WO2023153351A1 - 無機質粉末 - Google Patents

無機質粉末 Download PDF

Info

Publication number
WO2023153351A1
WO2023153351A1 PCT/JP2023/003739 JP2023003739W WO2023153351A1 WO 2023153351 A1 WO2023153351 A1 WO 2023153351A1 JP 2023003739 W JP2023003739 W JP 2023003739W WO 2023153351 A1 WO2023153351 A1 WO 2023153351A1
Authority
WO
WIPO (PCT)
Prior art keywords
inorganic powder
powder
cup
less
measured
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2023/003739
Other languages
English (en)
French (fr)
Japanese (ja)
Inventor
輝洋 相京
朋浩 川畑
純 山口
敦司 山下
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Denka Co Ltd
Original Assignee
Denka Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Denka Co Ltd filed Critical Denka Co Ltd
Priority to US18/837,068 priority Critical patent/US20250136461A1/en
Priority to CN202380020963.5A priority patent/CN118786183A/zh
Priority to KR1020247029272A priority patent/KR20240144980A/ko
Priority to JP2023580229A priority patent/JPWO2023153351A1/ja
Priority to EP23752815.3A priority patent/EP4467613A1/en
Publication of WO2023153351A1 publication Critical patent/WO2023153351A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Images

Classifications

    • 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
    • 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
    • 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
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • 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
    • 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
    • C01P2006/11—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
    • C08K2201/002—Physical properties
    • 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
    • C08K2201/003—Additives being defined by their diameter
    • 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.
  • Patent Document 1 has room for improvement in terms of fluidity when mixed with resin.
  • the following inorganic powder is provided.
  • An inorganic powder containing spherical alumina powder and spherical silica powder An inorganic powder having an angle of repose of 35° or more and 47° or less measured according to the following procedure A under conditions of room temperature of 25°C and humidity of 65%.
  • a funnel with an outlet diameter of 0.5 cm is attached at a height of 15 cm from the horizontal plate installed on the powder tester. Via a funnel, the mineral powder is continuously fed from a vertical direction onto the surface of the horizontal plate to form a conical deposit of constant shape.
  • Procedure B The inorganic powder is allowed to drop naturally from a height of 25 cm at an input amount of 5 to 10 g per minute, and is added into a measuring cup of 100 cm 3 until it overflows from the cup to prepare a heaping cup. Subsequently, without tapping, 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 ).
  • the diameter is D97
  • the inorganic powder according to any one of In the volume frequency particle size distribution measured by the wet laser diffraction scattering method, when the particle diameter at which the cumulative value is 10% is D 10 and the particle diameter at which the cumulative value is 50% is D 50 , An inorganic powder having a D 50 ⁇ D 10 of 0.5 ⁇ m or more and 17 ⁇ m or less.
  • an inorganic powder having excellent fluidity when mixed with resin is provided.
  • FIG. 1 is a schematic cross-sectional view showing the configuration of a thermal spraying device
  • the inorganic powder of this embodiment contains spherical alumina powder and spherical silica powder, and is configured to have an angle of repose of 35° or more and 47° or less.
  • the upper limit of the repose angle of the inorganic powder is 47° or less, preferably 46° or less, more preferably 45° or less. Thereby, the fluidity in the resin composition containing the inorganic powder can be improved.
  • the lower limit of the repose angle of the inorganic powder is, for example, 35° or more, preferably 36° or more, and more preferably 37° or more. As a result, an improvement in powder handling properties can be expected.
  • the upper limit of the collapse angle of the inorganic powder is 37° or less, preferably 36° or less, more preferably 35° or less. This can further improve the fluidity of the resin composition containing the inorganic powder.
  • the lower limit of the collapse angle of the inorganic powder is, for example, 20° or more, preferably 21° or more, and more preferably 22° or more. As a result, an improvement in powder handling properties can be expected.
  • the procedure A for measuring the angle of repose and the angle of decay in the inorganic powder is as follows.
  • a funnel with an outlet diameter of 0.5 cm is attached at a height of 15 cm from the horizontal plate installed on the powder tester.
  • the mineral powder is continuously fed from a vertical direction onto the surface of the horizontal plate to form a conical deposit of constant shape.
  • a protractor find the angle of elevation between the side surface of the conical deposit and the surface of the horizontal plate, which is defined as the angle of repose (°).
  • a 110 g weight is dropped three times from a height of 18 cm onto a horizontal plate to give an impact.
