WO2013039103A1 - Composite de charge inorganique, composition de résine conductrice de la chaleur et article moulé - Google Patents

Composite de charge inorganique, composition de résine conductrice de la chaleur et article moulé Download PDF

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Publication number
WO2013039103A1
WO2013039103A1 PCT/JP2012/073331 JP2012073331W WO2013039103A1 WO 2013039103 A1 WO2013039103 A1 WO 2013039103A1 JP 2012073331 W JP2012073331 W JP 2012073331W WO 2013039103 A1 WO2013039103 A1 WO 2013039103A1
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inorganic filler
boehmite
resin composition
filler composite
composite
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PCT/JP2012/073331
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English (en)
Japanese (ja)
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川村　孝
純司 山口
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Dic株式会社
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Priority to JP2013506375A priority Critical patent/JP5418720B2/ja
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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
    • 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
    • C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
    • C01F7/447—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by wet processes
    • C01F7/448—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by wet processes using superatmospheric pressure, e.g. hydrothermal conversion of gibbsite into boehmite
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/04—Compounds of zinc
    • C09C1/043—Zinc oxide
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/40—Compounds of aluminium
    • C09C1/42—Clays
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • 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
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/45—Aggregated particles or particles with an intergrown morphology
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
    • 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

Definitions

  • the present invention comprises a resin composition excellent in thermal conductivity and insulation, comprising a composite obtained from a thermoplastic resin or a thermosetting resin, a thermally conductive filler and alumina boehmite or zinc oxide.
  • the present invention relates to a molded body.
  • thermoplastic resin resins such as polypropylene (PP), ABS, polyamide (PA6, PA66, etc.), polyester (PET, PBT, etc.), polycarbonate (PC), etc. are known. Resins such as liquid crystal polyester (LCP) and polyphenylene sulfide (PPS), which have excellent heat resistance, mechanical strength, chemical resistance, and processability, are widely used in applications such as various electronic devices, electronic parts, and mechanical parts. It has become like this.
  • a thermosetting resin an epoxy resin, an unsaturated polyester resin, a urethane resin, an epoxy acrylate resin, and a polyimide resin are preferably used as materials that make use of excellent rigidity, dimensional stability, and insulation.
  • Patent Document 1 describes a thermally conductive resin molded product in which a thermoplastic resin is filled with graphite powder
  • Patent Document 2 describes a resin heat radiation plate in which polyphenylene sulfide resin is filled with magnesium oxide or aluminum oxide.
  • the molding fluidity was remarkably lowered and the moldability was greatly reduced.
  • a graphite filler is blended, there is a problem that the insulating property is lowered and the use is limited.
  • Patent Document 3 discloses a thermosetting resin or thermoplastic resin, a first inorganic filler having a microparticle size, SiO 2 (silica), Al 2 O 3 (alumina), alumina hydrate, TiO 2. (Titanium oxide), a resin composition for an electrical insulating material containing at least one second inorganic filler of nanoparticle size selected from the group consisting of AlN (aluminum nitride) is described.
  • AlN aluminum nitride
  • boehmite is described as alumina hydrate which is the second inorganic filler.
  • an object of the present invention is to provide a thermoplastic resin composition having good moldability. Therefore, a molded article that exhibits excellent thermal conductivity even if the volume content of the inorganic filler contained in the composition is small. And providing a resin composition used for the molded body.
  • an inorganic filler composite composed of boehmite having a shape of at least one of a granular shape, a square shape, a fiber shape, and a flat plate shape or a zinc oxide bonded or adhered to the surface of the thermally conductive filler. It has been found that the above-mentioned problems can be solved by providing the above.
  • FIG. 6 is a scanning electron micrograph of a composite of boron nitride and zinc oxide obtained in Synthesis Example 5.
  • FIG. 6 is a scanning electron micrograph of a composite of alumina and boehmite obtained in Synthesis Example 8.
  • 4 is a scanning electron micrograph of a composite of granular graphite and boehmite obtained in Synthesis Example 9. It is drawing which shows the flow direction and thickness direction which concern on thermal conductivity measurement. It is drawing which shows the measurement direction of the heat conductivity of a flow direction. It is drawing which shows the measurement direction of the heat conductivity of the thickness direction.
  • 3 is a scanning electron micrograph of a BN-BM composite after kneading with polystyrene.
