WO2025057768A1 - Composition de résine à base de polypropylène et article moulé - Google Patents

Composition de résine à base de polypropylène et article moulé Download PDF

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WO2025057768A1
WO2025057768A1 PCT/JP2024/031145 JP2024031145W WO2025057768A1 WO 2025057768 A1 WO2025057768 A1 WO 2025057768A1 JP 2024031145 W JP2024031145 W JP 2024031145W WO 2025057768 A1 WO2025057768 A1 WO 2025057768A1
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mass
propylene
parts
antistatic agent
polypropylene
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Japanese (ja)
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昂紀 坂本
悠 樋口
裕也 山本
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Sumitomo Chemical Co Ltd
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Sumitomo Chemical Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C08K3/013—Fillers, pigments or reinforcing additives
    • 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
    • C08K3/34—Silicon-containing compounds
    • 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
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • 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
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/20—Carboxylic acid amides
    • 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
    • C08K5/56—Organo-metallic compounds, i.e. organic compounds containing a metal-to-carbon bond
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/08—Copolymers of ethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene

Definitions

  • Molded articles containing polypropylene-based resin compositions are used in automobile interior and exterior materials, electrical component boxes, etc.
  • Such polypropylene-based resin compositions contain antistatic agents, and a method is known for improving the antistatic properties of the molded articles by adjusting the amount and ratio of the agents.
  • the present invention was made in consideration of these problems, and aims to provide a polypropylene resin composition that has excellent antistatic properties and can produce molded articles with relatively reduced VOC emissions, particularly acetaldehyde and acrolein emissions, and a molded article that contains the polypropylene resin composition.
  • the polypropylene-based resin composition according to this embodiment contains a polypropylene-based resin made of a propylene-based polymer as a resin component, talc as an inorganic filler, and a glycerin monostearate-based antistatic agent, an amine-based antistatic agent, and an amide-based antistatic agent as antistatic agents.
  • the polypropylene-based resin preferably contains, as a propylene-based polymer, at least one selected from the group consisting of propylene homopolymers and heterophasic propylene polymer materials, and more preferably contains a heterophasic propylene polymer material.
  • the isotactic pentad fraction of the propylene-based polymer is preferably 0.961 or more, more preferably 0.975 or more, and even more preferably 0.980 or more.
  • the isotactic pentad fraction of the propylene-based polymer is preferably 1.000 or less, and more preferably 0.995 or less.
  • the isotactic pentad fraction means the isotactic fraction in pentad units.
  • the isotactic pentad fraction indicates the content of structures in which five consecutive monomer units derived from propylene are meso-bonded when viewed in pentad units.
  • the isotactic pentad fraction refers to the value measured for the chain of monomer units derived from propylene.
  • the isotactic pentad fraction is a value measured by 13 C-NMR spectrum. Specifically, the isotactic pentad fraction is the ratio of the area of the mmmm peak to the area of all absorption peaks in the methyl carbon region obtained by 13 C-NMR spectrum. Note that the method for measuring the isotactic pentad fraction by 13 C-NMR spectrum is described, for example, in Macromolecules, 6, 925 (1973) by A. Zambelli et al. However, the assignment of the absorption peaks obtained by 13 C-spectrum is based on the description in Macromolecules, 8, 687 (1975).
  • the isotactic pentad fraction of the propylene-based polymer can be adjusted to the above range by appropriately selecting the catalyst, donor, polymerization conditions, etc. Also, a propylene-based polymer having the desired isotactic pentad fraction can be obtained from a commercial product.
  • the melt flow rate (MFR) of the propylene polymer is preferably 0.1 g/10 min or more and 300 g/10 min or less, and more preferably 1 g/10 min or more and 300 g/10 min or less.
  • the melt flow rate (MFR) of the propylene polymer may be 5 g/10 min or more and 100 g/10 min or less, or 10 g/10 min or more and 50 g/10 min or less.
  • the intrinsic viscosity (unit: dL/g) is a value measured at a temperature of 135°C using tetralin as a solvent by the following method.
  • Ubbelohde viscometer is used to measure the reduced viscosity at three concentrations: 0.1 g/dL, 0.2 g/dL, and 0.5 g/dL.
  • the reduced viscosity is plotted against the concentration, and the intrinsic viscosity is calculated by the extrapolation method, which extrapolates the concentration to zero.
  • the method for calculating the limiting viscosity using the extrapolation method is described, for example, on page 491 of "Polymer Solutions, Polymer Experiments 11" (published by Kyoritsu Publishing Co., Ltd. in 1982).
  • the molecular weight distribution (Mw/Mn) of the propylene homopolymer is preferably 3.0 or more, more preferably 4.0 or more.
  • the molecular weight distribution of the propylene homopolymer is preferably 15.0 or less, more preferably 10.0 or less.
  • the molecular weight distribution of the propylene homopolymer is preferably 3.0 or more and 15.0 or less, more preferably 4.0 or more and 10.0 or less.
  • the molecular weight distribution means the ratio (Mw/Mn) of the weight average molecular weight (Mw) to the number average molecular weight (Mn), calculated using the weight average molecular weight (Mw) and the number average molecular weight (Mn) measured by gel permeation chromatography (GPC) under the following conditions: Apparatus: Tosoh Corporation HLC-8121 GPC/HT Separation column: 3 GMHHR-H(S)HT manufactured by Tosoh Corporation Measurement temperature: 140°C Carrier: orthodichlorobenzene Flow rate: 1.0 mL/min Sample concentration: approximately 1 mg/mL Sample injection volume: 400 ⁇ L Detector: Differential refractometry Calibration curve creation method: Standard polystyrene is used
  • Propylene homopolymer can be produced, for example, by carrying out a polymerization process in which propylene is polymerized using a polymerization catalyst.
