WO2023153353A1 - 無機質粉末 - Google Patents

無機質粉末 Download PDF

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Publication number
WO2023153353A1
WO2023153353A1 PCT/JP2023/003742 JP2023003742W WO2023153353A1 WO 2023153353 A1 WO2023153353 A1 WO 2023153353A1 JP 2023003742 W JP2023003742 W JP 2023003742W WO 2023153353 A1 WO2023153353 A1 WO 2023153353A1
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Prior art keywords
inorganic powder
less
sphericity
cup
powder
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Ceased
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PCT/JP2023/003742
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English (en)
French (fr)
Japanese (ja)
Inventor
輝洋 相京
朋浩 川畑
純 山口
敦司 山下
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Denka Co Ltd
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Denka Co Ltd
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Filing date
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Application filed by Denka Co Ltd filed Critical Denka Co Ltd
Priority to EP23752817.9A priority Critical patent/EP4467615A1/en
Priority to CN202380020978.1A priority patent/CN118679222A/zh
Priority to US18/836,348 priority patent/US20250115484A1/en
Priority to JP2023580231A priority patent/JPWO2023153353A1/ja
Priority to KR1020247029274A priority patent/KR20240144982A/ko
Publication of WO2023153353A1 publication Critical patent/WO2023153353A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/021—After-treatment of oxides or hydroxides
    • C01F7/025—Granulation or agglomeration
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/42—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation
    • C01F7/422—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation by oxidation with a gaseous oxidator at a high temperature
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • 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
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • 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
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/10—Solid density
    • 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
    • C01P2006/11—Powder tap density
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
    • 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
    • C08K2201/016—Additives defined by their aspect ratio
    • 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