  • 2 is a scanning electron micrograph of a BN-BM complex in which fibrous BM is bonded to the BN surface. It is a scanning electron micrograph which expanded the coupling
  • the present invention includes the following items.
  • An inorganic filler composite composed of boehmite having at least one shape of a granular shape, a rectangular shape, a fibrous shape, a flat plate shape, or zinc oxide bonded or adhered to the surface of the thermally conductive filler, 2.
  • the inorganic filler composite according to 1 or 2 wherein the average particle size of the heat conductive filler is 0.5 to 100 ⁇ m, 4). 4.
  • a thermally conductive resin composition comprising a thermoplastic resin or a thermosetting resin, and the inorganic filler composite according to any one of 1 to 6, 9.
  • the content of the thermoplastic resin or thermosetting resin is 30% by volume or more of the total volume of the heat conductive resin composition, and the content of the inorganic filler composite according to any one of 1 to 6 is the heat conductive resin composition
  • the thermally conductive resin composition according to 8 which is 70% by volume or less of the total volume of the product, A heat conductive resin molding obtained by curing the heat conductive resin composition according to 10.8 or 9.
  • the thermally conductive filler used in the present invention is an inorganic compound having a thermal conductivity of 0.8 (W / m ⁇ K) or more.
  • the shape is a powdery inorganic compound composed of at least one of square, granular, fibrous, and flat.
  • the average particle size of the thermally conductive filler is preferably 0.1 to 500 ⁇ m, more preferably a thermally conductive filler having an average particle size of 1 to 200 ⁇ m.
  • These inorganic compounds may be subjected to a surface treatment with a silane coupling agent, an aluminum coupling agent, a titanium coupling agent, or the like, or a surface treatment with an acid, an alkali, an organic compound, or an inorganic compound. Also, the surface may be treated by mechanical processing.
  • Boron nitride used in the present invention is mainly used to improve thermal conductivity, and can be a known and commonly used one, and it is easy to produce an inorganic filler composite composed of boehmite and boron nitride.
  • Tabular grains or aggregates of tabular grains are preferred, and those having an average particle diameter of 0.5 to 100 ⁇ m are particularly preferred. When the average particle size is within this range, it is difficult to produce a composite, and when the average particle size is within this range, it is difficult to exhibit thermal conductivity.
  • Alignum nitride Known and commonly used ones are used, but it is preferably granular with an average diameter of 0.5 to 50 ⁇ m.
  • (Glass) Glass having at least one shape consisting of a granular shape, a rectangular shape, a fibrous shape, and a flat plate shape is preferable.
  • the average particle diameter is preferably 1 to 100 ⁇ m.
  • the fibrous glass is preferably a fibrous glass having a shape with an average diameter of 1 to 20 ⁇ m and an average length of 1 to 5000 ⁇ m.
  • As the flat glass scaly glass having an average particle size in the plane direction of 10 to 4000 ⁇ m and an aspect ratio of the particle size in the plane direction to the thickness of 2 to 2000 is preferably used.
  • alumina there are aluminas having various structures such as ⁇ -alumina, ⁇ -alumina, and ⁇ -alumina. In the present invention, any alumina can be used, or even if the structure is mixed in one particle. There is no problem. Furthermore, alumina silica which is a composite of alumina and silica may be used. The shape is preferably granular or fibrous. The average particle size is preferably 1 to 100 ⁇ m. A fiber having a diameter of 0.1 to 20 ⁇ m and a length of 1 to 5000 ⁇ m is preferably used. (graphite) Either natural or artificial graphite can be used. The shape can be any of granular, square, flat plate and the like.
  • the grain size is 0.1 to 500 ⁇ m in the case of granular or square, and the flat graphite has a mean particle size in the plane direction of 10 to 4000 ⁇ m, and a scale-like shape having an aspect ratio of the grain size in the plane direction to the thickness of 2 to 2000.
  • Magnesium oxide is preferably magnesium oxide that has been fired at a high temperature to improve water resistance, and preferably has a weight increase rate of 10% or less after being left under a saturated water pressure of 121 ° C./24 hrs.
  • the shape can be any of granular, square, and fibrous.
  • the average particle size is preferably 0.1 to 100 ⁇ m.
  • Boehmite The boehmite used in the present invention is mainly used for improving the thermal conductivity, and known and conventional ones can be used.
  • Boehmite is an alumina hydrate, such as mineral boehmite, typically Al 2 O 3 .H 2 O, having a water content of about 15% by mass, and, for example, pseudo-boehmite having 20 to 38% by mass. including.
