WO2015050263A1 - Composition de résine et élément de dissipation de chaleur comprenant cette dernière - Google Patents

Composition de résine et élément de dissipation de chaleur comprenant cette dernière Download PDF

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WO2015050263A1
WO2015050263A1 PCT/JP2014/076636 JP2014076636W WO2015050263A1 WO 2015050263 A1 WO2015050263 A1 WO 2015050263A1 JP 2014076636 W JP2014076636 W JP 2014076636W WO 2015050263 A1 WO2015050263 A1 WO 2015050263A1
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mass
resin
resin composition
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compound
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PCT/JP2014/076636
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English (en)
Japanese (ja)
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健二 池田
哲郎 土橋
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住友化学株式会社
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Priority to JP2015540578A priority Critical patent/JP6376135B2/ja
Publication of WO2015050263A1 publication Critical patent/WO2015050263A1/fr

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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
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/06—Elements
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
    • H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
    • H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
    • H01L23/3737—Organic materials with or without a thermoconductive filler
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00

Definitions

  • the present invention relates to a resin composition and a heat dissipation component comprising the same.
  • heat sinks made of aluminum-based alloys with high thermal conductivity have been used as heat-dissipating components such as heat sinks for cooling semiconductors such as LED elements and electronic devices used in LED lighting, and heat sinks for large power supplies such as industrial equipment and devices. It is used.
  • Patent Document 1 contains a thermoplastic resin, graphite particles, and a carbon fiber structure, and when the content of the graphite particles and the carbon fiber structure is 100 parts by mass of the thermoplastic resin, A resin composition characterized by 10 parts by mass or more and 300 parts by mass or less and 1 part by mass or more and 80 parts by mass or less is described.
  • Patent Document 2 contains a thermoplastic resin, carbon fiber, and graphite particles having an average particle diameter of more than 12 ⁇ m and not more than 50 ⁇ m, and is 230 ° C. and a load of 2.16 kg according to JIS-K-7210. Describes a resin composition having a melt flow rate of 0.5 g / 10 min to 30 g / 10 min.
  • the heat dissipating parts made of the resin composition described in any of the patent documents have low thermal conductivity, and further improvements have been demanded.
  • the present invention provides a resin composition capable of producing a heat dissipation component having good thermal conductivity, and a heat dissipation component comprising the resin composition and having good thermal conductivity. Objective.
  • the present invention 20% by mass or more and 59% by mass or less of the thermoplastic resin (A), 1% by mass or more and 10% by mass or less of carbon fiber (B) having a thermal conductivity of 150 W / m ⁇ K or more; A resin composition containing 40% by mass or more and 70% by mass or less of graphite particles (C) (provided that the total amount of (A), (B) and (C) is 100% by mass);
  • the thermoplastic resin (A) is a propylene resin (A1) having a melt flow rate measured at 230 ° C. and a load of 21.18 N of 1.0 g / 10 min to 200 g / 10 min, and 190 ° C. and a load of 21.18 N.
  • a resin composition which is a resin containing an ethylene resin (A2) having a melt flow rate of 5.0 g / 10 min to 300 g / 10 min and a density of 930 kg / m 3 to 990 kg / m 3 And a heat dissipating part comprising the resin composition.
  • A2 ethylene resin
  • the resin composition according to the present invention contains a predetermined amount of each of a thermoplastic resin (A), carbon fiber (B), and graphite particles (C).
  • a thermoplastic resin (A) contained in the resin composition contains a propylene resin (A1) and an ethylene resin (A2).
  • the content of the propylene resin (A1) is 5% by mass or more and 95% by mass or less, and 10% by mass or more when the total amount of the thermoplastic resin (A) is 100% by mass. It is preferably 90% by mass or less, and more preferably 15% by mass or more and 85% by mass or less.
  • the content of the ethylene resin (A2) is 95% by mass or less, 5% by mass or more, and 90% by mass or less when the total amount of the thermoplastic resin (A) is 100% by mass. It is preferably 10% by mass or more, and more preferably 85% by mass or less and 15% by mass or more.
  • the content of the propylene resin (A1) is 95% by mass or less (that is, the content of the ethylene resin (A2) is 5% by mass or more), it is possible to obtain a heat radiation component having a good thermal conductivity. It becomes.
  • the content of the thermoplastic resin (A) is 20% by mass or more and 59% by mass or less when the total amount of the thermoplastic resin (A), the carbon fiber (B) and the graphite particles (C) is 100% by mass. Yes, it is preferably 26 mass% or more and 56 mass% or less, and more preferably 28 mass% or more and 55 mass% or less.
  • the content of the thermoplastic resin (A) is 20% by mass or more, the impact resistance of the heat dissipation component can be improved.
