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Method for utilizing template to prepare silicon dioxide hollow microspheres

A silica and hollow technology, which is applied in the field of preparation of template particles and hollow nano-microspheres, can solve problems such as difficult operation in industrial production, influence of polyelectrolyte concentration, slow drop rate, etc., achieve simple and effective dispersion, and short experiment cycle , the effect of mild reaction conditions

Inactive Publication Date: 2015-07-22
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this patent, the template is removed by water washing, which is environmentally friendly and economical, but there are still certain problems in its work: the polyelectrolyte is dissolved with ammonia water, which is highly volatile and irritating, and the dissolution of the polymer electrolyte is difficult. It is a slow process, so the concentration of polyelectrolyte will be affected, and the operation is very inconvenient; on the other hand, the silicon source is added in a dropwise manner, and the dropping rate is extremely slow (0.2ml / h), which is time-consuming. Difficult to operate in industrial production

Method used

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  • Method for utilizing template to prepare silicon dioxide hollow microspheres
  • Method for utilizing template to prepare silicon dioxide hollow microspheres
  • Method for utilizing template to prepare silicon dioxide hollow microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0032] Take 3ml of PAANa aqueous solution with a mass percentage concentration of 4%, add it to 50ml of absolute ethanol under stirring, and stir at a constant speed for 30min; add 1ml of ammonia solution with a mass percentage concentration of 25% into the system, stir and disperse evenly; finally add 1ml of Tetraethyl silicate, sealed container, stirring reaction for 12h. After the reaction, the template was removed by washing with water, and the product was collected and dried.

[0033] figure 1 It is the TEM picture of the product in Example 1. From figure 1 It can be seen that the coating has been successfully achieved, and silica microspheres without a solid structure have been obtained. The size of the hollow spheres is about 100nm, the thickness of the shell layer is 20-30nm, and the dispersion is good.

Embodiment example 2

[0035] Take 3ml of PAANa aqueous solution with a mass percentage concentration of 4%, add it to 50ml of absolute ethanol under stirring, and stir at a constant speed for 30min; add 1m of ammonia solution with a mass percentage concentration of 25% into the system, stir and disperse evenly; finally add 2ml of Tetraethyl silicate, sealed container, stirring reaction for 12h. After the reaction, the template was removed by washing with water, and the product was collected and dried.

Embodiment example 3

[0037] Take 3ml of PAANa aqueous solution with a mass percentage concentration of 5%, add it to 50ml of absolute ethanol under stirring, and stir at a constant speed for 30min; add 1ml of ammonia solution with a mass percentage concentration of 25% into the system, stir and disperse evenly; finally add 1ml of Tetraethyl silicate, sealed container, stirring reaction for 12h. After the reaction, the template was removed by washing with water, and the product was collected and dried.

[0038] figure 2 It is the TEM picture of the product in Example 3. The product has good dispersion and no hollow structure, the size of the hollow sphere is about 140nm, and the shell wall thickness is 20-30nm.

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Abstract

The invention discloses a method for utilizing a template to prepare silicon dioxide hollow microspheres, and belongs to the field of inorganic nanometer materials. The silicon dioxide hollow microspheres are prepared from the following raw materials in parts by volume: 100 parts of alcohol, 0.5-5 parts of ammonia water (the concentration in mass percent is 25-28%), 1-30 parts of a silicon source precursor, and 1-15 parts of a template aqueous solution (the concentration in mass percent is 1-8%). The method is characterized by comprising the following steps: using water-soluble anionic sodium polyacrylate or sodium polymethacrylate, using aggregates separated out in the poor solvent alcohol as the template, adding ammonia water as a catalyst, at last, adding the silicon source precursor, enabling a hermetic reaction for 5-24 hours under the stirring condition at the temperature of 5-50 DEG C, after the reaction, washing out the template with water, and collecting the dried product, so as to obtain the nano-scale hollow structure microspheres. According to the method disclosed by the invention, the size of the product is adjusted by changing the feeding ratio of the raw materials; the method has the advantages of being simple and easy to operate, good in morphology of the product, free of solid particles and the like; furthermore, the manner of removing the template with water is mild, free of pollution and low in energy consumption.

Description

Technical field: [0001] The invention relates to a novel preparation method of template particles and hollow nano-microspheres, specifically belonging to the field of inorganic nano-materials. Background technique: [0002] In recent years, hollow microspheres, as a new type of particulate material, have attracted more and more attention. It refers to a group of spherical shell-type special structural materials with a size ranging from nanometers to several microns and a hollow interior. Because of the unique structural characteristics of hollow nano-microspheres, compared with solid particles or non-spherical particles of the same size, they have the characteristics of large specific surface area, low density, and light weight. Hollow silica nanospheres, as an important branch, have the characteristics of non-toxicity, good physical and chemical stability, and excellent biocompatibility. They can be loaded with drugs on the cavity or the outer wall of hollow spheres to prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12B82Y30/00
Inventor 石艳宋子敏付志峰
Owner BEIJING UNIV OF CHEM TECH
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