WO2024176859A1 - Composition de caoutchouc fluoré et joint pour véhicule électrique - Google Patents

Composition de caoutchouc fluoré et joint pour véhicule électrique Download PDF

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Publication number
WO2024176859A1
WO2024176859A1 PCT/JP2024/004315 JP2024004315W WO2024176859A1 WO 2024176859 A1 WO2024176859 A1 WO 2024176859A1 JP 2024004315 W JP2024004315 W JP 2024004315W WO 2024176859 A1 WO2024176859 A1 WO 2024176859A1
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Prior art keywords
fluororubber
fluororubber composition
seal
composition
vulcanized
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PCT/JP2024/004315
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English (en)
Japanese (ja)
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俊介 阿部
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Nok株式会社
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Publication of WO2024176859A1 publication Critical patent/WO2024176859A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers

Definitions

  • the present invention relates to a fluororubber composition.
  • Fluorororubber compositions have excellent resistance to oil and fuel, and are used as a material for sealing materials such as oil seals, O-rings, and packings in a wide range of fields, including automobiles and industrial machinery.
  • electric vehicles hereinafter sometimes referred to as "EVs”
  • EVs electric vehicles
  • a seal is installed between the motor, which acts as the prime mover, and the reduction gear.
  • Patent Document 1 Japanese Patent No. 62883978 discloses Tecnoflon BR9151 and BR9171 as rubbers that do not deteriorate due to reactions with additives in oil.
  • Patent Document 2 International Publication No. 2014/175079 discloses a fluororubber made of vinylidene fluoride-hexafluoropropylene-tetrafluoroethylene-ethylene-perfluoro(methyl vinyl ether) 5-component copolymer, and discloses Tecnoflon BR9151 and BR9171 as specific examples of such fluororubber.
  • insulating fluororubber compositions are generally used as materials for seals.
  • the seals are made of insulating fluororubber compositions, the seals will become charged and a potential difference will occur, raising concerns about the occurrence of electrolytic corrosion in the vehicle interior unit.
  • radio noise will be generated due to electromagnetic waves generated by the charging of the seals.
  • conductive parts such as carbon earth brushes and knuckle earths are connected to the reducer and body earth to prevent the charging and electrolytic corrosion of the vehicle interior unit.
  • conventional fluororubber compositions are desired to have excellent roll processability as well as excellent electrical conductivity from the viewpoint of preventing static electricity and electrolytic corrosion.
  • Patent No. 6288398 International Publication No. 2014/175079
  • the present invention provides a fluororubber composition that has excellent roll processability and electrical conductivity.
  • the gist and configuration of the present invention are as follows.
  • [1] A fluorororubber composition containing a peroxide-vulcanized fluororubber and 16 to 26 mass % of a conductive agent.
  • [2] The fluororubber composition according to the above [1], having a volume resistivity of 1.0 ⁇ cm or less.
  • [3] A seal for an electric vehicle, comprising the fluororubber composition according to the above [1] or [2].
  • FIG. 1 is a diagram illustrating a sealing device having a conductive part that includes a vulcanized fluororubber composition according to one embodiment as a seal.
  • the vulcanized fluororubber composition of the present invention contains a peroxide vulcanization-based fluororubber and 16 to 26% by mass of a conductive agent.
  • a peroxide vulcanization-based fluororubber as the fluororubber, the elongation of the fluororubber composition can be improved, and the roll processability of the fluororubber composition can be improved.
  • a conductive agent content of 16% by mass or more in the fluororubber composition the fluororubber composition can have excellent electrical conductivity.
  • the hardness and viscosity of the fluororubber composition become appropriate, and the roll processability of the fluororubber composition can be improved.
  • the seal itself has excellent electrical conductivity, so that extra parts such as earth brushes and knuckle earths are not required as in conventional EVs, and space can be saved in the EV.
  • the fluororubber composition is preferably a fluororubber composition for shaft seals or packing seals, and more preferably a fluororubber composition for seals such as shafts and packings of electric vehicles.
  • the volume resistivity of the fluororubber composition after vulcanization is preferably 1.0 ⁇ cm or less, more preferably 0.5 ⁇ cm or less, and even more preferably 0.3 ⁇ cm or less.
  • a sample made of the vulcanized fluororubber composition with dimensions of 140 mm x 100 mm x 2 mm is used. This sample is prepared by preparing the fluororubber composition, performing primary vulcanization at 160-200°C for 3-30 minutes in a molding press to obtain dimensions of 140 mm x 100 mm x 2 mm, and then performing secondary vulcanization at 150-250°C for 0.5-24 hours in a thermostatic bath.