  • the heat radiating component with favorable heat conductivity can be obtained by making content of a thermoplastic resin (A) into 59 mass% or less.
  • a propylene resin (A1) is resin which contains the structural unit derived from propylene exceeding 50 mass%.
  • the propylene resin (A1) includes a propylene homopolymer; a structural unit derived from at least one comonomer selected from the group consisting of ethylene and an ⁇ -olefin having 4 to 10 carbon atoms, and a structural unit derived from propylene.
  • a propylene copolymer a structural unit derived from at least one comonomer selected from the group consisting of ethylene and an ⁇ -olefin having 4 to 10 carbon atoms in a propylene homopolymer matrix, and a structural unit derived from propylene And a heterophasic polymerized material which is a mixture having a structure in which a copolymer having the above is dispersed. These may be used alone or in combination of two or more.
  • the content of structural units derived from at least one comonomer selected from the group consisting of ethylene and an ⁇ -olefin having 4 to 10 carbon atoms in the propylene copolymer and the heterophasic polymerization material is 0.01% by mass.
  • the content is preferably 20% by mass or less (however, the total amount of each of the propylene copolymer and the heterophasic polymerization material is 100% by mass).
  • Examples of the ⁇ -olefin having 4 to 10 carbon atoms include butene, hexene, octene and the like, butene is preferable.
  • propylene copolymer examples include propylene-ethylene copolymer, propylene-1-butene copolymer, propylene-1-hexene copolymer, propylene-1-octene copolymer, propylene-ethylene- Examples thereof include 1-butene copolymer, propylene-ethylene-1-hexene copolymer, and propylene-ethylene-1-octene copolymer. These may be random copolymers or block copolymers.
  • a propylene resin (A1) a propylene homopolymer, a propylene-ethylene copolymer, a propylene-1-butene copolymer, or a propylene-ethylene-1-butene copolymer is preferably used, and a propylene homopolymer is used. It is more preferable.
  • the melt flow rate of the propylene resin (A1) measured at 230 ° C. and a load of 21.18 N is 5.0 g / 10 min to 200 g / 10 min, preferably 10 g / 10 min to 150 g / 10 min. Yes, more preferably from 20 g / 10 min to 120 g / 10 min.
  • a resin composition having appropriate fluidity can be obtained, and by setting the melt flow rate to 200 g / 10 min or less, the impact resistance of the heat radiation component Can be improved.
  • Propylene resin (A1) can be produced by a known polymerization method using a polymerization catalyst.
  • the polymerization catalyst include a Ziegler type catalyst system, a Ziegler-Natta type catalyst system, a catalyst system comprising a transition metal compound of Group 4 of the periodic table having a cyclopentadienyl ring and an alkylaluminoxane, and a cyclopentadienyl ring.
  • Examples thereof include a catalyst system comprising a transition metal compound of Group 4 of the periodic table, a compound that reacts with the transition metal compound to form an ionic complex, and an organoaluminum compound.
  • a prepolymerized catalyst prepared by prepolymerizing ethylene or ⁇ -olefin in the presence of the above catalyst system may be used.
  • these catalyst systems include JP-A-61-218606, JP-A-61-287904, JP-A-5-194585, JP-A-7-216017, and JP-A-9-316147.
  • catalyst systems described in JP-A-10-212319 and JP-A-2004-182981 are examples of these catalyst systems described in JP-A-10-212319 and JP-A-2004-182981.
  • Examples of the polymerization method include bulk polymerization, solution polymerization, slurry polymerization, and gas phase polymerization.
  • Bulk polymerization is a method in which polymerization is performed using a liquid olefin as a medium at the polymerization temperature
  • gas phase polymerization is a method in which a gaseous monomer is used as a medium and a gaseous monomer is contained in the medium. This is a polymerization method.
  • These polymerization methods may be either batch type or continuous type, and these polymerization methods may be arbitrarily combined.
  • a production method by a continuous gas phase polymerization method, a bulk-gas phase polymerization method in which a bulk polymerization method and a gas phase polymerization method are continuously performed is preferable.
  • Various conditions in the polymerization step may be appropriately determined.
  • the heterophasic polymer material used as the propylene resin (A1) is a propylene homopolymer produced in the preceding polymerization step, and composed of propylene, ethylene, and an ⁇ -olefin having 4 to 10 carbon releases in the latter polymerization step. It is preferable to produce using a method of polymerizing at least one comonomer selected from the group, a so-called “multistage polymerization method”.
  • the isoform measured by 13 C-NMR of the portion produced by homopolymerization of propylene (the portion produced by propylene homopolymerization)
  • the tactic pentad fraction is preferably 0.95 or more, more preferably 0.98 or more.