  • polymerization catalysts examples include Ziegler catalysts; Ziegler-Natta catalysts; catalysts containing a compound of a transition metal of Group 4 of the periodic table having a cyclopentadienyl ring and an alkylaluminoxane; catalysts containing a compound of a transition metal of Group 4 of the periodic table having a cyclopentadienyl ring, a compound that reacts with the transition metal compound to form an ionic complex, and an organoaluminum compound; and modified catalysts in which catalytic components (a compound of a transition metal of Group 4 of the periodic table having a cyclopentadienyl ring, a compound that forms an ionic complex, an organoaluminum compound, etc.) are supported on inorganic particles (silica, clay minerals, etc.).
  • Examples of the polymerization catalyst include those described in JP-A-61-218606, JP-A-5-194685, JP-A-7-216017, JP-A-9-316147, JP-A-10-212319, JP-A-2004-182981, JP-A-2010-168545, and JP-A-2011-246699.
  • a polymer obtained by prepolymerizing propylene in the presence of the polymerization catalyst can also be used as the polymerization catalyst.
  • Polymerization methods include, for example, bulk polymerization, solution polymerization, and gas phase polymerization.
  • bulk polymerization refers to a method in which polymerization is carried out using a liquid olefin as a medium at the polymerization temperature.
  • Solution polymerization refers to a method in which polymerization is carried out in an inert hydrocarbon solvent such as propane, butane, isobutane, pentane, hexane, heptane, or octane.
  • Gas phase polymerization refers to a method in which a gaseous monomer is used as a medium and the gaseous monomer is polymerized in that medium.
  • Polymerization methods include, for example, batch, continuous, and combinations of these.
  • the polymerization method may be a multi-stage method in which multiple polymerization reaction tanks are connected in series.
  • the polymerization method is preferably a continuous gas phase polymerization method or a bulk-gas phase polymerization method in which bulk polymerization and gas phase polymerization are carried out continuously.
  • polymerization temperature polymerization pressure
  • monomer concentration polymer concentration
  • catalyst input amount polymerization time, and other polymerization conditions
  • the polymer may be dried at a temperature below the melting point of the polymer, if necessary, to remove residual solvent contained in the polymer and ultra-low molecular weight oligomers produced as by-products during production.
  • drying methods include those described in JP-A-55-75410 and Japanese Patent No. 2,565,753.
  • the random copolymer of propylene and a monomer other than propylene contains monomer units derived from propylene and monomer units derived from a monomer other than propylene, and preferably contains 0.01% by mass or more and 20% by mass or less of monomer units derived from a monomer other than propylene, based on 100% by mass of the total mass of the copolymer.
  • Examples of monomers other than propylene include ethylene and ⁇ -olefins having 4 to 12 carbon atoms.
  • ⁇ -olefins are aliphatic unsaturated hydrocarbons having a carbon-carbon unsaturated double bond at the ⁇ -position.
  • Examples of ⁇ -olefins having 4 to 12 carbon atoms include 1-butene, 1-pentene, 1-hexene, 1-heptene, 1-octene, 1-nonene, 1-decene, 1-dodecene, 4-methyl-1-pentene, and 4-methyl-1-hexene.
  • the monomer other than propylene is preferably at least one selected from the group consisting of ethylene and ⁇ -olefins having 4 to 10 carbon atoms, more preferably at least one selected from the group consisting of ethylene, 1-butene, 1-hexene, and 1-octene, and even more preferably at least one selected from the group consisting of ethylene and 1-butene.
  • random copolymers of propylene and monomers other than propylene include propylene-ethylene random copolymers, propylene-1-butene random copolymers, propylene-1-hexene random copolymers, propylene-1-octene random copolymers, propylene-ethylene-1-butene random copolymers, propylene-ethylene-1-hexene random copolymers, and propylene-ethylene-1-octene random copolymers.
  • the random copolymer of propylene and a monomer other than propylene preferably has an intrinsic viscosity ([ ⁇ ]) of 0.10 dL/g or more and 4.00 dL/g or less, more preferably 0.50 dL/g or more and 3.00 dL/g or less, and even more preferably 0.70 dL/g or more and 2.00 dL/g or less, from the viewpoint of improving the fluidity of the polypropylene resin composition when melted.
  • the molecular weight distribution (Mw/Mn) of the random polymer of propylene and a monomer other than propylene is preferably 3.0 or more, more preferably 4.0 or more.
  • the molecular weight distribution is preferably 10.0 or less, more preferably 7.0 or less.
  • the molecular weight distribution of the random polymer of propylene and a monomer other than propylene is preferably 3.0 or more and 10.0 or less, more preferably 4.0 or more and 7.0 or less.
  • a random copolymer of propylene and a monomer other than propylene can be produced, for example, by polymerizing propylene and a monomer other than propylene according to the polymerization catalyst, polymerization method, polymerization method, and polymerization conditions that can be used in the production of the propylene homopolymer described above.
  • the heterophasic propylene polymerization material is a mixture containing a polymer I containing 80% by mass or more of monomer units derived from propylene (wherein the total mass of the polymer I is taken as 100% by mass), and a polymer II containing monomer units derived from at least one ⁇ -olefin selected from the group consisting of ethylene and ⁇ -olefins having 4 to 12 carbon atoms, and monomer units derived from propylene.
  • the heterophasic propylene polymerization material can be produced, for example, by carrying out a first polymerization step of polymerizing polymer I and a second polymerization step of polymerizing polymer II. These polymerization steps can be carried out according to the polymerization catalyst, polymerization method, polymerization system, and polymerization conditions that can be used in the production of the above-mentioned propylene homopolymer.
  • the heterophasic propylene polymerization material may be such that the sum of polymer I and polymer II contained in the heterophasic propylene polymerization material is 100% by mass, relative to the total mass of the heterophasic propylene polymerization material being 100% by mass.
  • polymer I contains 80% by mass or more of monomer units derived from propylene (where the total mass of polymer I is 100% by mass).