  • the elevation angle formed by the side surface of the cone-shaped deposit and the surface of the horizontal plate is obtained, and this is defined as the collapse angle (°).
  • 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. Thereby, there is a possibility of improving 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 a laser diffraction light scattering method, and can be measured using, for example, "Model LS-13-230" (manufactured by Beckman Coulter, Inc.) 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 angle of repose, collapse angle, bulk density, and degree of compaction are controlled by appropriately selecting the type and amount of each component contained in the inorganic powder, the preparation method of the inorganic powder, and the like.
  • 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 and the like are factors for making the angle of repose, angle of collapse, bulk density, and degree of compression 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.
  • the degree of "sphericity" in the spherical alumina powder and/or spherical silica powder is, for example, an average sphericity of 0.90 or more for particles having a cumulative particle size distribution of less than 75% (d75), and a particle size of d75 or more.
  • the average sphericity of particles having is preferably 0.85 or more.
  • the average sphericity of spherical silica powder is increased, the fluidity tends to be improved.
  • the average sphericity of coarse particles having a particle size of d75 or more to 0.85 or more the effect of the present embodiment is obtained. can be further enhanced.
  • the average sphericity is obtained by taking a particle image taken with a stereoscopic microscope (for example, model "SMZ-10" manufactured by Nikon Corporation), a scanning electron microscope, etc. can be measured as That is, the projected area (A) and perimeter (PM) of the grain are measured from the photograph. Assuming that the area of the perfect circle corresponding to the perimeter (PM) is (B), the circularity of the particle can be expressed as A/B.
  • 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.
  • a combustible gas supply pipe 11, a combustion supporting gas supply pipe 12, and a Each of the tubes 13 is 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 Manufacture 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-supporting gas from the combustion-supporting gas supply pipe 12, and the burner In 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 . Air heated in the melting furnace 2 was used as the secondary air. Also, the lower opening of the cyclone 4 was set to 100%. As the raw material powder, alumina powder having a maximum average particle size (D 50 ) in the range of 2 to 45 ⁇ m was used.
  • D 50 maximum average particle size
  • 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.
  • silica powder having an average particle size (D 50 ) of 5 ⁇ m was obtained by changing the classification treatment conditions.
  • the obtained spherical silica powder and the above spherical alumina powder were mixed at a mass ratio of 90:10 to obtain an inorganic powder.
  • Example 3 Inorganic powder was obtained using the spherical alumina powder obtained in the same manner as in Example 1 above, except that the opening of the lower portion of the cyclone 4 was set to 0% without supplying secondary air.
  • Example 4 Inorganic powder was obtained using silica powder obtained in the same manner as in Example 3 above, except that the spherical silica powder was not stored in an aluminum bag.
  • 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.
  • ⁇ Angle of repose, Collapse angle> The repose angle and decay angle of the obtained inorganic powder were measured using a powder tester (manufactured by Hosokawa Micron Corporation, model PT-E) under conditions of room temperature of 25° C. and humidity of 65%. The specific steps are as follows. A funnel with an outlet diameter of 0.5 cm was attached at a height of 15 cm from the horizontal plate installed on the powder tester. Via a funnel, the mineral powder was continuously fed from a vertical direction onto the surface of the horizontal plate to form a conical deposit of constant shape. Using a protractor, the angle of elevation formed by the side surface of the cone-shaped deposit and the surface of the horizontal plate was determined and defined as the angle of repose (°).
  • 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-13-230, 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.
  • ⁇ Fluidity of Resin Composition 90 parts by mass of each inorganic powder obtained, 5.5 parts by mass of biphenyl type epoxy resin (YX-4000HK manufactured by Japan Epoxy Resin Co., Ltd.), and phenol resin (phenol aralkyl resin, MEHC-7800S manufactured by Meiwa Kasei Co., Ltd.) 4 .8 parts by mass, 0.15 parts by mass of triphenylphosphine (manufactured by Hokko Chemical Co., Ltd.: TPP), and N-phenyl-3-aminopropyltrimethoxysilane manufactured by Shin-Etsu Chemical Co., Ltd.: KBM-573)0.
  • the inorganic powders of Examples 1-4 showed results that could improve the fluidity of the resin composition compared to Comparative Examples 1-4.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Silicon Compounds (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
PCT/JP2023/003739 2022-02-09 2023-02-06 無機質粉末 Ceased WO2023153351A1 (ja)

