WO2011024659A1 - Composition de résine de polycarbonate ignifugeante et moulages réalisés à partir de celle-ci - Google Patents

Composition de résine de polycarbonate ignifugeante et moulages réalisés à partir de celle-ci Download PDF

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Publication number
WO2011024659A1
WO2011024659A1 PCT/JP2010/063774 JP2010063774W WO2011024659A1 WO 2011024659 A1 WO2011024659 A1 WO 2011024659A1 JP 2010063774 W JP2010063774 W JP 2010063774W WO 2011024659 A1 WO2011024659 A1 WO 2011024659A1
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mass
parts
polycarbonate resin
resin composition
flame
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PCT/JP2010/063774
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English (en)
Japanese (ja)
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敬直 竹内
誠一 前場
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出光興産株式会社
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
    • C08K5/41—Compounds containing sulfur bound to oxygen
    • C08K5/42—Sulfonic acids; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms

Definitions

  • the present invention relates to a flame retardant polycarbonate resin composition and a molded body thereof. Specifically, a molded article having good flame retardancy even at a thickness of about 1.2 to 1.0 mm and excellent in thermal conductivity, thermal stability, mechanical characteristics, impact resistance, flow characteristics and wettability.
  • the present invention relates to a flame retardant polycarbonate resin composition suitable for the electric / electronic field and the like, and a molded product thereof.
  • Patent Document 1 In order to obtain a resin composition excellent in thermal conductivity, it is known to contain specific graphite (see, for example, Patent Document 1). Further, for example, in Patent Document 2, in order to achieve good flame retardancy in addition to antistatic performance and the like, (A) 100 parts by mass of a thermoplastic resin, (B) 5 to 100 parts by mass of graphite having a specific particle size, (C) A flame-retardant resin composition comprising 0.001 to 1 part by mass of an alkali (earth) metal salt of an organic sulfonate is disclosed. However, in Patent Document 2, evaluation is made only at a thickness of 2.5 mm in the flame retardancy evaluation.
  • Patent Document 3 does not describe flame retardancy, and even such a resin composition does not provide sufficient flame retardancy at a thickness of about 1.5 mm required for a casing of an electronic device or the like. It is done.
  • a heat dissipating case in which a heating element is accommodated which is composed of a thermoplastic resin [A] and a specific heat conductive filler [B], and heat conduction to 100 parts by mass of the thermoplastic resin [A].
  • a heat dissipating case made of a heat conductive resin composition having a filler [B] content of 10 to 1,000 parts by mass is disclosed.
  • Patent Document 4 there is no description relating to flame retardancy required for a housing such as an electronic device, and since there is no addition of a flame retardant or an anti-drip agent, it does not have sufficient flame retardancy. Conceivable.
  • PTFE polytetrafluoroethylene
  • the prior art using polytetrafluoroethylene (PTFE) as an anti-drip agent is often intended for non-halogen flame retardant materials stipulated by various regulations and standards. Even if the addition amount of PTFE is widely taken, in the examples, the addition amount is almost 0.5% by mass or less of the whole resin composition (for example, see Patent Document 2).
  • the present invention even if a silicone compound is not added, even if the thickness is about 1.2 to 1.0 mm, it has good flame retardancy, thermal conductivity, thermal stability, mechanical properties, impact resistance It aims at providing the flame-retardant polycarbonate resin composition which gives the molded object excellent in the property, the flow characteristic, and the wettability, and the molded object.
  • this invention provides the following flame-retardant polycarbonate resin composition and its molded object.
  • the present invention even if it does not contain a silicone compound, it has a thickness of 1.2 to 1.V depending on the polycarbonate resin composition containing artificial graphite, a fluorine-containing anti-dripping agent, and a specific organic sulfonic acid alkali metal salt.
  • Flame retardant polycarbonate resin composition which has good flame retardancy even at about 0 mm, and gives a molded article excellent in thermal conductivity, thermal stability, mechanical properties, impact resistance, flow properties and wettability, and molding thereof The body can be provided.
  • the polycarbonate resin as the component (A) preferably has a viscosity average molecular weight of 19,000 to 30,000 in order to obtain excellent impact resistance. From the viewpoint of moldability, the viscosity average molecular weight Is more preferably 19,000-27,000. Moreover, when mixing and using two or more types of polycarbonate resin, it is desirable to adjust and use the viscosity average molecular weight in the said range as (A) component whole.