  • Polymer I may be, for example, a propylene homopolymer, or may contain monomer units derived from monomers other than propylene.
  • the content of such monomer units may be, for example, 0.01% by mass or more and less than 20% by mass relative to the total mass of polymer I, 100% by mass.
  • Monomers other than propylene include, for example, ethylene and ⁇ -olefins having 4 or more carbon atoms.
  • ⁇ -olefins having 4 or more carbon atoms include 1-butene, 1-pentene, 1-hexene, 1-heptene, 1-octene, 1-nonene, 1-decene, 1-dodecene, 4-methyl-1-pentene, 4-methyl-1-hexene, etc.
  • the monomer other than propylene is preferably at least one selected from the group consisting of ethylene and ⁇ -olefins having 4 to 10 carbon atoms, more preferably at least one selected from the group consisting of ethylene, 1-butene, 1-hexene, and 1-octene, and even more preferably at least one selected from the group consisting of ethylene and 1-butene.
  • polymer I containing monomer units derived from a monomer other than propylene examples include propylene-ethylene copolymer, propylene-1-butene copolymer, propylene-1-hexene copolymer, propylene-1-octene copolymer, propylene-ethylene-1-butene copolymer, propylene-ethylene-1-hexene copolymer, propylene-ethylene-1-octene copolymer, etc.
  • polymer I is preferably a propylene homopolymer, a propylene-ethylene copolymer, a propylene-1-butene copolymer, or a propylene-ethylene-1-butene copolymer, and more preferably a propylene homopolymer.
  • the isotactic pentad fraction of polymer I is preferably 1.000 or less, and may be, for example, 0.998 or less, 0.995 or less, 0.990 or less, or 0.985 or less.
  • the lower limit of the isotactic pentad fraction is not particularly limited, but may be, for example, 0.900 or more, 0.925 or more, 0.930 or more, 0.961 or more, 0.965 or more, or 0.968 or more.
  • the content of polymer I is preferably 50% by mass or more and 99% by mass or less, and more preferably 60% by mass or more and 95% by mass or less, relative to the total mass of the heterophasic propylene polymerization material (100% by mass).
  • polymer II contains monomer units derived from at least one ⁇ -olefin selected from the group consisting of ethylene and ⁇ -olefins having 4 to 12 carbon atoms, and monomer units derived from propylene.
  • ⁇ -olefins having 4 to 12 carbon atoms include 1-butene, 1-pentene, 1-hexene, 1-heptene, 1-octene, 1-nonene, 1-decene, 1-dodecene, 4-methyl-1-pentene, and 4-methyl-1-hexene.
  • Polymer II preferably contains 30% by mass or more of monomer units derived from at least one ⁇ -olefin selected from the group consisting of ethylene and ⁇ -olefins having 4 to 12 carbon atoms, and also contains monomer units derived from propylene (where the total mass of Polymer II is taken as 100% by mass).
  • the content of monomer units derived from at least one ⁇ -olefin selected from the group consisting of ethylene and ⁇ -olefins having 4 to 12 carbon atoms may be 30% by mass or more and 70% by mass or less, or 35% by mass or more and 60% by mass or less (where the total mass of polymer II is taken as 100% by mass).
  • the at least one ⁇ -olefin selected from the group consisting of ethylene and ⁇ -olefins having 4 to 12 carbon atoms is preferably at least one selected from the group consisting of ethylene and ⁇ -olefins having 4 to 10 carbon atoms, more preferably at least one selected from the group consisting of ethylene, 1-butene, 1-hexene, 1-octene, and 1-decene, and even more preferably at least one selected from the group consisting of ethylene and 1-butene.
  • polymer II examples include propylene-ethylene copolymer, propylene-ethylene-1-butene copolymer, propylene-ethylene-1-hexene copolymer, propylene-ethylene-1-octene copolymer, propylene-ethylene-1-decene copolymer, propylene-1-butene copolymer, propylene-1-hexene copolymer, propylene-1-octene copolymer, and propylene-1-decene copolymer.
  • polymer II is preferably a propylene-ethylene copolymer, a propylene-1-butene copolymer, or a propylene-ethylene-1-butene copolymer, and more preferably a propylene-ethylene copolymer.
  • the content of polymer II is preferably 1% by mass or more and 50% by mass or less, and more preferably 5% by mass or more and 40% by mass or less, relative to the total mass (100% by mass) of the heterophasic propylene polymerization material.
  • the content of monomer units derived from at least one ⁇ -olefin selected from the group consisting of ethylene and ⁇ -olefins having 4 to 12 carbon atoms may be 0.3% by mass or more and 35% by mass or less, or 0.7% by mass or more and 24% by mass or less (wherein the total mass of the heterophasic propylene polymerization material is 100% by mass).
  • the content of xylene insoluble components (CXIS components) in the heterophasic propylene polymerization material is preferably 50% by mass or more and 99% by mass or less, and more preferably 60% by mass or more and 95% by mass or less, relative to the total mass of the heterophasic propylene polymerization material (100% by mass).
  • the content of xylene soluble components (CXS components) in the heterophasic propylene polymerization material is preferably 1% by mass or more and 50% by mass or less, more preferably 5% by mass or more and 40% by mass or less, based on the total mass of the heterophasic propylene polymerization material (100% by mass).
  • the xylene insoluble component refers to a component contained in a polymer that is insoluble in p-xylene and is a solid obtained by the following method: About 2 g of the polymer is dissolved in boiling p-xylene for 2 hours to obtain a solution, which is then cooled to 20° C. to precipitate a solid.
  • xylene soluble components refer to components other than the "CXIS components" in the polymer.
  • the CXIS component in the heterophasic propylene polymerization material is mainly composed of polymer I
  • the CXS component in the heterophasic propylene polymerization material is mainly composed of polymer II.
