WO2006041186A1 - Composition de résine contenant une fibre de carbone produite par la vapeur et utilisation de celle-ci - Google Patents

Composition de résine contenant une fibre de carbone produite par la vapeur et utilisation de celle-ci Download PDF

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Publication number
WO2006041186A1
WO2006041186A1 PCT/JP2005/019150 JP2005019150W WO2006041186A1 WO 2006041186 A1 WO2006041186 A1 WO 2006041186A1 JP 2005019150 W JP2005019150 W JP 2005019150W WO 2006041186 A1 WO2006041186 A1 WO 2006041186A1
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Prior art keywords
resin composition
carbon fiber
vapor grown
resin
grown carbon
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PCT/JP2005/019150
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English (en)
Inventor
Yuji Nagao
Ryujji Yamamoto
Original Assignee
Showa Denko K.K
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Publication of WO2006041186A1 publication Critical patent/WO2006041186A1/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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/06—Elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/09—Articles with cross-sections having partially or fully enclosed cavities, e.g. pipes or channels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/09—Articles with cross-sections having partially or fully enclosed cavities, e.g. pipes or channels
    • B29C48/10—Articles with cross-sections having partially or fully enclosed cavities, e.g. pipes or channels flexible, e.g. blown foils
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
    • B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
    • B29C48/21—Articles comprising two or more components, e.g. co-extruded layers the components being layers the layers being joined at their surfaces
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
    • B29C45/0001—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor characterised by the choice of material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
    • B29C48/17—Articles comprising two or more components, e.g. co-extruded layers the components having different colours
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
    • B29C49/0005—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor characterised by the material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C51/00—Shaping by thermoforming, i.e. shaping sheets or sheet like preforms after heating, e.g. shaping sheets in matched moulds or by deep-drawing; Apparatus therefor
    • B29C51/002—Shaping by thermoforming, i.e. shaping sheets or sheet like preforms after heating, e.g. shaping sheets in matched moulds or by deep-drawing; Apparatus therefor characterised by the choice of material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2079/00—Use of polymers having nitrogen, with or without oxygen or carbon only, in the main chain, not provided for in groups B29K2061/00 - B29K2077/00, as moulding material
    • B29K2079/08—PI, i.e. polyimides or derivatives thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
    • B29K2995/0037—Other properties
    • B29K2995/0072—Roughness, e.g. anti-slip
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
    • B29K2995/0037—Other properties
    • B29K2995/0072—Roughness, e.g. anti-slip
    • B29K2995/0073—Roughness, e.g. anti-slip smooth
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
    • B29K2995/0037—Other properties
    • B29K2995/0089—Impact strength or toughness
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2023/00—Tubular articles
    • B29L2023/22—Tubes or pipes, i.e. rigid

Definitions

  • the present invention relates to a resin composition for a seamless belt and a seamless belt obtained by molding the composition. More specifically, the present invention relates to a resin composition for a seamless belt to be used for a photoreceptor, a charge belt, a transfer belt, a fixing belt, or the like in an image forming apparatus such as an electrophotographic copyingmachine or a laserprinter, the resin composition being excellent in durability, heat resistance and surface smoothness, and the resin composition having stable electrical resistance properties, and a seamless belt using the composition.
  • the present invention relates to a resin composition for a tray, excellent in heat resistance, antistatic property, etc., onto which tray a magnetic head for a hard disk drive is mounted, and onwhich tray themagnetichead is processed, washed, transferred, stored, etc.; and a tray using the composition, for carrying a magnetic head for magnetic disk drive.
  • the present invention relates to: an electroconductive thermoplasticresincomposition for afuel tube, containing as a conductive filler a specific vapor grown carbon fiber; and a fuel tube using the composition. More specifically, the present invention relates to: an electroconductive thermoplastic resin composition which has stable electrical resistance property, which is excellent in surface smoothness, toughness, extrusionmoldabiIityandthe like inabalancedmanner withoutimpairingtheelongationpropertyofathermoplasticresin itself, and which can be suitably used for a fuel tube for use inan automobile or the like; and a fuel tubeusing the composition.
  • a rotating body made of metal, plastic, rubber or the like is used for a photoreceptor, a charged body, a transferring member, a fixing member or the like.
  • rotating body include those having a drum-like shape and those made of resin having a belt-like shape.
  • the belt In a case where a seamless belt is used as a rotating body, the belt requires heat resistance and heat cycle durability as well as mechanical properties such as tensile strength.
  • a seamless belt used in such printer or copying machine must have a small coefficient of thermal expansion and be excellent in dimensional stability.
  • thermosetting polyimide or a heat-resistant fluorine-based resin has been used for a seamless belt.
  • a transfer belt, an intermediate transfer belt, a fixing belt or the like for electrophotography in a copying machine, a printer, or the like it is necessary to regulate the electrical resistivity to be 10 6 to 10 13 ⁇ -cm. Furthermore, it is required that difference between the surface resistivity and the volume resistivity be small, that fluctuation in the surface resistivity and the volume resistivity with time be small and that the surface resistivity and the volume resistivity depend little on environmental changes.
  • thermosetting polyimide or a heat-resistant fluorine-based resin used for a seamless belt has insulating property
  • conductive filler tobe generallyusedin include: carbon materials each having a graphite structure such as carbon black, graphite, vapor grown carbon fiber and carbon fiber; metal materials such as metal fiber, metal powder and metal foil, and metal oxides; and inorganic filler coated with metal (JP 2000-248086 A, JP 2003-255640 A and JP 2003-246927 A) .