  • the isotactic pentad fraction is a fraction of the propylene monomer unit at the center of the isotactic chain in the pentad unit in the propylene polymer molecular chain, in other words, 5 propylene monomer units. It is the fraction of propylene monomer units in a continuously meso-bonded chain (hereinafter referred to as mmmm).
  • the method for measuring the isotactic pentad fraction is as follows. It is the method described by Zambelli et al., Macromolecules, 6, 925 (1973), that is, the method measured by 13 C-NMR.
  • the ratio of the area of the NMR peak attributed to mmmm to the area of the absorption peak of the methyl carbon region measured by 13 C-NMR spectrum is the isotactic pentad fraction.
  • ethylene resin (A2) is resin containing 50 mass% or more of structural units derived from ethylene.
  • the ethylene resin (A2) is an ethylene homopolymer; an ethylene copolymer having a structural unit derived from ethylene, a structural unit derived from propylene, and a structural unit derived from an ⁇ -olefin having 4 to 10 carbon atoms. Is mentioned. These may be used alone or in combination of two or more.
  • the content of the structural unit derived from the ⁇ -olefin having 4 to 10 carbon atoms in the ethylene copolymer is preferably 0.01% by mass or more and 20% by mass or less (provided that the total amount of the ethylene copolymer is 100%). (Mass%).
  • Examples of the ⁇ -olefin having 4 to 10 carbon atoms include butene, hexene, octene and the like, butene is preferable.
  • ethylene copolymer examples include an ethylene-propylene copolymer, an ethylene-butene-1 copolymer, an ethylene-pentene-1 copolymer, an ethylene-hexene-1 copolymer, an ethylene-octene-1 copolymer, And ethylene-4-methyl-pentene-1.
  • the density of the ethylene resin (A2) is at 930 kg / m 3 or more 990kg / m 3 or less, preferably not more than 940 kg / m 3 or more 980 kg / m 3, more preferably 950 kg / m 3 or more 965 kg / m 3 or less is there.
  • the density of the ethylene resin (A2) is measured according to the method defined in Method A in JIS K7112-1980 after annealing described in JIS K6760-1995.
  • the melt flow rate of the ethylene resin (A2) measured at 190 ° C. and a load of 21.18 N is 5.0 g / 10 min to 300 g / 10 min, preferably 10 g / 10 min to 250 g / 10 min. More preferably, it is 20 g / 10 min or more and 200 g / 10 min or less.
  • an appropriately fluid resin composition can be obtained.
  • the melt flow rate By setting the melt flow rate to 300 g / 10 min or less, the heat resistance of the heat dissipation component It becomes possible to improve impact properties.
  • the ethylene resin (A2) can be produced using a known method.
  • Examples of such a method include polymerization using a catalyst containing a transition metal atom.
  • a catalyst containing a transition metal atom a transition metal compound (a), a composition comprising a transition metal compound (a) and an activator (b), and a transition metal compound (a) and an activator
  • carrier (c) is mentioned.
  • transition metal compound (a) examples include a transition metal compound containing a group 3-11 of the periodic table or a lanthanoid series transition metal atom, a halogen atom, and a group having a cyclopentadiene-type anion skeleton or a group containing a hetero atom. Can be mentioned. When there are a plurality of these groups, they may be the same or different.
  • a group having a cyclopentadiene type anion skeleton, a group having a cyclopentadiene type anion skeleton and a group containing a hetero atom, or a group containing a hetero atom may be directly connected to each other, such as a carbon atom, silicon It may be linked via a residue containing an atom, nitrogen atom, oxygen atom, sulfur atom or phosphorus atom.
  • Examples of the group having a cyclopentadiene-type anion skeleton include a substituted or unsubstituted cyclopentadienyl group, indenyl group, hydroindenyl group, and fluorenyl group.
  • Examples of the hetero atom in the group containing a hetero atom include an oxygen atom, a sulfur atom, a nitrogen atom, and a phosphorus atom. Examples of such a group include an alkoxy group, an aryloxy group, a thioalkoxy group, a thioaryloxy group, and an amino group.
  • the activator (b) may be any one that can activate the transition metal compound (a) and form an ion pair.
  • Examples of the activator (b) include organoaluminum compounds, organoaluminum oxy compounds, boron compounds, clay minerals, sulfonates, carboxylic acid derivatives, surface-treated solid oxides or halides. These compounds may be used alone or in combination of two or more.
  • Examples of the carrier (c) include inorganic substances such as inorganic oxides, clays and clay minerals, and particulate organic polymers.
  • examples of the inorganic oxide include SiO 2 , Al 2 O 3 , MgO, ZrO 2 , TiO 2 , B 2 O 3 , CaO, ZnO, BaO, ThO 2 , and mixtures thereof.