  • Boehmite (including pseudo-boehmite) has a unique X-ray diffraction pattern and distinguishes it from other aluminum materials, such as other hydrated aluminas, such as the common precursor material aluminum hydroxide. be able to.
  • the boehmite used in the present invention can be produced by heating a commonly known aluminum hydroxide. Although there is no restriction
  • Zinc oxide It is represented by ZnO in the chemical formula, and is also called zinc white.
  • a shape A fibrous form, a granular form, a square shape, and a flat form thing are used preferably. In the case of a granular shape or a rectangular shape, a granular shape having an average particle diameter of 1 to 100 ⁇ m is preferable.
  • the fibrous form is preferably a fibrous form having an average diameter of 1 to 20 ⁇ m and an average length of 1 to 5000 ⁇ m.
  • a scaly shape having an average particle size in the plane direction of 10 to 4000 ⁇ m and an aspect ratio of the plane direction particle size to the thickness of 2 to 2000 is preferably used.
  • the inorganic filler used in the present invention is boehmite having at least one shape of a granular, fibrous, or tabular shape on the surface of a thermally conductive filler that is an aggregate of tabular grains or tabular grains, or It is characterized by being an inorganic filler composite composed of zinc oxide bonded or adhered.
  • the bond or adhesion used here is a thermally conductive filler after molding by a known method using a resin composition in which the inorganic filler composite of the present invention is dispersed in a resin by a known method, It means a state in which boehmite or zinc oxide is firmly attached and not separated.
  • the resin and the filler of the present invention are dispersed using an extruder or the like, and then the resin component is dissolved and filtered with a solvent.
  • a method of separating only the filler complex and confirming with a scanning electron microscope (SEM) or the like or a method of directly observing the filler with a transmission electron microscope-electron beam energy loss spectroscopy (TEM-EELS) or the like.
  • SEM scanning electron microscope
  • TEM-EELS transmission electron microscope-electron beam energy loss spectroscopy
  • the inorganic filler composite of the present invention is constituted by bonding or adhering boehmite or zinc oxide to the surface of the thermally conductive filler.
  • the mode of this bonding or adhesion is unknown, but it can be produced by heating an aluminum compound such as aluminum hydroxide or a zinc compound such as zinc nitrate and a thermally conductive filler in an aqueous solution, and the resulting composite As shown in FIG. 1 and FIG. 2, boehmite or zinc oxide is present in a form firmly adhered on the surface of the thermally conductive filler.
  • the temperature is 50 to 300 ° C. in an autoclave. It is manufactured by bringing the components into a pressurized state within a range and reacting (hydrothermal synthesis) those components.
  • boron nitride used by this invention A well-known thing is used as boron nitride used by this invention. That is, hexagonal or cubic boron nitride mainly composed of boron and nitrogen. In particular, hexagonal boron nitride produced by a normal pressure method is preferably used. Boron nitride is produced by a known method.
  • the invention is not particularly limited to this.
  • the surface of the thermally conductive filler of the present invention may contain an organic functional group such as amino group, hydroxyl group, carboxyl group, isocyanate group, epoxy group, unsaturated group.
  • organic functional groups such as amino group, hydroxyl group, carboxyl group, isocyanate group, epoxy group, unsaturated group.
  • surface treatment agents include coupling agents containing silicon, aluminum, titanium, etc., anionic and cationic surfactants or dispersants containing phosphorus atoms, or epoxy groups, amino groups, isocyanate groups, unsaturated groups,
  • the inorganic filler composite of the present invention is obtained by hydrothermally synthesizing boehmite or zinc oxide raw material components in the presence of the above-described heat conductive filler to obtain a heat conductive filler and boehmite or zinc oxide composite.
  • a hydrothermal synthesis method to obtain boehmite (1) A method of hydrolyzing an aluminum alkoxide compound in the presence of an organic or inorganic acidic catalyst to obtain aluminum hydroxide, and then hydrothermally heating the obtained aluminum hydroxide in an autoclave.
  • a method of hydrothermally synthesizing aluminum compounds such as aluminum chloride and aluminum sulfate in an autoclave (3) A method of hydrothermal synthesis as an aluminum hydroxide raw material may be mentioned, but any method may be used.
  • a hydrothermal synthesis method using aluminum hydroxide as a raw material is preferably used for controlling the size and shape of boehmite.