  • aromatic polycarbonate resin as (A) component
  • the various aromatic polycarbonate resin manufactured by reaction of bivalent phenol and a carbonate precursor can be used.
  • Various divalent phenols can be mentioned, and in particular, 2,2-bis (4-hydroxyphenyl) propane [bisphenol A], bis (4-hydroxyphenyl) methane, 1,1-bis (4- Hydroxyphenyl) ethane, 2,2-bis (4-hydroxy-3,5-dimethylphenyl) propane, 4,4'-dihydroxydiphenyl, bis (4-hydroxyphenyl) cycloalkane, bis (4-hydroxyphenyl) ether Bis (4-hydroxyphenyl) sulfide, bis (4-hydroxyphenyl) sulfone, bis (4-hydroxyphenyl) sulfoxide and bis (4-hydroxyphenyl) ketone.
  • dihydric phenols may be used alone or in combination of two or more. Particularly preferred dihydric phenols are those based on bis (bisphenol A), bis (4-hydroxyphen
  • Examples of the carbonate precursor include carbonyl halide, carbonyl ester and haloformate, specifically phosgene, dihaloformate of dihydric phenol, diphenyl carbonate, dimethyl carbonate and diethyl carbonate.
  • the aromatic polycarbonate may have a branched structure, and examples of the branching agent include 1,1,1-tris (4-hydroxyphenyl) ethane, ⁇ , ⁇ ′, ⁇ ′′ -tris (4- Bidroxyphenyl) -1,3,5-triisopropylbenzene, phloroglysin, trimellitic acid, and isatin bis (o-cresol).
  • the component (A) for example, a commercially available aromatic polycarbonate resin such as Teflon FN3000A, FN2600A, FN2500A, FN2200A, FN1900A, FN1700A, FN1500A (trade name, manufactured by Idemitsu Kosan Co., Ltd.) is used. be able to. These aromatic polycarbonate resins may be used alone or in admixture of two or more.
  • the resin composition can obtain thermal conductivity by containing artificial graphite as the component (B).
  • Artificial graphite is obtained by molding and firing petroleum coke, etc., and further highly graphitized at ultra-high temperatures. Since artificial graphite is difficult to orient during molding, it is easy to obtain strength and has excellent mechanical strength. It can be a composition.
  • the object of the present invention is to obtain flame retardancy with a thin wall, and in addition to natural graphite, expanded graphite, spherical graphite, flake graphite obtained by pulverizing natural graphite, and the like, the above object of the present invention. Therefore, artificial graphite is used in the present invention.
  • the component (B) is not particularly limited as long as it is artificial graphite, but the average particle diameter (50% cumulative diameter) is preferably in the range of about 20 to 180 ⁇ m, more preferably in the range of 30 to 170 ⁇ m. . If the average particle size of the artificial graphite is in the range of about 20 to 180 ⁇ m, the impact strength of the molded product obtained from the composition containing the artificial graphite will not decrease.
  • the average particle diameter of artificial graphite can be measured by a laser diffraction scattering method according to JIS R 1629.
  • those having a fixed carbon content of 99.0% by mass or more are preferable, those having an ash content of 0.5% by mass or less are preferable, and those having a volatile content of 0.4% by mass or less are preferable. If the volatile content is large, gas winding may occur during molding, which may impair the appearance.
  • the component (B) commercially available products such as PAG series and HAG series manufactured by Nippon Graphite Industry Co., Ltd. can be used. These artificial graphites may be used alone or in combination of two or more.
  • the content of the component (B) is 30 to 70 parts by mass with respect to 100 parts by mass of the component (A). If it is less than 30 parts by mass, sufficient thermal conductivity cannot be obtained, and if it exceeds 70 parts by mass, flame retardancy with a thin wall cannot be obtained, impact strength is lowered, and molecular weight of polycarbonate resin is reduced during granulation. cause.
  • the amount is preferably 40 to 50 parts by mass.
  • the fluorine-containing dripping inhibitor which is (C) component is polytetrafluoroethylene which has fibril formation ability.
  • the fibril forming ability refers to a tendency of the resins to be bonded and become fibrous due to an external action such as shearing force.
  • Polytetrafluoroethylene having fibril-forming ability imparts an effect of preventing melt dripping to the polycarbonate resin composition of the present invention, and exhibits excellent flame retardancy.
