WO2024106403A1 - 無機粉末、樹脂用充填剤、樹脂組成物及び無機粉末の製造方法 - Google Patents
無機粉末、樹脂用充填剤、樹脂組成物及び無機粉末の製造方法 Download PDFInfo
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- WO2024106403A1 WO2024106403A1 PCT/JP2023/040831 JP2023040831W WO2024106403A1 WO 2024106403 A1 WO2024106403 A1 WO 2024106403A1 JP 2023040831 W JP2023040831 W JP 2023040831W WO 2024106403 A1 WO2024106403 A1 WO 2024106403A1
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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
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
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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
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- 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
- C01F7/023—Grinding, deagglomeration or disintegration
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- 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
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
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- 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
- C08K3/28—Nitrogen-containing compounds
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- 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
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- 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
- C01P2002/74—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by peak-intensities or a ratio thereof only
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- 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
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- 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
Definitions
- the present invention relates to inorganic powders, fillers for resins, resin compositions, and methods for producing inorganic powders.
- Powdered inorganic metal compounds such as silica, alumina, and boron nitride are widely used as inorganic fillers for resins, taking advantage of their thermal conductivity and insulating properties.
- inorganic fillers when inorganic fillers are mixed into resins, the fluidity of the resin composition tends to decrease.
- Patent Documents 1 and 2 propose an inorganic powder for use as an additive to a resin composition, which has a specific particle size distribution and average circularity.
- an object of the present invention is to provide an inorganic powder that can achieve excellent fluidity when blended with a resin, a filler for resin containing the inorganic powder, a resin composition containing the inorganic powder, and a method for producing the inorganic powder.
- the inventors of the present application discovered that the above-mentioned problems can be solved by using an inorganic powder having a Hausner ratio, defined as the ratio of tap density to bulk density, within a certain range, and thus completed the present invention. That is, the present invention has the following aspects.
- the inorganic powder according to [1] having an average particle diameter (D50) of 30 ⁇ m or less.
- D50 average particle diameter
- the inorganic powder according to [1] or [2] which has a specific surface area of 0.3 m 2 /g or more.
- [6] The inorganic powder according to [5], having a semi-quantitative value of 0.6 or more calculated from the O 1s peak intensity measured by X-ray photoelectron spectroscopy.
- [7] The inorganic powder according to any one of [1] to [6], which is for use in resin filling.
- a filler for resin comprising the inorganic powder according to any one of [1] to [7].
- a resin composition comprising the inorganic powder according to any one of [1] to [8] and at least one resin selected from the group consisting of thermoplastic resins and thermosetting resins.
- the dispersing step includes breaking up agglomerated particles in the raw powder with the cavitation bubbles.
- the present invention provides an inorganic powder that can achieve excellent fluidity when blended with a resin, a filler for resin containing the inorganic powder, a resin composition containing the inorganic powder, and a method for producing the inorganic powder.
- the inorganic powder according to this embodiment has a Hausner ratio of 1.00 to 1.33.
- the "Hausner ratio” is the ratio of tap density to bulk density, and is expressed as “tap density (g/cm 3 )/bulk density (g/cm 3 )."
- the tap density and bulk density for determining the Hausner ratio can be measured by the following method. (Method of measuring tap density and bulk density) First, the inorganic powder is dried at 120°C for 5 hours.
- the bulk density and tap density of the inorganic powder are calculated from the following formulas (1) to (2).
- the bulk density and tap density are calculated to two decimal places by rounding off the third decimal place.
- the bulk density and tap density are calculated in "g/cm 3 ", assuming that 1 mL of a graduated cylinder is 1 cm 3.
- the tap density and bulk density are measured under conditions of a temperature of 21 to 25°C and a humidity of 50% ⁇ 4%.
- Tap density (g/cm 3 ) mass of inorganic powder (M1)/V2 (2)
- the Hausner ratio of the inorganic powder according to this embodiment is 1.00 to 1.33.
- the preferred range of the Hausner ratio of the inorganic powder may be 1.00 to 1.11, 1.12 to 1.18, 1.19 to 1.25, or 1.26 to 1.33.
- an inorganic powder with a small tap density has a large volume and a small bulk density, so that the powder is likely to have a Hausner ratio of more than 1.33.
- the inorganic powder according to this embodiment can have a Hausner ratio in the range of 1.00 to 1.33 even if the tap density is low.