  • clay or clay mineral examples include kaolin, bentonite, kibushi clay, gyrome clay, allophane, hysinger gel, bayophyllite, talc, unmo group, montmorillonite group, vermiculite, ryokdeite group, palygorskite, kaolinite, nacrite, dickite, Halloysite and the like.
  • carrier (c) those subjected to surface treatment or chemical treatment as necessary may be used.
  • the catalyst containing a transition metal atom examples include a solid catalyst component prepared by using a transition metal compound in Group 4 to 6 of the periodic table and an organometallic compound of Group 1, 2, or 13 metal in the periodic table. Examples include so-called Ziegler-Natta catalysts.
  • Examples of the polymerization method used for producing the ethylene resin (A2) include a slurry polymerization method, a gas phase polymerization method, and a solution polymerization method using the catalyst containing the transition metal atom.
  • the polymerization conditions such as polymerization temperature, polymerization time, polymerization pressure and monomer concentration are not particularly limited. Moreover, you may coexist components, such as surfactant, an antistatic agent, and an electron-donating compound, in a polymerization reaction system as needed.
  • the thermal conductivity of the carbon fiber (B) used in the present invention is 150 W / m ⁇ K or more, preferably 200 W / m ⁇ K or more. When the thermal conductivity of the carbon fiber (B) is less than 150 W / m ⁇ K, the thermal conductivity of the resin composition may decrease.
  • the thermal conductivity of the carbon fiber (B) is preferably as high as possible from the viewpoint of imparting heat radiation performance, but is usually 1950 W / m ⁇ K or less, and usually 800 W / m ⁇ K or less from the viewpoint of availability. It is. From the viewpoint of thermal conductivity, pitch-based carbon fibers are preferable, and specific examples include trade name DIALEAD manufactured by Mitsubishi Plastics Co., Ltd.
  • the surface of this carbon fiber (B) may be treated with a sizing agent.
  • the sizing agent include polyolefin, polyurethane, polyester, acrylic, epoxy resin, starch, vegetable oil and the like.
  • the sizing agent may contain a surface treatment agent such as acid-modified polyolefin and silane coupling agent, and a lubricant such as paraffin wax.
  • the method for treating the carbon fiber (B) with a sizing agent include a method of immersing the carbon fiber (B) in an aqueous solution in which the sizing agent is dissolved, a method of applying the aqueous solution to the fiber by spraying, and the like.
  • the number average fiber length of the carbon fibers (B) in the resin composition in the present invention is preferably 0.5 mm or more, and more preferably 0.7 mm or more. By setting the fiber length in such a range, the thermal conductivity of the resin composition can be made higher than the thermal conductivity of the resin composition containing carbon fibers having a number average fiber length of less than 0.5 mm.
  • the number average fiber length (unit: mm) of the carbon fibers is a method described in JP-A No. 2002-5924, in which the resin is removed from the sample for evaluation by a Soxhlet extraction method (solvent: xylene) and the fibers are recovered. Can be measured.
  • the fiber diameter of carbon fiber (B) is 5 micrometers or more, and it is more preferable that it is 7 micrometers or more.
  • the content of the carbon fiber (B) is 1% by mass or more and 10% by mass or less when the total amount of the thermoplastic resin (A), the carbon fiber (B), and the graphite particles (C) is 100% by mass. More preferably, it is 2 mass% or more and 9 mass% or less.
  • the graphite constituting the graphite particles (C) used in the present invention may be either artificial graphite or natural graphite. Specifically, trade name CB-150 manufactured by Nippon Graphite Industry Co., Ltd. can be mentioned.
  • the average particle diameter of the graphite particles (C) is preferably more than 12 ⁇ m and 50 ⁇ m or less, and more preferably 19 ⁇ m or more and 40 ⁇ m or less. By making the average particle diameter larger than 12 ⁇ m, it becomes possible to improve the fluidity of the resin composition, and by setting the average particle diameter to 50 ⁇ m or less, the thermal conductivity of the heat dissipation component is improved.
  • the average particle diameter can be measured using a laser scattering type particle size distribution measuring apparatus.
  • the content of the graphite particles (C) is 40% by mass or more and 70% by mass or less when the total amount of the thermoplastic resin (A), the carbon fiber (B), and the graphite particles (C) is 100% by mass. 42 mass% or more and 65 mass% or less is preferable, and 43 mass% or more and 63 mass% or less is more preferable.
  • the melt flow rate (MFR) of the resin composition according to the present invention is from 0.1 g / 10 min to 30 g / 10 min, preferably from 0.2 g / 10 min to 25 g / 10 min, more preferably. Is 0.3 g / 10 min or more and 20 g / 10 min or less.
