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WO2007135749A1 - Composition de résine à conduction thermique élevée - Google Patents

Composition de résine à conduction thermique élevée Download PDF

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Publication number
WO2007135749A1
WO2007135749A1 PCT/JP2006/310821 JP2006310821W WO2007135749A1 WO 2007135749 A1 WO2007135749 A1 WO 2007135749A1 JP 2006310821 W JP2006310821 W JP 2006310821W WO 2007135749 A1 WO2007135749 A1 WO 2007135749A1
Authority
WO
WIPO (PCT)
Prior art keywords
magnesium oxide
parts
phosphorus
weight
resin composition
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2006/310821
Other languages
English (en)
Japanese (ja)
Inventor
Takayuki Miyashita
Satomi Nakada
Takashi Usami
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Polyplastics Co Ltd
Original Assignee
Polyplastics Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Polyplastics Co Ltd filed Critical Polyplastics Co Ltd
Priority to PCT/JP2006/310821 priority Critical patent/WO2007135749A1/fr
Priority to CN200680054686.6A priority patent/CN101448899B/zh
Publication of WO2007135749A1 publication Critical patent/WO2007135749A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances

Definitions

  • the present invention relates to a highly heat conductive resin composition having excellent moldability and heat and heat resistance.
  • PPS Polyphenylene sulfide
  • PAS Polyarylene sulfide represented by resin
  • An object of the present invention is to solve the above-mentioned problems of the prior art, and to provide a material having high thermal conductivity that is free from problems such as screw wear and that is excellent in moldability and wet heat resistance.
  • the present inventors have found that when a specific phosphorus-containing coated magnesium oxide and an alkoxysilane compound are combined with a PAS resin, there is no problem of wear such as screw and molding. As a result, the present invention has been completed.
  • the present invention is a highly heat conductive resin composition
  • a highly heat conductive resin composition comprising 100 to 500 parts by weight of a polyarylene sulfide resin and 100 to 500 parts by weight of a phosphorus-containing coated magnesium oxide and 0.1 to 5 parts by weight of an alkoxysilane compound. is there.
  • the PAS resin used in the present invention has a repeating unit of — (Ar—S) — (wherein Ar is an arylene group), and the c arylene group is, for example, a p-phenylene group. , M-phenylene group, _Phenylene group, substituted phenyl group, p, p '— diphenylsulfone group, p, p' — biphenylene group, p, p '-diphenylene ether group, p, p' — diphenylene A carbonyl group, a naphthalene group, etc. can be used.
  • those having p-phenylene sulfide group as a repeating unit, in which p-phenylene group is used as the arylene group are particularly preferably used.
  • the copolymer two or more different combinations of the arylene sulfide groups consisting of the above-mentioned arylene groups can be used, and among them, p_phenylene sulfide groups and m-phenolic groups can be used.
  • a combination containing a lensulfide group is particularly preferably used.
  • those containing 80 mol% or more are suitable from the viewpoint of physical properties such as heat resistance, fluidity (moldability) and mechanical properties.
  • a high molecular weight polymer having a substantially linear structure obtained by condensation polymerization from a monomer mainly composed of a bifunctional halogen aromatic compound can be particularly preferably used.
  • a partially branched or crosslinked structure is formed by using a small amount of a monomer such as a polyhaloaromatic compound having three or more halogen substituents when polycondensation is performed.
  • a polymer with a relatively low molecular weight is heated at a high temperature in the presence of oxygen or an oxidant to increase the melt viscosity by oxidative crosslinking or thermal crosslinking. It is also possible to use polymers with improved or mixtures thereof.
  • the PAS resin used in the present invention is mainly composed of the linear PAS resin (310 ° C. Shear rate ⁇ OOsec- 1 having a viscosity of 10 to 300 Pa ⁇ s), and a part thereof (1 to 30 weight 0 / 0 , preferably 2 to 25% by weight) Force A mixed system with a branched or crosslinked PAS resin having a relatively high viscosity (300 to 3000 Pa ⁇ s, preferably 500 to 2000 Pa ⁇ s) may be used.
  • the PAS resin used in the present invention is preferably one that has been purified by removing acid by-products, hot water washing, organic solvent washing (or a combination thereof), etc. after polymerization to remove by-product impurities.
  • the high thermal conductive resin composition of the present invention is obtained by blending phosphorus-containing coated magnesium oxide and an alkoxysilane compound with the PAS resin.
  • the phosphorus-containing coated magnesium oxide used in the present invention includes magnesium oxide having a coating layer made of a magnesium phosphate compound, and a covering layer made of a double oxide on the surface, and at least a part of the surface thereof.