- the tap density of the inorganic powder may be, for example, 2.30 g/cm 3 or less, 2.00 g/cm 3 or less, 1.70 g/cm 3 or less, 1.50 g/cm 3 or less, 1.30 g/cm 3 or less, or 1.00 g/cm 3 or less. Even if it has such a tap density, the Hausner ratio is likely to be in the above range, so that the fluidity is easily improved.
- the lower limit of the tap density of the inorganic powder is not particularly limited, but may be, for example, 0.10 g/cm 3 or more, 0.20 g/cm 3 or more, or 0.30 g/cm 3 or more.
- the tap density of the inorganic powder according to this embodiment can be any combination of the above-mentioned preferable upper and lower limits within the range in which the Hausner ratio is 1.00 to 1.33.
- the inorganic powder according to this embodiment can have a Hausner ratio in the range of 1.00 to 1.33 even if the bulk density is low.
- the bulk density of the inorganic powder may be 1.60 g/cm 3 or less, 1.40 g/cm 3 or less, 1.20 g/cm 3 or less, 1.00 g/cm 3 or less, or 0.80 g/cm 3 or less. Even if it has such a bulk density, the Hausner ratio is likely to be in the above range, so the flowability is easily improved.
- the lower limit of the bulk density of the inorganic powder is not particularly limited, but may be, for example, 0.05 g/cm 3 or more, 0.10 g/cm 3 or more, or 0.20 g/cm 3 or more.
- the bulk density of the inorganic powder according to this embodiment can be any combination of the above-mentioned preferred upper and lower limits within the range in which the Hausner ratio is 1.00 to 1.33.
- the inorganic powder according to this embodiment particularly preferably has a tap density of 1.00 g/ cm3 or less and a bulk density of 1.00 g/ cm3 or less.
- inorganic powders with a small difference between tap density and bulk density can be easily prepared by a manufacturing method that includes dispersing the raw powder of the inorganic powder in a liquid containing cavitation bubbles, recovering it, and drying it.
- the manufacturing method of the inorganic powder will be described later.
- the manufacturing method of the inorganic powder of this embodiment is particularly suitable for inorganic powders with a tap density of 1.00 g/ cm3 or less and a bulk density of 1.00 g/ cm3 or less.
- the average particle diameter (D50) of the inorganic powder according to this embodiment is preferably 30 ⁇ m or less.
- the average particle diameter (D50) of the inorganic powder refers to the volume-based cumulative diameter (D50) evaluated by a laser diffraction scattering method after a specific dispersion treatment, for example, a homogenizer treatment.
- volume-based cumulative diameter (D50) means a particle diameter corresponding to a cumulative value of 50% in the volume-based cumulative particle size distribution measured by a laser diffraction scattering method.
- the cumulative particle size distribution is represented by a distribution curve with the particle diameter ( ⁇ m) on the horizontal axis and the cumulative value (%) on the vertical axis.
- the Hausner ratio is likely to be outside the range of this embodiment, but according to this embodiment, even if the D50 is small, the Hausner ratio is likely to be in the range of 1.00 to 1.33. Therefore, even if the D50 is 30 ⁇ m or less, the fluidity is likely to be improved.
- the D50 of the inorganic powder may be 30 ⁇ m or less, 27 ⁇ m or less, 25 ⁇ m or less, 22 ⁇ m or less, 20 ⁇ m or less, 17 ⁇ m or less, 15 ⁇ m or less, 12 ⁇ m or less, or 9 ⁇ m or less.
- the lower limit of D50 of the inorganic powder is not particularly limited, but may be, for example, 0.05 ⁇ m or more, 0.08 ⁇ m or more, 0.12 ⁇ m or more, 0.15 ⁇ m or more, 0.17 ⁇ m or more, 0.20 ⁇ m or more, 0.22 ⁇ m or more, or 0.25 ⁇ m or more.
- the D50 of the inorganic powder according to this embodiment can be any combination of the above-mentioned preferred upper and lower limits within the range in which the Hausner ratio is 1.00 to 1.33.
- the specific surface area of the inorganic powder may be 0.1 m 2 /g or more, 0.2 m 2 /g or more, 0.3 m 2 /g or more, 0.4 m 2 /g or more, 0.5 m 2 /g or more, 0.6 m 2 /g or more, 0.7 m 2 /g or more, 0.8 m 2 /g or more, 0.9 m 2 /g or more, or 1.0 m 2 /g or more. Even if the specific surface area is above the lower limit, the inorganic powder tends to have excellent flowability.
