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Preparation method of high-purity micron-sized spherical silica micropowder

A technology of silica and microspheres, which is applied in the direction of silica and silica, can solve the problems affecting industrialization and production capacity, the metal content is easy to exceed the standard, and the reaction is not easy to control, so as to improve elasticity, shrinkage rate and curing time. fast effect

Active Publication Date: 2017-10-27
ETERNAL SPECIALTY MATERIALS ZHUHAI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The oil-in-water emulsification method (O / W) disclosed by CN104556076B has a long curing time, which affects industrialization and production capacity. The water-in-oil emulsification method (W / O) disclosed by CN104030302B uses a large amount of flammable and explosive organic solvents (for example: diesel oil) As a reaction medium, there are certain hazards to the human body and the environment. Mix it with sodium silicate solution, add acid (H2SO4, HCl, etc.) dropwise for precipitation reaction, and obtain SiO through filtration, drying, crushing, and calcination. 2 Powder, precipitation formation speed is fast, but the reaction is not easy to control, and the metal content is easy to exceed the standard

Method used

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  • Preparation method of high-purity micron-sized spherical silica micropowder
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  • Preparation method of high-purity micron-sized spherical silica micropowder

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preparation example Construction

[0038] The preparation method of silicon dioxide microsphere provided by the invention, it comprises the steps:

[0039] i) providing a silicon-containing precursor solution;

[0040] ii) adding the silicon-containing precursor solution into the oil phase containing an emulsifier and stirring to obtain a mixed solution;

[0041] iii) adding the basic catalyst into the mixed solution, and after standing for aging, washing the precipitate with a mixture of solvent and water, and drying to obtain the silica microspheres.

[0042] Step i) the silicon-containing precursor is Si(OR) 4 , ethyl silicate 40, ethyl silicate 32 and SiR 2 (OR 1 ) 3 One or a mixture of two or more, wherein, R, R 1 , R 2 each independently as C 1-3Alkyl; preferably tetramethyl orthosilicate (TMOS), tetraethyl orthosilicate (TEOS), methyltrimethoxysilane (methyltrimethoxysilane) or ethyltrimethoxysilane (Ethyltrimethoxysilane) A mixture of one or more than two, more preferably tetraethyl silicate (TE...

Embodiment 1

[0062] Ethyl orthosilicate (TEOS) and ethyl acetate were distilled under reduced pressure for use.

[0063] Step i) Take 200g of deionized water, add acid to PH=1.50, mix with 90g of tetraethyl orthosilicate (TEOS), and react for 0.5h to form a clear and transparent silicon-containing precursor solution. Based on the total weight of silicon precursors, the SiO 2 Content is 15 parts by weight;

[0064] Step ii) Take 2.63g Span-80, 0.36g Tween-80, 85g kinematic viscosity (40°C)=5mm 2 / s white oil, rotating speed 200rpm, time 15min; take 40g of silica sol and add to mixed white oil, rotating speed 20000rpm, time 15min, get white emulsion;

[0065] Step iii) adding ammonia water to react for 2 hours, standing and aging for 2 hours, taking white precipitate; washing with water and ethyl acetate several times in sequence, and drying to obtain high-purity micron-sized spherical silica microspheres 1 .

[0066] The SEM image of the obtained high-purity micron-sized spherical silica...

Embodiment 2

[0068] Ethyl orthosilicate (TEOS) and ethyl acetate were distilled under reduced pressure for use.

[0069] Step i) Take 90g of deionized water, add acid to PH = 2.5, mix with 180g of tetraethyl orthosilicate (TEOS), and react for 1.5h to form a clear and transparent silicon-containing precursor solution. Based on the total weight of silicon precursors, the SiO 2 Content is 30 parts by weight;

[0070] Step ii) Take 8.76g Span-80, 1.24g Tween-80, 85g kinematic viscosity (40°C)=10mm 2 / s oil phase, rotation speed 200rpm, time 25min; take 85g of silica sol and add it to the mixed white oil, rotation speed 10000rpm, time 10min, to obtain white emulsion;

[0071] Step iii) adding diethylamine to react for 2 hours, standing and aging for 2 hours, take the white precipitate; successively wash with water and ethyl acetate several times, and dry to obtain high-purity micron-sized spherical silica microspheres 2 .

[0072] The SEM image of the obtained high-purity micron-sized spher...

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Abstract

The invention discloses a preparation method of high-purity micron-sized spherical silica micropowder. The preparation method comprises the following steps: firstly, providing a precursor solution containing silicon; secondly, adding the precursor solution into an oil phase containing an emulsifier and then stirring to obtain a mixed solution; thirdly, adding a basic catalyst into the mixed solution, standing and ageing, washing precipitate with a mixture of a solvent and water, and then drying to obtain silica microspheres, wherein the precursor solution containing the silicon is one or a mixture of two or more of Si(OR)4, ethyl silicate 40, ethyl silicate 32 and SiR2(OR1)3, and R, R1 and R2 are C1-3 alkyl groups which are independent of one another. The silica microspheres disclosed by the invention have the advantages that the purity is excessively-high and the contents of all metal impurities are below 0.2 ppm; in addition, the preparation method disclosed by the invention is easy to operate and products in the preparation process are easy to treat; and particle sizes of the finally-obtained silica microspheres are 0.3 to 0.4 [mu]m.

Description

technical field [0001] The invention relates to a preparation method of high-purity micron-level spherical silica powder. Background technique [0002] High-purity silica microspheres, with low content of radioactive elements and micron-scale spheroidization, can reduce the expansion coefficient, enhance the mechanical and electrical properties of the material, improve the flame retardancy, and reduce the water absorption of the molding compound. At present, it has been widely used in the fields of aviation, aerospace, electronic information, new coatings, special ceramics, high-grade cosmetics, high-efficiency catalysts, liquid chromatography fillers, pigments, large-screen liquid crystal displays, and VLSI molding compounds. [0003] At present, Japan and the United States are the most successful countries in the research on the spheroidization of silica powder. The raw materials for preparing high-purity micron-sized materials include water glass, purified quartz, ethyl o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
CPCC01B33/18C01P2004/03C01P2004/61C01P2004/62C01P2006/80
Inventor 韩露卓胜池花玉芳陆树苹朱元清
Owner ETERNAL SPECIALTY MATERIALS ZHUHAI CO LTD
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