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Synthetic method of metallic oxide nanospheres

A technology of nano-microspheres and synthesis methods, applied in the direction of rare earth metal oxides/hydroxides, rare earth metal compounds, chemical instruments and methods, etc., can solve the problems of difficult process control and difficult to obtain nanostructures, and achieve easy operation, Good repeatability and controllable nanoparticle size

Active Publication Date: 2018-12-11
SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Using microemulsion as a template is an ideal method for synthesizing microspheres. However, when synthesizing metal oxide microspheres, the hydrolysis rate of metal alkoxides or metal organic salts is too fast, and the whole process is difficult to control. Only solid particles with irregular shapes can be obtained. , it is difficult to obtain nanostructures with regular morphology

Method used

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  • Synthetic method of metallic oxide nanospheres
  • Synthetic method of metallic oxide nanospheres
  • Synthetic method of metallic oxide nanospheres

Examples

Experimental program
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Effect test

Embodiment 1

[0033]Take 6.23 g of cetyl alcohol ethoxylate-20 (Brij®58) and 30 mL of cyclohexane in an oil bath environment at 50°C, stir magnetically at a rate of 500 rpm for 1 h to form a microemulsion system, and then add Add 0.6 mL of ethylene glycol and 0.45 mL of glacial acetic acid, stir well, then add 0.05 g of N-sulfonic acid butylpyridine bisulfate, stir well to obtain a mixed solution, and finally add 0.3 mL of tetra-n-titanate to the mixed solution Butyl ester, after mixing evenly, placed in 50 ° C constant temperature stirring reaction for 8 h, after the completion of the reaction, the system was cooled to room temperature, and then added ethanol and water in the final reaction liquid with a volume ratio of 1:3 prepared eluent Perform demulsification and precipitation, centrifuge to obtain solid particles, elute the solid particles with an eluent prepared with ethanol and water at a volume ratio of 1:3, then centrifuge at 8000 rpm for 30 min, repeat the elution 2 to 3 times, an...

Embodiment 2

[0036] Under anhydrous conditions, take 5.98 g of nonylphenol polyoxyethylene ether and 30 mL of cyclohexane in an oil bath at 50°C, stir magnetically at a rate of 500 rpm for 1 h, then add 3 mL of butanol to form a microemulsion system, and then Add 0.6 mL of ethylene glycol and 0.45 mL of glacial acetic acid to the microemulsion system, stir well, then add 0.05 g of mixed acid (concentrated sulfuric acid and concentrated nitric acid in a volume ratio of 1:1), stir well to obtain a mixed solution, and finally Add 0.3 mL of tetra-n-butyl titanate to the mixed solution, mix evenly, place it at 50 °C and stir for 8 h, after the reaction is completed, the system is cooled to room temperature, and then ethanol and water are added to the final reaction solution to The eluent prepared with a volume ratio of 1:3 was used for demulsification and precipitation, and the solid particles were obtained by centrifugation. The solid particles were eluted with ethanol and water with an eluent ...

Embodiment 3

[0039] Under anhydrous conditions, take 6.67 g of isomeric tridecanol polyoxyethylene ether and 30 mL of cyclohexane in an oil bath at 50°C, stir magnetically at a rate of 500 rpm for 1 h, then add 2 mL of butanol to form a microemulsion system , then add 0.6mL ethylene glycol and 0.45 mL glacial acetic acid to the microemulsion system, stir well and then add 0.05 g Hβ molecular sieve into it, stir well to obtain a mixed solution, take 0.5mL isopropanol solution (containing 0.25 g isopropanol aluminum propoxide), and then add it to the mixed solution, after mixing evenly, place it at 50°C for constant temperature and stir for 8 h. The eluent prepared at a ratio of 1:4 was used for demulsification and precipitation, and centrifuged to obtain solid particles. The eluent prepared with acetonitrile and water at a volume ratio of 1:4 was used to elute the solid particles, and then centrifuged at 8000 rpm for 30 minutes, and the elution was repeated for 2~ Three times, the separated...

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Abstract

The invention discloses a synthetic method of metallic oxide nanospheres. The synthetic method is characterized by taking microemulsion as a template, hydrolyzing metal alcoholate or organic metal salt in the microemulsion, and finally forming nanospheres. The reaction is capable of introducing matters which can react with each other to generate water into a microemulsion system under an anhydrouscondition, and the water content of the microemulsion system is controlled by controlling the speed of chemical reaction which is capable of generating water, so that effective control on the hydrolysis speed of the metal alcoholate or the organic metal salt can be realized; meanwhile, the micelle diameter of the microemulsion in the microemulsion system can be regulated, and the metallic oxide nanospheres are controllable in particle diameter and narrow in particle diameter distribution; the particle diameter of the metallic oxide nanospheres obtained by utilizing the technology is controllable within a range from 10 to 2000 nm, and the polydispersion index of the particle diameter of the metallic oxide nanospheres ranges from 1 to 5 percent. The synthetic method disclosed by the invention is simple in a synthetic process, easy to operate and good in repeatability and has a 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 nano-microspheres. Background technique [0002] Among many inorganic materials, metal oxide microsphere materials occupy an important position, and metal oxide microspheres are widely used in daily life and industry. 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-alumina is a white crystalline powder, and it has been confirmed that there are eleven kinds of crystals such as α, β, γ, δ, η, θ, κ and χ. The structure of n...

Claims

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Application Information

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IPC IPC(8): C01G23/047C01G25/02C01G49/06C01G9/02C01G3/02C01F17/00C01F11/02C01F7/30B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01F7/30C01F11/02C01F17/206C01G3/02C01G9/02C01G23/047C01G25/02C01G49/06C01P2004/32C01P2004/52C01P2004/64
Inventor 邹伟王宇向佳杨虎颜杰郑汶江郑丹李颜利
Owner SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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