- the upper limit of the specific surface area of the inorganic powder is not particularly limited, and may be, for example, 35 m 2 /g or less, 32 m 2 /g or less, 30 m 2 /g or less, 27 m 2 /g or less, 25 m 2 /g or less, 22 m 2 /g or less, 20 m 2 /g or less, 17 m 2 /g or less, or 15 m 2 /g or less.
- the specific surface area of the inorganic powder according to this embodiment can be any combination of the above-mentioned preferred upper and lower limits within the range in which the Hausner ratio is 1.00 to 1.33.
- the specific surface area of the inorganic powder can be measured by a BET multipoint method using nitrogen gas in accordance with JIS Z 8830:2013.
- the inorganic powder according to the present embodiment preferably contains at least one selected from alumina powder, aluminum nitride powder, silica powder, silicon nitride powder, magnesium oxide powder, titanium oxide powder, zirconia powder, zinc oxide powder, aggregated boron nitride powder, scaly boron nitride powder, and spherical boron nitride powder, more preferably contains at least one selected from alumina powder, aluminum nitride powder, silica powder, silicon nitride powder, aggregated boron nitride powder, scaly boron nitride powder, and spherical boron nitride powder, and more preferably contains at least one selected from alumina powder, silica powder, aggregated boron nitride powder, scaly boron nitride powder, and spherical boron nitride powder.
- the inorganic powder may contain one of the above-mentioned powders alone, or may be a mixed powder containing two or more of them.
- the blending ratio of each powder can be set arbitrarily.
- the shape of the alumina powder, aluminum nitride powder, silica powder, silicon nitride powder, magnesium oxide powder, titanium oxide powder, zirconia powder, and zinc oxide powder is not particularly limited and may be spherical or amorphous. From the viewpoints of flowability and low viscosity during filling, however, a spherical shape is preferred.
- the inorganic powder is preferably at least one powder selected from agglomerated boron nitride powder, flaky boron nitride powder, and spherical boron nitride powder, and is more preferably flaky boron nitride powder or spherical boron nitride powder.
- Boron nitride powder has lubricity, high thermal conductivity, and insulating properties, and is widely used as a solid lubricant, a release agent for molten gas and aluminum, and a filler for heat dissipation materials.
- the inorganic powder according to the present embodiment is at least one powder selected from the above-mentioned aggregated boron nitride powder, scaly boron nitride powder, and spherical boron nitride powder, it is easy to provide a solid lubricant, a release agent, and a filler for heat dissipation materials that are more fluid than conventional ones.
- aggregated boron nitride powder refers to a powder in which hexagonal boron nitride having scaly primary particles is aggregated to form a mass.
- spherical powder means that the powder is observed to have a circular or rounded grain shape when observed at a magnification of 10,000 times using a scanning electron microscope.
- the average circularity of the spherical boron nitride powder may be 0.70 or more, 0.75 or more, 0.80 or more, or 0.87 or more.
- the "average circularity" can be calculated by the following method.
- the projected area (S) and perimeter (L) of one particle are calculated by image analysis using image analysis software (e.g., MacView, product name, manufactured by Mountec Co., Ltd.) for an image of the powder taken with a scanning electron microscope (SEM) (magnification: 10,000 times, image resolution: 1280 x 1024 pixels).
- image analysis software e.g., MacView, product name, manufactured by Mountec Co., Ltd.
- SEM scanning electron microscope
- the circularity is calculated by substituting the projected area (S) and perimeter (L) into the following formula (3).
- the semi-quantitative value calculated from the O 1s peak intensity measured by X-ray photoelectron spectroscopy of the inorganic powder (hereinafter sometimes referred to as "O 1s semi-quantitative value”) is preferably 0.6 or more, more preferably 0.65 or more, and even more preferably 0.7 or more.
- "semi-quantitative value calculated from the O 1s peak intensity measured by X-ray photoelectron spectroscopy” refers to a semi-quantitative value calculated from the O 1s peak intensity by removing the background by the Shirley method from the spectrum obtained by measuring the inorganic powder using an X-ray photoelectron spectrometer (for example, Thermo Fisher Scientific, product name: K-Alpha type X-ray photoelectron spectrometer, monochromator-equipped Al-X - ray source, measurement area: 400 x 200 ⁇ m).
