size, favorable dispersivity, ordered crystalline structure, favorable photoluminescence and photocatalysis performance, high photoelectric transformation efficiency and simple preparation method.

Description

technical field [0001] The invention relates to the field of nanotechnology, in particular to a method for preparing nano titanium dioxide under high pressure and microwave conditions. Background technique [0002] Nano-titanium dioxide is an n-type semiconductor material. Due to the large surface area of ​​nano-materials, it has unique surface effects, small size effects, quantum size effects, and macroscopic quantum tunneling effects, so it exhibits many unique physical and chemical properties. Nano-titanium dioxide has excellent chemical stability, thermal stability, weather resistance and photocatalytic properties, so it has a wide range of application values ​​in various fields such as coatings, ceramics, environmental protection, cosmetics, industrial catalysis and solar cells. [0003] There are many methods for preparing nano-titanium dioxide, such as uniform precipitation method, sol-gel method, microemulsion synthesis method, alkoxide hydrolysis method and hydrothe...

Claims

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Application Information

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IPC IPC(8): C01G23/053B82B3/00
Inventor 杜国平付敏
Owner SHANGHAI NORMAL UNIVERSITY
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