  • Aluminum hydroxide includes gibbsite type and buyer light type, but any aluminum hydroxide cannot be used.
  • a method for obtaining zinc oxide a known method is used, but it is preferable to use a water-soluble inorganic zinc compound.
  • a hydrate of zinc nitrate is preferably used.
  • the shape of the boehmite and zinc oxide components it is desirable to control the shape of the boehmite and zinc oxide components.
  • a method of controlling the shape of the boehmite component (1) A method of controlling the pH of water, which is a medium component during hydrothermal synthesis, to a specific value, (2) A hydrothermal synthesis method may be used in the presence of inorganic or organic compounds such as magnesium compounds, sodium compounds, calcium compounds, barium compounds, strontium compounds, cerium compounds. These methods are arbitrarily used according to the shape of the boehmite component in the inorganic filler composite of the present invention.
  • the shape of the boehmite component of the inorganic filler composite of the present invention can be any of granular, fibrous, rectangular and flat shapes, but preferred shapes include fibrous and flat shapes.
  • fibrous boehmite it is preferable to use magnesium compounds such as magnesium hydroxide, magnesium oxide, magnesium chloride, magnesium carbonate, magnesium sulfate, magnesium nitrate, magnesium acetate, magnesium borate, magnesium formate and magnesium phosphate.
  • magnesium compounds such as magnesium hydroxide, magnesium oxide, magnesium chloride, magnesium carbonate, magnesium sulfate, magnesium nitrate, magnesium acetate, magnesium borate, magnesium formate and magnesium phosphate.
  • sodium compounds such as sodium sulfate, sodium sulfite, sodium carbonate, sodium hydroxide, sodium acetate and sodium chloride.
  • a calcium compound, a strontium compound, a barium compound, a cerium compound or the like may be used.
  • zinc oxide it is preferable to use an inorganic compound that becomes the nucleus of growth, and in the case of fibrous zinc oxide, it is preferable to use a colloidal aqueous dispersion made of pseudoboehmite.
  • the inorganic filler composite of the present invention can be obtained by hydrothermal synthesis in an autoclave when the above-described raw materials are performed at 100 ° C. or higher.
  • the temperature for the hydrothermal synthesis is preferably 50 to 300 ° C, more preferably 70 to 300 ° C.
  • a preferable temperature is 130 ° C to 300 ° C. If it is less than 130 ° C., the hydrolysis of aluminum hydroxide does not proceed sufficiently, and boehmite does not grow sufficiently. If it exceeds 300 ° C., boehmite having a sufficient crystal structure is not generated.
  • Hydrothermal synthesis is usually performed for 3 to 30 hours. When it is less than 3 hours, hydrolysis of the aluminum hydroxide salt is insufficient and boehmite does not grow sufficiently. Also, hydrothermal treatment exceeding 30 hours is not economical in production.
  • the inorganic filler composite of the present invention is hydrothermal synthesis, water is used as a medium.
  • the concentration during hydrothermal synthesis is 5 to 50% by mass, preferably 10 to 40% by mass.
  • the shape of the thermally conductive filler of the inorganic filler composite of the present invention is preferably such that the average particle size of the thermally conductive filler is 0.1 to 500 ⁇ m. If it is 0.1 ⁇ m or less, the thermal conductivity is not improved, and if it exceeds 500 ⁇ m, the physical properties of the molded product are remarkably lowered.
  • the shape of boehmite or zinc oxide is preferably granular, square, or flat. When the particle size of the granular or square boehmite is less than 0.01 ⁇ m, the thermal conductivity is not improved, and when it is 100 ⁇ m or more, the strength of the finally obtained resin composition is significantly reduced.
  • the size of the fibrous boehmite or zinc oxide is preferably a fibrous boehmite having a diameter of 0.05 to 50 ⁇ m and an aspect ratio of 1 to 1000. If the diameter is less than 0.05 ⁇ m and the aspect ratio is less than 1, there is no effect of improving thermal conductivity, and if the diameter exceeds 50 ⁇ m and the aspect ratio exceeds 1000, the molding fluidity of the finally obtained resin composition is significantly impaired. It is not preferable.
  • the flat boehmite or zinc oxide preferably has a diameter of 0.05 to 50 ⁇ m and an aspect ratio of 10 or more. If the diameter is less than 0.05 ⁇ m and the aspect ratio is less than 10, the effect of improving thermal conductivity is small, and if the diameter exceeds 50 ⁇ m, the strength of the resulting resin composition is remarkably lowered, which is not preferable.