  • magnesium oxide having a coating layer made of a double oxide means that at least one element of aluminum, iron, silicon, and titanium and a matrix are formed on the surface of the magnesium oxide.
  • Gnesium Specific examples the mixed oxide, Fuorusuterai preparative (M g S i 4), spinel (A 1 2 M g J, magnesium Blow wells (F e 2 M g O, magnesium titanate (M g T I_ ⁇ 3 Etc., preferably forsterite.
  • magnesium oxide which is a magnesium oxide having a coating layer made of magnesium oxide and a double oxide, which is used for producing phosphorus-containing coated magnesium oxide.
  • Magnesium oxide having the characteristics of the present invention can be produced using a known method such as an electrofusion method or a sintering method.
  • a method for producing magnesium oxide having a coating layer made of a double oxide is to melt at a high temperature in the presence of a compound that forms a double oxide on the surface of the magnesium oxide produced by the above method.
  • the surface is coated with a double oxide.
  • a compound that forms a double oxide is wet-added to the magnesium oxide powder, and then mixed and stirred, or a compound that forms a double oxide is present on the surface of the magnesium oxide. It can be produced by a method of firing at a temperature higher than the melting point of the coating material.
  • the compound used to form the double oxide is preferably one or more compounds selected from the group consisting of aluminum compounds, iron compounds, silicon compounds and titanium compounds.
  • the form of the compound is not limited, but nitrates, sulfates, chlorides, oxynitrates, oxysulfates, oxychlorides, hydroxides, oxides and the like are used. Specific examples of this compound include fumed silica, aluminum nitrate, and iron nitrate.
  • the method for producing a phosphorus-containing coated magnesium oxide is a method in which a magnesium oxide having a coating layer made of magnesium oxide or a double oxide produced by the above method is subjected to a surface treatment with a phosphorus compound, and the surface thereof is converted into a magnesium phosphate compound. A covering layer is formed.
  • Phosphorus compounds used for this surface treatment include phosphoric acid, phosphate, and acidic phosphoric acid.
  • An ester etc. can be mentioned, These may be used individually or may use 2 or more types simultaneously.
  • the phosphate include sodium phosphate, potassium phosphate, and ammonium phosphate.
  • the acidic phosphate ester include isopropyl acid phosphate, methenorea acid phosphate, etheno rare acid phosphate, propyl acid phosphate, and butyl acid. Examples include dophosphate, lauryl urea acid phosphate, stearino rare acid phosphate, 2-ethynolehexyl acid phosphate, and oleyl acid phosphate. Of these, isopropyl acid phosphate is preferred because a coating layer having excellent water resistance can be easily formed.
  • a predetermined amount of phosphorus compound is added to magnesium oxide having a coating layer made of magnesium oxide or a double oxide, and stirred for 5 to 60 minutes, for example. Thereafter, it is baked at a temperature of 300 ° C. or more for 0.5 to 5 hours.
  • Phosphorus-containing coated magnesium oxide produced by such a method is generally available as COOLFILER 1 C F 2-10 O A (Tateho Chemical Co., Ltd.).
  • the addition amount of the phosphorus-containing coated magnesium oxide is important. If the addition amount is too small, the desired thermal conductivity does not appear, and conversely if the addition amount is too large, the moldability is deteriorated. . Therefore, the addition amount of the phosphorus-containing coated magnesium oxide is 100 to 500 parts by weight, preferably 150 to 400 parts by weight with respect to 100 parts by weight of the PAS resin. In addition, the particle size distribution of the phosphorus-containing coated magnesium oxide is also important. If the average particle size is too small, when it is kneaded with a resin, there is a problem that the viscosity is severely increased and the moldability is remarkably lowered.
  • the average particle size and to the 10 ⁇ 50 ⁇ ⁇ , preferably 15 ⁇ 30 ⁇ ⁇ , and the maximum particle size is 300 mu m or less, preferably 150 ⁇ ⁇ below.
  • the alkoxysilane compound used in the present invention is aminoalkoxysilane, vinylanoloxysilane, epoxyanoloxysilane, menolecaptoanoloxysilane. It may be at least one selected from the group consisting of lan and arylalkoxysilanes.
  • a silane compound having one or more amino groups in one molecule and two or three alkoxy groups is also effective.
  • Examples include ⁇ -aminopropyl trimethoxysilane;
  • any silane compound having one or more vinyl groups in one molecule and having two or three alkoxy groups is effective.
  • any silane compound having one or more epoxy groups in one molecule and two or three alkoxy groups is effective, for example, ⁇ -glycidoxypropyl trimethyl.
  • a silane compound having one or more mercapto groups in one molecule and having two or three alkoxy groups is also effective.
  • ⁇ -mercaptopropyl trimethoxysilane ⁇ -mercaptopropyltriethoxysilane and the like.
  • any silane compound having one or more aryl groups and two or three alkoxy groups in one molecule is effective.
