A kind of titanium dioxide mesoporous microsphere with high-energy crystal surface exposure and preparation method thereof

A titanium dioxide and mesoporous technology, applied in the field of photocatalytic materials, can solve the problems of insufficient mesoporous structure, complex preparation system, introduction of impurity environment, etc., to increase impurities and treatment process, simple preparation system, and good monodispersity. Effect

Active Publication Date: 2022-06-07
HUBEI UNIV OF TECH
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  • Abstract
  • Description
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Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcomings of the prior art microspheres that are small (nano-scale), uneven particle size, lack of mesoporous structure, complex preparation system, introduction of impurities and harm to the environment, and provide a method for preparing high-energy crystals under simple conditions. Method for face-exposed TiO2 mesoporous microspheres

Method used

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  • A kind of titanium dioxide mesoporous microsphere with high-energy crystal surface exposure and preparation method thereof
  • A kind of titanium dioxide mesoporous microsphere with high-energy crystal surface exposure and preparation method thereof
  • A kind of titanium dioxide mesoporous microsphere with high-energy crystal surface exposure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] (1) Add 0.25 mL of NaCl solution (0.05 mol / L) to 100 mL of ethanol in a cold bath at -40°C, and stir at a speed of 500 r / min for 30 min to mix well to obtain a mixed solution.

[0055] (2) 4 mL of tetrabutyl titanate was added to the above mixed solution and continued to be stirred for 10 h at a speed of 500 r / min in a -40° C. cold bath to obtain suspension A.

[0056] (3) The above-mentioned suspension A was centrifuged at 5000 r / min to collect the precipitated product and washed with alcohol for 3 times and water for 3 times to obtain a white product, and then freeze-dried the white product at -80 °C for 2 h to obtain the precursor of titanium dioxide mesoporous microspheres .

[0057] (4) adding the prepared titanium dioxide mesoporous microsphere precursor to a mixture of 70 mL of ethanol and 10 mL of deionized water and stirring to form suspension B;

[0058] (5) Place the above-mentioned suspension B in a 100 mL stainless steel reaction kettle with a polytetraflu...

Embodiment 2

[0061] (1) Add 0.5 mL of KCl solution (0.001 mol / L) to 100 mL of butanol in a cold bath at -25°C, and stir at a speed of 100 r / min for 15 min to mix well to obtain a mixed solution.

[0062] (2) 1 mL of titanium isopropoxide was added to the above mixed solution and continued to be stirred at a speed of 100 r / min in a -25° C. cold bath for 4 h to react to obtain suspension A.

[0063] (3) The above-mentioned suspension A was centrifuged at 2000 r / min to collect the precipitated product and washed with alcohol for 3 times and water for 3 times to obtain a white product, and then freeze-dried the white product at -10°C for 12 h to obtain titanium dioxide mesoporous microspheres.

[0064] (4) adding the prepared titanium dioxide mesoporous microsphere precursor to a mixture of 50 mL of isopropanol and 30 mL of deionized water and stirring to form suspension B;

[0065] (5) Place the above-mentioned suspension B in a 100 mL stainless steel reaction kettle with a polytetrafluoroeth...

Embodiment 3

[0067] (1) Put 1 mL of KNO in a cold bath at -10°C 3 with Na 2 SO 4 mixed solution (KNO 3 with Na 2 SO 4 The concentration was 0.1 mol / L) into 100 mL of ethanol and propanol mixed solution, and stirred at a rotational speed of 1000 r / min for 240 min to mix uniformly to obtain a mixed solution.

[0068] (2) 10 mL of a mixture of tetrabutyl titanate and titanium isopropoxide was added to the above mixed solution, and the mixture was continued to be stirred at 1000 r / min for 6 h in a -10°C cooling bath to obtain suspension A.

[0069] (3) The above-mentioned suspension A was centrifuged at 4000 r / min to collect the precipitated product and washed with alcohol for 3 times and water for 3 times to obtain a white product, and then freeze-dried the white product at -50°C for 6 h to obtain titanium dioxide mesoporous microspheres.

[0070] (4) adding the prepared titanium dioxide mesoporous microsphere precursor to 80 mL of deionized water and stirring to form suspension B;

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Abstract

The invention relates to a titanium dioxide mesoporous microsphere exposed by a high-energy crystal plane and a preparation method thereof. That is, using titanium alkoxide as the titanium source and organic alcohol as the solvent, by controlling the hydrolysis of titanium alkoxide in the alcohol-water solution at low temperature, changing the titanium source, reaction temperature, reaction time, metal salt solution, organic alcohol and water The formation of titanium dioxide mesoporous microspheres is controlled by the ratio of titanium dioxide, and an environmentally friendly and economical metal salt solution is selected to control its sphericity and particle size. The precursor of mesoporous microspheres is obtained by centrifugal collection combined with freeze-drying. Using the alcohol / water mixed system, the mesoporous microsphere precursor is prepared into a high-energy surface such as (001) crystal surface by controlling the volume ratio of alcohol / water, hydrothermal reaction temperature, and hydrothermal reaction time by hydrothermal / solvothermal method Exposed mesoporous TiO 2 Microspheres. The preparation system of the invention is simple and the cycle is short, and the method can prepare titanium dioxide mesoporous microspheres with good sphericity, uniform particle size distribution, rich mesoporous structure and exposed high-energy crystal planes.

Description

technical field [0001] The invention belongs to the field of photocatalytic materials, and relates to a photocatalytic material titanium dioxide microsphere and a preparation method, in particular to a titanium dioxide mesoporous microsphere with exposed high-energy crystal planes and a preparation method thereof. Background technique [0002] TiO 2 As the most studied photocatalyst material, it is one of the best photocatalysts due to its good chemical stability, non-toxicity and low cost. But TiO 2 Disadvantages of its own, such as micron-sized TiO 2 Fewer active sites and easy recombination of photogenerated electron-hole pairs lead to low quantum efficiency; nanoscale TiO 2 Easy agglomeration also leads to fewer active sites, and at the same time, fine nanoparticles will be dispersed in water and cannot be recovered when they are used for photocatalytic treatment of water, becoming a secondary pollution source. The above disadvantages limit TiO 2 as a further develo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/053B01J21/06B01J35/08
CPCC01G23/053B01J35/004B01J21/063B01J35/08C01P2004/03C01P2004/61C01P2004/32Y02W10/37
Inventor 常鹰魏志顺谌援王莉何鹏浩
Owner HUBEI UNIV OF TECH
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