  • Heterophasic propylene polymerization materials include, for example, (propylene)-(propylene-ethylene) polymerization materials, (propylene)-(propylene-ethylene-1-butene) polymerization materials, (propylene)-(propylene-ethylene-1-hexene) polymerization materials, (propylene)-(propylene-ethylene-1-octene) polymerization materials, (propylene)-(propylene-1-butene) polymerization materials, (propylene)-(propylene-1-hexene) polymerization materials, (propylene)-(propylene-1-octene) polymerization materials, (propylene)-(propylene-1-decene) polymerization materials, (propylene- (ethylene)-(propylene-ethylene) polymerization material, (propylene-ethylene)-(propylene-ethylene-1-butene) polymerization material, (propylene-ethylene)-(propylene-ethylene
  • (propylene)-(propylene-ethylene) polymer material means "a heterophasic propylene polymer material in which polymer I is a propylene homopolymer and polymer II is a propylene-ethylene copolymer.” The same applies to other similar expressions.
  • the heterophasic propylene polymeric material is preferably a (propylene)-(propylene-ethylene) polymeric material, a (propylene)-(propylene-ethylene-1-butene) polymeric material, a (propylene-ethylene)-(propylene-ethylene) polymeric material, a (propylene-ethylene)-(propylene-ethylene-1-butene) polymeric material, or a (propylene-1-butene)-(propylene-1-butene) polymeric material, and more preferably a (propylene)-(propylene-ethylene) polymeric material.
  • the intrinsic viscosity number ([ ⁇ ]I) of polymer I is preferably 0.10 dL/g or more and 4.00 dL/g or less, more preferably 0.50 dL/g or more and 3.00 dL/g or less, and even more preferably 0.70 dL/g or more and 2.00 dL/g or less.
  • the intrinsic viscosity number ([ ⁇ ]II) of polymer II is preferably 1.00 dL/g or more and 10.00 dL/g or less, more preferably 2.00 dL/g or more and 10.00 dL/g or less, and even more preferably 2.00 dL/g or more and 9.00 dL/g or less.
  • the ratio ([ ⁇ ]II/[ ⁇ ]I) of the intrinsic viscosity number ([ ⁇ ]II) of polymer II to the intrinsic viscosity number ([ ⁇ ]I) of polymer I is preferably 1 or more and 20 or less, more preferably 1 or more and 10 or less.
  • a method for measuring the intrinsic viscosity number ([ ⁇ ]I) of polymer I for example, a method can be used in which polymerized polymer I is extracted from a reactor in which polymer I is polymerized, and the intrinsic viscosity number of the polymer is measured.
  • the intrinsic viscosity number ([ ⁇ ]II) of polymer II can be calculated, for example, by the following formula (i) using the intrinsic viscosity number ([ ⁇ ]Total) of the heterophasic propylene polymerization material, the intrinsic viscosity number ([ ⁇ ]I) of polymer I, and the contents of polymer II and polymer I.
  • [ ⁇ ]II ([ ⁇ ]Total-[ ⁇ ]I ⁇ XI)/XII...(i) [ ⁇ ]Total: Intrinsic viscosity number (dL / g) of the heterophasic propylene polymer material
  • XII Ratio of the mass of polymer II to the total mass of the heterophasic propylene polymer material (mass of polymer II/mass of heterophasic propylene polymer material)
  • XI and XII can be determined from the material balance during polymerization.
  • the intrinsic viscosity of the CXIS component is preferably 0.10 dL/g or more and 4.00 dL/g or less, more preferably 0.50 dL/g or more and 3.00 dL/g or less, and even more preferably 0.70 dL/g or more and 2.00 dL/g or less.
  • the intrinsic viscosity of the CXS component is preferably 1.00 dL/g or more and 10.00 dL/g or less, more preferably 2.00 dL/g or more and 10.00 dL/g or less, and even more preferably 2.00 dL/g or more and 9.00 dL/g or less.
  • the ratio ([ ⁇ ]CXS/[ ⁇ ]CXIS) of the intrinsic viscosity number of the CXS component ([ ⁇ ]CXS) to the intrinsic viscosity number of the CXIS component ([ ⁇ ]CXIS) is preferably 1 or more and 20 or less, more preferably 1 or more and 10 or less.
  • the molecular weight distribution (Mw(I)/Mn(I)) of polymer I is preferably 3.0 or more, and more preferably 4.0 or more.
  • the molecular weight distribution of the CXIS component is preferably 3.0 or more, and more preferably 4.0 or more.
  • the content of polypropylene resin is from 50 parts by mass to 99.9 parts by mass, preferably from 60 parts by mass to 99.9 parts by mass, more preferably from 70 parts by mass to 99.9 parts by mass, and even more preferably from 75 parts by mass to 99.9 parts by mass, per 100 parts by mass of the total content of resin components and talc, from the viewpoint of obtaining good mechanical strength for automotive materials, industrial materials, etc.
  • the polypropylene resin composition according to the present embodiment may further include an ethylene- ⁇ -olefin copolymer as a resin component.
  • the ethylene- ⁇ -olefin copolymer may be an ethylene- ⁇ -olefin random copolymer.
  • the ethylene- ⁇ -olefin copolymer refers to a copolymer that contains monomer units derived from ethylene and monomer units derived from an ⁇ -olefin having 4 or more carbon atoms, and is substantially free of monomer units derived from propylene.
  • the ethylene- ⁇ -olefin copolymer may have a total content of monomer units derived from ethylene and monomer units derived from ⁇ -olefins having 4 or more carbon atoms of 100% by mass, where the total mass of the copolymer is 100% by mass.
  • Examples of ⁇ -olefins having 4 or more carbon atoms include ⁇ -olefins having 4 to 12 carbon atoms.
  • Examples of ⁇ -olefins having 4 to 12 carbon atoms include 1-butene, 1-pentene, 1-hexene, 4-methyl-1-pentene, 1-octene, and 1-decene.