Definitions

  • the present invention relates to inorganic powder.
  • Patent Document 1 describes, as an inorganic powder, a spherical alumina powder having a silica coating layer, which is sphericalized by flame spraying.
  • the following inorganic powder is provided.
  • An inorganic powder containing spherical alumina powder and spherical silica powder S 1 is the sphericity of the inorganic powder with a particle diameter of 5 ⁇ m or more and less than 10 ⁇ m
  • S 2 is the sphericity of the particle diameter of 10 ⁇ m or more and less than 20 ⁇ m
  • the particle diameter is 20 ⁇ m, measured using a wet flow image analysis device.
  • the sphericity of 30 ⁇ m or more is S 3
  • the sphericity of particles with a diameter of 30 ⁇ m or more and less than 45 ⁇ m is S 4
  • the sphericity of particles with a diameter of 45 ⁇ m or more is S 5
  • At least two or more of S 1 , S 3 , S 4 and S 5 are 0.89 or more
  • S2 is 0.75 or more and less than 0.89
  • inorganic powder 2.
  • the inorganic powder according to S AVE is 0.89 or more when S AVE is the average sphericity obtained from the average value of four of S 1 , S 3 , S 4 , and S 5 (excluding those with a value of 0).
  • the inorganic powder is an inorganic powder. 3. 1. or 2.
  • the mass (g) is measured and the bulk density (g/cm 3 ) is calculated. 5. 1. ⁇ 4. The inorganic powder according to When the loose bulk density is A and the firm bulk density is P, An inorganic powder having a degree of compression determined based on ((P ⁇ A)/P) ⁇ 100 of 30% or more and 44% or less. 6. 1. ⁇ 5. The inorganic powder according to any one of In the volume frequency particle size distribution measured by the wet laser diffraction scattering method, the particle diameter at which the cumulative value is 10% is D 10 , the particle diameter at which the cumulative value is 50% is D 50 , and the cumulative value is 97%.
  • an inorganic powder is provided that, when mixed with a resin, can suppress the generation of burrs during molding and can improve the mechanical strength of molded articles.
  • FIG. 1 is a schematic cross-sectional view showing the configuration of a thermal spraying device
  • the inorganic powder of the present embodiment includes spherical alumina powder and spherical silica powder, and S 1 is the sphericity of particles having a particle diameter of 5 ⁇ m or more and less than 10 ⁇ m, and a particle diameter of 10 ⁇ m or more, which is measured using a wet flow image analyzer.
  • the sphericity of less than 20 ⁇ m is S 2
  • the sphericity of particles with a diameter of 20 ⁇ m or more and less than 30 ⁇ m is S 3
  • the sphericity of particles with a diameter of 30 ⁇ m or more and less than 45 ⁇ m is S 4
  • the sphericity of particles of 45 ⁇ m or more is S 5 .
  • At least two of S 1 , S 3 , S 4 , and S 5 are 0.89 or more
  • S 2 is 0.75 or more and less than 0.89.
  • At least two of S 1 , S 3 , S 4 and S 5 are 0.89 or more, preferably 0.91 or more, more preferably 0.92 or more. As a result, the fluidity, bending strength, and burr properties of the resin composition can be improved.
  • the fluidity, bending strength, and burr properties of the resin composition can be improved.
  • the lower limit of S2 is 0.75 or more, preferably 0.81 or more, more preferably 0.83 or more. Thereby, bending strength can be improved.
  • the upper limit of S2 is, for example, less than 0.89, preferably 0.87 or less, more preferably 0.86 or less. Thereby, bending strength can be improved.
  • S AVE is the average sphericity obtained from the average value of S 1 , S 3 , S 4 , and S 5 (excluding those with a value of 0), and is measured using a wet flow image analyzer.
  • S 50 ( ⁇ m) is the median diameter of the spherical silica powder.
  • the lower limit of SAVE is, for example, 0.89 or more, preferably 0.90 or more, and more preferably 0.91 or more. Thereby, the fluidity of the resin composition can be improved.
  • the upper limit of SAVE may be, for example, 0.99 or less.
  • S AVE and S 50 may be configured to satisfy 0.20 ⁇ (S AVE ) 2 /S 50 ⁇ 0.50.
  • the lower limit of (S AVE ) 2 /S 50 is, for example, 0.20 or more, preferably 0.21 or more, and more preferably 0.22 or more. Thereby, the fluidity of the resin composition can be improved.
  • the upper limit of (S AVE ) 2 /S 50 is, for example, 0.50 or less, preferably 0.45 or less, and more preferably 0.40 or less. Thereby, bending strength can be improved.
  • the upper limit of the degree of compaction in the inorganic powder is, for example, 44% or less, preferably 43% or less, more preferably 42% or less. This can be expected to improve the mixing property of the inorganic powder with the resin.
  • the lower limit of the degree of compaction in the inorganic powder is, for example, 30% or more, preferably 31% or more, and more preferably 32% or more. As a result, an improvement in powder handling properties can be expected.
  • the upper limit of the bulk density (P) of the inorganic powder is, for example, 2.3 g/cm 3 or less, preferably 2.2 g/cm 3 or less, more preferably 2.1 g/cm 3 or less. As a result, the denseness is increased, and there is a possibility of improving the strength of the resin composition.
  • the lower limit of the bulk density (P) of the inorganic powder is, for example, 1.5 g/cm 3 or more, preferably 1.6 g/cm 3 or more, more preferably 1.7 g/cm 3 or more. This makes it possible to improve the handleability of the powder.
  • the volume frequency particle size distribution of the inorganic powder is measured by a wet laser diffraction scattering method, and in the volume frequency particle size distribution, the particle size at which the cumulative value is 10% is D 10 , and the particle size at which the cumulative value is 50% is D 50. , and the particle diameter at which the cumulative value is 97% is defined as D97 .
  • the lower limit of (D 97 ⁇ D 10 )/D 50 is, for example, 4 or more, preferably 5 or more, and more preferably 6 or more. If the particle size distribution is too narrow or the D50 is too large, the fluidity and filling properties of the powder itself may deteriorate.
  • the upper limit of (D 97 -D 10 )/D 50 is, for example, 30 or less, preferably 25 or less, more preferably 20 or less. When the particle size distribution is in an appropriate range without excessively broadening the D50 , the fluidity and filling properties of the powder itself can be improved.
  • the upper limit of D 50 -D 10 is, for example, 17 ⁇ m or less, preferably 16 ⁇ m or less, more preferably 15 ⁇ m or less. Thereby, appropriate fluidity, thermal conductivity, etc. can be secured.
  • the lower limit of D 50 -D 10 is, for example, 0.5 ⁇ m or more, preferably 1 ⁇ m or more, more preferably 2 ⁇ m or more. Thereby, filling property can be ensured.
