Classifications

• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B33/00—Silicon; Compounds thereof
  • C01B33/113—Silicon oxides; Hydrates thereof
  • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
  • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K7/00—Use of ingredients characterised by shape
  • C08K7/22—Expanded, porous or hollow particles
  • C08K7/24—Expanded, porous or hollow particles inorganic
  • C08K7/26—Silicon- containing compounds
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K3/00—Use of inorganic substances as compounding ingredients
  • C08K3/34—Silicon-containing compounds
  • C08K3/36—Silica
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L101/00—Compositions of unspecified macromolecular compounds
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2004/00—Particle morphology
  • C01P2004/60—Particles characterised by their size
  • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2004/00—Particle morphology
  • C01P2004/60—Particles characterised by their size
  • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2006/00—Physical properties of inorganic compounds
  • C01P2006/12—Surface area
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2006/00—Physical properties of inorganic compounds
  • C01P2006/40—Electric properties
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2006/00—Physical properties of inorganic compounds
  • C01P2006/80—Compositional purity
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K2201/00—Specific properties of additives
  • C08K2201/002—Physical properties
  • C08K2201/006—Additives being defined by their surface area

Definitions

• Step A A step of preparing a hydrophobic liquid aqueous emulsion using a cationic surfactant
• Step B A step of adding a silanol precursor, an alkaline substance, and a cationic surfactant B to the aqueous emulsion obtained in Step A to generate a hollow silica particle precursor
• Step C A step of heat-treating the hollow silica particle precursor obtained in Step B above 1000 ° C. and 1200 ° C.
• the total content of alkali metals and alkaline earth metals relative to the content of silica in the hollow silica particles is 50 mass ppm or less, preferably 30 mass ppm or less, more preferably 20 mass ppm or less, more preferably 15 mass ppm or less, and from the viewpoint of productivity of hollow silica particles, preferably 1 mass ppb or more, more preferably 5 mass ppb or more.
• the alkali metal content and alkaline earth metal content in the hollow silica particles can be measured by the method described in US EPA METHOD 3051A. Lithium, rubidium, and cesium in hollow silica particles can also be measured by the method described in US EPA METHOD 3051A.
• the porosity of the hollow silica particles is preferably 50% by volume or more, more preferably 55% by volume or more, and still more preferably 60% by volume or more from the viewpoint of lowering the dielectric constant of the hollow silica particles. From the viewpoint of the hollow silica particles having sufficient strength, it is preferably 80% by volume or less, more preferably 77% by volume or less, and further preferably 74% by volume or less.
• the porosity of hollow silica particles can be determined by the method described in Examples.
• R 1 and R 2 each independently represent a linear or branched alkyl group having 4 to 22 carbon atoms
• R 3 represents an alkyl group having 1 to 3 carbon atoms
• a plurality of R 3 may be different groups
• X — represents a monovalent anion.
• alkyl groups having 4 to 22 carbon atoms include various butyl groups, various pentyl groups, various hexyl groups, various heptyl groups, various octyl groups, various nonyl groups, various decyl groups, various dodecyl groups, various tetradecyl groups, various hexadecyl groups, various octadecyl groups, various eicosyl groups, and the like.
• the alkyl group having 1 to 3 carbon atoms includes methyl group, ethyl group, n-propyl group and isopropyl group.
• R 3 is preferably a methyl group.
• dialkyldimethylammonium salts represented by general formula (2) include dibutyldimethylammonium chloride, dihexyldimethylammonium chloride, dioctyldimethylammonium chloride, dihexyldimethylammonium bromide, dioctyldimethylammonium bromide, dilauryldimethylammonium bromide, ditetradecyldimethylammonium bromide, and the like.
• quaternary ammonium hydroxide salts include tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, tributylmethylammonium hydroxide, trimethylhydroxyethylammonium hydroxide (choline), tetraethanolammonium hydroxide, methyltriethanolammonium hydroxide, and dimethylbis(2-hydroxyethyl)ammonium hydroxide.