- X-ray photoelectron spectrometer for example, Thermo Fisher Scientific, product name: K-Alpha type X-ray photoelectron spectrometer, monochromator-equipped Al-X - ray source, measurement area: 400 x 200 ⁇ m.
- the "O 1s semi-quantitative value” can be the value of the O 1s peak area in the inorganic powder measured according to the manual of the X-ray photoelectron spectrometer.
- the “Shirley method” refers to a method for determining the shape of the background to be subtracted, assuming that the inelastically scattered electrons that cause the background are independent of energy and that the number of inelastically scattered electrons is proportional to the peak intensity.
- the inorganic powder according to the present embodiment can provide a resin composition having excellent flowability, and therefore can be preferably used as a filler for resins.
- the resin filler according to the present embodiment includes the inorganic powder described above. From the viewpoint of obtaining a resin composition with better fluidity, the resin filler may be composed of only the inorganic powder described above.
- the resin that can be mixed with the resin filler according to the present embodiment is not particularly limited, and can be mixed with conventionally known thermosetting resins and thermoplastic resins.
- the method for producing an inorganic powder according to the present embodiment includes dispersing a raw material powder in a liquid containing cavitation bubbles (step (I)), and recovering the raw material powder from the liquid and then drying it (step (II)). According to the production method according to the present embodiment, an inorganic powder having a Hausner ratio of 1.00 to 1.33 can be efficiently produced.
- the manufacturing method according to the present embodiment includes dispersing a raw material powder in a liquid containing cavitation bubbles (step (I)).
- cavitation bubbles refers to bubbles that are generated by vaporization of a liquid when the liquid is in a low-pressure state.
- Methods for dispersing the raw material powder in a liquid containing cavitation bubbles include, for example, a method in which the raw material powder is poured into a liquid containing cavitation bubbles and mechanically stirred, and a method in which the raw material powder is dispersed in the liquid by utilizing cavitation bubbles.
- step (I) includes disintegrating the aggregated particles in the raw powder with cavitation bubbles (i.e., disintegrating the aggregated particles).
- the disintegration includes disintegrating the aggregated particles to primary particles.
- the state of the particle surface is easily changed by increasing the proportion of hydroxyl groups on the particle surface through step (I), which is also considered to be one of the reasons why an inorganic powder having a small Hausner ratio can be obtained.
- the raw powder is not particularly limited. An inorganic powder prepared by any method can be used as the raw powder.
- the average particle size (D50) of the raw powder is preferably 0.05 to 30 ⁇ m, more preferably 0.5 to 25 ⁇ m.
- the specific surface area of the raw powder may be 1 to 30 m 2 /g, or 1 to 15 m 2 /g.
- the Hausner ratio of the raw material powder is preferably 1.35 to 3.00, and more preferably 1.50 to 2.50.
- Examples of methods for preparing a liquid containing cavitation bubbles include a method of reducing the pressure of the liquid, a method using ultrasonic waves, and a hydrodynamic method.
- a liquid containing cavitation bubbles can be prepared by these methods using a commercially available device.
- a hydrodynamic method may be adopted.
- the powder suction continuous dissolving and dispersing device generally has a mechanism for generating a flow rate by an agitating blade.
- the rotation speed of the agitating blade is preferably 2,000 to 10,000 rpm, more preferably 4,000 to 9,000 rpm, even more preferably 4,500 to 8,000 rpm, even more preferably 5,000 to 8,000 rpm, and particularly preferably 6,000 to 7,200 rpm.
- the step (I) preferably includes generating cavitation bubbles in the liquid. That is, by dispersing the raw material powder in the liquid while generating cavitation bubbles, agglomerated particles in the raw material powder are easily disintegrated.
- the process of generating cavitation bubbles is preferably performed 50 or more times, more preferably 100 or more times, and even more preferably 150 or more times, as the number of cavitation processes calculated from the rotation speed (rpm) of the stirring blades of the device and the discharge volume.
- the liquid in which the raw material powder is dispersed is not particularly limited as long as it has the effect of the present invention.
- the liquid may be a liquid consisting of only an organic solvent such as ethanol, or a mixed solution of water and an organic solvent.
- the content of water in the mixed solution is preferably 80% by mass or more, more preferably 90% by mass or more, and even more preferably 95% by mass or more.
- it is particularly preferable that the liquid is a liquid consisting of only water.