  • the particle size distribution of the inorganic powder is a value based on particle size measurement by the laser diffraction light scattering method, and can be measured using, for example, "Model LS-13230" (manufactured by Beckman Coulter) as a particle size distribution analyzer.
  • Water is used as a solvent, and as a pretreatment, an output of 200 W is applied for 1 minute using a homogenizer for dispersion treatment.
  • the PIDS (Polarization Intensity Differential Scattering) concentration is adjusted to 45 to 55%.
  • 1.33 is used as the refractive index of water, and the refractive index of the material of the powder is taken into consideration as the refractive index of the powder. For example, amorphous silica is measured with a refractive index of 1.50, and alumina with a refractive index of 1.68.
  • the sphericity, median diameter, bulk density, and degree of compaction are controlled by appropriately selecting the type and amount of each component contained in the inorganic powder, the method for preparing the inorganic powder, and the like. It is possible to Among these, for example, the alumina powder and / or silica powder immediately after collection are subjected to appropriate storage treatment, the opening degree of these powders during classification treatment is appropriately adjusted, spherical alumina powder of different particle size and the combined use of spherical silica powder, etc. are factors for setting the sphericity, median diameter, bulk density, and degree of compaction within desired numerical ranges.
  • the spherical alumina powder and spherical silica powder contained in the inorganic powder are also called molten spherical particles, respectively. Manufactured by melting and spheroidizing. If necessary, the molten spherical particles thus obtained may be classified and sieved. For example, an inorganic powder can be obtained by producing spherical alumina powder and spherical silica powder and mixing them.
  • FIG. 1 An example of a schematic diagram of a thermal spray apparatus used to produce fused spherical particles is shown in FIG.
  • the melting furnace 2 is composed of a vertical furnace body, but is not limited to this, and may be a horizontal furnace or a tilt furnace in which a flame is blown out horizontally.
  • the hot exhaust gas is cooled by pipes 3, 5 with water cooling jackets.
  • the blower 9 may be connected to a suction gas amount control valve (not shown) and a gas exhaust port. Under the melting furnace 2, the cyclone 4, and the back filter 8, a collected powder extraction device (not shown) may be connected.
  • Classification can be performed using known equipment such as a heavy subsidence chamber, a cyclone, and a classifier having rotary blades. This classification operation may be incorporated in the transportation process of the molten spheroidized product, or may be carried out in a separate line after collective collection.
  • the combustible gas for example, one or more of acetylene, propane, butane, and the like are used, but propane, butane, or a mixed gas thereof, which has a relatively small calorific value, is preferable.
  • a gas containing oxygen for example, is used as the combustion support gas. In general, it is inexpensive and most preferable to use pure oxygen of 99% by mass or more.
  • an inert gas such as air or argon can be mixed with the combustion support gas.
  • alumina powder having an average particle size of 3 to 70 ⁇ m may be used as the alumina raw material powder, which is the raw material powder.
  • the supply of the aluminum hydroxide powder into the high-temperature flame may be either a dry method or a wet method in which it is slurried with water or the like.
  • Silica raw material powder which is a raw material powder, is prepared by adjusting the particle size structure so that the ratio of particles of 1 ⁇ m or less is 15 to 50% and the ratio of particles of 5 ⁇ m or more is 50 to 80%. may be used.
  • the content of the spherical silica powder in the inorganic powder is, for example, 3 to 30% by mass, preferably 3 to 20% by mass, more preferably 3 to 10% by mass, based on 100% by mass of the total amount of the spherical alumina powder and the spherical silica powder. %.
  • the spherical silica powder may be amorphous and/or crystalline.
  • the spherical silica powder preferably has an amorphous rate of, for example, 95% or more, more preferably 97% or more, as measured by the method described below.
  • the amorphous rate is determined by X-ray diffraction analysis using a powder X-ray diffractometer (for example, RIGAKU's trade name "Model MiniFlex") in the range of 26 ° to 27.5 ° for CuK ⁇ ray 2 ⁇ . Measured from peak intensity ratios.
  • a powder X-ray diffractometer for example, RIGAKU's trade name "Model MiniFlex”
  • crystalline silica has a main peak at 26.7°, but amorphous silica does not.
  • a resin composition containing the inorganic powder of the present invention can be suitably used as a resin molding material.
  • the resin composition contains, in addition to the inorganic powder of the present invention, resins and known resin additives.
  • the inorganic powder may be used alone, or may be used by mixing with other fillers.
  • the resin composition may contain 10 to 99% by mass of inorganic powder, or 10 to 99% by mass of mixed inorganic powder containing inorganic powder and other fillers.
  • the content of other fillers in the mixed inorganic powder may be, for example, 1 to 20% by mass or 3 to 15% by mass with respect to 100% by mass of the inorganic powder.
  • "-" means including upper and lower limits unless otherwise specified.
  • fillers include titania, silicon nitride, aluminum nitride, silicon carbide, talc, calcium carbonate, and the like.
  • Other fillers having an average particle size of about 5 to 100 ⁇ m are used, and there are no particular restrictions on their particle size configuration and shape.
  • polyester resins examples include epoxy resins, silicone resins, phenolic resins, melamine resins, urea resins, unsaturated polyesters, fluorine resins, polyamides such as polyimides, polyamideimides and polyetherimides, polybutylene terephthalate, polyethylene terephthalate, and the like.
  • the resin composition is produced by, for example, blending raw material components at a predetermined ratio using a blender, Henschel mixer, or the like, kneading the mixture using a heating roll, a kneader, a single-screw or twin-screw extruder, or the like, and then pulverizing the mixture after cooling. be able to.
  • FIG. 1 Various spherical alumina powders and spherical silica powders were produced using the thermal spraying apparatus 100 shown in FIG.
  • the burner 1 has a double-tube structure capable of forming an inner flame and an outer flame, and is installed at the top of the melting furnace 2. 13 are connected.