  • the volume resistivity of the fluororubber composition does not change within the above temperature and vulcanization time ranges.
  • the volume resistivity of the fluororubber composition is measured according to the four-probe method in accordance with JIS K7194:1994, using a Hioki Milliohm High Tester 3540 (product name) measuring device, and is measured at room temperature using the parallel terminal electrode method.
  • the fluorororubber is not particularly limited as long as it is a peroxide vulcanized fluororubber after vulcanization, but one or more homopolymers or copolymers of fluorine-containing olefins can be used.
  • fluorine-containing olefins examples include vinylidene fluoride, hexafluoropropylene, pentafluoropropylene, trifluoroethylene, trifluorochloroethylene, tetrafluoroethylene, vinyl fluoride, perfluoroacrylic acid ester, perfluoroalkyl acrylate, perfluoromethyl vinyl ether, perfluoroethyl vinyl ether, and perfluoropropyl vinyl ether. These fluorine-containing olefins can be used alone or in combination of two or more.
  • fluorine-containing rubbers examples include vinylidene fluoride-hexafluoropropylene binary copolymers, vinylidene fluoride-tetrafluoroethylene-hexafluoropropylene ternary copolymers, and vinylidene fluoride-hexafluoropropylene-perfluoroalkyl vinyl ether ternary copolymers.
  • Fluorororubber may be obtained by solution polymerization, suspension polymerization, or emulsion polymerization, or may be obtained as a commercially available product.
  • Examples of commercially available fluororubber include Chemours' products “VITON (registered trademark) GBL-600S” and “VITON (registered trademark) GLT-600S,” and Daikin Industries' products “DAI-EL (registered trademark) GBR-6002” and “DAI-EL (registered trademark) G-901.”
  • Fluororubber is a peroxide-vulcanized fluororubber that is vulcanized with peroxide.
  • Peroxide-vulcanized fluororubber is a polymer that introduces cure sites such as Br or I to the molecular chain end at the time of polymerization and uses this to undergo a vulcanization reaction.
  • Peroxide-vulcanized fluororubber can be confirmed by, for example, (a) detecting Br or I in the fluororubber by elemental analysis using XRF (X-ray fluorescence analysis), or (b) not detecting elements derived from an acid acceptor such as Mg or Ca in the molded fluororubber composition by elemental analysis.
  • Peroxide-vulcanized fluororubber does not require an acid acceptor compared to polyol-vulcanized fluororubber, so the fluororubber composition can achieve excellent roll processability. For this reason, in a preferred embodiment of the present invention, the fluororubber composition does not contain an acid acceptor.
  • the fluororubber composition after vulcanization contains 16 to 26% by mass of the conductive agent.
  • the fluororubber composition can have excellent electrical conductivity and roll processability by containing 16 to 26% by mass of the conductive agent.
  • the conductive agent is not particularly limited as long as it can impart electrical conductivity to the fluororubber composition, but the conductive agent is preferably at least one material selected from the group consisting of Ketjen black, graphite, carbon nanotubes, and carbon fibers.
  • the content of the conductive agent in the fluororubber composition is preferably 18 to 26% by mass, more preferably 20 to 26% by mass, and even more preferably 22 to 26% by mass.
  • the conductive agent in the fluororubber composition may be one type or two or more types.
  • the fluororubber composition may further contain a processing aid.
  • the processing aid is not particularly limited, but is preferably at least one material selected from the group consisting of vegetable wax, polyester, and fluoropolyether derivatives.
  • the content of the processing aid in the fluororubber composition is preferably 3 to 14 mass%, more preferably 6 to 10 mass%, and even more preferably 6 to 7 mass%.
  • the fluororubber composition of the present invention contains a fluororubber and a conductive agent, and the fluororubber composition may further contain, as components other than the fluororubber and the conductive agent, an antioxidant; a thermoplastic resin; a plasticizer; a softener; a foaming agent; a foaming assistant; a colorant; a dispersant; a flame retardant; a tackifier; a release agent; various metal powders, and the like.
  • the fluororubber composition can be obtained by kneading 16 to 26% by mass of a conductive agent, a peroxide-vulcanized fluororubber, and, if necessary, materials such as a processing aid, using kneading equipment (rolls, kneaders, etc.).
  • the vulcanized fluororubber composition of the present invention can be obtained by adding a vulcanizing agent to the fluororubber composition obtained as described above, and then heating the composition in a molded state into a predetermined shape.
  • a known manufacturing device can be used.
  • the fluororubber composition can be put into a cavity of a predetermined shape using an injection molding machine, a compression molding machine, or the like, and heated under appropriate conditions to obtain a vulcanized fluororubber composition.
  • the vulcanization may be performed in multiple stages.
  • the fluororubber composition may be pressed into a predetermined shape and subjected to primary vulcanization, and the fluororubber composition after the primary vulcanization may be further subjected to secondary vulcanization.