- the liquid temperature in step (I) is preferably 10 to 60°C, more preferably 20 to 40°C, from the viewpoints of effectively generating cavitation in the liquid and suppressing volatilization of the liquid.
- the proportion of the raw powder dispersed in the liquid is preferably 5 to 30 mass%, more preferably 5 to 20 mass%, and even more preferably 5 to 15 mass%, relative to the total of the liquid and raw powder (100 mass%). In one embodiment, the proportion of the raw powder may be 5 to 10 mass%, or may be 8 to 10 mass%.
- the time for carrying out step (I) is not particularly limited as long as the effect of the present invention is achieved.
- the time for step (I) may be extended from the viewpoint of increasing the recovery efficiency of the crushed powder or preventing variation in crushing in the treated powder.
- the time for step (I) may be 5 minutes or more and 24 hours or less, 5 minutes or more and 20 hours or less, or 5 minutes or more and 10 hours or less.
- Step (II) is a step of recovering the raw material powder from the liquid after step (I) and drying the recovered raw material powder.
- the method for recovering the raw material powder from the liquid include filtration (reduced pressure filtration, vacuum filtration, etc.) and centrifugation.
- methods for drying the recovered raw material powder include high-temperature air drying and reduced-pressure drying.
- the drying temperature of the raw material powder is preferably 80 to 150° C., and more preferably 100 to 120° C.
- the drying time is preferably 2 to 24 hours, and more preferably 5 to 12 hours.
- the manufacturing method according to this embodiment may include steps (other steps) other than the above-mentioned steps (I) and (II). Examples of other steps include dissolving inorganic powder.
- the resin composition according to this embodiment contains the inorganic powder described above and at least one resin selected from the group consisting of thermoplastic resins and thermosetting resins.
- the proportion of the inorganic powder in the resin composition is not particularly limited and can be appropriately adjusted depending on the purpose. For example, it may be in the range of 1 to 99 mass % or in the range of 5 to 80 mass % based on the total mass of the resin composition.
- the resin composition according to the present embodiment contains at least one resin selected from thermoplastic resins and thermosetting resins. More specifically, for example, polyethylene resin; polypropylene resin; epoxy resin; silicone resin; phenol resin; melamine resin; urea resin; unsaturated polyester resin; fluororesin; polyamide-based resins such as polyimide resin, polyamideimide resin, and polyetherimide resin; polyester-based resins such as polybutylene terephthalate resin and polyethylene terephthalate resin; polyphenylene sulfide resin; wholly aromatic polyester resin; polysulfone resin; liquid crystal polymer resin; polyethersulfone resin; polycarbonate resin; maleimide-modified resin; ABS resin; AAS (acrylonitrile-acrylic rubber-styrene) resin; AES (acrylonitrile-ethylene-propylene-diene rubber-styrene) resin; hydrocarbon-based elastomer resin; polyphenylene ether resin; aromatic polyene-
- additives may be blended into the resin composition as long as they do not impair the effects of the present invention.
- examples of other additives include rubber-like substances such as silicone rubber, polysulfide rubber, acrylic rubber, butadiene rubber, styrene block copolymer, and saturated elastomer; resin-like substances such as silicone resin; resins in which epoxy resin or phenolic resin is partially or entirely modified with aminosilicone, epoxysilicone, alkoxysilicone, and the like; flame retardant assistants such as Sb 2 O 3 , Sb 2 O 4 , and Sb 2 O 5 ; flame retardants such as halogenated epoxy resin and phosphorus compounds; colorants such as carbon black, iron oxide, dyes, and pigments. These may be used alone or in combination of two or more.
- the method for producing the resin composition is not particularly limited, and the resin composition can be produced by stirring, dissolving, mixing, and dispersing a predetermined amount of each material.
- the apparatus for mixing, stirring, dispersing, etc. of the mixture is not particularly limited, but a mortar and pestle machine equipped with a stirring and heating device, a three-roll mill, a ball mill, a planetary mixer, etc. can be used. These apparatuses may also be used in appropriate combination.
- raw material powder As the raw material powder, powders of the following inorganic metal compounds were used.
- the average particle size (D50), specific surface area, bulk density, tap density of the raw material powder, and viscosity ( ⁇ 1) of the resin composition are values measured under the same conditions as those for the inorganic powder described below.
- Example 1 Raw material powder 1 (10% by mass) was dispersed in ion-exchanged water in which cavitation bubbles were generated using a powder suction continuous dissolution and dispersion device (manufactured by Japan Spindle Manufacturing Co., Ltd., product name: Jet Paster (registered trademark), model number: JPSS) (step (I)).