  • the melt flow rate is a value measured at a measurement temperature of 230 ° C. and a load of 21.18 N in accordance with the method defined in JIS K7210.
  • the resin composition contains an adsorbent (D), an antioxidant (E), at least one compound (F) selected from the following compound group S, and the like. You may let them.
  • the compound group S is represented by a compound represented by the general formula C n H n-2 (OH) n (wherein n represents an integer of 4 or more), the following alkoxy compound, and the following formula (2). It is a group of compounds consisting of a compound, trehalose, sucrose, lactose, maltose, meletitose, stachyose, curdlan, glycogen, glucose and fructose.
  • An alkoxy compound is a compound in which a hydrogen atom of at least one hydroxyl group of a hydroxyl group contained in a compound represented by the following formula (1) is substituted with an alkyl group having 1 to 12 carbon atoms, and the formula (1) Is a compound containing one aldehyde group or one ketone group and m-1 hydroxyl groups.
  • C m H 2m O m (1) In the formula, m represents an integer of 3 or more.) (In the formula, p represents an integer of 2 or more.)
  • the adsorbent (D) is at least one compound selected from the group consisting of calcium hydroxide, zeolite, and hydrotalcite. Among these, it is preferable to use calcium hydroxide because fogging resistance can be improved with a smaller amount of use.
  • the average particle diameter of calcium hydroxide used as the adsorbent (D) is preferably 0.1 ⁇ m or more and 150 ⁇ m or less, and more preferably 1 ⁇ m or more and 10 ⁇ m or less. By setting the average particle diameter within this range, the adsorbent (D) can be uniformly dispersed in the resin composition.
  • the average particle diameter can be measured using a laser scattering type particle size distribution measuring apparatus.
  • the content of the adsorbent (D) is 100 parts by mass with respect to the total amount of the thermoplastic resin (A), carbon fiber (B), and graphite particles (C). And 0.05 parts by mass or more and 1 part by mass or less, and preferably 0.2 parts by mass or more and 1 part by mass or less.
  • antioxidant (E) a known antioxidant can be used.
  • phenolic antioxidants, hydroquinone antioxidants, sulfur antioxidants, phosphorus antioxidants and the like can be mentioned. These may be used alone or in combination of two or more, and it is preferable to use a phenolic antioxidant and a phosphorus antioxidant alone or in combination.
  • phenolic antioxidants examples include alkylated monophenols, alkylthiomethylphenols, alkylidene bisphenols and derivatives thereof, acylaminophenol derivatives, and ⁇ - (3,5-di-tert-butyl-4-hydroxyphenyl) propionic acid.
  • hydroquinone antioxidant examples include hydroquinone, 2,6-di-tert-butyl-4-methoxyphenol, 2,5-di-tert-butylhydroquinone, 2,5-di-tert-amylhydroquinone, 2,6-diphenyl-4-octadecyloxyphenol, 2,6-di-tert-butylhydroquinone, 2,5-di-tert-butyl-4-hydroxyanisole, 3,5-di-tert-butyl-4- Examples include hydroxyphenyl stearate, bis (3,5-di-tert-butyl-4-hydroxyphenyl) adipate and mixtures thereof.
  • sulfur-based antioxidant examples include 2,4-bis [(octylthio) methyl] -O-cresol, 4,6-bis (dodecylthiomethyl) -O-cresol, dilauryl 3,3′-thiodipropio.
  • phosphorus antioxidants include triphenyl phosphite, tris (nonylphenyl) phosphite, tris (2,4-di-tert-butylphenyl) phosphite, 6- [3- (3-tert-butyl).
  • Content of antioxidant (E) is 0.05 mass part or more and 1 mass part or less with respect to 100 mass parts of total amounts of the said thermoplastic resin (A), carbon fiber (B), and graphite particle (C). It is preferable that it is 0.1 mass part or more and 0.5 mass part or less.
  • the compound (F) is at least one compound selected from the following compound group S.
  • the compound group S is represented by a compound represented by the general formula C n H n-2 (OH) n (wherein n represents an integer of 4 or more), the following alkoxy compound, and the following formula (2). It is a group of compounds consisting of a compound, trehalose, sucrose, lactose, maltose, meletitose, stachyose, curdlan, glycogen, glucose and fructose.
  • An alkoxy compound is a compound in which a hydrogen atom of at least one hydroxyl group of a hydroxyl group contained in a compound represented by the following formula (1) is substituted with an alkyl group having 1 to 12 carbon atoms, and the formula (1) Is a compound containing one aldehyde group or one ketone group and m-1 hydroxyl groups.
  • C m H 2m O m (1) In the formula, m represents an integer of 3 or more.) (In the formula, p represents an integer of 2 or more.)