  • miniaturization of conductive filler increase in aspect ratio of the filler, increase in specific surface area of the filler or the like is effective for obtaining high conductivity with a small addition amount of the filler.
  • carbon black having an extremely large specific surface area and a hollow carbon fiber
  • carbon black and carbon nanotube each have a large specific surface area and hence has large surface energy, so that agglomeration readily occurs and the dispersibility into a resin is poor.
  • carbon black or the carbon nanotube is blended into a resin, there are problems of reduction in mechanical strength and variations in electrical resistance properties.
  • compositioncompoundedwithanantistatic agent whose electroconductive mechanism depends on ionic conduction, is susceptible to moisture in the environment.
  • the antistatic agent flows out during washing or long-term use of the composition, which leads to reduction in the antistatic property.
  • addition of a large amount of antistatic agent causes a problem such as decrease in heat resistance.
  • carbonblack and a carbon fiber are not influenced by humidity, washing and the like, they involve, for example, a problem that carbon particles or carbon fibers are apt to fall out of a molded product, to thereby damage a magnetic head.
  • thermoplastic resins have been mainly used for, for example, the ducts in the engine rooms of automobiles, and are produced by subjecting polyamide-based resins to blow molding or by extrusion molding saturated polyester-basedresins, polyamide resins, polyolefin resins, and thermoplastic polyurethane into tubes.
  • Polyamideresins polyamide 11 andpolyamide 12
  • polyester resins polyester resins
  • fluorine-based resins each having flexibility have been widely used for fuel tubes for automobiles.
  • a blow hollow molded product and a tube molded product are used inapplicationswhere anon-conductive liquidsuchas a fuel flows, there arises a seriousproblem.
  • JP 08-261374 Adiscloses amulti-layer synthetic resin tube having an inner layer composed of an electroconductive thermoplastic molding material.
  • the document shows a graphite-fibril having a fiber diameter of 10 ran and an aspect ratio of about 500 to 1,000 (that is, a carbon nanofiber) as a conductivityimpartingmaterial.
  • carbon black and a carbon nanotube each have a large specific surface area and hence has large surface energy, so each of them is apt to generate an agglomerate and has poor dispersibilityinto aresin.
  • thesematerials involve many problems when blended into a resin, such as reduction in mechanical strength, difficulty in obtaining surface smoothness and wide variation in elecrtoconductivity due to localization.
  • An object of the present invention is to provide a resin composition for a seamless belt showing stable electrical resistance properties and excellent in surface smoothness, durability and heat resistance and a seamless belt using the composition.
  • Another object of the present invention is to provide a tray for carrying amagnetic head for a magnetic disk drive, which tray is inexpensive, excellent in mechanical strength and an antistatic property, from which carbon fibers do not fall off .
  • Still another object of the present invention is to provide an electroconductive thermoplastic resin composition that can be suitably used for a tube for a fuel, the composition showing stable electrical resistance property, and the compositionbeing excellent insurface smoothness, durability, andheat resistance.
  • the inventors of the present invention have made extensive studies with a view to achieving the above object. As a result, they have found that the above objects can be achieved by using a resin composition with a specific vapor grown carbon fiber blended therein as a conductive filler, thereby completing the present invention.
  • one aspect of the present invention relates to: a resin composition for a seamless belt having the following constitution; a method of producing the resin composition; and a seamless belt using the resin composition.
  • a resin composition for a seamless belt containing a heat-resistant resin having a glass transition temperature of 100 0 C or higher and/or a melting point of 200 0 C or higher and a vapor grown carbon fiber having an average filament diameter of 50 to 130 nm in an amount of 1 to 30 parts by mass with respect to 100 parts by mass of the heat-resistant resin, wherein the volume resistivity of the resin composition is within a range of 1 x 10 5 to 1 x 10 13 ⁇ cm.
  • the resin composition for a seamless belt according to the above item Al further containing conductive carbon black in an amount of 1 to 10 parts by mass with respect to 100 parts by mass of the heat-resistant resin.
  • thermoplastic resin and thermosetting resin are examples of thermoplastic resin and thermosetting resin.
  • heat-resistant resin is at least one kind selected from a fluorine-based resin, polyimide, polyamide imide, polyether imide, polyether ether ketone, polysulfone, polyether sulfone, polybenzimidazole, polyphenylene sulfide, polyethylene naphthalate, polyallylate and an aromatic polyamide resin.
  • 2.5 mm is 10 ⁇ m or less.
  • AlO to A16 which is used for a transfer belt, an intermediate transfer belt, a transfer/fixing belt, an intermediate transfer/fixing belt or a fixing belt for use in an image forming apparatus utilizing an electrophotographic technique.
  • the seamless belt of the present invention which uses a specific vapor grown carbon fiber as a conductive filler, can showmore stable electrical resistance properties (such as small difference between the surface resistivity and the volume resistivity, small fluctuation in the surface resistivity and thevolumeresistivitywithtime, andlowdependenceof the surface resistivityandthevolume resistivityonenvironmental changes) .
  • the belt is excellent in surface smoothness, flexibility, durabilityandheat resistance (that is, inthebelt, wrinkles and dimensional changes hardly generate when it is repeatedly used for a long time period at a high temperature and underpressure) . Therefore, the belt can be preferably used for a photoreceptor belt, a charge belt, a transfer belt, a fixing belt or the like in an image forming apparatus such as a (color) laser printer or a (color) electrophotographic copying machine.
  • a resin composition for a tray for carrying a magnetic head for a magnetic disk drive composed of the following constitution; a carrier tray using the same; and methods of producing them.