  • the raw material powder is fed into the high-temperature flame from the raw material supply pipe 13 and melted to form spherical molten spherical particles.
  • Molten spherical particles that have passed through the melting furnace 2 are sucked by the blower 9 together with combustion exhaust gas, move through the pipes 3 and 5 by air, and are classified and collected by the cyclone 4 or the bag filter 8 .
  • Example 1 ⁇ Production of spherical alumina powder Using the above thermal spraying apparatus 100, LPG is supplied as a combustible gas from the combustible gas supply pipe 11, atmospheric air is supplied as a combustion auxiliary gas from the combustion auxiliary gas supply pipe 12, and in the burner 1 , a high-temperature flame was formed by the combustion of LPG and oxygen. Secondary air is supplied to the cyclone 4 by a rotary valve (not shown) installed in the pipe 3 . Atmospheric air was used as the secondary air. The opening/closing degree (lower opening degree) of the lower valve in the cyclone 4 was set to 100%.
  • alumina powder having a maximum average particle size (D 50 ) in the range of 2 to 45 ⁇ m was used as the raw material powder.
  • the fused spherical particles collected by the bag filter 8 were recovered as spherical alumina powder.
  • Natural silica powder with an average particle size (D 50 ) of 5 ⁇ m was used as the raw material powder, the carrier gas for the raw material was 10 Nm 3 /hr, and the combustible gas supplied to the burner was 10 Nm 3 /hr.
  • the production of the spherical alumina powder was carried out in the same manner as described above, except that the supply amount of the auxiliary combustion gas was 25 Nm 3 /hr.
  • the fused spherical particles collected by the bag filter 8 were recovered as spherical silica powder having an average particle size (D 50 ) of 0.3 ⁇ m.
  • the spherical silica powder was stored in an aluminum bag (manufactured by Japan Co., Ltd., Lamizip AL) at a humidity of 60 to 80% and a temperature of 20 to 30 ° C within 28 days immediately after collection ( storage processing).
  • the spherical silica powder immediately after the aluminum bag was opened and taken out was mixed with the spherical alumina powder immediately after the above production at a mass ratio of 90:10 to obtain an inorganic powder.
  • Example 2-4 Spherical alumina powder obtained in the same manner as in Example 1 above was used, except that the lower opening was changed to 20%, 25%, and 35%, respectively, during the classification process in the production of the spherical alumina powder. , to obtain an inorganic powder.
  • Example 2 In the production of spherical alumina powder, the amount of combustible gas supplied to the burner and the amount of combustion support gas supplied to the burner were 1.5 times that of Example 1, and the above-mentioned powder was stored in the atmosphere for 28 days without the above storage treatment. An inorganic powder was obtained in the same manner as in Example 1, except that spherical silica powder was used.
  • the sphericity of the obtained inorganic powder was determined as follows under conditions of room temperature of 25° C. and humidity of 70%. Using a wet flow image analyzer (manufactured by Sysmex Corporation, FPIA-3000), the obtained inorganic powder was evaluated for a sphericity (S 1 ) with a particle size of 5 ⁇ m or more and less than 10 ⁇ m, and a spherical shape with a particle size of 10 ⁇ m or more and less than 20 ⁇ m.
  • Circularity (Perimeter of projected particle image)/(Perimeter of circle corresponding to area of projected particle image)
  • Sphericity and circularity are average values of particles within each particle size class.
  • the sphericity was the squared value of the circularity of each particle size class.
  • the average sphericity (S AVE ) was calculated from the average values of the four values of S 1 , S 3 , S 4 and S 5 (except those with a value of 0).
  • the obtained inorganic powder was measured for loose bulk density and firm bulk density using a powder tester (manufactured by Hosokawa Micron Corporation, PT-E model) under conditions of room temperature of 25° C. and humidity of 55%.
  • the specific steps are as follows. Inorganic powder, which is a measurement sample, is charged at a rate of 5 to 10 g per minute, allowed to fall naturally from a height of 25 cm, charged into a 100 cm 3 measurement cup, and continued until it overflows from the cup. Got ready.
  • the heaped cup was scraped off the top surface of the cup, and then the mass (g) of the inorganic powder filled in the cup was measured to obtain the loose bulk density (g/cm 3 ). was calculated.
  • the mass (g) was measured and the bulk density (g/cm 3 ) was calculated.
  • the degree of compression (%) was determined based on the formula: ((P ⁇ A)/P) ⁇ 100, where A is the loose bulk density and P is the hard bulk density obtained by the above procedure.
  • the volume frequency particle size distribution of the obtained inorganic powder was determined by a wet laser diffraction scattering method using a particle size distribution analyzer (LS-13230 manufactured by Beckman Coulter, Inc.). Water was used as a solvent, and as a pretreatment, an output of 200 W was applied for 1 minute using a homogenizer to disperse the particles. Also, the PIDS (Polarization Intensity Differential Scattering) concentration was adjusted to 45 to 55% and measured. Based on the obtained volume frequency particle size distribution, the particle diameter DX at which the cumulative value is X% was calculated.
  • the resulting resin composition was molded into a size of 4 mm ⁇ 16 mm ⁇ 80 mm at a mold temperature of 180 ° C., cured at 180 ° C. for 6 hours, and then measured for bending strength (MPa) according to JIS K 6911. complied with the law. When the bending strength was 135 MPa or more, the mechanical strength was evaluated as good, and when it was less than 135 MPa, the mechanical strength was evaluated as poor.
  • the resulting resin composition was molded using molds having slits of 2 ⁇ m, 5 ⁇ m, 10 ⁇ m, and 30 ⁇ m for burr measurement at a molding temperature of 175° C. and a molding pressure of 7.4 MPa.
  • the resin was measured with vernier calipers, and the values measured at each slit were averaged to obtain the burr length ( ⁇ m).
  • the burr length was 1 mm or less, it was evaluated as being able to suppress the generation of burrs during molding (good), and when it exceeded 1 mm, it was evaluated as being likely to generate burrs during molding (poor).
  • the inorganic powders of Examples 1 to 4 were able to improve the mechanical strength of molded articles of the resin composition as compared with Comparative Examples 1 and 2, and as compared with Comparative Example 1, were able to suppress the generation of burrs during molding. Indicated.

