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A method for synthesizing metal oxide microspheres based on the Stober method

A metal alcoholate and oxide technology, which is applied in the field of metal oxide microspheres based on the Stober method, can solve the problems of not meeting the basic requirements of sol-gel, fast hydrolysis, polydispersity and even agglomeration, and achieve microsphere Controllable nanoparticle size, not easy to agglomerate, and uniform size

Active Publication Date: 2022-02-22
SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When using this method to synthesize metal oxide microspheres, most metal alcoholates or metal organic salts are easily hydrolyzed and the hydrolysis speed is extremely fast, which does not meet the basic requirements of sol-gel, and the result is often polydisperse or even agglomerated. sample

Method used

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  • A method for synthesizing metal oxide microspheres based on the Stober method
  • A method for synthesizing metal oxide microspheres based on the Stober method
  • A method for synthesizing metal oxide microspheres based on the Stober method

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Under anhydrous conditions, 0.3 g of tetra-n-butyl titanate was added to 10 mL of ethylene glycol, and the reaction was fully stirred to form a stable precursor solution. 0.55 mL of ethanol and 0.45 mL of glacial acetic acid were added to the obtained precursor solution, and Add 0.5 g of N-sulfonic acid butylpyridinium bisulfate, fully disperse and dissolve and stir for 0.5 h, and finally add 20 mL of acetone to it, stir and mix evenly to obtain a reaction solution. The prepared reaction liquid is packed in a high-pressure container, and heated to 120°C, fully reacted for 3 h, centrifuged the final reaction liquid after the reaction, centrifuged at 2000 rpm for 30 min to obtain solid particles, and used ethanol and water at a volume ratio The eluent prepared at 1:3 elutes the solid particles 2 to 3 times, and the separated product is dried in an oven at 80°C for 8h, and then in a tube furnace, air is roasted at 500°C for 10 h, the air flow rate is 3.6 L / min, and titaniu...

Embodiment 2

[0034] Under anhydrous conditions, add 0.45 g of aluminum isopropoxide to 10 mL of ethylene glycol, stir the reaction to form a stable precursor solution, add 0.75 mL of ethanol and 0.55 mL of glacial acetic acid to the obtained precursor solution, and add Add 0.36 g of mixed acid (concentrated sulfuric acid and concentrated nitric acid in a volume ratio of 1:1), fully disperse and dissolve, and stir for 0.8 h. Finally, add 20 mL of acetone to it and mix well to obtain a reaction solution. The prepared reaction solution was packed into a high-pressure container, and heated to 125° C., fully reacted for 3 h, centrifuged the final reaction solution after the reaction, centrifuged at 2000 rpm for 30 min to obtain solid particles, and used ethanol and water at a volume ratio The eluent prepared at 1:2 elutes the solid particles 2 to 3 times, and the separated product is dried in an oven at 90°C for 6 h, and then roasted in air at 450°C in a tube furnace After 10 h, the air flow ra...

Embodiment 3

[0037] Under anhydrous conditions, add 0.38 g of zirconium n-propoxide to 10 mL of ethylene glycol, stir the reaction to form a stable precursor solution, add 0.65 mL of ethanol and 0.55 mL of glacial acetic acid to the obtained precursor solution, and add Add 0.46 g of Hβ molecular sieve, fully disperse and dissolve and stir for 0.8 h, and finally add 20 mL of acetone to it, stir and mix evenly to obtain a reaction solution. The prepared reaction solution was packed into a high-pressure container, and heated to 125° C., fully reacted for 2 h, centrifuged the final reaction solution after the reaction, centrifuged at 5000 rpm for 30 min to obtain solid particles, and used ethanol and water at a volume ratio The eluent prepared at 1:5 elutes the solid particles 2 to 3 times, and the separated product is dried in an oven at 100° C. for 6 hours, and then in a tube furnace, roasted with air at 600° C. for 9 h, the air flow rate is 2.26 L / min, and the zirconia microspheres are obta...

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Abstract

The invention discloses a method for synthesizing metal oxide microspheres based on the Stober method, which utilizes the advantages of the Stober method in combination with the characteristics of easy hydrolysis of metal alkoxides or metal organic salts, and controls the water release rate of the chemical reaction during the synthesis process. The hydrolysis rate of metal alkoxide or metal organic salt is effectively controlled, the nucleation and growth rate of metal oxide microspheres are realized, and the nucleation and growth process is divided into two steps. The invention obtains the dispersibility of metal oxide microspheres Well, it is not easy to agglomerate, the particle size of microspheres and nanoparticles is controllable, and the size is uniform. The invention has simple synthesis process, easy operation, good repeatability and good application prospect.

Description

technical field [0001] The invention relates to the technical field of inorganic materials, in particular to a method for synthesizing metal oxide microspheres based on the Stober method. Background technique [0002] Metal oxide microsphere materials are widely used in various fields due to their shape characteristics. For example, titanium dioxide nanospheres have always been considered to be the most ideal object for producing photonic crystals. In addition, they also play an important role as pigments and paper whitening agents, photocatalysts, and optical catalysts. In the field of catalysis, titanium dioxide can be used as both a catalyst and a catalyst. Carrier, titanium dioxide particles are often added in cosmetics as the anti-ultraviolet component of sunscreen; nano-zirconia microspheres have the characteristics of strong thermal shock resistance, high temperature resistance, good chemical stability, and outstanding material compounding. Combining nano zirconia mi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B13/32
CPCC01B13/326C01P2004/62
Inventor 邹伟王宇颜杰杨虎向佳郑汶江郑丹李颜利
Owner SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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