  • N in the general formula of the compound represented by the general formula C n H n-2 (OH) n (hereinafter referred to as compound S1) represents an integer of 4 or more.
  • n is preferably an integer of 5 to 8, and more preferably 6.
  • Compound S1 includes sugar alcohols having 4 or more carbon atoms.
  • Compound S1 may be D-form or L-form, or a mixture of D-form and L-form. Further, it may be optically active or optically inactive.
  • the compound S1 is preferably a sugar alcohol having 6 carbon atoms.
  • the alkoxy form means that the hydrogen atom of at least one hydroxyl group of the hydroxyl group contained in the compound represented by the following formula (1) (hereinafter sometimes referred to as the compound (1)) has 1 to 12 carbon atoms. This is a compound substituted with an alkyl group, and the compound (1) contains one aldehyde group or ketone group and m-1 hydroxyl groups.
  • M of the compound (1) is an integer of 3 or more, preferably 3 to 60, and particularly preferably 6 or 12.
  • Compound (1) has one aldehyde carbonyl group or one ketonic carbonyl group.
  • Compound (1) has m-1 hydroxyl groups.
  • the compound (1) is preferably a monosaccharide, specifically, glycerose, erythrose, threose, ribose, lyxose, xylose, arabinose, aldohexose, allose, talose, gulose, glucose, altrose, mannose, galactose, idose.
  • Monosaccharides having an aldehyde group such as octose monosaccharides having a ketone group such as ketotriose, dihydroxyacetone, ketotetorose, erythrulose, ketopentose, xylulose, ribulose, ketohexose, psicose, fructose, sorbose, tagatose;
  • Compound (1) may be an optically active substance such as D-form or L-form, or an optically inactive substance such as DL-form.
  • D-form or L-form an optically active substance
  • DL-form an optically inactive substance
  • hexoses such as allose, talose, growth, glucose, altrose, mannose, galactose, idose, psicose, fructose, sorbose, tagatose are preferable, and glucose is particularly preferable.
  • the alkoxy form is a compound in which a hydrogen atom of at least one hydroxyl group contained in the compound (1) is substituted with an alkyl group.
  • the alkoxy compound preferably has at least one hydroxyl group. Particularly preferred is an alkoxy compound in which one hydrogen atom of a hydroxyl group contained in the compound (1) is substituted with an alkyl group, and the other group remains a hydroxyl group.
  • the alkyl group has 1 to 12 carbon atoms, preferably 1 or 2, and particularly preferably 1.
  • Preferable alkoxy compounds include, for example, formula (1-2) (Wherein, R represents an alkyl group having 1 to 12 carbon atoms, preferably 5 to 12 carbon atoms).
  • Examples of the compound represented by the formula (1-2) include methyl ⁇ -D-glucopyranoside, methyl ⁇ -D-glucopyranoside, ethyl ⁇ -D-glucopyranoside, ethyl ⁇ -D-glucopyranoside, and n-propyl ⁇ -D.
  • alkyl of compound (1) examples thereof include a method in which hydrogen chloride gas is circulated through an alcohol solution at ⁇ 10 ° C. or more and 25 ° C. or less, for example, a method in which a mixed solution of compound (1), alkyl alcohol and hydrochloric acid is heated to reflux for alkoxylation.
  • methyl ⁇ -D-glucopyranoside, n-octyl ⁇ -D-glucopyranoside, and the like can be obtained from Tokyo Chemical Industry Co., Ltd.
  • p represents an integer of 2 or more, preferably 2 to 6, Particularly preferably, it represents 5.
  • Examples of the compound (2) include 1,2,3-trihydroxycyclopropane, 1,2,3,4-tetrahydroxycyclopentane, 1,2,3,4,5-pentahydroxycyclopentane, 2,3,4,5,6-hexahydroxycyclohexane, 1,2,3,4,5,6,7-heptahydroxycycloheptane, 1,2,3,4,5,6,7,8-octa And hydroxycyclooctane.
  • 1,2,3,4,5,6-hexahydroxycyclohexane such as myo-inositol, epi-inositol, allo-inositol, muco-inositol, neo-inositol, chiro-inositol, scyllo-inositol, etc.
  • myo-inositol and scyllo-inositol represented by the following formula are preferred.
  • the content of at least one compound (F) selected from the compound group S is 100 parts by mass of the total mass of the thermoplastic resin (A), the carbon fiber (B), and the graphite particles (C). On the other hand, it is 0.01 mass part or more and 1 mass part or less, and it is preferable that it is 0.05 mass part or more and 0.5 mass part or less.
  • the resin composition used in the present invention may contain an organic fiber (G).