  • a resin composition for a tray for carrying a magnetic head for a magnetic disk drive comprising a heat-resistant resin having a glass transition temperature of 100 0 C or higher and/or a melting point of 200 0 C or higher and a vapor grown carbon fiber having an average filament diameter of 50 to 130 nm in an amount of 1 to 30 parts by mass with respect to 100 parts by mass of the heat-resistant resin, wherein the volume resistivity of the resin composition is in the range of 1 x 10 2 to 1 x 10 8 ⁇ cm.
  • the resin composition for a carrier tray according to Bl wherein the heat-resistant resin is at least one kind selected from afluorine resin, polyimide, polyamide imide, polyether imide, polyether ether ketone, polysulfone, polyether sulfone, polybenzimidazole, polyphenylene sulfide, polyethylene naphthalate, polyallylate, aromatic polyamide, polycarbonate, modified polyphenylene ether, polybutylene terephthalate, polyethylene terephthalate, and a cycloolefin polymer.
  • the heat-resistant resin is at least one kind selected from afluorine resin, polyimide, polyamide imide, polyether imide, polyether ether ketone, polysulfone, polyether sulfone, polybenzimidazole, polyphenylene sulfide, polyethylene naphthalate, polyallylate, aromatic polyamide, polycarbonate, modified polyphenylene ether, polybutylene tere
  • the resin composition for a carrier tray according to Bl wherein theheat-resistant resinis apolyether ether ketone resin, a polycarbonate resin, a modified polyphenylene ether resin, polyphenylene sulfide, or a cycloolefin polymer.
  • the resin composition for a carrier tray according to Bl wherein the vapor grown carbon fiber has a specific surface area of 10 to 50 m 2 /g and an average aspect ratio of 65 to 500.
  • the resin composition for a carrier tray according to B4 wherein the vapor grown carbon fiber has a specific surface area of 15 to 40 m 2 /g, and have an average aspect ratio of 100 to 200.
  • the resin composition for a carrier tray according to Bl, wherein the number of branches of the vapor grown carbon fiber per length is 0.3/ ⁇ m or less.
  • a tray for carrying a magnetic head for a magnetic disk composed of the resin composition according to any one of Bl to B6, comprising an arm part, a head chip attached to the tip of the arm part and a lead wire connected to the head chip.
  • the ten point average roughness (Rz) at a cut-off wavelength of 2.5 mm is 10 ⁇ m or less.
  • a method of producing a tray for carrying a magnetic head for a magnetic disk drive wherein the resin composition for a tray for carrying a magnetic head for a magnetic disk drive according to any one of Bl to B6 is subjected to injectionmolding.
  • the tray for carrying a magnetic head for a magnetic disk drive of the present invention uses a specific vapor grown carbon fiber which can be favorably dispersed as a conductive filler into a heat-resistant resin; and provide desired antistatic property even in a small amount. Unlike a case where carbon black is used, in a case of using the tray of the present invention, no falling-off of particles from the tray occurs and therefore, a magnetic head can be prevented from being damaged.
  • Still another aspect of the present invention relates to: an electroconductive thermoplastic resin composition for a fuel tube composed of the following constitution; and a fuel tube using the composition.
  • thermoplastic resin composition for a fuel tube comprising a thermoplastic resin and vapor grown carbon fiber having an average filament diameter of 50 to 130 nm, wherein the volume resistivity is 1 x 10 8 ⁇ cm or less and the stretch at break of the resin composition is 80% or more of the stretch at break of the thermoplastic resin alone.
  • thermoplastic resin is polyamide, polyester, or a fluorine-based resin.
  • [CIl] Afuel tubeusingthe electroconductivethermoplasticresin composition for a fuel tube according to any one of the above Cl to ClO.
  • the fuel tube according to the above CIl comprising a multi-layer structure where at least the innermost layer of the multi-layer structure is made of the resin composition.
  • a method of producing a fuel tube having a multi-layer structure comprising a multi-layer structure where at least the innermost layer of the multi-layer structure is made of the resin composition for a fuel tube according to any one of the above Cl to ClO, whereinthe resincompositionandthe same thermoplastic resin composition as the former or another thermoplastic resin composition different from the former are subjected to co-extrusion molding.
  • the electroconductive thermoplastic resin composition for a fuel tube of the present invention is excellent in physical properties such as surface smoothness, toughness, and extrusion moldability in abalancedmannerwithout impairing the elongation property of a thermoplastic resin itself, so it can be suitably used for a fuel tube or any other tubular molded product for use in an automobile or the like.
  • FIG. I 1 is an electron micrograph (magnification : X 2000) of the electroconductive resin composition obtained in Example 9.
  • Aheat-resistant resin to be used in the present invention is required to be a heat-resistant resinhaving a glass transition temperature of 100 0 C or higher and/or a melting point of 200 0 C or higher, and any one of thermoplastic and thermosetting resins can be used as long as the resin satisfies the above requirement .
  • At least one kind selected from a fluorine-based resin, a polyimide resin, a polyamide imide resin, a polyether imide resin, a polyether ether ketone resin, a polysulfone resin, a polyether sulfone resin, a polybenzimidazole resin, a polyphenylene sulfide resin, a polyethylene naphthalate resin, a polyallylate resin and an aromatic polyamide resin is preferable.
  • a fluorine-based resin a polyimide resin (PI) , a polyamide imide resin (PAI) , or a polyether ether ketone resin (PEEK) is suitable.
  • PI polyimide resin
  • PAI polyamide imide resin
  • PEEK polyether ether ketone resin
  • fluorine-based resin refers to generally known fluorine resins of thermoplastic homopolymer or copolymer type.