  • ⁇ -diarylaminopro Examples thereof include biltrimethoxysilane, ⁇ -arylaminopropyl trimethoxysilane, and ⁇ -arylthiopropyl trimethoxysilane.
  • aminoalkoxy Sisilane is most preferred.
  • the addition amount of the alkoxysilane compound is important. If the amount of the alkoxysilane compound is small, the mechanical properties after the PCT are significantly decreased. Therefore, the addition amount of the alkoxysilane compound is 0.1-5 parts by weight, preferably 0.5-4 parts by weight with respect to 100 parts by weight of the PAS resin.
  • the present invention is a method for producing a highly thermally conductive resin composition.
  • (1) A method in which all raw materials are mixed and kneaded.
  • the effect of the present invention is exhibited by any method, such as a method of adding a coated magnesium oxide, (3) a method of adding a alkoxysilane compound to a phosphorus-containing coated magnesium oxide after the PAS resin is melted, and the like.
  • the (2) alkoxysilane compound is added to the PAS resin and melted so that the PAS resin and the alkoxysilane compound react more efficiently. After kneading, it is preferable to produce by a method of adding phosphorus-containing coated magnesium oxide.
  • the high thermal conductive resin composition of the present invention is within the object range of the present invention, and is used for improving the performance such as mechanical strength, heat resistance, dimensional stability (deformation resistance, warpage) and electrical properties.
  • fibrous, granular or plate-like fillers are used depending on the purpose.
  • fibrous filler examples include inorganic fibrous materials such as glass fiber, asbestos fiber, boron fiber, and titanic acid lithium fiber.
  • a particularly typical fibrous filler is glass fiber.
  • High melting point organic fiber materials such as polyamide, fluorine resin, and acrylic resin can also be used.
  • the granular fillers include quartz powder, glass beads, glass powder, calcium silicate, aluminum silicate, kaolin, talc, clay, diatomaceous earth, silicates such as wollastonite, iron oxide, titanium oxide, zinc oxide.
  • silicates such as wollastonite, iron oxide, titanium oxide, zinc oxide.
  • metal oxides such as calcium carbonate, metal carbonates such as magnesium carbonate, calcium sulfate, and metal sulfates such as barium sulfate.
  • the plate-like filler include My strength and glass flakes.
  • These inorganic fillers can be used alone or in combination of two or more.
  • thermoplastic resins that is, flame retardants, colorants such as dyes and pigments, stabilizers such as antioxidants and ultraviolet absorbers, lubricants, crystallization accelerators, crystal nucleating agents, etc.
  • flame retardants colorants such as dyes and pigments
  • stabilizers such as antioxidants and ultraviolet absorbers
  • lubricants such as talc, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, kaolin, etc.
  • crystallization accelerators such as crystallization accelerators, crystal nucleating agents, etc.
  • Molded products obtained by injection molding, extrusion molding, blow molding, etc. using the high thermal conductive resin composition of the present invention thus obtained have high moisture and heat resistance, chemical resistance, dimensional stability, Shows flame retardancy and excellent heat dissipation. Taking advantage of this advantage, it can be suitably used for components that radiate heat generated internally, such as heat exchangers, heat sinks, and optical pickups.
  • LEDs for example, LEDs, sensors, connectors, sockets, terminal blocks, printed circuit boards, motor parts, ECU cases, and other electrical and electronic parts, lighting parts, TV parts, rice cooker parts, microwave oven parts, irons, etc. It can be used for household and office electrical product parts such as parts, copier-related parts, printer-related parts, facsimile-related parts, heaters, and air conditioner parts.
  • Example 1 LEDs, sensors, connectors, sockets, terminal blocks, printed circuit boards, motor parts, ECU cases, and other electrical and electronic parts, lighting parts, TV parts, rice cooker parts, microwave oven parts, irons, etc. It can be used for household and office electrical product parts such as parts, copier-related parts, printer-related parts, facsimile-related parts, heaters, and air conditioner parts.
  • the thermal conductivity was measured by the hot disk method using a sample with a disk-shaped molded product with a diameter of 30 mm and a thickness of 2 mm.
  • a rod-shaped product having a width of 20 mm and a thickness of 1 mm was molded under the conditions of a cylinder temperature of 340 ° C and an injection pressure of lOOMPa, and the flow distance was measured.
  • the components used and the method of adding alkoxysilane compounds are as follows: 'Polyphenylene sulfide resin (PPS resin); Pho-Tron w 202 A manufactured by Kureha Chemical Industry Co., Ltd.
  • Filler 2 (comparative product): Silica-coated magnesium oxide, average particle size 27 ⁇ m, maximum particle size 100 / xm (Categote Cf 2-100 manufactured by Tateho Chemical Co., Ltd.)

