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Process for producing silica-based particle, coating composition for coating film formation, and base material with coating film

By growing and removing inorganic oxides in the presence of electrolyte salts, silica-based particles with internal cavities are prepared, which solves the problems of poor low refractive index and complicated preparation in the existing technology, and achieves high stability and The formation of strong coating film improves the performance and production efficiency of the coating film.

Inactive Publication Date: 2007-05-30
JGC CATALYSTS & CHEMICALS LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the particles proposed by the applicant of the present application mentioned above may not be able to obtain a sufficient low refractive index effect depending on the purpose and application of the particles.
In addition, in the production method described in Patent Document 6, inorganic oxides other than the above-mentioned silica are removed in advance, and then a silica coating layer is formed. The production process is complicated, and there are major difficulties in terms of reproducibility and productivity.
[0006] In addition, the above-mentioned conventional microparticles sometimes have the problem that the stability of the coating film-forming coating material used to prepare the substrate coated with the coating film is not sufficient, and the thickness of the coating film obtained by using the coating film-forming coating material is not uniform. , or insufficient membrane strength

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0043] 〔Method for producing silica-based microparticles〕

[0044]The method for producing silica-based microparticles of the present invention includes the following steps (a) and (b), which are essential steps. Moreover, the following process (c), (d) or (e) is included besides the said process. That is, the preparation method of the silica-based microparticles involved in the present invention includes (a)+(b), (a)+(b)+(c), (a)+(b)+(d), (a)+ (b)+(c)+(d), (a)+(b)+(d)+(e), and (a)+(b)+(c)+(d)+(e) A combination of processes. Next, each step will be described.

[0045] Step (a) is to add silicate aqueous solution and / or acidic silicic acid solution and alkali-soluble inorganic compound aqueous solution at the same time in alkaline aqueous solution, or in alkaline aqueous solution in which seed particles are dispersed as required, to prepare the molar ratio MO X / SiO 2 Composite oxide particle dispersion in the range of 0.3 to 1.0, wherein SiO 2 Indicates silica, MO X In...

Embodiment 1

[0126] Preparation of silica-based microparticles (P-1)

[0127] Heating 100g of SiO with an average particle size of 5nm at 80°C 2 A mixture of silica sol at a concentration of 20% by weight and 1900 g of pure water. The pH of this reaction mother liquor is 10.5, adds 9000g with SiO 2 The concentration is 1.17% by weight of sodium silicate aqueous solution and 9000g of Al 2 o 3 A sodium aluminate aqueous solution having a concentration of 0.83% by weight. At this time, the temperature of the reaction solution was kept at 80°C. Immediately after the addition of the above-mentioned substances, the pH of the reaction liquid rose to 12.5, and remained almost unchanged thereafter. After the addition, the reaction solution was cooled to room temperature, washed with an ultrafiltration membrane, and prepared with a solid content concentration of 20% by weight of SiO 2 ·Al 2 o 3 Primary particle dispersion.

[0128] Add 1,700 g of pure water to 500 g of the primary particl...

Embodiment 2

[0150] Preparation of silica-based microparticles (P-2)

[0151] 1,500 g of an aqueous dispersion of silica-based microparticles (P-1-1) having a solid content concentration of 20% by weight, 500 g of pure water, 1,750 g of ethanol, and 626 g of 28% ammonia water were prepared in the same manner as in Example 1 by heating at 35°C. The mixed solution, then add 104g ethyl silicate (SiO 2 Concentration of 28% by weight) to form a silica coating film, wash with an ultrafiltration membrane while adding 5L of pure water, and obtain silica-based microparticles (P-2-1) water with a solid content concentration of 20% by weight Dispersions.

[0152] Next, after maturing the silica-based fine particle (P-2-1) dispersion at 200°C for 1 hour, it was washed with an ultrafiltration membrane while adding 5 L of pure water to obtain a silica-based fine particle (P-2-1) with a solid content concentration of 20% by weight. Silicon microparticles (P-2-2) aqueous dispersion. At this time, the...

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Abstract

Fine hollow spherical silica-based particles which each comprises a shell having a void inside and which hence have a low refractive index. An aqueous silicate solution and / or an acidic silicic acid solution is added to an aqueous alkali solution simultaneously with an aqueous solution of an alkali-soluble inorganic compound to prepare a dispersion of fine particles of a composite oxide. During this operation, an electrolyte salt is added in such an amount that the ratio of the number of moles of the electrolyte salt.

Description

technical field [0001] The present invention relates to silica-based microparticles having voids therein, a method for producing the same, a paint for forming a coating film containing the silica-based microparticles, and a method for forming a coating film containing the silica-based microparticles on the surface of a substrate Coated substrates. Background technique [0002] Hollow silica particles having a particle diameter of approximately 0.1 to 300 μm have been disclosed (see Patent Document 1, Patent Document 2, etc.). In addition, a method for preparing hollow particles composed of a dense shell of silica by precipitating active silica from an aqueous alkali metal silicate solution onto a core composed of a material other than silica is disclosed. On the other hand, it is obtained by removing the material without breaking the silica shell (see Patent Document 3, etc.). [0003] In addition, a micron-sized spherical silica particle is also disclosed. The particle ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18C09C1/28C09D201/00C09D7/12
CPCC09C1/3045B82Y30/00C01P2004/34C09C1/3081C09D7/1266C09D7/1275C01B13/363C01P2004/62C09C1/309C08K7/26C01B33/146C08K9/06C09D7/1291C01P2004/64C09D7/61C09D7/67C09D7/68C09D7/70Y10T428/26Y10T428/2984C01B33/18C09C1/28C09D201/00
Owner JGC CATALYSTS & CHEMICALS LTD