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Method for preparing bi12tio20 nanometer powder by microwave-assisted sol-gel method

A sol-gel method, nano-powder technology, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve problems such as unreported, low purity, complex process, etc., and achieve wide application prospects and process time. Short, small powder particle size effect

Active Publication Date: 2016-05-25
PINGLUO XIANGTAI COAL CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The bismuth titanate crystal prepared by the chemical solution deposition method has better photocatalytic performance to the methyl orange solution in the ultraviolet range, and is also suitable for the research of doping modification (Journal of Molecular Catalysis A: Chemical, 2003: 305-311), but There are problems of low purity, large pollution, and difficult to control the shape; solvothermal synthesis method can synthesize zero-dimensional, one-dimensional, and two-dimensional nano-Bi 12 TiO 20 material (Chemical Communication, 2009: 3937-3939), but the process is relatively complicated, the requirements for production equipment and operators are high, and the yield is low, so it is not suitable for industrialization
In summary, the preparation of Bi by microwave-assisted sol-gel method 12 TiO 20 Powder has not been reported yet

Method used

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  • Method for preparing bi12tio20 nanometer powder by microwave-assisted sol-gel method
  • Method for preparing bi12tio20 nanometer powder by microwave-assisted sol-gel method
  • Method for preparing bi12tio20 nanometer powder by microwave-assisted sol-gel method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Will 11.64gBi (NO 3 ) 3 ·5H 2 O was added to 20ml of 1.0mol / LHNO 3solution, and stirred until completely dissolved to obtain solution A; 0.68g (CH 3 (CH 2 ) 3 O) 4 Ti was added to 10ml of ethylene glycol, and stirred until completely mixed to obtain solution B; under the condition of stirring, the A solution and the B solution were completely mixed to obtain a clear solution C; 2.5g of citric acid, and stirred until the solution was completely mixed uniformly; under the condition of continuing to stir, dropwise added mass concentration of 28% ammonia water to adjust the pH value of the solution to 8, and obtained a transparent sol; the obtained transparent sol was condensed at 110°C, Dry for 40 hours to obtain a xerogel; under low vacuum conditions (absolute pressure 0.02MPa), heat the obtained xerogel to 600°C by microwave, and heat it for 10 minutes, then thermally decompose it to obtain light yellow Bi 12 TiO 20 Powder.

[0030] By XRD analysis (attached fi...

Embodiment 2

[0032] Will 11.64gBi (NO 3 ) 3 ·5H 2 O was added to 20ml of 1.0mol / LHNO 3 solution, and stirred until completely dissolved to obtain solution A; 0.68g (CH 3 (CH 2 ) 3 O) 4 Ti was added to 10ml of ethylene glycol, and stirred until completely mixed to obtain solution B; under the condition of stirring, the A solution and the B solution were completely mixed to obtain a clear solution C; 2.5g of citric acid, and stirred until the solution was completely mixed uniformly; under the condition of continuous stirring, the pH value of the solution was adjusted by dropping 25% mass concentration of ammonia water to obtain a transparent sol; the obtained transparent sol was condensed at a temperature of 100°C, Dry for 60 hours to obtain a dry gel; under low vacuum conditions (absolute pressure 0.01MPa), heat the obtained dry gel to 640°C by microwave, and keep it warm for 10 minutes. The main component of the obtained product is Bi 12 TiO 20 , there exists Bi 2 o 3 impurity ph...

Embodiment 3

[0034] Will 11.64gBi (NO 3 ) 3 ·5H 2 O was added to 20ml of 1.0mol / LHNO 3 solution, and stirred until completely dissolved to obtain solution A; 0.68g (CH 3 (CH 2 ) 3 O) 4 Ti was added to 10ml of ethylene glycol, and stirred until completely mixed to obtain solution B; under the condition of stirring, the A solution and the B solution were completely mixed to obtain a clear solution C; 2.5g of citric acid, and stirred until the solution was completely mixed uniformly; under the condition of continuous stirring, dropwise added mass concentration of 26% ammonia water to adjust the pH value of the solution to 8, and obtained a transparent sol; the obtained transparent sol was condensed at 115°C, Dry for 36 hours to obtain a dry gel; under low vacuum conditions (absolute pressure 0.013MPa), heat the obtained dry gel to 560°C by microwave and keep it warm for 10 minutes. The main component of the obtained product is Bi 12 TiO 20 , there exists Bi 4 Ti 3 o 12 and Bi 2 o ...

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Abstract

The invention relates to a method for preparing Bi12TiO20 nano-powder by virtue of a microwave-assisted sol-gel method. The method is characterized by comprising the following steps: (1) adding Bi(NO3)3.5H2O into an HNO3 solution to obtain a solution A; (2) adding (CH3(CH2)3O)4Ti into glycol to obtain a solution B; (3) mixing the solution A with the solution B obtained in the step (2) to obtain a clarified solution C; (4) adding citric acid into the solution C, dropwise adding ammonia water to regulate the pH value of the solution to be 6-10, and stirring to obtain transparent sol; (5) condensing and drying the transparent sol at 100-130 DEG C to obtain dried gel; and (6) carrying out microwave heating decomposition on the obtained dried gel under a low vacuum condition. The method is short in technological process and reaction time and applicable to industrial batch production, and the microwave heating decomposition time is 7-15 minutes.

Description

technical field [0001] The invention relates to a microwave-assisted sol-gel method for preparing Bi 12 TiO 20 nanopowder method. Background technique [0002] Bi 12 TiO 20 It has a cubic structure, a symmetrical structure, and no residual dipole moment, so it has excellent photoelectric, electro-optic, and photocatalytic properties, and can be used in optical information processing, catalytic degradation, and other fields. Controlled synthesis of Bi with high purity and uniform morphology 12 TiO 20 The powder has a great influence on its photoelectric and photocatalytic properties, so the controlled synthesis of Bi with uniform morphology and pure phase 12 TiO 20 Powder is very necessary to broaden its application. [0003] Currently, the preparation of Bi 12 TiO 20 Powder methods mainly include solid-state reaction method, chemical solution deposition method, solvothermal synthesis method, etc. Bi synthesized by traditional solid-state reaction method 12 TiO 20...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/00B82Y30/00
CPCC01G29/00C01P2002/72C01P2004/03C01P2004/04C01P2004/62C01P2004/64
Inventor 房国丽王立辉严祥辉
Owner PINGLUO XIANGTAI COAL CHEM
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