- the cavitation bubbles in the ion-exchanged water were generated by rotating the stirring blade of the device at 7,200 rpm.
- step (I) was carried out for 60 minutes, the raw material powder was recovered by filtration. Thereafter, it was dried at 120°C for 5 hours to obtain the inorganic powder of Example 1 (spherical boron nitride powder).
- the average particle size (D50), specific surface area (BET specific surface area), O 1s semi-quantitative value, bulk density and tap density of the obtained inorganic powder were measured under the following conditions.
- the flowability of the resin composition containing the inorganic powder was also evaluated under the following conditions. The results are shown in Table 2.
- the bulk density and tap density of the inorganic powder were measured by the following method. First, the inorganic powder was dried at 120 ° C. for 5 hours. After that, 5.00 ⁇ 0.02 g (M1) of the dried inorganic powder was weighed with a precision balance (precision balance with a minimum weighing value of 0.001 g) and poured into a 50 mL graduated cylinder. After pouring, the volume (V1) (to one decimal place) of the inorganic powder in the graduated cylinder was measured visually. Next, the graduated cylinder was lifted and dropped 500 times from a height of 3.5 cm.
- the graduated cylinder was dropped onto a rubber mat (thickness 40 mm) so that the impact on the graduated cylinder was the same each time.
- the volume (V2) (to one decimal place) of the inorganic powder in the graduated cylinder was measured visually.
- the bulk density and tap density of the inorganic powder were calculated from the following formulas (1) to (2).
- the bulk density and tap density were calculated to two decimal places by rounding off the third decimal place.
- the bulk density and tap density were calculated in "g/cm 3 " assuming that 1 mL of a graduated cylinder is 1 cm 3.
- the tap density and bulk density were measured under conditions of a temperature of 23°C and a humidity of 50%.
- the flowability of the resin composition containing the inorganic powder was evaluated by the ratio of the shear viscosity of the raw material powder to that of the inorganic powder (the ratio of the shear viscosity before and after the cavitation treatment). Specifically, the resin composition was prepared by the following method, and the viscosity ratio of the obtained resin composition at a shear of 0.1 (1/s) was evaluated.
- a dispersant manufactured by BYK Japan Co., Ltd., product name "DISPERBYK-111", 0.3% by mass
- an SC material manufactured by Tokyo Chemical Industry Co., Ltd., product name "3-glycidyloxypropyltrimethoxysilane", 1% by mass
- raw material powder (15% by mass) were added to an epoxy resin (manufactured by Nippon Steel Chemical & Material Co., Ltd.), and the mixture was kneaded for 3 minutes at room temperature, revolution speed of 2,000 rpm, and rotation speed of 800 rpm using a hybrid mixer (manufactured by Thinky Corporation, product name "Awatori Rentaro (registered trademark) AR-250").
- Examples 2 to 7 and Comparative Examples 1 to 4 Inorganic powders were produced in the same manner as in Example 1, except that the type of raw material powder and the production conditions were as shown in Table 2.
- Comparative Examples 1 to 4 the raw material powder was stirred and dispersed in a liquid containing no cavitation bubbles, and then the raw material powder was filtered and recovered and dried.
- the average particle size (D50), specific surface area, bulk density and tap density were measured in the same manner as in Example 1, and the flowability of the resin composition containing the inorganic powder was evaluated.
- the O 1s semi-quantitative value was measured in the same manner as in Example 1. The results are shown in Table 2.
- the notation "-" means that the device was not used or the measurement was not performed.
- the inorganic powder according to this embodiment can produce a resin composition with excellent fluidity. Therefore, it can be preferably used as a filler for resins.
