Preparation method and product of Bi12TiO20 micro-spheres

A technology of microspheres and precursor solutions, applied in chemical instruments and methods, nanotechnology, nanotechnology, etc., to achieve the effects of easy control, simple preparation process, and simple preparation process

Inactive Publication Date: 2014-12-17
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] But with Bi(NO 3 ) 3 When preparing bismuth titanate nanopowders as raw materials by hydrothermal method, the biggest difficulty lies in the fact that Bi(NO 3 ) 3 React, hydrolyze to generate BiONO 3 , resulting in a large amount of Bi in the hydrothermal reaction product 2 o 3 or pyrochlore compared to 2 Ti 2 o 7 Miscellaneous

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  • Preparation method and product of Bi12TiO20 micro-spheres
  • Preparation method and product of Bi12TiO20 micro-spheres
  • Preparation method and product of Bi12TiO20 micro-spheres

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1) Weighing 6 mmol of tetrabutyl titanate and dissolving it in ethylene glycol methyl ether to finally obtain an ethylene glycol methyl ether solution with a tetrabutyl titanate concentration of 0.4 mol / L.

[0037] 2) In a state of stirring, ammonia water is added dropwise to the ethylene glycol methyl ether solution of tetrabutyl titanate prepared in step 1) to hydrolyze the tetrabutyl titanate to obtain titanium oxyhydroxide precipitates. Thereafter, wash and filter with deionized water more than 3 times.

[0038] 3) Weigh 8mmol of ammonium bismuth citrate, dissolve it in deionized water, and finally obtain an aqueous solution of ammonium bismuth citrate with a concentration of 0.4mol / L;

[0039]4) Under stirring, disperse the precipitated titanium oxyhydroxide prepared in step 2) in the aqueous solution of ammonium bismuth citrate prepared in step 3), forming a suspension solution containing titanium oxyhydroxide and ammonium bismuth citrate.

[0040] 5) Weigh 0.12 ...

Embodiment 2

[0047] 1) Weighing 6 mmol of tetrabutyl titanate and dissolving it in ethylene glycol methyl ether to finally obtain an ethylene glycol methyl ether solution with a tetrabutyl titanate concentration of 0.5 mol / L.

[0048] 2) In a state of stirring, ammonia water is added dropwise to the ethylene glycol methyl ether solution of tetrabutyl titanate prepared in step 1) to hydrolyze the tetrabutyl titanate to obtain titanium oxyhydroxide precipitates. Thereafter, wash and filter with deionized water more than 3 times.

[0049] 3) Take 8mmol of ammonium bismuth citrate, dissolve it in deionized water, and finally obtain an aqueous solution of ammonium bismuth citrate with a concentration of 0.5mol / L;

[0050] 4) Under stirring, disperse the precipitated titanium oxyhydroxide prepared in step 2) in the aqueous solution of ammonium bismuth citrate prepared in step 3), forming a suspension solution containing titanium oxyhydroxide and ammonium bismuth citrate.

[0051] 5) Weigh 0.10 ...

Embodiment 3

[0055] 1) Weigh 6 mmol of tetrabutyl titanate, dissolve it in ethylene glycol methyl ether, and finally obtain an ethylene glycol methyl ether solution with a tetrabutyl titanate concentration of 0.7 mol / L.

[0056] 2) In a state of stirring, ammonia water is added dropwise to the ethylene glycol methyl ether solution of tetrabutyl titanate prepared in step 1) to hydrolyze the tetrabutyl titanate to obtain titanium oxyhydroxide precipitates. Thereafter, wash and filter with deionized water more than 3 times.

[0057] 3) Weigh 8mmol of ammonium bismuth citrate, dissolve it in deionized water, and finally obtain an aqueous solution of ammonium bismuth citrate with a concentration of 0.7mol / L;

[0058] 4) Under stirring, disperse the precipitated titanium oxyhydroxide prepared in step 2) in the aqueous solution of ammonium bismuth citrate prepared in step 3), forming a suspension solution containing titanium oxyhydroxide and ammonium bismuth citrate.

[0059] 5) Weigh 0.13 mol o...

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Abstract

The invention discloses a preparation method and products of Bi12TiO20 micro-spheres. The preparation method comprises the following steps: by using a titanium oxyhydroxide precipitate which is obtained by hydrolyzing tetrabutyl titanate by virtue of an ammonia-water solution as a titanium source, fully dispersing the titanium oxyhydroxide precipitate in an ammonium bismuth citrate aqueous solution; then, adding a certain potassium hydroxide as a mineralizer; fully stirring and oscillating; transferring to a reaction kettle; sealing; and carrying out hydrothermal treatment at 150-300 DEG C for 6-48 hours to finally obtain the Bi12TiO20 micro-spheres with the diameters of 2-4 mu m, wherein each micro-sphere is self-assembled by smaller nano-particles. According to the preparation method of the Bi12TiO20 micro-spheres, by using the ammonium bismuth citrate as a bismuth source for the first time, the Bi12TiO20 micro-spheres which are self-assembled by the nano-particles by means of precise regulation of reaction conditions without additionally adding a surface modifier. The preparation method disclosed by the invention is simple and controllable in preparation process.

Description

technical field [0001] The present invention relates to the preparation method of bismuth titanate material, relate in particular to a kind of Bi 12 TiO 20 Preparation method and product of microspheres. Background technique [0002] In recent years, the heterogeneous photocatalytic technology using semiconductor oxides as catalysts has become an ideal environmental pollution control technology, and the application of photohydrolysis hydrogen production has been extensively studied. Among them, titanium dioxide is considered to be the most promising semiconductor photocatalyst due to its chemical and biological inertness, high stability, non-toxicity and low cost. However, two inherent defects of titanium dioxide limit its practical application: (1) TiO 2 The band gap is wide, and it can only be excited by ultraviolet light with a wavelength less than 386.5nm; (2) TiO 2 The electrons and holes generated by photoexcitation are easy to recombine, resulting in extremely low...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G29/00B82Y30/00
Inventor 徐刚白惠文邓世琪沈鸽韩高荣
Owner ZHEJIANG UNIV
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