  • the ⁇ -olefins having 4 to 12 carbon atoms are preferably 1-butene, 1-hexene, or 1-octene.
  • the ⁇ -olefins having 4 to 12 carbon atoms may be ⁇ -olefins having a cyclic structure, such as vinylcyclopropane and vinylcyclobutane.
  • ethylene- ⁇ -olefin copolymers examples include ethylene-1-butene copolymers, ethylene-1-hexene copolymers, ethylene-1-octene copolymers, ethylene-1-decene copolymers, ethylene-(3-methyl-1-butene) copolymers, and copolymers of ethylene and ⁇ -olefins having a cyclic structure.
  • the content of monomer units derived from ⁇ -olefins having 4 or more carbon atoms is preferably 1% by mass or more and 49% by mass or less, more preferably 5% by mass or more and 49% by mass or less, and even more preferably 24% by mass or more and 49% by mass or less, relative to the total mass (100% by mass) of the ethylene- ⁇ -olefin copolymer.
  • the density of the ethylene- ⁇ -olefin copolymer is preferably 0.85 g/ cm3 or more and 0.89 g/ cm3 or less, more preferably 0.85 g/ cm3 or more and 0.88 g/ cm3 or less, and even more preferably 0.85 g/ cm3 or more and 0.87 g/ cm3 or less.
  • the melt flow rate (MFR) of the ethylene- ⁇ -olefin copolymer is preferably 0.1 g/10 min or more and 80 g/10 min or less.
  • the melt flow rate (MFR) of the ethylene- ⁇ -olefin copolymer is measured by Method A under conditions of a temperature of 190°C and a load of 2.16 kg in accordance with the method specified in JIS K7210-1:2014 and K7210-2:2014.
  • an ethylene- ⁇ -olefin copolymer When an ethylene- ⁇ -olefin copolymer is included, its content is preferably 1 part by mass or more, and more preferably 5 parts by mass or more, per 100 parts by mass of polypropylene-based resin. Also, the content of the ethylene- ⁇ -olefin copolymer is preferably 50 parts by mass or less, and more preferably 30 parts by mass or less, per 100 parts by mass of polypropylene-based resin.
  • Ethylene- ⁇ -olefin copolymers can be produced by polymerizing ethylene and an ⁇ -olefin with 4 or more carbon atoms using a polymerization catalyst.
  • polymerization catalysts examples include homogeneous catalysts such as metallocene catalysts, Ziegler-Natta catalysts, etc.
  • homogeneous catalysts include catalysts containing a compound of a transition metal of Group 4 of the periodic table having a cyclopentadienyl ring and an alkylaluminoxane; catalysts containing a compound of a transition metal of Group 4 of the periodic table having a cyclopentadienyl ring, a compound that reacts with the transition metal compound to form an ionic complex, and an organoaluminum compound; and catalysts modified by supporting catalytic components (a compound of a transition metal of Group 4 of the periodic table having a cyclopentadienyl ring, a compound that forms an ionic complex, an organoaluminum compound, etc.) on inorganic particles (silica, clay minerals, etc.).
  • Ziegler-Natta catalysts include catalysts that combine a titanium-containing solid transition metal component with an organometallic component.
  • ethylene- ⁇ -olefin copolymer commercially available products may be used.
  • examples of commercially available ethylene- ⁇ -olefin copolymers include Engage (registered trademark) manufactured by Dow Chemical Japan, Tafmer (registered trademark) manufactured by Mitsui Chemicals, Inc., Neozex (registered trademark) and Ultzex (registered trademark) manufactured by Prime Polymer Co., Ltd., Excellen FX (registered trademark), Sumikathene (registered trademark), and Esprene SPO (registered trademark) manufactured by Sumitomo Chemical Co., Ltd., etc.
  • the content thereof is preferably 1 part by mass or more and 50 parts by mass or less, more preferably 5 parts by mass or more and 40 parts by mass or less, and even more preferably 15 parts by mass or more and 30 parts by mass or less, per 100 parts by mass of the total of the resin component content and the talc content, from the viewpoint of obtaining good mechanical strength for automotive materials, industrial materials, etc.
  • the polypropylene-based resin composition according to the present embodiment contains talc as an inorganic filler.
  • the talc is hydrous magnesium silicate having a pyrophyllite-type three-layered crystal structure.
  • the talc is preferably obtained by pulverizing hydrous magnesium silicate, and more preferably, is a plate-like particle obtained by finely pulverizing molecular crystals of hydrous magnesium silicate to the order of unit layers.
  • the average particle size of talc is preferably 3 ⁇ m or less.
  • the average particle size of talc means the 50% equivalent particle size D50 obtained from the integral distribution curve of the sieve size measurement method using a centrifugal sedimentation type particle size distribution measurement device, in which the talc is suspended in a dispersion medium of water or alcohol.
  • the talc content is from 0.1 to 50 parts by mass, preferably from 0.1 to 40 parts by mass, more preferably from 0.1 to 30 parts by mass, and even more preferably from 0.1 to 25 parts by mass, per 100 parts by mass of the total of the resin component content and the talc content.
  • the polypropylene resin composition according to this embodiment may contain inorganic fillers other than talc.
  • inorganic fillers include calcium carbonate, barium sulfate, mica, crystalline calcium silicate, and fibrous magnesium oxysulfate.
  • the polypropylene-based resin composition according to the present embodiment contains, as an antistatic agent, a glycerin monostearate-based antistatic agent, an amine-based antistatic agent, and an amide-based antistatic agent.
  • Glycerin monostearate-based antistatic agents are ester compounds obtained from glycerin and stearic acid.
  • Examples of glycerin monostearate-based antistatic agents include monoglycerin monostearate and diglycerin monostearate.
  • Commercially available glycerin monostearate-based antistatic agents include "Electrostripper TS-5" manufactured by Kao Corporation, "Rikemal S-71-D” manufactured by Riken Vitamin Co., Ltd., and "MG-100” manufactured by Toho Chemical Co., Ltd.