  • a molded product of a desired shape can be produced by molding and vulcanizing the fluororubber composition.
  • the product containing the fluororubber composition is preferably a seal such as a shaft seal or a packing seal for an electric vehicle.
  • the seal for an electric vehicle preferably has an overall electrical conductivity of 10 ⁇ or less, more preferably 9 ⁇ or less, and even more preferably 5 ⁇ or less.
  • the electrical conductivity of the entire seal can be evaluated as an electrical resistance value measured under the conditions of 500kHz/5V using an impedance analyzer (IM3570 (device name), manufactured by Hioki E.E.C. Co., Ltd.) after the seal is placed so as to be engaged between the shaft and the housing of a rotation tester and the shaft and the housing are in contact with a conductor.
  • IM3570 impedance analyzer
  • FIG. 1 is a diagram showing one embodiment of a sealing device having a conductive part 120 containing the vulcanized fluororubber composition of the present invention as a seal, and shows a schematic cross-sectional view (schematic cross-sectional view) of the rotating shaft 20 and housing 38 of the sealing device 40, taken along a plane including the axis ⁇ of the rotating shaft 20.
  • the sealing device 40 is disposed in a gap 107 between the outer surface 20s of the rotating shaft 20 and the inner surface 38s that constitutes the shaft hole in the housing 38, which has a shaft hole into which the rotating shaft 20 is inserted.
  • the rotating shaft 20 may be, for example, the motor shaft of a drive motor in an EV (Electric Vehicle) or HEV (Hybrid Electric Vehicle).
  • the rotating shaft 20 is rod-shaped (cylindrical) and its cross section is typically circular.
  • the housing 38 is typically grounded.
  • the sheath pipe portion 110 of the sealing device 40 shown in FIG. 1 will be described below.
  • the sheath pipe portion 110 is an annular portion that is directly or indirectly fixed to the outer surface 20s of the rotating shaft 20.
  • the sheath pipe portion 110 is directly fixed to the outer surface 20s of the rotating shaft 20.
  • the means for fixing the sheath pipe portion 110 to the outer surface 20s of the rotating shaft 20 is not particularly limited.
  • the sheath pipe portion 110 and the outer surface 20s of the rotating shaft 20 may be fitted together by a press fit method to fix the sheath pipe portion 110 to the outer surface 20s of the rotating shaft 20.
  • the sheath pipe portion 110 may be fixed to the outer surface 20s of the rotating shaft 20 using an adhesive or the like.
  • the sheath tube portion 110 comprises a fixed portion 110a extending in a direction parallel to the axis ⁇ of the rotating shaft 20, and a support portion 110b connecting to the end of the fixed portion 110a and extending in a direction approaching the inner surface 38s of the housing 38.
  • the fixed portion 110a and the support portion 110b are each plate-shaped.
  • the fixed portion 110a is cylindrical
  • the support portion 110b is disk-shaped with a through hole in the center.
  • the fixed portion 110a and the support portion 110b are approximately perpendicular in a cross section obtained by cutting the rotating shaft 20 along a plane including the axis ⁇ . Therefore, the sheath tube portion 110 has an approximately L-shaped cross section.
  • approximately vertical means that it does not have to be completely vertical.
  • the fixed portion 110a and the support portion 110b form an angle of 90 degrees, but this angle may be 75 to 105 degrees (preferably 80 to 100 degrees, and more preferably 85 to 95 degrees).
  • the sheath tube portion 110 is preferably made of a metal, and more preferably a metal having electrical conductivity. Such metals include stainless steel, cold rolled steel (SPCC), brass, and aluminum.
  • the sheath tube portion 110 does not have to be made of a metal. For example, it may be made of resin.
  • the sheath tube portion 110 can be formed by pressing or forging.
  • the conductive part 120 of the sealing device 40 shown in FIG. 1 will be described below.
  • the conductive part 120 is ring-shaped, with the ring outer peripheral part 120a in contact with the inner surface 38s of the housing 38, and the main surface 120s of the conductive part 120 being fixed to the sleeve pipe part 110.
  • the main surface 120s of the conductive part 120 is fixed to the support part 110b of the sleeve pipe part 110.
  • the conductive part 120 functions as a seal containing the vulcanized fluororubber composition of the present invention, and is sheet-shaped or plate-shaped.
  • the cross section is substantially L-shaped, and the main surface 120s of the conductive part 120 is in contact with the main surface of the plate-shaped support part 110b in the sleeve pipe part 110.
  • the main surface 120s of the conductive part 120 is in close contact with the main surface of the support part 110b.
  • the main surface 120s of the ring outer periphery 120a is in contact with the inner surface 38s of the housing 38.
  • centrifugal force is applied to the sealing device 40, and it is preferable that the main surface 120s of the ring outer periphery 120a is in close contact with the inner surface 38s of the housing 38.
