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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 without adding any additives to directly apply high-pressure microwaves to prepare nano-titanium dioxide

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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Embodiment 1

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

[0032] (2) ultrafiltration, get the solid and wash to no SO 4 2- , and finally washed with absolute ethanol for 1 to 2 times, and vacuum-dried at 75° C. for 1 hour to obtain nano-sized titanium dioxide particles.

[0033] XRD results such as figure 1 as shown, figure 2 It is TEM image (a) and TEM fine structure image (b), image 3 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 in any ratio can also be used as the reaction medium, configured as a 0.05mol / L titanium sulfate solution for the reaction,...

Embodiment 2

[0037] (1) With titanium tetrachloride as the titanium source, put the mixture of ethanol / deionized water=1:0.5 (volume ratio) in the ice-water bath in the fume hood, and gradually add TiCl dropwise while stirring. 4 Be made into the stock solution of the concentration of 0.2mol / L, this solution is light golden yellow. Take 10ml of the stock solution and add deionized water (or ethanol, or a mixture of ethanol and deionized water in any ratio, the result is the same) to dilute to 50ml, pour it into a 100ml polytetrafluoroethylene microwave reactor, at 1.0Mpa about 180 React at ℃ for 20 minutes, and 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 - Finally, wash with absolute ethanol for 1 to 2 times, and vacuum dry at 80° C. for 1.5 hours to obtain nano-titanium dioxide particles.

[0039] Characterization results, XRD results such as Figure 5 as shown, Figure 6 It is TEM ima...

Embodiment 3

[0041](1) Use metatitanic acid as the titanium source and deionized water as the reaction medium to prepare a 0.25mol / L metatitanic acid solution, take 5ml and add deionized water (or ethanol, or ethanol and deionized water in any ratio) The mixed solution formed, the result is the same) diluted to 50ml, poured into a polytetrafluoroethylene microwave reactor with a volume of 100ml, reacted at 2.0Mpa, 210°C for 15min, cooled to room temperature, and obtained a milky white suspension;

[0042] (2) ultrafiltration, get solid washing to no SO 4 2- Till this time (neutral at this time), finally wash with absolute ethanol for 1-2 times, and vacuum-dry at 60°C for 2 hours to obtain nano titanium dioxide particles.

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

[0044] In step (1), ethano...

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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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