  • a resin having a glass transition temperature of 100 0 C or higher and/or a melting point of 200 0 C or higher is selected from such fluorine-based resins.
  • Preferable examples of such resin include perfluoro-based copolymers.
  • perfluoro-based copolymers include: a copolymer of tetrafluoroethylene andperfluoroalkyl vinyl ether; a copolymer of tetrafluoroethylene and hexafluoropropylene; a copolymer of tetrafluoroethyleneandethylene (ETFE) ; andatertiarycopolymer of tetrafluoroethylene, hexafluoropropylene and perfluoroalkyl vinyl ether.
  • Those polymers each have a heat distortion temperature under load of about 70 to 100 0 C and a heat resistance up to about 150 to 260°C.
  • polyimide resin refers to all resins each having an imide bond in its structure, and examples of such resin include thermoplastic and thermosetting polyimide.
  • Thermoplastic polyimide has an imide group and has thermoplasticity. Therefore, the polyimide itself can melt or soften at a predetermined temperature or higher, so the polyimide can be directly subjected to extrusion molding.
  • the property is found in polyimide having in its main chain, (2 or more) ether bonds, an alkylene bond (having 3 or more carbon atoms) and a functional group that provides intramolecular flexibility such as a carbonyl group.
  • an organic dianhydride such as pyromellitic dianhydride, 2, 2 ' , 3, 3'-biphenyltetracarboxylic dianhydride, 3, 3' , 4, 4 '-benzophenonetetracarboxylic dianhydrideorbis (2, 3-dicarboxyphenyl)methanedianhydride
  • an organic diamine such as bis ⁇ 4- [3- (4-aminophenoxy)benzoyl]phenyl ⁇ ether, 4,4"-bis (3-aminophenoxy)biphenyl, bis ⁇ 4- (3-aminophenoxy)phenyl ⁇ sulfone or
  • 2, 2 '-bis ⁇ 4- (3-aminophenoxy)phenyl ⁇ propane) equal to each other in amount are allowed to gradually react with each other while being stirred in an organic polar solvent (such as N-methylpyrrolidone or N,N-dimethylacetamide) .
  • the reaction involves polycondensation into a polymer having a necessary molecular weight and imide ring closure after the polycondensation.
  • the organic dianhydride and the organic diamine react to form polyimide in a single stroke.
  • the temperature of extruding polyimide into a film is about 300 to 400 0 C.
  • thermosettingpolyimide does notmelt in apolyimide state . Therefore, molding of the thermosettingpolyimide into a seamless belt involves the two steps of: subjecting its precursor having thermoplasticity, i.e. polyamic acid to primary molding; and subsequently transforming the resultant into an imide.
  • the polyimide can be produced by allowing an organic dianhydride (such as pyromellitic dianhydride, 2, 2 ' , 3, 3 '-biphenyltetracarboxylic dianhydride,
  • the reaction is a polycondensation reaction for producing a polyamic acid having a desiredmolecular weight, andmust not involve a ring closure reaction to transform the resultant into an imide.
  • the organic dianhydride and the organic diamine must be allowed to gradually react with each other while the reaction temperature is kept low.
  • the above examples of polyimide have no amino group, but so-called polyamide imide containing an amino group can also be used.
  • the polyamide imide can be produced through a polycondensation reaction between a tricarboxylic monoanhydride to serve as an organic acid and anyone of the organic diamines exemplified above equal to each other in amount in an organic solvent.
  • the polyimide-based resin has a heat distortion temperature of 200 to 400 0 C and heat resistance up to about 250 to 350 0 C.
  • the vapor grown carbon fiber to be used in the present invention preferably has an average filament diameter of 50 to 130 nm.
  • An average filament diameter of less than 50 nm results in an exponential increase in surface energy, with the result that an agglomeration force between filaments drastically increases. If a vapor grown carbon fiber having such average filament diameter is merely kneadedwith a resin, the fiber cannot be sufficiently dispersed into the resin, which results in agglomerates of the fiber scattered in a resin matrix and therefore, a conductive network cannot be formed. When a large shearingforce is appliedat the time ofkneading, the agglomerates can be raveled out and the fiber can be dispersed into the matrix.
  • the vapor grown carbon fiber to be used in the present invention have an aspect ratio of 65 to 500, more preferably 100 to 200.
  • the larger the aspect ratio of the fiber (that is, the longer the filament) the more entangled with each other and the more difficult it is to ravel out. As a result, the fiber cannot be sufficiently dispersed.
  • the aspect ratio is less than 65, 10 mass% or more of a filler must be added in order to form a conductive linked skeleton structure, which is not preferred in that fluidity and tensile strength of the resin is remarkably decreased.
  • the degree of branching of the vapor grown carbon fiber to be used in the present invention is preferably 0.3/ ⁇ m or less, more preferably 0.2/ ⁇ m or less, or still more preferably 0.1/ ⁇ m or less. If the degree of branching is in excess of 0.3/ ⁇ m, the carbon fiber forms strongaggregates, therebymaking it difficult to impart conductivity efficiently with a small amount of the fiber.
  • the average interplaner spacing d O o2 is preferably 0.345 nm or less, more preferably 0.343 nm or less, or still more preferably 0.340 nm or less.
  • the average interplaner spacing doos is in excess of 0.345 nm, graphite crystals have not sufficiently grown, so the resistivity of the carbon fiber alone increases to be 10 or more times as high as that of a crystallized fiber.
  • the carbon fiber is mixed with a resin or the like, electron transfer to and fro between the carbon fiber and the resin becomes difficult.
