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Low-temperature preparation method of nano mixed crystal of brookite and rutile titanium dioxide

A technology of rutile titanium dioxide and brookite, which is applied in the field of nanomaterials, can solve the problems of lack of low-temperature preparation methods of brookite and rutile titanium dioxide nano-mixed crystals, and achieve the effects of mild conditions, low cost and easy operation

Inactive Publication Date: 2015-03-25
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there is a lack of a low-temperature preparation method for brookite and rutile titanium dioxide nano-mixed crystals with adjustable ratio

Method used

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  • Low-temperature preparation method of nano mixed crystal of brookite and rutile titanium dioxide
  • Low-temperature preparation method of nano mixed crystal of brookite and rutile titanium dioxide

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Experimental program
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Embodiment 1

[0021] The invention provides a low-temperature preparation method of brookite and rutile titanium dioxide nano-mixed crystals, comprising the following steps:

[0022] (1) Precursor preparation: use tetraethyl titanate as the titanium source, mix ultrapure water, tetraethyl titanate, and absolute ethanol at a volume ratio of 1:3:15, and 9ml tetraethyl titanate The ester was added to 45ml of absolute ethanol, and 3ml of ultrapure water was added dropwise while stirring; stirred at room temperature for 30min at a stirring rate of 8000rmp; the product was centrifuged for 3min and dried under reduced pressure at 60°C for 12h to obtain an amorphous hydrated titanium oxide, to which 36ml mass fraction of 30% hydrogen peroxide was added to complete the reaction to obtain a yellow peroxotitanic acid sol;

[0023] (2) In the peroxotitanic acid sol, add the ammoniacal liquor of 9ml mass fraction 25% as pH regulator, add the glycolic acid of 1.5ml massfraction 70% as template agent; Add...

Embodiment 2

[0029] The difference between embodiment 2 and embodiment 1 is:

[0030] (1) Precursor preparation: use tetraethyl titanate as the titanium source, mix ultrapure water, tetraethyl titanate, and absolute ethanol at a volume ratio of 1:3.2:16, and mix 9.6ml of tetraethyl titanate Ethyl ester was added to 48ml of absolute ethanol, and 3ml of ultrapure water was added dropwise while stirring; stirred at room temperature for 40min at a stirring rate of 8000rmp; the product was centrifuged for 4min, and dried under reduced pressure at 60°C for 8h to obtain Shaped hydrated titanium oxide, to which 45ml mass fraction 30% hydrogen peroxide was added, completely reacted to obtain yellow peroxotitanic acid sol;

[0031] (2) Add 9.6ml of mass fraction 25% ammoniacal liquor as pH regulator in peroxotitanic acid sol, add the glycolic acid of 1.6ml massfraction 70% as template agent; Add pH regulator and template agent to peroxotitanic acid in the sol;

[0032] (3) Place the sol in a water...

Embodiment 3

[0036] The difference between embodiment 3 and embodiment 1 is:

[0037] (1) Precursor preparation: use tetraethyl titanate as the titanium source, mix ultrapure water, tetraethyl titanate, and absolute ethanol at a volume ratio of 3:10:50, and mix 10ml of tetraethyl titanate The ester was added to 50ml of absolute ethanol, and 3ml of ultrapure water was added dropwise while stirring; stirred at room temperature for 45min at a stirring rate of 9000rmp; the product was centrifuged for 4min and dried under reduced pressure at 70°C for 8h to obtain an amorphous hydrated titanium oxide, 45ml mass fraction 30% hydrogen peroxide was added therein, and the complete reaction made yellow peroxotitanic acid sol;

[0038] (2) In peroxotitanic acid sol, add 10ml mass fraction 25% ammoniacal liquor as pH regulator, add the glycolic acid of 1.8ml massfraction 70% as template agent; Add pH regulator and template agent to peroxotitanate sol middle;

[0039] (3) Place the sol in a water bath...

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Abstract

The invention discloses a low-temperature preparation method of nano mixed crystal of brookite and rutile titanium dioxide. The low-temperature preparation method comprises the following steps: (1) preparing a precursor: mixing ultrapure water, tetraethyl titanate and absolute ethyl alcohol in a volume ratio of 1 to (3-4) to (15-20) to obtain a mixture by taking the tetraethyl titanate as a titanium source, and drying the mixture to obtain hydrated titanium oxide, adding 30% hydrogen peroxide into the hydrated titanium oxide to completely react to prepare peroxo titanic acid sol; (2) adding a pH regulator and a template agent into the peroxo titanic acid sol; (3) stirring the sol under a water bath condition with a temperature of 40-60 DEG C and removing excessive hydrogen peroxide; and (4) filling the sol into a reaction kettle and performing hydrothermal reaction for 24-48 hours at 160-200 DEG C to obtain a product, washing the product until neutral, drying and grinding the neutral product under reduced pressure to prepare the mixed crystalline-phase nano titanium dioxide. The low-temperature preparation method is performed at a relatively low temperature, simple and convenient to operate, capable of being synthesized on a large scale, and low in cost.

Description

technical field [0001] The invention belongs to the field of nanometer materials, and in particular relates to a low-temperature preparation method of brookite and rutile titanium dioxide nano-mixed crystals. Background technique [0002] Due to its excellent photoelectric properties, chemical resistance, high activity, and non-toxicity, nano-titanium dioxide plays an important role in the fields of optics, electricity, magnetism, and sensors. As an excellent photocatalytic material, at present, anatase and rutile have been deeply studied in both theory and practical application. The most typical example is the commercial titanium dioxide P25, which is composed of anatase and rutile according to the mass ratio It is a mixed crystal composed of 71 / 29, which has a very good effect of sterilization and oxidation degradation of pollutants. Recent studies have shown that brookite has unique advantages in the photocatalytic reduction of specific pollutants, while rutile has bette...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053
CPCC01G23/053C01P2004/64C01P2004/30
Inventor 王冰杨则伟安浩崔皓潘旸翟建平
Owner NANJING UNIV