  • the heat conductive resin composition of this invention is comprised by including a thermoplastic resin or a thermosetting resin, and the said inorganic filler composite_body
  • thermoplastic resins include, for example, polypropylene (PP) resin, polystyrene, acrylonitrile-butadiene-styrene copolymer resin (ABS), polyamide (PA6, PA66 etc.) resin, polyester (PET, PBT etc.) resin, polycarbonate ( PC) resin, liquid crystal polyester (LCP) resin, polyphenylene sulfide (PPS) resin, polyphenylene ether resin, polysulfone resin, polyether ether ketone resin, etc. with excellent heat resistance, mechanical strength, chemical resistance and processability Can be mentioned.
  • PP polypropylene
  • ABS acrylonitrile-butadiene-styrene copolymer resin
  • PA6 PA66 etc. polyamide
  • polyester PET, PBT etc.
  • PC polycarbonate
  • LCP liquid crystal polyester
  • PPS polyphenylene sulfide
  • PPS polyphenylene sulfide
  • PES polyphenylene ether resin
  • thermosetting resins examples include liquid thermosetting resins such as epoxy resins; radical polymerization thermosetting resins such as unsaturated polyester resins, polyimide resins, polyurethane resins, and vinyl ester resins; Used. Moreover, a hardening
  • the amount of the inorganic filler composite of the present invention to be used with respect to the resin is 10 to 70% by volume in terms of volume%. Preferably, it is 20 to 60% by volume.
  • the blending amount of the inorganic filler composite is less than 10% by volume, sufficient thermal conductivity cannot be obtained.
  • it exceeds 70% by volume the molding fluidity is remarkably lowered and the mechanical properties are lowered, making it difficult to use in practical use.
  • the inorganic filler composite of the present invention may be used in combination with a thermal conductive filler that is a raw material inorganic filler, boehmite of various shapes, or zinc oxide alone. Further, it may be used in combination with one or more other fillers.
  • Preferred inorganic fillers that can be used in combination are aluminum hydroxide, magnesium oxide, boehmite, zirconia, aluminum oxide, mullite, silicon carbide, silicon nitride, aluminum nitride, wollastonite, boron nitride, magnesium sulfate, titanium oxide, magnesium carbonate, calcium carbonate , Bentonite, montmorillonite, mica, synthetic mica, talc, graphite powder, carbon nanotube, glass fiber, aramid fiber, carbon fiber, graphite fiber, and various metal powders.
  • the shape of these fillers may be any shape such as granular, fibrous, or flat. The shape, particle size, aspect ratio, etc. can be appropriately selected and used according to the purpose.
  • additives can be used in combination when producing the resin composition.
  • Additives include antioxidants, heat stabilizers, light stabilizers, polymerization inhibitors, UV absorbers, lubricants, dispersants, mold release agents, plasticizers, organic or inorganic colorants, antistatic agents, copper Examples thereof include harm prevention agents, water repellents, silane coupling agents, titanium coupling agents, and aluminum coupling agents.
  • thermoplastic resin composition preparation of thermal conductive resin composition
  • dissolved in the solvent the method of melt-kneading using the said inorganic filler composite body, the said thermoplastic resin, a twin screw extruder, etc.
  • a method for synthesizing a thermoplastic resin can be mentioned below.
  • thermosetting resin a method of directly stirring and mixing a liquid resin or a resin dissolved in a solvent using a disper, a homogenizer, etc., a method of synthesizing a thermosetting resin in the presence of the present inorganic filler composite, .
  • the molded body using the thermally conductive resin composition obtained in the present invention is an inorganic filler composite of a thermally conductive filler and various shapes of boehmite or zinc oxide, so that each of them contains not a composite but a thermal conductive. Compared to a molded body obtained from the conductive resin composition, it has a characteristic of excellent thermal conductivity. Moreover, the molded object of this invention has the characteristics with few differences in thermal conductivity by the direction of a molded object.
  • the molded product obtained from the heat conductive resin composition of the present invention is obtained from the heat conductive resin composition containing each of them, not the composite, by using the inorganic filler composite of the present invention. It became clear that it has the characteristic which is excellent in heat conductivity compared with a molded object.
  • the molded article of the present invention has a feature that there is little difference in thermal conductivity depending on the direction of the molded article, and in particular, has a feature of high thermal conductivity in the thickness direction that is perpendicular to the flow direction. It became.