  • the vapor grown carbon fiber to be used in the present invention has a BET specific surface area of preferably 10 to 50 m 2 /g, or more preferably 15 to 40 m 2 /g.
  • BET specific surface area increases, surface energy of the carbon fiber also increases to make adhesive and agglomeration forces stronger, which leads to difficulty in dispersing the fiber.
  • the interfacial areabetween thematrix and the carbon fiber increases, it is impossible to sufficiently cover the fiber with the matrix, or more carbon fiber may be peeled off the matrix.
  • As aresult whenacompositeofthe fiber andthe resin isproduced, not only electrical conductivity but also mechanical strength deteriorates, which is not preferred.
  • the peak height ratio (Id/Ig) of a band ranging from 1341 to 1349 cm “1 (Id) to a band ranging from 1570 to 1578 cm “1 (Ig) in the Raman scattering spectrum of the vapor grown carbon fiber to be used in the present invention is preferably 0.1 to 1.4, more preferably 0.15 to 1.3, or still more preferably 0.2 to 1.2.
  • the vapor grown carbon fiber to be used in the present invention having the above physical properties can be produced by thermally decomposing a carbon source (an organic compound) in the presence of an organic transition metal compound.
  • Examples of carbon source (organic compound) to serve as a rawmaterial for the carbon fiber include gases such as toluene, benzene, naphthalene, ethylene, acetylene, ethane, anaturalgas, andcarbonmonoxide, andmixtures ofthegases .
  • gases such as toluene, benzene, naphthalene, ethylene, acetylene, ethane, anaturalgas, andcarbonmonoxide, andmixtures ofthegases .
  • aromatic hydrocarbons such as toluene and benzene are preferable.
  • the organictransitionmetal compound contains atransition metal to serve as a catalyst.
  • the transition metal is an element belonging to any one of Groups 4 to 10 in the periodic table.
  • Examples of preferable organic transitionmetal compound include ferrocene and nickelocene.
  • a sulfur compound such as sulfur or thiophene can be used as a catalyst aidwhichenhances catalytic activitybyefficiently removing a gas such as hydrogen adsorbing to the surface of a transitionmetal catalyst particle in the atmosphere of a thermal decomposition reaction.
  • the above organic compound, the organic transitionmetal compound and the sulfur compound are supplied into a reactor heated to 800 to 1300 °C and cause a thermal decomposition, to thereby generate carbon fiber.
  • a reducing gas such as hydrogen as carrier gas
  • the organic transition metal compound and the sulfur compound dissolved in aromatic hydrocarbon may be used, or the materials gasified at a temperature of 500 0 C or less maybe used.
  • the raw material is in liquid form, vaporization and decomposition of the raw material occur on the inner wall of the reaction tube, causing an uneven concentration- distribution , andthus generatedcarbon fibertends to aggregate.
  • the rawmaterial gasified in advance is preferred for the purposed of making the concentration of the material uniform inside the reaction tube.
  • the ratio of the transition metal catalyst to sulfur compoundcatalystaid is preferably 15 to 35 mass %. If the ratio is less thanl5mass%, the catalyst activitybecomes too high, increasing the number of branching in the carbon fiber or producing radial carbon fiber filaments, which leads to increase in interaction betweenfilaments andunpreferable formationofstrongaggregates. If the ratio exceeds 35 mass%, since gas such as hydrogen adsorbed onto the catalyst cannot be sufficiently removed, which disturbs carbon source supply to the catalyst and leads to generation of particles other than carbon fiber, it is not preferred.
  • the branching number of carbon fiber and the raveling level of filament agglomerates depend on raw material concentration at the time of reaction.
  • the ratio of the supply amount of rawmaterial to the amount of carrier gas in the reaction tube be 1 g/1 or less, more preferably 0.5 g/1, even more preferably 0.2 g/1.
  • the furnace used for heat treatment to develop crystals may be any furnace as far as the furnace can hold the target temperatureof2000 °Corhigher, morepreferably2300 °Corhigher.
  • Acheson furnace, resistance furnace or high-frequency furnace may be used.
  • the heat treatment may be conducted by directly applying an electrical current to the powder material or formed product in some cases.
  • the atmosphere of the heat treatment is non-oxidation, preferably inert atmosphere constitutedby one ormore rare gases of argon, helium and neon.
  • inert atmosphere constitutedby one ormore rare gases of argon, helium and neon.
  • the shorter, the more preferable, and generally 1 hour is sufficient.
  • the carbon fiber is sinteredandsolidified, so production yield deteriorates. Therefore, it is sufficient that, after the temperature at the central portion of a molded product or the like has reached a target temperature, the temperature at the central portion be kept at the target temperature for 10 minutes to 1 hour.
  • boron compound such as boron carbide (B 4 C) , boron oxide (B 2 O 3 ) , elemental boron, boric acid(H 3 BO 3 ) or borate salt may be mixed into carbon fiber in conducting graphitization with heat treatment at 2000 to 3500 °C in inert atmosphere.
  • the amount of the boron compound to be added depends on the chemical property and physical property of the compound and cannot be flatly limited. For instance, in a case where boron carbide (B 4 C) is used, the amount is preferably 0.05 to 10 mass %, more preferably 0.1 to 5 mass % based on the carbon fiber.
  • the boron amount contained in the crystals of carbon fiber or in the surface of the crystals is preferably 0.01 to 5 mass %.
  • the boron content be 0.1 mass % ormore.
  • the upper limit of the boron amount which can substitute carbon in the graphenesheet is about 3 mass %, a larger amount of boron, especially 5 mass % or more of boron, which will remain as boron carbides or boron oxides to cause decrease in electroconductivity, is unpreferable.