  • Glycerin monostearate-based antistatic agents may be used alone or in combination of two or more types.
  • the content of the glycerin monostearate-based antistatic agent is from 0.01 to 0.09 parts by mass, preferably from 0.03 to 0.09 parts by mass, and more preferably from 0.05 to 0.09 parts by mass, per 100 parts by mass of the total of the resin component content and the talc content, from the viewpoint of reducing the amount of VOCs emitted in the molded product and obtaining good bleed resistance and antistatic properties.
  • the amine-based antistatic agent is preferably an ester compound of a fatty acid and a polyoxyalkylene alkylamine.
  • the fatty acid is preferably a saturated fatty acid having 12 to 22 carbon atoms. Examples of such fatty acids include lauric acid, tridecylic acid, myristic acid, pentadecylic acid, palmitic acid, margaric acid, stearic acid, nonadecylic acid, arachidic acid, henicosylic acid, and behenic acid.
  • the amine-based antistatic agent is preferably stearyl diethanolamine monostearate. Only one type of amine-based antistatic agent may be used, or two or more types may be used in combination.
  • the amide-based antistatic agent is preferably an amide compound of a fatty acid and diethanolamine, specifically, an N,N'-di(hydroxyethyl)alkylamide represented by the following formula (I).
  • C n H 2n+1 CON(CH 2 CH 2 OH) 2 Formula (I) (In formula (I), n represents an integer of 17 or more.)
  • N,N'-di(hydroxyethyl)alkylamides include coconut fatty acid diethanolamide, lauric acid diethanolamide, tridecylic acid diethanolamide, pentadecylic acid diethanolamide, palmitic acid diethanolamide, heptadecylic acid diethanolamide, oleic acid diethanolamide, stearic acid diethanolamide, nonadecanoic acid diethanolamide, arachidic acid diethanolamide, etc.
  • the N,N'-di(hydroxyethyl)alkylamide is preferably stearyl diethanolamide.
  • the total content of the amine-based antistatic agent and the amide-based antistatic agent is from 0.09 to 0.7 parts by mass, preferably from 0.15 to 0.5 parts by mass, and more preferably from 0.2 to 0.3 parts by mass, per 100 parts by mass of the total of the resin component content and the talc content, from the viewpoint of reducing the amount of VOCs emitted in the molded product and obtaining good bleed resistance and antistatic performance.
  • the ratio of the amine-based antistatic agent to the amide-based antistatic agent is from 40/60 to 89/11, preferably from 45/55 to 75/25, and more preferably from 55/45 to 60/40, from the viewpoint of reducing the amount of VOCs emitted in the molded product and obtaining good bleed resistance and antistatic performance.
  • the total content of the glycerin monostearate-based antistatic agent, the amine-based antistatic agent, and the amide-based antistatic agent is from 0.10 parts by mass to 0.79 parts by mass, preferably from 0.10 parts by mass to 0.50 parts by mass, and more preferably from 0.20 parts by mass to 0.40 parts by mass, from the viewpoint of reducing the amount of VOCs emitted in the molded product and obtaining good bleed resistance and antistatic performance.
  • the polypropylene resin composition according to the present embodiment further contains a lubricant.
  • the lubricant include higher fatty acid amides that do not contain a hydroxyl group in their chemical structure.
  • the higher fatty acid amide may be at least one selected from the group consisting of fatty acid monoamides and fatty acid bisamides.
  • the fatty acid monoamides include lauric acid amide, stearic acid amide, oleic acid amide, behenic acid amide, and erucic acid amide.
  • the fatty acid bisamides include methylene bisstearylamide, ethylene bisstearylamide, ethylene bisoleylamide, and hexamethylene bisstearylamide.
  • the lubricant content is preferably 0.01 parts by mass or more and 1.0 parts by mass or less, and more preferably 0.01 parts by mass or more and 0.5 parts by mass or less, per 100 parts by mass of the total of the resin component content and the talc content.
  • the polypropylene resin composition according to the present embodiment further contains at least one pigment selected from the group consisting of carbon black, titanium oxide, fatty acid metal salts, phthalocyanine metal compounds, red iron oxide, ultramarine, and polyolefin wax.
  • the pigment may be in the form of a dry color or a master batch type.
  • the pigment content is preferably 0.1 parts by mass or more and 10 parts by mass or less, more preferably 0.1 parts by mass or more and 6 parts by mass or less, even more preferably 0.2 parts by mass or more and 3 parts by mass or less, and particularly preferably 0.4 parts by mass or more and 3 parts by mass or less, relative to 100 parts by mass of the total of the resin component content and the talc content.
  • the polypropylene resin composition according to the present embodiment may contain other additives as necessary, such as neutralizing agents, antioxidants, processing stabilizers, UV absorbers, nucleating agents, transparent nucleating agents, processing aids, metal soaps, foaming agents, antibacterial agents, plasticizers, flame retardants, crosslinking agents, crosslinking aids, and brightness enhancers.
  • additives such as neutralizing agents, antioxidants, processing stabilizers, UV absorbers, nucleating agents, transparent nucleating agents, processing aids, metal soaps, foaming agents, antibacterial agents, plasticizers, flame retardants, crosslinking agents, crosslinking aids, and brightness enhancers.
  • the method for producing the polypropylene resin composition according to this embodiment is not particularly limited, and can be produced, for example, by melt-kneading each component.
  • kneaders used for melt-kneading include single-screw extruders, twin-screw extruders, Banbury mixers, and heated rolls.
  • the melt-kneading temperature is preferably 170°C or higher and 250°C or lower, and the melt-kneading time is preferably 1 minute or higher and 20 minutes or lower.
  • the melt-kneading of each component may be performed simultaneously or sequentially.
  • the molded product according to this embodiment includes the polypropylene-based resin composition described above.