  • polytetrafluoroethylene examples include polytetrafluoroethylene, tetrafluoroethylene-based copolymers (for example, tetrafluoroethylene / hexafluoropropylene copolymers) and the like.
  • polytetrafluoroethylene hereinafter sometimes referred to as “PTFE”
  • PTFE polytetrafluoroethylene
  • PTFE having the ability to form fibrils has a very high molecular weight, and the number average molecular weight determined from the standard specific gravity is usually 500,000 or more, preferably 500,000 to 15 million, more preferably 1,000,000 to 10 million.
  • such PTFE is obtained by polymerizing tetrafluoroethylene in an aqueous solvent in the presence of sodium, potassium or ammonium peroxydisulfide at a pressure of 7 to 700 kPa at a temperature of 0 to 200 ° C., preferably 20 to 100 ° C.
  • Such PTFE can be used in solid form or in the form of an aqueous dispersion.
  • PTFE having such fibril-forming ability examples include those classified as type 3 in the ASTM standard. Specific examples thereof include, for example, Teflon 6-J (manufactured by Mitsui DuPont Fluorochemical Co., Ltd.), Polyflon D-1, Polyflon F-103, Polyflon F201 (manufactured by Daikin Industries, Ltd.), CD076 (Asahi Glass Fluoro) Polymers Co., Ltd.] and the like.
  • Algoflon F5 manufactured by Solvay Solexis Co., Ltd.
  • polyflon MPA manufactured by Polyflon FA-100
  • PTFE may be used independently and may combine 2 or more types.
  • the content of component (C) is 1 to 5 parts by mass with respect to 100 parts by mass of component (A). If it is less than 1 part by mass, the effect of preventing dripping cannot be obtained, and if it exceeds 5 parts by mass, the impact strength is reduced.
  • the amount is preferably 1 to 4 parts by mass.
  • an organic sulfonic acid alkali metal salt selected from sodium paratoluenesulfonate, potassium perfluorobutanesulfonate, and potassium trifluoromethanesulfonate is used as the flame retardant as the component (D), and these are specified. Include in proportions.
  • the content thereof is 0.15 to 0.73 parts by mass with respect to 100 parts by mass of the component (A). If it is less than 0.15 parts by mass, the effect as a flame retardant is not exhibited, and if it exceeds 0.73 parts by mass, the thermal stability is lowered.
  • the amount is preferably 0.15 to 0.4 parts by mass.
  • potassium perfluorobutanesulfonate and / or potassium trifluoromethanesulfonate is used as the component (D), the content thereof is 0.15 to 0.25 parts by mass with respect to 100 parts by mass of the component (A). It is.
  • the resin composition of the present invention can contain an antioxidant as the component (E).
  • antioxidant As antioxidant, phosphorus antioxidant, a phenolic antioxidant, etc. are used suitably. These may be used alone or in combination of two or more. Examples of phosphorus antioxidants include triphenyl phosphite, diphenyl nonyl phosphite, diphenyl (2-ethylhexyl) phosphite, tris (2,4-di-t-butylphenyl) phosphite, trisnonyl phenyl phosphite.
  • Diphenylisooctyl phosphite 2,2′-methylenebis (4,6-di-t-butylphenyl) octyl phosphite, diphenylisodecyl phosphite, diphenylmono (tridecyl) phosphite, phenyldiisodecyl phosphite, phenyldi ( Tridecyl) phosphite, Tris (2-ethylhexyl) phosphite, Tris (isodecyl) phosphite, Tris (tridecyl) phosphite, Dibutyl hydrogen phosphite, Trilauryl trithiophosphite, Te Trakis (2,4-di-t-butylphenyl) -4,4′-biphenylenediphosphonite, 4,4′-isopropylid
  • Examples of phosphorus antioxidants include Irgafos 168 (trade name, manufactured by Ciba Specialty Chemicals Co., Ltd.), Irgafos 12 (trade name, manufactured by Ciba Specialty Chemicals Co., Ltd.), Irgafos 38 (trade name, manufactured by Ciba Specialty Chemicals Co., Ltd.) ), ADKSTAB C (trademark), ADKSTAB ⁇ 329K (trademark, ADEKA Corp.), ADKSTAB PEP36 (trademark, ADEKA Corp.), ADKSTAB PEP-8 (trademark, ADEKA Corporation), JC263 (trademark) Johoku Chemical Industry Co., Ltd., Trademark), Sardstab P-EPQ (Clariant, Trademark), Weston 618 (GE, Trademark), Weston 619G (GE, Trademark) and West n 624 (GE Co., trademark) can be exemplified commercially available products such as.