  • carbon fiber may be subjected to oxidation treatment to thereby introduce phenolic hydroxyl group, carboxyl group, quinone group or lactone group to the surface of the carbon fiber. Further, the carbon fiber may be subjected to surface treatment with a silane coupling agent, titanate coupling agent, aluminium coupling agent or phosphoric ester coupling agent or the like.
  • carbon black may also be added as a conductive filler.
  • a vapor growncarbon fiber andcarbon black are used in combination and the carbon black is uniformly dispersed, a phenomenon that the range of variation in conductivity is narrowed is observed.
  • Carbon black that can be used generally has an average particle size of 1 to 500 ⁇ m and a volume resistivity of about 10 1 to 10 4 ⁇ -cm. Examples thereof include acetyleneblack, Ketjen Black, oil furnace black and thermal black.
  • the resin composition for a seamless belt of the present invention contains theheat-resistantresinandvapor growncarbon fiber described above, and optionally contains carbon black.
  • the blending amount of the vapor grown carbon fiber is 1 to 30 parts by mass, or preferably 3 to 15 parts by mass with respect to 100 parts by mass of the heat-resistant resin. If the blending amount of the vapor grown carbon fiber is less than
  • the blending amount of carbonblack is preferably 1 to 10 partsbymass, ormorepreferably
  • breaking of the vapor grown carbon fiber filaments be suppressed as much as possible.
  • the breaking ratio of the vapor grown carbon fiber is suppressed to preferably 20 % or less, more preferably 15% or less, or still more preferably 10 % or less.
  • the breaking ratio can be evaluated by comparing the aspect ratios (measured by means of, for example, a scanning electron microscope photographic image) of the carbon fiberbefore andafterthemixing and kneading.
  • procedure as described below can be used in order to perform the mixing and kneading step while suppressing thebreakingofthevaporgrowncarbonfiberto the extentpossible.
  • an inorganic filler when melt-kneaded with a thermoplastic resin or a thermosetting resin, a high shearing force is applied to agglomerated inorganic filler to break the inorganic filler to thereby pulverize the inorganic filler, so that the inorganic filler isuniformlydispersedinamoltenresin.
  • a high shearing force examples include a large number of kneaders such as one utilizing astonemillmechanismanda co-rotatingtwin screwextruderhaving a kneading disk introduced into screw elements, which can apply a high shearing force.
  • kneader when any such kneader is used, filaments of the vapor grown carbon fiber are broken in a kneading step. Althoughbreaking of the fiber filaments canbe suppressed in case of using a uniaxial extruder having a weak shearing force, it is impossible to uniformly disperse the fiber. Therefore, in order to uniformly disperse the fiber while suppressing breaking of filaments, a co-rotating twin screw extruder using no kneading disk is desirably used to reduce a shearing force. Alternatively, a kneader such as a pressure kneader that does not apply a high shearing force and achieves dispersion over a long time period is desirably used.
  • a special mixing element is desirably employed in a uniaxial extruder.
  • the wettability of an inorganic filler with respect to a molten resin is important for filling the resinwith the inorganic filler.
  • An example of a method of improving wettability includes a method wherein the surface of vapor grown carbon fiber is oxidized.
  • the fiber When the vapor grown carbon fiber to be used in the present invention is downy with a bulk specific gravity of about 0.01 to 0.1 g/cm 3 , the fiber tends to involve the air, so deaeration by means of an ordinary uniaxial extruder or co-rotating twin screw extruder is difficult, and therefore it is difficult to fill the resinwith the carbon fiber.
  • abatch-type pressure kneader is preferably used as a kneader that has good filling property and can suppress breaking of filaments to the extent possible.
  • the fiber kneaded by means of a batch-type pressure kneader can be fed into a uniaxial extruder before being solidified, to thereby be formed into pellets.
  • the resin composition for a seamless belt of the present invention can have a volume specific resistivity of 1 x 10 6 to 1 x 10 13 ⁇ cm, preferably 1 x 10 7 to 1 x 10 10 ⁇ cm, or more preferably 1 x 10 8 to 1 x 10 9 ⁇ cmby adjustingphysical properties andblending amount of the vapor grown carbon fiber.
  • the composition After preparing a composition by mixing and dispersing the above components, the composition is molded into a seamless belt .
  • a dry molding method or a wet molding method can be preferably used as a molding method.
  • the dry molding method is a method involving directly subjecting a matrix resin to melt extrusion molding through a ring die in a state where substantially no organic solvent is present.
  • the wet molding method involves: subjecting a composition in a plasticized state or a solution state to primary molding in the presence of an organic solvent; removing a solvent or the like; and molding the resultant into a target seamless belt shape.
  • the composition in a plasticized state is molded into a tubular shape while casting the composition toward the outer periphery of a metal drum, or by directly subjecting the composition to extrusion molding through a ring die.
  • a centrifugal casting method where a composition is poured in a solution state into a metal drum and molded while rotating the drum.
  • An organic solvent to be used in the wet molding method is selected from those which can swell or dissolve the heat-resistant resin (apolyamic acidinthe case of thermosetting polyimide) .
  • the centrifugal casting method involves the use of an organic solvent into which the heat-resistant resin can be completely dissolved, and it is necessary to select the amount of the solvent.
  • thermosetting polyimide as a heat-resistant resin.
  • starting materials are subjected to a polycondensation reaction in the organic solvent to produce a polyamic acid solution.
  • a conductive filler is mixed therewith and dispersed into the solution as described above.