  • the molded product is a molded product molded by a conventionally known method. Examples of such molded products include injection molded products, press molded products, vacuum molded products, vacuum press molded products, pressure molded products, foam molded products, extrusion molded products, etc. Examples of the molding method for such molded products include injection molding, press molding, vacuum molding, vacuum press molding, pressure molding, foam molding, extrusion molding, etc.
  • the molded article according to this embodiment is preferably an injection molded article.
  • injection molding methods for forming the injection molded article include general injection molding, injection foam molding, supercritical injection foam molding, ultra-high speed injection molding, injection compression molding, injection press molding, gas-assisted injection molding, sandwich molding, sandwich foam molding, and insert-outsert molding.
  • the molded article according to this embodiment is preferably used as an automobile interior part.
  • automobile interior parts include door trims, pillars, instrument panels, consoles, rocker panels, arm rests, door panels, spare tire covers, etc.
  • the molded article according to this embodiment may be obtained by the method described in the following steps (A') and (B').
  • Step (A') A step of pulverizing a molded product containing the above-mentioned polypropylene-based resin composition to obtain a pulverized product.
  • Step (B') A step of molding the pulverized product to obtain a molded product containing the above-mentioned polypropylene-based resin composition.
  • a polypropylene-based resin made of a propylene-based polymer as a resin component, talc as an inorganic filler, and a glycerin monostearate-based antistatic agent, an amine-based antistatic agent, and an amide-based antistatic agent as antistatic agents With respect to 100 parts by mass of the total of the content of the resin component and the content of the talc, The content of the polypropylene-based resin is 50 parts by mass or more and 99.9 parts by mass or less, The content of the talc is 0.1 parts by mass or more and 50 parts by mass or less, the total content of the glycerin monostearate-based antistatic agent, the amine-based antistatic agent, and the amide-based antistatic agent is 0.10 parts by mass or more and 0.79 parts by mass or less; The content of the glycerin monostearate-based antistatic agent is 0.01 parts by mass or more and 0.09 parts by mass or less,
  • the reduced viscosity was measured for three concentrations of 0.1 g/dL, 0.2 g/dL, and 0.5 g/dL, the reduced viscosity was plotted against the concentration, and the intrinsic viscosity was calculated by the method of extrapolating the concentration to zero.
  • Resin Component ⁇ Propylene-Based Polymer Heterophagic Propylene Polymer Material (A)> Using a polymerization catalyst obtained by the method described in Example 1 of JP 2004-182981 A, a heterophasic propylene polymerization material (A) was produced as a propylene-based polymer by a liquid phase-gas phase polymerization method, the heterophasic propylene polymerization material (A) containing 87 parts by mass of a propylene homopolymer component (a) as a polymer (I) and 13 parts by mass of an ethylene-propylene random copolymer component (b) as a polymer (II).
  • heterophasic propylene polymer material (A) was as follows: Melt flow rate (temperature 230°C, load 2.16 kg): 55 g/10 min (a) Propylene homopolymer component Isotactic pentad fraction: 0.983 Intrinsic viscosity number: 0.90dL/g (b) Ethylene-propylene random copolymer Intrinsic viscosity: 6.0 dL/g Content of structural units derived from ethylene: 32% by mass
  • the physical properties of the ethylene- ⁇ -olefin copolymer (B) were as follows: Content of structural units derived from ethylene EG8200: 65% by mass (content of structural units derived from 1-octene: 35% by mass) EG8842: 44% by mass (content of structural units derived from 1-octene: 56% by mass) ⁇ Melt flow rate (temperature 190°C, load 2.16 kg) EG8200: 5g/10min EG8842: 1g/10min ⁇ Density EG8200: 0.870g/cm 3 EG8842: 0.857g/ cm3
  • Lubricant ⁇ Lubricant 1: Ethylene bis stearic acid amide: CAS No. 324-27431> "Alflow H-50S” manufactured by NOF Corporation was used. ⁇ Lubricant 2 Erucic acid amide: CAS No. 112-84-5> "Neutron S” manufactured by Nippon Fine Chemicals was used.
  • Neutralizing agent ⁇ Neutralizing agent 1 Calcium stearate: CAS No. 1592-23-0> Calcium stearate manufactured by Sakai Chemical Industry Co., Ltd. was used.
  • Antioxidant ⁇ Antioxidant 1 CAS No. 90498-90-1> "Sumilizer GA80” manufactured by Sumitomo Chemical Co., Ltd.
  • Antioxidant 2 CAS No. 26741-53-7> Songwon "SONGNOX6260”
  • Antioxidant 3 CAS No. 16545-54-3> "Sumilizer TPM” manufactured by Sumitomo Chemical Co., Ltd.
  • Antistatic Agent 1 Glycerin monostearate-based antistatic agent; CAS No. 31566-31-1> Kao Corporation "Electrostripper TS-5"
  • Antistatic agent 2 Mixture of ester compound of stearyldiethanolamine and stearic acid and stearyldiethanolamide compound> A known material was used.
  • Antistatic agent 3 stearyl diethanolamide compound> A known material was used.
  • HALS Hindered amine weathering agent
  • ADEKASTAB LA-52 "ADEKASTAB LA-52” manufactured by ADEKA Corporation
  • ⁇ Ultraviolet absorber CAS No. 4221-80-1> "Sumisorb 400” manufactured by Sumika Chemtex Co., Ltd. was used.
  • ⁇ Organic peroxide 8% masterbatch of di(2-tert-butylperoxyisopropyl)benzene> Perkadox 14, manufactured by Kayaku Akzo Co., Ltd. A mixture of 8% by mass of organic peroxide, 88% by mass of propylene homopolymer, and 4% by mass of SiO2 was used.