  • the organic fibers (G) include plant fibers such as polyester fibers, polyamide fibers, polyurethane fibers, polyimide fibers, polyolefin fibers, polyacrylonitrile fibers, and kenaf.
  • the organic fiber (G) is preferably an organic fiber-containing resin composition in which the thermoplastic resin (A), a modified polyolefin modified with an unsaturated carboxylic acid or a derivative thereof, or a resin such as an elastomer is mixed. Used as a thing.
  • Examples of the method for producing the organic fiber-containing resin composition include methods described in JP-A-2006-8995 and JP-A-3-121146.
  • the resin composition of the present invention contains organic fibers (G)
  • the content is 100 parts by mass of the total amount of the thermoplastic resin (A), the carbon fibers (B), and the graphite particles (C). It is preferably 3 parts by mass or more and 10 parts by mass or less, and more preferably 3 parts by mass or more and 5 parts by mass or less.
  • the resin composition of the present invention comprises the above components (D) and (E) in order to improve the processing characteristics, mechanical characteristics, electrical characteristics, thermal characteristics, surface characteristics, light stability and the like of the resin composition.
  • other resins and additives may be contained.
  • the “other resins” include polyolefins modified with unsaturated carboxylic acids or derivatives thereof, and rubbers such as polyolefin elastomers, polyester elastomers, polyurethane elastomers, and polyvinyl chloride elastomers.
  • the additive examples include inorganic fillers, neutralizers, plasticizers, lubricants, mold release agents, adhesion preventing agents, nucleating agents, light stabilizers, flame retardants, pigments, dyes, and the like.
  • the inorganic filler examples include glass fiber, talc, wollastonite, glass flake and the like.
  • the method for producing the resin composition of the present invention is not limited, but the thermoplastic resin (A), carbon fiber (B), graphite particles (C), and adsorbent (D) used as necessary, A method in which an antioxidant (E), a compound (F), an organic fiber (G), a modifier and the like are uniformly mixed using a mixing device such as a Henschel mixer or a tumbler and then melt kneaded using a plasticizing device. Is mentioned. In melt-kneading, it is preferable to appropriately adjust the temperature and agitation of the plasticizing apparatus in order to prevent the carbon fiber (B) from being broken and becoming too short.
  • a resin composition containing organic fibers is prepared in advance as in the method disclosed in Japanese Patent Application Laid-Open No. 2006-8995, and the resin composition and the thermoplastic resin are prepared.
  • Carbon fiber, graphite particles, and optionally modified polyolefin and modifier may be uniformly mixed using a mixing device such as a Henschel mixer or tumbler, and then melt-kneaded using a plasticizing device. .
  • the plasticizing device is a device that heats a thermoplastic resin to a temperature higher than its melting point and stirs the thermoplastic resin in a molten state.
  • a Banbury mixer for example, a single-screw extruder, a twin-screw co-rotating extruder (for example, TEM [registered trademark] manufactured by Toshiba Machine Co., Ltd., TEX [registered trademark] manufactured by Nippon Steel Works, Ltd., etc.) can be used.
  • 2 axis different direction rotary extruder Kobe Steel Works Co., Ltd. FCM [registered trademark], Nippon Steel Works Co., Ltd. CMP [registered trademark] etc.
  • the heat dissipation component according to the present invention is obtained by molding the above resin composition.
  • the molding method is not particularly limited, and molding can be performed using methods such as extrusion molding, injection molding, compression molding, and blow molding.
  • the heat radiating component include a lighting fixture component.
  • parts for lighting equipment include a heat sink, a sealing cover, and a shade.
  • the heat radiating component include a heat sink for cooling a semiconductor such as an electronic device, and a heat sink for a large power source such as an industrial device or apparatus.
  • Compound (F) selected from Compound Group S: D-(+)-trehalose dihydrate (manufactured by Tokyo Chemical Industry Co., Ltd.)
  • the evaluation items of the molded articles prepared in Examples and Comparative Examples and the measurement methods thereof are as follows.
  • Melt flow rate (MFR, unit: g / 10 minutes) The melt flow rate was measured according to JIS K7210.
  • the melt flow rate of the resin composition and the propylene resin (A1) was measured at a temperature of 230 ° C. and a load of 21.18N.
  • the melt flow rate of the ethylene resin (A2) was measured at a temperature of 190 ° C. and a load of 21.18N.
  • Izod impact strength (Izod, unit: kJ / m 2 ) Using the test pieces (63.5 mm ⁇ 10 mm ⁇ thickness 4 mm) produced in the examples and comparative examples, according to the method defined in JIS K7110, notching was performed after molding to evaluate the notched impact strength. The measurement was performed at a temperature of 23 ° C.
  • Thermal conductivity of the molded body was measured using a laser flash method.