  • a predetermined amount of the polyamic acid solution is injected into a metal drum corresponding to a seamless belt having desired dimensions (diameter and width) , and rotation is started while the drum is heated fromthe outside of the drum.
  • the solvent is gradually evaporated and removed while the solution is uniformly flown over the entire inner surface of the drum.
  • a predetermined temperature generally a temperature slightly higher than the boiling point of the organic solvent and lower than the temperature at which the solution is transformed into an imide
  • the solvent is gradually evaporated and removed while the solution is uniformly flown over the entire inner surface of the drum.
  • the polyamic acid is solidified and molded into an endless belt.
  • the resultant endless belt is peeled off the drum and fit into a cylindrical mold, and the whole is placed into a heating oven, gradually heated to 250 0 C at first, and then gradually heated to 400 0 C (secondary molding) .
  • an imidation reaction gradually proceeds, whereby a seamless belt using thermosetting polyimide as a matrix is produced.
  • the cylindrical moldused in the secondarymolding is intendedmainly for performing a secondary treatment while keeping the shape of the belt, and is not essential.
  • a heat-resistant resin other than thermosetting polyimide can be molded by means of the centrifugal casting method in accordance with the same procedure as in the case of polyimide.
  • molding conditions are not particularly limited in both of the dry molding method and the wet molding method, and optimumconditions are desirably selected in correspondence with a selected composition.
  • the melt extrusion of the composition through a ring die is preferably performed at room temperature and the composition is preferably taken up substantially without stretching.
  • the seamless belt of the present invention thus produced is excellent in surface smoothness, and its ten point average roughness (Rz) at a cut-off wavelength of 2.5 mm is 10 ⁇ m or less, or preferably 8 ⁇ m or less.
  • the seamlessbelt ofthepresent invention canhave a thermal conductivity of 0.8 W/mK or more. If the thermal conductivity is 0.8 W/mK or more, the temperature of the seamless belt can be uniform, to thereby suppress the occurrence of, for example, wrinkles. In addition, the seamless belt can have good heat discharge property, and the maximum temperature that the belt can reach at the time of continuous use can be lowered, whereby the durability of the belt can be improved.
  • the seamless belt of the present invention has stable electrical resistance properties. To be specific:
  • the ratio of the surface resistivity to the volume resistivity is within 2 or less orders of magnitude
  • the ratio (Ra/Rh) of the volume resistivity Ra at normal temperature and a normal humidity to the volume resistivity Rh at a high temperature and a high humidity can be in the range of 0.03 to 30.
  • the fluctuation range of the surface resistivity upon application of a charging voltage can be within 2 or less orders of magnitude (less than 10 2 ) , or preferably 1 or less order of magnitude (less than 10 1 ) .
  • a ratio (Rioov/Riooov) of the volume resistivity Rioov when 100 V is applied to a volume resistivity Riooov when 1, 000 V is applied can fall within the range of 0.03 to 30, or preferably 0.1 to 10.
  • an intermediatetransferbeltorthelike, fluctuationinresistivity due to the environment is preferably small .
  • a ratio (Ra/Rh) of a volume resistivity Ra at normal temperature and a normal humidity to a volume resistivity Rh at a high temperature and a high humidity can be adjusted to fall within the range of 0.03 to 30, or preferably 0.1 to 10.
  • At normal temperature and a normal humidity refers to an environment having a temperature of 23 0 C and a humidity of 55 %Rh and the term "at a high temperature andahighhumidity” as usedherein refers to an environment having a temperature of 30 0 C and a humidity of 80 %Rh.
  • Aheat-resistant resin to be used in the present invention is a heat-resistant resin having a glass transition temperature of 100 0 C or higher and/or a melting point of 200 0 C or higher, and any one of thermoplastic and thermosetting resins can be used as long as the resin satisfies the conditions.
  • PC polycarbonate
  • PEEK polyether ether ketone
  • PPE modifiedpolyphenylene ether
  • PPS polyphenylene sulfide
  • the vapor grown carbon fiber to be used is the same as used in above (A) .
  • the resin composition for a tray for carrying a magnetic head for a magnetic disk drive contains the above heat-resistant resin and the vapor grown carbon fiber.
  • the blending amount of the vapor grown carbon fiber is 1 to 30 parts by mass, or preferably 3 to 15 parts by mass with respect to 100 parts by mass of the heat-resistant resin. If the blending amount of the vapor grown carbon fiber is less than 1 part by mass, it is difficult to form a conductive network, with the result that desired conductivity cannot be obtained. On the other hand, if the amount exceeds 30 parts by mass, impact resistance significantly deteriorates. Mixing/kneading of the above components maybe carried out in the same manner as described in the above (A) .
  • the resin composition for a carrier tray of the present invention can be controlled to have a volume specific resistivity of 1 x 10 2 to 1 x 10 8 ⁇ cm, preferably 1 x 10 3 to 1 x 10 8 ⁇ cm, or more preferably 1 x 10 4 to 1 x 10 7 ⁇ cm which is suitable for a tray for carrying a magnetic head for a magnetic disk drive, by adjusting physical properties, blending amount, and the like of the vapor grown carbon fiber.
  • the surface resistivity of the resin composition can be regulated to be 1 x 10 2 to 1 x 10 10 ⁇ /D or preferably 1 x 10 4 to 1 x 10 8 ⁇ /D.
  • resistivity controllable to be within the above range not only an excellent antistatic property but also prevention of excessive contact current from flowing into a magnetic head which is caused by contact between the magnetic head and the tray can be achieved.
  • the above respective components are mixed and dispersed to prepare a composition, and the composition is molded into a carrier tray.