  • the conductive part 120 deformed so that the cross section is approximately L-shaped the ring outer periphery 120a is cylindrical, and the remaining part is disk-shaped with a through hole in the center.
  • the centrifugal force F generated by the rotation of the rotating shaft 20 increases the force with which the conductive part 120 is pressed against the inner surface 38s of the housing 38 compared to before the rotating shaft 20 rotates.
  • centrifugal force F is applied to the conductive part 120, and the ring outer periphery 120a of the conductive part 120 is pressed against the inner surface 38s of the housing 38.
  • the ring outer periphery 120a of the conductive part 120 is stably attached to the inner surface 38s of the housing 38, ensuring electrical continuity between the rotating shaft 20 and the housing 38.
  • the method of fixing the main surface 120s of the conductive portion 120 to the main surface of the support portion 110b of the sheath tube portion 110 is not particularly limited, and for example, they can be fixed using an adhesive. However, if they are fixed using metal bolts and nuts without using an adhesive, it is easier to ensure electrical continuity between the conductive portion 120 and the sheath tube portion 110, which is preferable as it results in easier electrical continuity between the rotating shaft 20 and the housing 38.
  • a fluororubber composition was produced by kneading materials in the proportions shown in the following Table 1.
  • the names of the materials used in each example are shown below.
  • Type 1 (ASTM) fluororubber VITON (registered trademark) A-500 (manufactured by Chemours)
  • Type 2 (ASTM) fluororubber VITON (registered trademark) B-600 (manufactured by Chemours)
  • Type 3 (ASTM) fluororubber VITON (registered trademark) GLT-600S (manufactured by Chemours)
  • Type 6 (ASTM) fluororubber Daiel (registered trademark) GBR-6002 (manufactured by Daikin Industries, Ltd.)
  • Ketjenblack A KETJENBLACK EC600JD (manufactured by Lion Specialty Chemicals)
  • Ketjen Black B Denka Black
  • the fluororubber compositions produced as described above were evaluated for hardness (Durometer A hardness), hardness (IRHD (International Rubber Hardness Degree) hardness), volume resistivity, seal conductivity, and roll processability. The preparation and measurement methods for the samples for each evaluation are shown below.
  • Hardness (Durometer A hardness): A fluororubber composition was vulcanized under the conditions of primary vulcanization at 180°C for 4 minutes and secondary vulcanization at 230°C for 9 hours to prepare a sample having a thickness of 2 mm. The durometer A hardness of this sample was then measured at room temperature using a constant pressure rubber hardness tester P1-A (device name) manufactured by Kobunshi Keiki Co., Ltd. in accordance with JIS K6253-2:2012.
  • P1-A device name
  • IRHD hardness The fluororubber composition was vulcanized under the conditions of primary vulcanization at 180°C for 4 minutes and secondary vulcanization at 230°C for 9 hours to prepare a sample having dimensions of 140 mm x 100 mm x 2 mm. The IRHD hardness of this sample was then measured under IRHD (micro) conditions using a Digitest II (device name) manufactured by Burleis Co., Ltd. in accordance with JIS K6253-2:2012.
  • volume resistivity The fluororubber composition was vulcanized under the conditions of primary vulcanization at 180°C for 4 minutes and secondary vulcanization at 230°C for 9 hours to prepare a sample having dimensions of 140 mm x 100 mm x 2 mm. Next, the sample was measured according to the four-probe method in accordance with JIS K7194:1994, and the volume resistivity was measured at room temperature using a milliohm high tester 3540 (device name) manufactured by Hioki E.E.C., using the parallel terminal electrode method.
  • the fluororubber composition was vulcanized under the conditions of primary vulcanization at 180°C for 4 minutes and secondary vulcanization at 230°C for 9 hours to mold an oil seal with an inner diameter of 85 mm, an outer diameter of 105 mm, and a width of 13 mm.
  • the oil seal was installed so as to be fitted between the shaft and housing of a rotation tester, and the electrical resistance value was measured under the conditions of 500 kHz/5 V using an impedance analyzer (IM3570 (device name), manufactured by Hioki E.E.C. Co., Ltd.) with the shaft and housing in contact with a conductor.
  • IM3570 impedance analyzer
  • the fluororubber compositions of the present invention had a volume resistivity of 0.3 ⁇ cm or less, a seal conductivity of 9 ⁇ or less, and roll processability was also rated "good.”
  • the fluororubber compositions of the comparative examples all had very high volume resistivities and seal conductivity values, or the fluororubber compositions could not be kneaded, or the roll processability was rated "poor.” From the above, it was confirmed that the present invention can provide a fluororubber composition with excellent conductivity and roll processability.
  • Rotating shaft 20s Outer surface of rotating shaft 38 Housing 38s Inner surface of housing 40 Sealing device 107 Gap 110 Sleeve tube portion 110a Fixed portion 110b in sleeve tube portion Support portion 120 Conducting portion 120a Ring outer periphery portion 120s in conducting portion Main surface of conducting portion ⁇ Axial center of rotating shaft

