Process for producing porous silica particles, resin composition for antireflection coatings, article with antireflection coating, and antireflection film

A technology of silicon dioxide and a manufacturing method, which is applied in the treatment of silicon dioxide, silicon oxide, dyed organosilicon compounds, etc., can solve the problems of low output of porous silicon dioxide particles and poor manufacturing efficiency, and achieves good production efficiency, The effect of low dielectric constant and high yield

Inactive Publication Date: 2013-09-25
DIC CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the production method described in Patent Document 3 needs to be carried out under the condition that the amount of the aforementioned mixed solution is overwhelmingly greater than the amount of the alkoxysilane. It is carried out under the condition that the total mass of water and polyol is about 120 times, so there is a problem that the yield of porous silica particles is small, and the production efficiency is very poor.

Method used

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  • Process for producing porous silica particles, resin composition for antireflection coatings, article with antireflection coating, and antireflection film
  • Process for producing porous silica particles, resin composition for antireflection coatings, article with antireflection coating, and antireflection film
  • Process for producing porous silica particles, resin composition for antireflection coatings, article with antireflection coating, and antireflection film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0129] 213.2 g of methanol, 61.3 g of pure water, and 27.4 g of 28% by mass ammonia water were put into a 500 mL 4-necked flask equipped with a thermometer and a stirring blade, and were uniformly mixed by stirring (liquid B), and the inner temperature was kept at 20°C. Separately, 34.3 g of tetramethoxysilane (hereinafter abbreviated as “TMOS”), 45.1 g of methanol, and 6.5 g of octylamine were uniformly mixed in another container (liquid A). The inside of the flask was kept at 20°C, and liquid A was poured into liquid B over 120 minutes while stirring. After the liquid A was injected, the reaction was continued at 20° C. for 60 minutes. After the reaction, the reaction solution was centrifuged at 10,000 rpm for 10 minutes, and then the supernatant was discarded and the precipitate was taken out.

[0130] 200 g of methanol was added to the precipitate obtained above, followed by stirring and mixing to obtain a suspension. The suspension was centrifuged at 10,000 rpm for 10 m...

Embodiment 2

[0132] 213.2 g of methanol, 61.3 g of pure water, and 27.4 g of 28% by mass ammonia water were put into a 500 mL 4-necked flask equipped with a thermometer and a stirring blade, and were uniformly mixed by stirring (liquid B), and the inner temperature was kept at 20°C. Separately, 34.3 g of TMOS, 45.1 g of methanol, and 39.3 g of decylamine were uniformly mixed in another container (liquid A). The inside of the flask was kept at 20°C, and liquid A was poured into liquid B over 120 minutes while stirring. After the liquid A was injected, the reaction was continued at 20° C. for 60 minutes. After the reaction, the reaction solution was centrifuged at 10,000 rpm for 10 minutes, and then the supernatant was discarded and the precipitate was taken out.

[0133]200 g of methanol was added to the precipitate obtained above, followed by stirring and mixing to obtain a suspension. The suspension was centrifuged at 10,000 rpm for 10 minutes, the supernatant was discarded, and the pre...

Embodiment 3

[0135] 213.2 g of methanol, 61.3 g of pure water, and 27.4 g of 28% by mass ammonia water were put into a 500 mL 4-necked flask equipped with a thermometer and a stirring blade, and were uniformly mixed by stirring (liquid B), and the inner temperature was kept at 20°C. Separately, 34.3 g of TMOS, 45.1 g of methanol, and 9.3 g of laurylamine were uniformly mixed in another container (liquid A). The inside of the flask was kept at 20° C., and liquid A was poured into liquid B over 120 minutes. After the liquid A was injected, the reaction was continued at 20° C. for 60 minutes. After the reaction, the reaction solution was centrifuged at 10,000 rpm for 10 minutes, and then the supernatant was discarded and the precipitate was taken out.

[0136] 200 g of methanol was added and mixed to the precipitate obtained above to obtain a suspension. The suspension was centrifuged at 10,000 rpm for 10 minutes, the supernatant was discarded, and the precipitate was washed with methanol. ...

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Abstract

The purpose of the present invention is to provide a process for producing porous silica particles which enables reduction in the particle diameter and which attains, in the production, a high yield relative to the volume of a reaction solution. A process for producing porous silica particles which have pores on the surface is provided in order to achieve the purpose. This process is characterized by including: a step of adding a mixed fluid (A) which comprises a tetraalkoxysilane, an alkylamine and an alcohol to a mixed fluid (B) which comprises ammonia, an alcohol and water to conduct the hydrolysis and condensation of the tetraalkoxysilane and thus obtain silica particles; and a step of removing the alkylamine from the silica particles.

Description

technical field [0001] The present invention relates to a method for producing porous silica particles having a particle diameter as small as, for example, 100 to 250 nm and having fine pores on the surface, which can be mass-produced (mass-produced) with respect to the mass of the reaction system. Background technique [0002] Porous silica particles are silica particles having fine pores on the particle surface. Among such porous silica particles, porous silica particles whose pores have a size of 2 to 50 nm in the mesoporous region are called mesoporous silica particles. Porous silica particles contain air in their pores and have excellent optical and electrical properties, so they are used as materials for antireflection films, interlayer insulating films, and the like. When porous silica particles are used for the antireflection film, the low refractive index properties of the porous silica particles can be utilized as a material for the low refractive index layer. In...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18C08G77/02C08K9/06C08L101/00C09C1/28C09C3/12C09D5/33C09D7/62C09D201/00
CPCC01B33/18C08K3/36C08K7/26C09D7/70C09D5/006C09D7/62C09D7/61
Inventor 所宽树山科洋三高野圣史下垣知代田渊穰出口朋枝
Owner DIC CORP
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