  • a sample for measuring the flow direction thermal conductivity is a section obtained by cutting the injection molded product of FIG. 5 from the above-mentioned molded plate as shown in the test piece for measuring the flow direction thermal conductivity, as shown in FIG.
  • the samples were bonded so as to be 10 mm ⁇ width 8 to 10 mm ⁇ thickness 2 mm to obtain a sample for measuring the thermal conductivity in the flow direction.
  • the thermal conductivity in the arrow direction (resin flow direction) in FIG. 6 was measured and used as the flow direction thermal conductivity.
  • Thickness direction thermal conductivity measurement As shown in the thickness direction thermal conductivity measurement test piece, a test piece cut into a size of 8 to 10 mm in length, 8 to 10 mm in width, and 2 mm in thickness was obtained. The thickness direction thermal conductivity measurement test piece was used (FIG. 7), the thermal conductivity in the direction of the arrow shown in FIG. 7 was measured, and the thickness direction thermal conductivity was obtained.
  • the thermal conductivity was measured by using a Xenon flash laser analyzer LFA447 manufactured by Bruca Ax Co., Ltd., and the thermal diffusivity was measured.
  • FIG. 9 shows an enlarged view of the BN-BM coupling part in FIG. As is clear from FIGS. 10 and 11, no clear boundary line was observed between BN and BM, and it was confirmed that BN and fibrous BM were bonded.
  • Example 1 The above BN-BM composite-A and high density polyethylene (HDPE) having a density of 0.96 g / cm 3 were used as the thermoplastic resin and mixed according to the formulation shown in Table-3. The mixture was melt kneaded at a cylinder temperature of 160 ° C. using a twin screw extruder TEM-37 (manufactured by Toshiba Machine) to obtain pellets for injection molding. After the obtained pellets were dried at 90 ° C. for 4 hours, a test for heat conduction measurement shown in FIG. 5 was performed using an injection molding machine Cycap 75 (manufactured by Sumitomo Heavy Industries) at a cylinder temperature of 180 ° C. and a mold temperature of 40 ° C.
  • Cycap 75 manufactured by Sumitomo Heavy Industries
  • the piece was injection molded to produce a test piece for measuring thermal conductivity, and the thermal conductivity was measured.
  • the specific heat and density of the molded product necessary for obtaining the thermal conductivity from the obtained thermal diffusivity were obtained by calculation since the additivity of components generally holds. The following values were used for the density and specific heat of each component.
  • Example 2 Using BN-BM composite-A, injection molding was carried out in the same manner as in Example 1 with the formulations shown in Tables 1 and 2, and the thermal conductivity was measured. The results are shown in Table 3.
  • Example 3 Polyamide 6 having a specific gravity of 1.14 (product name: 1011FB, manufactured by Ube Industries) and BN-BM composite-B were used as the thermoplastic resin and blended according to the formulation shown in Table-3. After mixing the compound until uniform, it is melt kneaded at a cylinder temperature of 240 ° C using a twin screw extruder TEM-37 (manufactured by TOSHIBA MACHINE), pelletized for injection molding, and immediately put into a paper bag with aluminum interior. , Heat sealed and sealed. After the obtained pellets were dried at 100 ° C. for 4 hours, a test for heat conduction measurement shown in FIG.
  • Example 5 Using polybutylene terephthalate (hereinafter PBT product name Novaduran 5008, manufactured by Mitsubishi Engineering Plastics) as a thermoplastic resin, the mixture shown in Table 3 was mixed until uniform, and then a twin screw extruder TEM-37 (manufactured by Toshiba Machine) was used. It was melt-kneaded at a cylinder temperature of 250 ° C. and pelletized for injection molding. After the obtained pellets were dried at 120 ° C. for 4 hours, the heat conduction measurement test shown in FIG. 5 was performed using an injection molding machine Cycap 75 (manufactured by Sumitomo Heavy Industries) at a cylinder temperature of 250 ° C. and a mold temperature of 40 ° C. Pieces were injection molded.
  • the obtained test piece was cut into a test piece for measuring thermal conductivity as shown in FIGS. 5 and 6, and the thermal conductivity was measured.
  • the density and specific heat of PBT were determined using the following values, and the density and specific heat of the molded product were calculated. PBT density 1.31 g / cm 3 , specific heat 1.24 J / g ⁇ K The results are shown in Table 3.