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| CN202380078237.9A CN120187666A (zh) | 2022-11-14 | 2023-11-13 | 无机粉末、树脂用填充剂、树脂组合物及无机粉末的制造方法 |
| KR1020257019176A KR20250107899A (ko) | 2022-11-14 | 2023-11-13 | 무기 분말, 수지용 충전제, 수지 조성물 및 무기 분말의 제조 방법 |
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| JP2004505875A (ja) * | 2000-08-04 | 2004-02-26 | アトフィナ | 流動性を改善し五酸化燐粉末の製造方法 |
| JP2013040062A (ja) * | 2011-08-12 | 2013-02-28 | Mitsubishi Chemicals Corp | 六方晶窒化ホウ素粉末、それを含有する熱伝導性樹脂組成物及びそれによる成形体 |
| JP2017132653A (ja) * | 2016-01-27 | 2017-08-03 | 信越化学工業株式会社 | セラミックス成型品及び透明焼結体の製造方法 |
| US20170326641A1 (en) * | 2014-12-05 | 2017-11-16 | Industry-University Cooperation Foundation Hanyang University Erica Campus | Metal powder, feedstock, and preparation method therefor |
| JP2022025568A (ja) * | 2020-07-29 | 2022-02-10 | 株式会社フジミインコーポレーテッド | 粉末材料及びこれを用いた焼結体 |
| JP2022047494A (ja) * | 2020-09-11 | 2022-03-24 | クエステック イノベーションズ リミテッド ライアビリティ カンパニー | 付加製造用ステンレス鋼粉末 |
| WO2022106923A1 (en) * | 2020-11-18 | 2022-05-27 | BioPharma Synergies, S. L. | Orodispersible powder composition comprising an antihistamine compound |
| US20220242732A1 (en) * | 2019-06-05 | 2022-08-04 | Deepak Nitrite Limited | A free flowing sodium nitrite and method of production |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7976941B2 (en) * | 1999-08-31 | 2011-07-12 | Momentive Performance Materials Inc. | Boron nitride particles of spherical geometry and process for making thereof |
| JP5281250B2 (ja) | 2007-03-29 | 2013-09-04 | 株式会社アドマテックス | 樹脂組成物添加用無機粉末及び樹脂組成物 |
| JP5236198B2 (ja) | 2007-03-29 | 2013-07-17 | 株式会社アドマテックス | 樹脂組成物添加用無機粉末及び樹脂組成物 |
| CN104271677A (zh) * | 2012-05-04 | 2015-01-07 | 纳幕尔杜邦公司 | 用于制备具有增强的堆积处理特性的粉末的方法 |
| CN113831685B (zh) * | 2021-09-16 | 2023-09-26 | 中国科学院工程热物理研究所 | 一种取向排布的氮化硼高导热复合材料及制备方法 |
-
2023
- 2023-11-13 CN CN202380078237.9A patent/CN120187666A/zh active Pending
- 2023-11-13 JP JP2024558876A patent/JPWO2024106403A1/ja active Pending
- 2023-11-13 WO PCT/JP2023/040831 patent/WO2024106403A1/ja not_active Ceased
- 2023-11-13 KR KR1020257019176A patent/KR20250107899A/ko active Pending
- 2023-11-14 TW TW112143889A patent/TWI906694B/zh active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004505875A (ja) * | 2000-08-04 | 2004-02-26 | アトフィナ | 流動性を改善し五酸化燐粉末の製造方法 |
| JP2013040062A (ja) * | 2011-08-12 | 2013-02-28 | Mitsubishi Chemicals Corp | 六方晶窒化ホウ素粉末、それを含有する熱伝導性樹脂組成物及びそれによる成形体 |
| US20170326641A1 (en) * | 2014-12-05 | 2017-11-16 | Industry-University Cooperation Foundation Hanyang University Erica Campus | Metal powder, feedstock, and preparation method therefor |
| JP2017132653A (ja) * | 2016-01-27 | 2017-08-03 | 信越化学工業株式会社 | セラミックス成型品及び透明焼結体の製造方法 |
| US20220242732A1 (en) * | 2019-06-05 | 2022-08-04 | Deepak Nitrite Limited | A free flowing sodium nitrite and method of production |
| JP2022025568A (ja) * | 2020-07-29 | 2022-02-10 | 株式会社フジミインコーポレーテッド | 粉末材料及びこれを用いた焼結体 |
| JP2022047494A (ja) * | 2020-09-11 | 2022-03-24 | クエステック イノベーションズ リミテッド ライアビリティ カンパニー | 付加製造用ステンレス鋼粉末 |
| WO2022106923A1 (en) * | 2020-11-18 | 2022-05-27 | BioPharma Synergies, S. L. | Orodispersible powder composition comprising an antihistamine compound |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20250107899A (ko) | 2025-07-14 |
| TWI906694B (zh) | 2025-12-01 |
| JPWO2024106403A1 (https=) | 2024-05-23 |
| CN120187666A (zh) | 2025-06-20 |
| TW202421706A (zh) | 2024-06-01 |
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