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  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Polymers & Plastics (AREA)
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PCT/JP2023/003742 2022-02-09 2023-02-06 無機質粉末 Ceased WO2023153353A1 (ja)

Priority Applications (5)

Application Number Priority Date Filing Date Title
EP23752817.9A EP4467615A1 (en) 2022-02-09 2023-02-06 Inorganic powder
CN202380020978.1A CN118679222A (zh) 2022-02-09 2023-02-06 无机粉末
US18/836,348 US20250115484A1 (en) 2022-02-09 2023-02-06 Inorganic powder
JP2023580231A JPWO2023153353A1 (https=) 2022-02-09 2023-02-06
KR1020247029274A KR20240144982A (ko) 2022-02-09 2023-02-06 무기질 분말

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JP2022018511 2022-02-09

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JP2004244491A (ja) * 2003-02-13 2004-09-02 Denki Kagaku Kogyo Kk 高熱伝導性無機質粉末およびその樹脂組成物
JP2012020900A (ja) * 2010-07-14 2012-02-02 Denki Kagaku Kogyo Kk 球状アルミナ粉末、その製造方法及び用途
JP2013014513A (ja) 2004-12-24 2013-01-24 Nippon Steel & Sumikin Materials Co Ltd 球状アルミナ粉末
JP2022018511A (ja) 2020-07-15 2022-01-27 浜松ホトニクス株式会社 レーザ加工装置及びレーザ加工方法

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JP2004244491A (ja) * 2003-02-13 2004-09-02 Denki Kagaku Kogyo Kk 高熱伝導性無機質粉末およびその樹脂組成物
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WO2025229849A1 (ja) * 2024-04-30 2025-11-06 デンカ株式会社 アルミナ粉末、無機粉末および樹脂組成物

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