Preparation method of hydrophobic nano-silica

A nano-silicon dioxide and silicon dioxide technology, applied in the field of nano-materials, can solve the problems of insufficient yield of trichlorosilane, poor dispersion of silica, and high investment scale, and achieve good industrial application prospects and high hydrophobicity. performance, low energy consumption

Active Publication Date: 2012-06-20
河南海博瑞硅材料科技有限公司
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Problems solved by technology

Silicon tetrachloride is a poisonous and harmful liquid with strong corrosiveness. It is easy to react with water to form silicic acid and hydrogen chloride, which will seriously pollute the environment and seriously threaten people's life safety. How to safely deal with silicon tetrachloride has been Become a bottleneck restricting the development of polysilicon
The biggest problem with this method at present is that the yield of the product trichlorosilane is not high enough, the project consumes a lot of energy, the investment scale is high, and the cost of recycling trichlorosilane may be higher than the cost of direct production of trichlorosilane
[0004] Recently, there are patent reports on the use of silicon tetrachloride to prepare silicon dioxide under alkaline conditions. Although this method is simple to operate and low in economic cost, the prepared silicon dioxide has poor dispersion, is easy to agglomerate, and is difficult to be used in organic materials and polymerization. good dispersion in

Method used

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  • Preparation method of hydrophobic nano-silica
  • Preparation method of hydrophobic nano-silica

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 23g of sodium metasilicate in 140ml of deionized water and transfer to a 250ml three-neck flask. Under mechanical stirring at room temperature, gradually add silicon tetrachloride dropwise until the pH value of the solution is 8, control the dropping time for 8 minutes, and then react for 1 hour; then add modifier KH151 according to the molar ratio of modifier: silicon dioxide is 1:2 (Vinyltriethoxysilane), react at 60°C for 8h to obtain a silica emulsion. The resulting emulsion was washed with deionized water until by-products were removed. The resulting product was suction filtered and dried at 100°C to obtain hydrophobic nano-silica.

Embodiment 2

[0030] Weigh 23g of sodium metasilicate in 160ml of deionized water and transfer to a 250ml three-neck flask. Under mechanical stirring, gradually add silicon tetrachloride dropwise until the pH value of the solution is 4, control the dropping time to 15min, and the reaction temperature is 40°C, and then react for 2h after the dropping; (γ-(methacryloyloxy)propyltrimethoxysilane): dichlorodimethylsilane: silicon dioxide = 1:4:20, react at 50°C for 3 hours, and react at 80°C for 4 hours to obtain silica lotion. The resulting emulsion was washed with deionized water until by-products were removed. The resulting product was suction filtered and dried at 150°C to obtain hydrophobic nano-silica.

Embodiment 3

[0032] Weigh 31g of natron in 170ml of deionized water and transfer to a 250ml three-neck flask. Under mechanical stirring, silicon tetrachloride was gradually added dropwise until the pH value of the solution was 9, the reaction temperature was controlled at 50°C, the dropwise addition time was 5min, and after the dropwise addition was completed, reacted for 4h to obtain a silicon dioxide emulsion. The resulting emulsion was washed with tap water until by-products were removed. Disperse the washed filter cake in deionized water, add a mixed modifier, wherein, in molar ratio, isooctanoic acid: perfluorooctanoic acid: silicon dioxide = 1:6:15, and react at 70°C for 7 hours to obtain a silica emulsion. The product is filtered by suction and dried at 190°C to obtain hydrophobic nano-silica.

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Abstract

The invention belongs to the technical field of nanometer material, particularly relates to a preparation method of hydrophobic nano-silica. Silicon tetrachloride is added to alkaline solution to perform a hydrolysis reaction so as to prepare silica, and organic modifiers are added to liquid reactant for reaction; then hydrophobic nano-silica is obtained through water washing and drying; or the organic modifiers are added for reaction after the liquid reactant is processed through water washing, and then hydrophobic nano-silica is obtained through drying. The preparation method effectively solves the utilization problem of a by-product that is silicon tetrachloride in photovoltaic industry and other industrial productions, is simple, fast, safe and controllable, achieves lower cost, and can process silicon tetrachloride massively.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and in particular relates to a method for preparing hydrophobic nano silicon dioxide. Background technique [0002] With the accelerated development of my country's photovoltaic industry in recent years, the output of polysilicon has increased sharply, and for every 1 ton of polysilicon produced, 10-20 tons of silicon tetrachloride by-products will be produced. Silicon tetrachloride is a poisonous and harmful liquid with strong corrosiveness. It is easy to react with water to form silicic acid and hydrogen chloride, which will seriously pollute the environment and seriously threaten people's life safety. How to safely deal with silicon tetrachloride has become a problem. Become a bottleneck restricting the development of polysilicon. [0003] At present, there are two main methods for processing silicon tetrachloride: one is the gas phase method to prepare silicon dioxide, and this m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12B82Y40/00
Inventor 张治军李小红刘凯李庆华蔡天聪
Owner 河南海博瑞硅材料科技有限公司
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