  • Example 6 Each material was mixed according to the formulation shown in Table 3, and the thermal conductivity was determined in the same manner as in Example 4. The results are shown in Table 3. The density and specific heat of ZnO were determined using the following values, and the density and specific heat of the molded product were obtained by calculation. ZnO density 5.5 g / cm 3 , specific heat 0.50 J / g ⁇ K
  • thermoplastic resin As a thermoplastic resin, a high density polyethylene (HDPE) having a melt flow rate (MFR) of 7.0 g / 10 min and a density of 0.96 g / cm 3 measured at a temperature of 190 ° C. and a load of 2160 g, boron nitride-A and Table-1 A needle-shaped BM (BM-A) shown in Table 4 was used and mixed according to the formulation shown in Table-4. The blend was melt kneaded at a cylinder temperature of 160 ° C. using a twin screw extruder TEM-37 (manufactured by Toshiba Machine) to obtain pellets for injection molding. After the obtained pellets were dried at 90 ° C.
  • HDPE high density polyethylene
  • MFR melt flow rate
  • a test for heat conduction measurement shown in FIG. 5 was performed using an injection molding machine Cycap 75 (manufactured by Sumitomo Heavy Industries) at a cylinder temperature of 180 ° C. and a mold temperature of 40 ° C. Pieces were injection molded. The obtained test piece was cut into a test piece for measuring thermal conductivity as shown in FIGS. 5 and 6, and the thermal diffusivity was measured. The results are shown in Table-4.
  • thermo conductivity was measured in the same manner as in the Examples with the formulation shown in Table 4 without using the thermal conductive particle-BM composite of the present invention.
  • Example 7 The GB-BM composite-B, alumina-BM composite-A, and granular graphite-BM composite-A of the present invention were used and blended in the formulation shown in Table-5. Conductivity was measured. The results are shown in Table-5.
  • the density and specific heat of the glass beads, alumina, and graphite were determined using the following values, and the density and specific heat of the molded product were obtained by calculation. Glass beads density 2.5g / cm 3 , specific heat 0.83J / g ⁇ K Alumina density 3.7 g / cm 3 , specific heat 0.75 J / g ⁇ K Graphite density 2.2g / cm 3 , specific heat 0.84J / g ⁇ K
  • the composition using the inorganic filler composite of the present invention has a feature that is excellent in thermal conductivity as compared with a molded body obtained from a thermally conductive resin composition used without making each composite. Further, the molded article of the present invention has a feature that there is little difference in thermal conductivity depending on the direction of the molded article, and in particular, has a feature of high thermal conductivity in the thickness direction that is perpendicular to the flow direction. It is.
  • a resin composition comprising an inorganic filler composite formed by bonding or adhering boehmite or zinc oxide to the surface of the heat conductive filler of the present invention to a thermoplastic resin or a quenching resin is a heat conductive resin composition It can be used as
  • Test piece for measuring flow direction thermal conductivity 2 Test piece for measuring thickness direction thermal conductivity 3: Flow direction surface 4: Thickness direction surface 5: Thickness direction 6: Right angle direction 7: Flow method 8: Injection molded product 9 : Flow direction surface 10: Measurement direction of flow direction thermal conductivity 11: Measurement direction of thickness direction thermal conductivity

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Abstract

Les compositions de résine classiques ont des inconvénients tels qu'un manque de conductivité de chaleur suffisante ou, de façon à améliorer la conductivité de la chaleur, que la nécessité de l'addition de grandes quantités de charges, ce qui conduit à une aptitude inférieure au moulage. Ainsi, le problème que se propose de résoudre la présente invention est de proposer une composition de résine thermoplastique ayant une bonne aptitude au moulage et de ce fait fournir un article moulé qui présente une excellente conductivité thermique même avec une faible teneur en volume de charge inorganique ajoutée à la composition, et une composition de résine utilisée dans l'article moulé. On résout le problème en fournissant un composite de charge inorganique dans lequel de la boehmite ou de l'oxyde de zinc, qui se présente sous la forme d'au moins l'un parmi sphérique, angulaire, fibreuse ou tabulaire, est lié à ou déposé sur la surface d'une charge conductrice de la chaleur.
PCT/JP2012/073331 2011-09-13 2012-09-12 Composite de charge inorganique, composition de résine conductrice de la chaleur et article moulé WO2013039103A1 (fr)

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