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

La présente invention concerne un matériau de résine de poly(sulfure d'arylène) exempt de problème d'usure de vis, etc., qui est excellent en termes de capacité de moulage et de résistance à la chaleur et à l'humidité et qui présente une conductivité thermique élevée. En particulier, on propose une composition de résine à conduction thermique élevée comprenant 100 parties en poids de résine de poly(sulfure d'arylène), de 100 à 500 parties en poids d'oxyde de magnésium avec un revêtement à base de phosphore et de 0,1 à 5 parties en poids d'un composé alcoxysilane.
PCT/JP2006/310821 2006-05-24 2006-05-24 Composition de résine à conduction thermique élevée Ceased WO2007135749A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/JP2006/310821 WO2007135749A1 (fr) 2006-05-24 2006-05-24 Composition de résine à conduction thermique élevée
CN200680054686.6A CN101448899B (zh) 2006-05-24 2006-05-24 高热传导性树脂组合物

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2006/310821 WO2007135749A1 (fr) 2006-05-24 2006-05-24 Composition de résine à conduction thermique élevée

Publications (1)

Publication Number Publication Date
WO2007135749A1 true WO2007135749A1 (fr) 2007-11-29

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PCT/JP2006/310821 Ceased WO2007135749A1 (fr) 2006-05-24 2006-05-24 Composition de résine à conduction thermique élevée

Country Status (2)

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CN (1) CN101448899B (fr)
WO (1) WO2007135749A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013500352A (ja) * 2009-07-24 2013-01-07 ティコナ・エルエルシー 熱伝導性ポリマー組成物およびそれから製造される物品

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015137468A1 (fr) 2014-03-14 2015-09-17 大日精化工業株式会社 Oxyde complexe thermoconducteur, son procédé de production, composition contenant un oxyde complexe thermoconducteur et son utilisation
CN104119587B (zh) * 2014-07-02 2016-03-30 合肥和安机械制造有限公司 一种耐高温高压胶管材料用改性铝矾土及其制备方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01236270A (ja) * 1988-03-17 1989-09-21 Showa Denko Kk 樹脂組成物
JPH06256654A (ja) * 1993-03-03 1994-09-13 Polyplastics Co ポリアリーレンサルファイド樹脂組成物
JP2001151905A (ja) * 1999-11-24 2001-06-05 Tonen Chem Corp 樹脂製放熱板
JP2001214065A (ja) * 1999-11-22 2001-08-07 Kyowa Chem Ind Co Ltd 半導体封止用材料およびその樹脂組成物およびその成型品
JP2004027177A (ja) * 2001-12-25 2004-01-29 Tateho Chem Ind Co Ltd 酸化マグネシウム粉末を含む樹脂組成物
JP2005264124A (ja) * 2004-03-22 2005-09-29 Asahi Kasei Chemicals Corp ポリフェニレンスルフィド樹脂組成物

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01236270A (ja) * 1988-03-17 1989-09-21 Showa Denko Kk 樹脂組成物
JPH06256654A (ja) * 1993-03-03 1994-09-13 Polyplastics Co ポリアリーレンサルファイド樹脂組成物
JP2001214065A (ja) * 1999-11-22 2001-08-07 Kyowa Chem Ind Co Ltd 半導体封止用材料およびその樹脂組成物およびその成型品
JP2001151905A (ja) * 1999-11-24 2001-06-05 Tonen Chem Corp 樹脂製放熱板
JP2004027177A (ja) * 2001-12-25 2004-01-29 Tateho Chem Ind Co Ltd 酸化マグネシウム粉末を含む樹脂組成物
JP2005264124A (ja) * 2004-03-22 2005-09-29 Asahi Kasei Chemicals Corp ポリフェニレンスルフィド樹脂組成物

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013500352A (ja) * 2009-07-24 2013-01-07 ティコナ・エルエルシー 熱伝導性ポリマー組成物およびそれから製造される物品

Also Published As

Publication number Publication date
CN101448899A (zh) 2009-06-03
CN101448899B (zh) 2011-05-18

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