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

Abstract

Le but de la présente invention est de fournir une composition de caoutchouc fluoré qui présente d'excellentes propriétés d'usinage au rouleau et une excellente conductivité électrique.　La composition de caoutchouc fluoré contient un caoutchouc fluoré vulcanisé au peroxyde et 16 à 26% en masse d'un agent conducteur.
PCT/JP2024/004315 2023-02-24 2024-02-08 Composition de caoutchouc fluoré et joint pour véhicule électrique WO2024176859A1 (fr)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003013042A (ja) * 2001-06-28 2003-01-15 Mitsubishi Cable Ind Ltd 摺動部用シール材
JP2011001478A (ja) * 2009-06-19 2011-01-06 Tigers Polymer Corp カーボンブラック含有高導電性フッ素ゴム組成物
JP2011032465A (ja) * 2009-07-08 2011-02-17 Mitsubishi Cable Ind Ltd ゴム組成物及びゴム部材
WO2012026553A1 (fr) * 2010-08-25 2012-03-01 ダイキン工業株式会社 Composition de caoutchouc fluoré
JP2016000806A (ja) * 2014-05-23 2016-01-07 ダイキン工業株式会社 フッ素ゴム組成物及びフッ素ゴム成形品
JP2019137838A (ja) * 2018-02-09 2019-08-22 ダイキン工業株式会社 フッ素ゴム組成物及びその成形品
JP2021143306A (ja) * 2020-03-13 2021-09-24 株式会社フコク ゴム組成物およびそれを用いたゴム部材

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003013042A (ja) * 2001-06-28 2003-01-15 Mitsubishi Cable Ind Ltd 摺動部用シール材
JP2011001478A (ja) * 2009-06-19 2011-01-06 Tigers Polymer Corp カーボンブラック含有高導電性フッ素ゴム組成物
JP2011032465A (ja) * 2009-07-08 2011-02-17 Mitsubishi Cable Ind Ltd ゴム組成物及びゴム部材
WO2012026553A1 (fr) * 2010-08-25 2012-03-01 ダイキン工業株式会社 Composition de caoutchouc fluoré
JP2016000806A (ja) * 2014-05-23 2016-01-07 ダイキン工業株式会社 フッ素ゴム組成物及びフッ素ゴム成形品
JP2019137838A (ja) * 2018-02-09 2019-08-22 ダイキン工業株式会社 フッ素ゴム組成物及びその成形品
JP2021143306A (ja) * 2020-03-13 2021-09-24 株式会社フコク ゴム組成物およびそれを用いたゴム部材

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