  • phenolic antioxidants examples include n-octadecyl-3- (3,5-di-t-butyl-4-hydroxyphenyl) propionate, 2,6-di-t-butyl-4-methylphenol, 2, Hindered phenols such as 2'-methylenebis (4-methyl-6-tert-butylphenol), pentaerythrityl-tetrakis [3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate] It is done.
  • antioxidants bis (2,6-di-tert-butyl 4-methylphenyl) pentaerythritol diphosphite, bis (2,4-di-tert-butylphenyl) pentaerythritol diphosphite, etc.
  • Those having a pentaerythritol diphosphite structure and triphenylphosphine are preferred.
  • phenolic antioxidants examples include Irganox 1010 (trade name, manufactured by Ciba Specialty Chemicals Co., Ltd.), Irganox 1076 (trade name, manufactured by Ciba Specialty Chemicals Co., Ltd.), Irganox 1330 (trade name, manufactured by Ciba Specialty Chemicals Co., Ltd.) Irganox 3114 (trade name, manufactured by Ciba Specialty Chemicals Co., Ltd.), Irganox 3125 (trade name, manufactured by Ciba Specialty Chemicals Co., Ltd.), BHT (trade name, manufactured by Takeda Pharmaceutical Company Limited), Cyanox 1790 (trade name, manufactured by Cyanamid Co., Ltd.), and Examples include commercial products such as Sumilizer GA-80 (trademark, manufactured by Sumitomo Chemical Co., Ltd.).
  • the content of the component (E) is preferably about 0.001 to 1 part by mass, more preferably 0.1 to 1 part by mass with respect to 100 parts by mass of the component (A). If it is 0.001 part by mass or more, thermal stability does not decrease during granulation and molding, and if it is 1 part by mass or less, there is no possibility of causing a decrease in molecular weight.
  • the resin composition of the present invention may contain a release agent as the component (F) for the purpose of improving productivity during molding and improving dimensional accuracy of the molded body.
  • a release agent for example, fatty acid ester, polyolefin wax, fluorine oil, paraffin wax, etc. can be used.
  • fatty acid esters are preferred, for example, stearic acid monoglyceride, stearic acid diglyceride, stearic acid monosorbate, behenic acid monoglyceride, pentaerythritol monostearate, pentaerythritol distearate, propylene glycol monostearate, sorbitan monostearate, etc. Partial esters are preferable, and stearic acid monoglyceride, stearic acid monosorbate, pentaerythritol monostearate, and pentaerythritol distearate are more preferable. These release agents may be used alone or in combination of two or more.
  • the content of component (F) is preferably about 0.3 to 2 parts by mass with respect to 100 parts by mass of component (A).
  • the content of the component (F) is within the above range, the physical properties are not greatly lowered, and the sustainability during continuous molding and the residual distortion and yield of the molded body are improved.
  • the resin composition of the present invention may contain various additives as long as the object of the present invention is not impaired.
  • Various additives include, for example, ultraviolet absorbers such as benzotriazoles and benzophenones, light stabilizers such as hindered amines, talc, mica, kaolin, diatomaceous earth, calcium carbonate, calcium sulfate, barium sulfate, glass fiber, and carbon fiber.
  • inorganic fillers such as potassium titanate.
  • a silicone compound such as a silicone-based flame retardant for the purpose of improving the flame retardancy as an additive.
  • the resin composition of the present invention is excellent in paintability by not containing a silicone compound, and is further made into a resin composition that gives a molded article having good flame retardancy and the like by containing each of the aforementioned components. Can do.
  • the flame-retardant polycarbonate resin composition of the present invention can be obtained by blending the above-described components (A) to (F) and various additives by a conventional method and melt-kneading.
  • some (C) fluorine-containing anti-dripping agents and the like may aggregate when blended as they are, and may be blended after (A) masterbatch with a polycarbonate resin.
  • a high-speed mixer or the like it may not always be necessary to make a master batch.