• the mixture of the alkaline substance and the cationic surfactant B may be brought into contact with the silanol precursor by adding the mixture of the alkaline substance and the cationic surfactant B to the reaction system containing the silanol precursor, or by adding the silanol precursor to the reaction system containing the mixture of the alkaline substance and the cationic surfactant B.
• the mixture of the alkaline substance and the cationic surfactant B is added to the reaction system containing the silanol precursor. addition is preferred.
• the dielectric constant at a measurement frequency of 5.8 GHz is preferably 1.1 or more, more preferably 1.2 or more, still more preferably 1.3 or more, and preferably 2.8 or less, more preferably 2.5 or less.
• the dielectric constant of the resin composition can be determined by the method described in Examples.
• the resin composition of the present invention has a dielectric loss tangent at a measurement frequency of 5.8 GHz.
• the dielectric loss tangent of the resin composition can be obtained by the method described in Examples.
• the BET specific surface area of the hollow silica particles was measured using a specific surface area measuring device (manufactured by Shimadzu Corporation, trade name "Flowsorb III2305"). The sample was pretreated by heating at 200° C. for 15 minutes.
• the dielectric constant and dielectric loss tangent of the resin composition were measured at a frequency of 5.8 GHz by molding the resin composition into a diameter of 2.5 mm and a length of 4 mm and using the cavity resonator perturbation method in the same manner as in "Measurement of relative dielectric constant and dielectric loss tangent of hollow silica particles".
• Example 1 342.2 g of ion-exchanged water, 150 g of dodecane (manufactured by Kishida Chemical Co., Ltd.: primary n-dodecane), and 7.8 g of Kotamine 2285E (manufactured by Kao Corporation: containing 58% by mass of behenyltrimethylammonium chloride) were mixed and stirred to obtain emulsion A.
• the volume average particle diameter of the particles in the obtained emulsion A was 0.5 ⁇ m.
• AH212-CS manufactured by Yokkaichi Gosei Co., Ltd., containing 50% by mass of dimethylbis(2-hydroxyethyl)ammonium hydroxide
• Cortamine 24P 711.6 g of Cortamine 24P were uniformly mixed to obtain a preparation liquid C.
• Preparation liquid C was added to preparation liquid B at a constant rate, and then stirred at 40° C. for 3 hours to obtain cloudy liquid D.
• the resulting cloudy liquid D was filtered using a 5C filter paper (manufactured by Advantec Toyo Co., Ltd.), washed with water, and dried at 110° C. to obtain a white hollow silica particle precursor. Hollow silica particles were obtained by firing the obtained hollow silica particle precursor at 1100° C. for 1 hour. Table 1 shows the physical properties of the obtained hollow silica particles.
• Example 2 388.6 g of ion-exchanged water, 200 g of dodecane (manufactured by Kishida Chemical Co., Ltd.: primary n-dodecane), and 11.4 g of Kotamine 86W (manufactured by Kao Corporation: containing 28% by mass of stearyltrimethylammonium chloride) were mixed and stirred to obtain emulsion A.
• the volume average particle diameter of the particles in the obtained emulsion A was 0.9 ⁇ m.
• Hollow silica particles were obtained in the same manner as in Example 1, except that the amount of ion-exchanged water was 13192.5 g and the amount of emulsion A was 138.1 g. Table 1 shows the physical properties of the obtained hollow silica particles.
• Comparative example 3 Hollow silica particles were obtained in the same manner as in Example 1, except that the firing temperature was changed to 1000°C. Table 1 shows the physical properties of the obtained hollow silica particles.
• Example 4 Epoxy resin (manufactured by Mitsubishi Chemical Corporation: jER (trademark) 828) 23.7 g, acid anhydride curing agent (manufactured by Mitsubishi Chemical Corporation: YH-306) 28.8 g, imidazole curing agent (manufactured by Mitsubishi Chemical Corporation: EMI24) 0.3 g Using a kneader (manufactured by Thinky Corporation: Planetary Vacuum Mixer), under atmospheric pressure, 1400 rpm for 1 minute, 2000 rpm under reduced pressure of 0.3 kPa. The mixture was kneaded for 5 minutes at a temperature of 100 m to obtain an epoxy resin kneaded liquid.
• a kneader manufactured by Thinky Corporation: Planetary Vacuum Mixer
• Example 6 A resin composition was obtained in the same manner as in Example 4, except that the hollow silica particles obtained in Example 1 were replaced with the hollow silica particles obtained in Example 3.
• Table 2 shows the physical properties of the obtained resin composition.

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• Compositions Of Macromolecular Compounds (AREA)

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• 2023
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