Priority Applications (5)

Application Number Priority Date Filing Date Title
US18/837,068 US20250136461A1 (en) 2022-02-09 2023-02-06 Inorganic powder
CN202380020963.5A CN118786183A (zh) 2022-02-09 2023-02-06 无机粉末
KR1020247029272A KR20240144980A (ko) 2022-02-09 2023-02-06 무기질 분말
JP2023580229A JPWO2023153351A1 (https=) 2022-02-09 2023-02-06
EP23752815.3A EP4467613A1 (en) 2022-02-09 2023-02-06 Inorganic powder

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2022-018507 2022-02-09
JP2022018507 2022-02-09

Publications (1)

Publication Number Publication Date
WO2023153351A1 true WO2023153351A1 (ja) 2023-08-17

Family

ID=87564413

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2023/003739 Ceased WO2023153351A1 (ja) 2022-02-09 2023-02-06 無機質粉末

Country Status (7)

Country Link
US (1) US20250136461A1 (https=)
EP (1) EP4467613A1 (https=)
JP (1) JPWO2023153351A1 (https=)
KR (1) KR20240144980A (https=)
CN (1) CN118786183A (https=)
TW (1) TW202344478A (https=)
WO (1) WO2023153351A1 (https=)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001139725A (ja) * 1999-11-15 2001-05-22 Denki Kagaku Kogyo Kk 無機質粉末及びそれが充填された樹脂組成物
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
JP2022018507A (ja) 2020-07-15 2022-01-27 フジモールド工業株式会社 被検物判定用の画像処理装置及び画像処理方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001139725A (ja) * 1999-11-15 2001-05-22 Denki Kagaku Kogyo Kk 無機質粉末及びそれが充填された樹脂組成物
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
JP2013014513A (ja) 2004-12-24 2013-01-24 Nippon Steel & Sumikin Materials Co Ltd 球状アルミナ粉末
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
JP2022018507A (ja) 2020-07-15 2022-01-27 フジモールド工業株式会社 被検物判定用の画像処理装置及び画像処理方法

Also Published As

Publication number Publication date
CN118786183A (zh) 2024-10-15
JPWO2023153351A1 (https=) 2023-08-17
US20250136461A1 (en) 2025-05-01
EP4467613A1 (en) 2024-11-27
KR20240144980A (ko) 2024-10-04
TW202344478A (zh) 2023-11-16

Similar Documents

Publication Publication Date Title
WO2023153353A1 (ja) 無機質粉末
WO2023153351A1 (ja) 無機質粉末
WO2023153352A1 (ja) 無機質粉末
JP7787917B2 (ja) 球状シリカ粉末
JP7804705B2 (ja) 球状シリカ粉末
WO2024128321A1 (ja) 球状アルミナ粉末
WO2024128318A1 (ja) 球状アルミナ粉末
WO2024128320A1 (ja) 球状アルミナ粉末
JP7787916B2 (ja) 球状シリカ粉末
WO2024128317A1 (ja) 球状アルミナ粉末
WO2024128316A1 (ja) 球状アルミナ粉末
JP2025168739A (ja) アルミナ粉末、無機粉末および樹脂組成物
JP2025168735A (ja) アルミナ粉末、無機粉末および樹脂組成物
JP2025168731A (ja) アルミナ粉末、無機粉末および樹脂組成物
TW202525718A (zh) 無機質粉末

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 23752815

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2023580229

Country of ref document: JP

Kind code of ref document: A

WWE Wipo information: entry into national phase

Ref document number: 18837068

Country of ref document: US

Ref document number: 202380020963.5

Country of ref document: CN

WWE Wipo information: entry into national phase

Ref document number: 2023752815

Country of ref document: EP

Ref document number: 23752815

Country of ref document: EP

ENP Entry into the national phase

Ref document number: 2023752815

Country of ref document: EP

Effective date: 20240819

ENP Entry into the national phase

Ref document number: 20247029272

Country of ref document: KR

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

WWW Wipo information: withdrawn in national office

Ref document number: 1020247029272

Country of ref document: KR

WWW Wipo information: withdrawn in national office

Ref document number: 2023752815

Country of ref document: EP

WWP Wipo information: published in national office

Ref document number: 18837068

Country of ref document: US