  • Three test pieces (80 mm ⁇ 10 mm ⁇ thickness 4 mm) manufactured in Examples and Comparative Examples were stacked and bonded to obtain a 12 mm thick laminate.
  • Two substantially central portions of the laminate were cut from a direction perpendicular to the bonding surface, and each cut surface was polished to prepare a test piece of 10 mm ⁇ 12 mm ⁇ 1 mm thickness.
  • the thermal conductivity in the in-plane direction of the molded body was determined by a laser flash method thermal constant measuring apparatus (TC-7000, ULVAC-RIKO Co., Ltd.).
  • Example 1 In the ratio shown in Table 1-1 and Table 1-2 below, each component was put in a polyethylene bag and shaken vigorously to mix uniformly, and then a 20 mm single screw extruder VS20-26 made by Tanabe Plastics Machinery was used. After melt-kneading at a cylinder temperature of 240 ° C., it was cut into pellets of about 3 mm.
  • “mass%” is a value when the total amount of the thermoplastic resin (A), carbon fiber (B), and graphite particles (C) is 100 mass%.
  • Mass part is a value when the total amount of the thermoplastic resin (A), the carbon fiber (B), and the graphite particles (C) is 100 parts by mass.
  • the obtained pellets were injection molded using an injection molding machine (Toyo Seiki TOYO SI-30III) at a cylinder temperature of 230 ° C., a mold temperature of 50 ° C., an injection speed of 20 mm / sec, and a holding pressure of 25 MPa.
  • a molded body was obtained.
  • Table 2 shows the evaluation results of the physical properties of this molded body.
  • Example 2 Except that the blending amounts of (A-1), (A-4), (B-1), and (C) used in Example 1 were changed as shown in Table 1-1 and Table 1-2, A molded body was obtained in the same procedure as in Example 1, and its physical properties were evaluated. Table 2 shows the evaluation results of the physical properties of this molded body.
  • Example 3 Except that the blending amounts of (A-1), (A-4), (B-1), and (C) used in Example 1 were changed as shown in Table 1-1 and Table 1-2, A molded body was obtained in the same procedure as in Example 1, and its physical properties were evaluated. Table 2 shows the evaluation results of the physical properties of this molded body.
  • Example 1 The procedure similar to that of Example 1 was followed except that the thermoplastic resin (A-4) was replaced with (A-6) and the amount of (C) was changed as shown in Table 1-1 and Table 1-2. Molded bodies were obtained and their physical properties were evaluated. Table 2 shows the evaluation results of the physical properties of this molded body.
  • Example 4 The molded product was prepared in the same procedure as in Example 1 except that (A-1) and (A-2) were used as the propylene resin (A1) and blended as shown in Table 1 and the ethylene polymer was not blended. Obtained and evaluated its physical properties. Table 2 shows the evaluation results of the physical properties of this molded body.

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Abstract

L'invention porte sur : une composition de résine avec laquelle un élément de dissipation de chaleur ayant une bonne conductivité thermique peut être fabriqué ; et un élément de dissipation de chaleur comprenant la composition de résine. Plus précisément l'invention porte sur une composition de résine contenant 20 % en masse à 59 % en masse d'une résine thermoplastique (A), 1 % en masse à 10 % en masse de fibres de carbone (B), qui ont une conductivité thermique d'au moins 150 W/m∙K, et 40 % en masse à 70 % en masse de particules de graphite (C). (Le poids total de (A), (B) et (C) est fixé à 100 % en masse.) La résine thermoplastique (A) contient : une résine de propylène (A1) ayant un indice de fluage à l'état fondu, mesuré à 230 °C sous une charge de 21,18 N, de 1,0 g/10 min à 200 g/10 min ; et une résine d'éthylène (A2) ayant un indice de fluage à l'état fondu, mesuré à 190 °C sous une charge de 21,18 N, de 5,0 g/10 min à 300 g/10 min et ayant une masse volumique de 930 kg/m3 à 990 kg/m3. L'invention porte en outre sur un élément de dissipation de chaleur comprenant la composition de résine.
PCT/JP2014/076636 2013-10-01 2014-09-29 Composition de résine et élément de dissipation de chaleur comprenant cette dernière WO2015050263A1 (fr)

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JPWO2018123012A1 (ja) * 2016-12-28 2019-10-31 日立化成株式会社 熱伝導シート、熱伝導シートの製造方法及び放熱装置
JP2021050270A (ja) * 2019-09-24 2021-04-01 日本ポリプロ株式会社 ポリプロピレン樹脂組成物
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KR20180133842A (ko) * 2016-04-11 2018-12-17 세키수이 폴리머텍 가부시키가이샤 열전도성 시트
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