  • Aldehydes (acetaldehyde and acrolein) were measured using the following method. First, 5 L of nitrogen gas and the test strip were sealed in a 10 L Tedlar bag and heated at 80°C for 1 hour. 2 L of the resulting sample gas was collected into a 2,4-dinitrophenylhydrazine (DNPH) cartridge. After collection, the cartridge was eluted with acetonitrile, and the components eluted from the cartridge were measured using a high-performance liquid chromatograph (HPLC; Shimadzu Corporation, model: LC-20AD).
  • HPLC high-performance liquid chromatograph
  • the detection limit for acetaldehyde and acrolein was 0.15 ⁇ g/test strip, and when the amount of acetaldehyde and acrolein emitted was 0.15 ⁇ g/test strip, it was considered to be "below the detection limit.”
  • a flat plate of the resin composition having a length of 150 mm, a width of 90 mm, and a thickness of 3.0 mm was molded in the same manner as in the preparation of the test piece for the aldehyde measurement described above. Then, the measurement was performed in accordance with JIS-K-6911 using a HIOKI SM7110 (manufactured by Hioki E.E. Corporation).
  • Example 1 A resin composition containing 63 parts by mass of a propylene-based polymer: heterophasic propylene polymerization material (A) and a total of 26 parts by mass of an olefin-based polymer: ethylene- ⁇ -olefin copolymer (B) as resin components, (2) 11 parts by mass of talc as an inorganic filler, (3) 0.05 parts by mass of "Alflow H-50S” and 0.2 parts by mass of "Neutron S” as lubricants, (4) 0.05 parts by mass of calcium stearate as a neutralizing agent, (5) 0.05 parts by mass of "Sumilizer GA80” and 0.05 parts by mass of "SONGNOX 6260” as antioxidants, and 0.03 parts by mass of "Sumilizer TPM", (6) 0.05 parts by mass of "Electrostripper” as an antistatic agent, (7) Other additives were added in the proportions of 0.08 parts by mass of "ester compound of stearyl diethanolamine and
  • the melt-kneading conditions were a cylinder temperature of 230°C, a discharge rate of 50 kg/hour, a screw speed of 200 rpm, and an oxygen concentration of 2% in the feed hopper.
  • the oxygen concentration in the feed hopper was measured by inserting a sensor equipped in a portable oxygen concentration meter into the purge resin inlet attached to the feed hopper.
  • the condition of an oxygen concentration of 2% was also achieved by circulating nitrogen gas into the feed hopper.
  • the resulting resin composition was used to measure aldehydes and surface resistivity according to the evaluation method described above.
  • Example 2 Comparative Examples 1 to 4
  • Example 2 The same procedure as in Example 1 was carried out, except that the amounts of the antistatic agent “Electrostripper TS-5”, “ester compound of stearyl diethanolamine and stearic acid”, and “stearyl diethanolamide compound” were changed as shown in Table 1.
  • Table 1 shows the blending amount of (6) antistatic agent in Examples 1 and 2 and Comparative Examples 1 to 4, as well as the aldehyde measurement results and surface resistivity measurement results for the injection molded bodies of the polypropylene resin composition obtained by granulation.
  • the injection molded articles of each embodiment that satisfy all of the constituent requirements of the present invention have excellent antistatic properties and can relatively reduce the amount of VOC emissions, particularly the amount of acetaldehyde and acrolein emitted.

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Abstract

La présente invention concerne : une composition de résine à base de polypropylène qui présente d'excellentes propriétés antistatiques et permet d'obtenir un corps moulé dans lequel la quantité d'émission d'acétaldéhyde et d'acroléine est relativement réduite ; et un corps moulé.　Une composition de résine à base de polypropylène selon la présente invention contient une résine à base de polypropylène qui est composée d'un polymère à base de propylène et sert de composant de résine, du talc qui sert de charge inorganique, et un agent antistatique à base de monostéarate de glycérol, un agent antistatique à base d'amine et un agent antistatique à base d'amide qui servent d'agents antistatiques. Par rapport à un total de 100 parties en masse de la teneur en composant de résine et de la teneur en talc, la teneur en résine à base de polypropylène est de 50 parties en masse à 99,9 parties en masse, la teneur en talc est de 0,1 partie en masse à 50 parties en masse, la teneur totale en agent antistatique à base de monostéarate de glycérol, en agent antistatique à base d'amine et en agent antistatique à base d'amide est de 0,10 partie en masse à 0,79 partie en masse, et la teneur en agent antistatique à base de monostéarate de glycérol est de 0,01 partie en masse à 0,09 partie en masse. Le rapport entre l'agent antistatique à base d'amine et l'agent antistatique à base d'amide est de 40/60 à 89/11.
PCT/JP2024/031145 2023-09-12 2024-08-30 Composition de résine à base de polypropylène et article moulé Pending WO2025057768A1 (fr)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002212353A (ja) * 2001-01-19 2002-07-31 Grand Polymer Co Ltd ポリプロピレン樹脂組成物
JP2009167406A (ja) * 2007-12-21 2009-07-30 Sumitomo Chemical Co Ltd ポリプロピレン系樹脂組成物及びそれからなる成形体
CN101851373A (zh) * 2010-06-02 2010-10-06 王锦江 一种bopp薄膜用的高效抗静电滑爽母料及其生产工艺
JP2014201615A (ja) * 2013-04-02 2014-10-27 住友化学株式会社 プロピレン樹脂組成物及びそれからなる成形体

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002212353A (ja) * 2001-01-19 2002-07-31 Grand Polymer Co Ltd ポリプロピレン樹脂組成物
JP2009167406A (ja) * 2007-12-21 2009-07-30 Sumitomo Chemical Co Ltd ポリプロピレン系樹脂組成物及びそれからなる成形体
CN101851373A (zh) * 2010-06-02 2010-10-06 王锦江 一种bopp薄膜用的高效抗静电滑爽母料及其生产工艺
JP2014201615A (ja) * 2013-04-02 2014-10-27 住友化学株式会社 プロピレン樹脂組成物及びそれからなる成形体

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