  • the melt kneading can be performed using, for example, a ribbon blender, a Henschel mixer, a Banbury mixer, a drum tumbler, a single screw extruder, a twin screw extruder, a kneader, a multi-screw extruder, or the like.
  • the heating temperature in melt kneading is usually about 250 to 330 ° C.
  • the flame-retardant polycarbonate resin composition of the present invention is applied to a known molding method such as hollow molding, injection molding, extrusion molding, vacuum molding, pressure forming, hot bending molding, compression molding, calendar molding, rotational molding, and the like.
  • a thin molded article excellent in flame retardancy, thermal conductivity, thermal stability, mechanical properties, impact resistance, flow properties and wettability can be obtained.
  • the flame-retardant polycarbonate resin composition of the present invention is a molded product that is used in a part that requires a thin wall thickness (about 1.2 to 1.0 mm) and flame resistance when used, for example, for electrical and electronic use. It is suitably used for manufacturing parts, chassis for electric / electronic devices, heat dissipation components, heat transfer components, communication device components, and the like.
  • Examples and Comparative Examples The composition shown in each table is blended in a twin screw extruder (manufactured by Toshiba Machine Co., Ltd., model name TEM35), and melt kneaded at a barrel temperature of 300 to 320 ° C., a screw rotation speed of 100 to 600 rotations, and a discharge of 10 to 30 kg / hr. Thus, a sample for evaluation was obtained. The physical properties of the obtained evaluation samples were measured and evaluated according to the above methods, and the results are shown in the table.
  • a twin screw extruder manufactured by Toshiba Machine Co., Ltd., model name TEM35
  • the flame-retardant polycarbonate resin composition of the present invention has good flame retardancy even with a thickness of about 1.2 to 1.0 mm, and has thermal conductivity, thermal stability, mechanical properties, impact resistance, flow Because it can give molded products with excellent characteristics and wettability, it can be used in the electric and electronic fields, and in particular, projectors, digital equipment (CCD, etc.), personal computers, LED lighting, digital that require countermeasures against heat It is suitable for heat dissipation parts around a heat source such as a camera, a chassis, a case, and the like.
  • a heat source such as a camera, a chassis, a case, and the like.
  • the flame retardant polycarbonate resin composition of the present invention does not contain a silicone compound, so it has excellent wettability, and from the viewpoint of paintability, a mobile that requires a metal-like tactile feel as a part of the design. It is suitable for uses such as equipment casings.

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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 une composition de résine de polycarbonate ignifugeante capable de donner des moulages présentant de remarquables qualités ignifugeantes, une très bonne conductivité thermique, une très grande stabilité thermique, d'exceptionnelles caractéristiques mécaniques, une très bonne résistance aux chocs, de remarquables caractéristiques en termes d'écoulement et de mouillabilité, même quand ces moulages présentent une épaisseur d'environ 1,0 à 1,2 mm et qu'ils ne contiennent pas de composés de silicone. L'invention concerne également des moulages réalisés à partir de ladite composition de résine. L'invention concerne, plus précisément, une composition de résine de polycarbonate ignifugeante et sans silicone contenant (A) 100 parties en poids d'une résine de polycarbonate, (B) 30 à 70 parties en poids de graphite artificiel, (C) 1 à 5 parties en poids d'un agent anti-goutte contenant du fluor et (D) un retardateur de flamme constitué de 0,15 à 0,73 parties en poids de p-toluènesulfonate de sodium et de 0,15 à 0,25 parties en poids d'au moins un composé choisi parmi le perfluorobutanesulfonate de potassium et le trifluorométhanesulfonate de potassium ; ainsi que des moulages réalisés à partir de ladite composition.
PCT/JP2010/063774 2009-08-28 2010-08-13 Composition de résine de polycarbonate ignifugeante et moulages réalisés à partir de celle-ci WO2011024659A1 (fr)

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JP2009198583A JP5616599B2 (ja) 2009-08-28 2009-08-28 難燃性ポリカーボネート樹脂組成物及びその成形体

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CN109810404B (zh) * 2018-12-24 2021-11-23 浙江大学宁波理工学院 一种聚丙烯/金属氢氧化物/稀土化合物阻燃材料
JP2021009788A (ja) * 2019-07-01 2021-01-28 日本製鉄株式会社 金属黒鉛質ブラシ
JP7200057B2 (ja) 2019-07-01 2023-01-06 日本製鉄株式会社 金属黒鉛質ブラシ

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