  • the molding can be performed bymeans of a general method.
  • the resin composition obtained by means of the above method is molded by means of any one of various melt-moldingmethods .
  • amoldingmethod includepress molding, extrusion molding, vacuum molding, blow molding, and injection molding. Of those, injection molding is preferable.
  • any one of various molding methods such as: integral molding of a metal part and any other part by means of an insert injection molding method; a two-color injection molding method; a core back injection molding method; a sandwich injection molding method; and an injection press molding method can be used as an injection moldingmethod. Sincethe surface resistivityof aproductvaries depending on a resin temperature, a die temperature and a molding pressure, appropriateconditionsmustbe set ininjectionmolding.
  • a side gate, a film gate, a submarine gate, a pin gate or the like can be used as a gate (inlet) for injecting the resin composition from a cavity of a die in an injectionmoldingmethod.
  • the sectional areas of those gates are each desirably 0.2 mm 2 or more.
  • the diameter of the pin gate be 0.5 to 3 mm, or particularly desirably 1.0 to 2.5 mm.
  • the gate diameter of the pin gate smaller, themore preferable, as far as the die can be sufficiently filled with a resin, and the gate diameter is generally 0.2 to 0.5 mm.
  • the gate diameter sectional area
  • the conductive network formed by vapor grown carbon fiber is apt to be broken due to excessive shear force imposed to the resin composition when it flows through the gate.
  • an excessively large gate diameter makes the gate portion of a molded product less clear, with the result that the molded product is badly finished.
  • the resin composition of the present invention has good fluidity and good mold transferability. With a gate relatively large as described above, the transferability can be enhanced.
  • a flat portionhavinganangle of 80 to 100 degrees (nearlyperpendicular) against the parting face have a smooth surface.
  • the plane nearly perpendicular to the parting face has a rough surface, since such irregularities are transferred onto the resin, a large force is required to take a product out of the mold, which leads to defects such as breakage of the molded product.
  • the ten point average roughness (Rz) of the plane nearly perpendicular to the parting plane at a cut-off wavelength of 2.5 mm is preferably 10 ⁇ m or less, more preferably 5 ⁇ m or less, or still more preferably 3 ⁇ m or less.
  • the carrier tray sometimes corrodes and damages a magnetic head by virtue of a gas generated from the tray.
  • the amount of such a gas generated fromthe carrier trayof thepresent invention is preferably small.
  • the total amount of outgas from a surface area of 12.8 cm 2 measured by means of a headspace gas chromatogram under the conditions of a heating temperature of 85 0 C and an equilibrium time of 16 hours is preferably 1 ⁇ g/g or less, more preferably 0.5 ⁇ g/g or less, the amount of methylene chloride generated is 0.1 ⁇ g/g or less, more preferably 0.02 ⁇ g/g or less, and the amount of hydrocarbons genetated is 0.5 ⁇ g/g or less, more preferably 0.2 ⁇ g/g or less.
  • hydrocarbon examples include n-heptane, n-hexane, cyclohexane, benzene, and toluene, which are used in producing a resin.
  • the resin composition be degassed to remove volatile components during its production process or that a heat-resistant resin polymerized by a method not using a polymerization solvent.
  • the carrier tray of the present invention preferably has a surface excellent inuniformity and stability.
  • the tray having a surface area of 100 to 1 000 cm 2 is immersed in 500 ml of pure water and an ultrasonic wave of 40 KHz is applied to the tray for 60 seconds, the number of particles each having a particle size of 1 ⁇ m or more and falling off from the surface of the tray (particle generation) is 5, 000 pcs/cm 2 or less.
  • Such a tray can prevent a magnetic head from being physically or chemically contaminated and damaged by particles that fall out as a result of scratching, abrasion and washing.
  • the particle generation exceeds 5, 000 pcs/cm 2 , it causes contamination and damage by the particles that fall off at the timeofscratching, abrasion, washing, orthe like. Inthepresent invention, it is particularly desirable that the particle generation be 1,000 pcs/cm 2 or less.
  • the carrier trayof thepresent invention canhave a thermal conductivity of 0.8 W/mK or more.
  • thermal conductivity of 0.8 W/mK or more heat radiation can contribute to drastic improvement in deformation and damage of the tray at the time of handling on and after heat treatment step.
  • thermoplastic resin composition for a fuel tube and a fuel tube
  • thermoplastic resin used in the present invention includes polyamide, polyester and fluorine-based resin.
  • the polyamide is a resin mainly composed of an amino acid, lactam, or a diamine and a dicarboxylic acid, and examples of its main component include: amino acids such as 6-aminocapronic acid, 11-aminoundecylic acid, 12-aminododecanoic acid and para-aminomethylbenzoic acid; lactams such as ⁇ -aminocaprolactam and ⁇ -laurolactam; aliphatic, alicyclic, and aromatic diamines such as tetramethylenediamine, hexamethylenediamine, undecamethylenediamine, dodecamethylenediamine,
  • 2-methylpentamethylenediamine and aliphatic, alicyclic, and aromatic dicarboxylic acids such as adipic acid, spelic acid, azelaicacid, sebacicacid, dodecanedioic acid, terephthalicacid, isophthalic acid, 2-chloroterephthalic acid, 2-methylterephthalic acid, 5-methylisophthalic acid, 5-sodium sulfoisophthalic acid, hexahydroterephthalic acid and hexahydroisophthalic acid.
  • each of polyamide homopolymers and copolymers derived fromthose rawmaterials maybe used alone, or two or more of them may be used as a mixture.
  • polyamide homopolymers and copolymers include PA6, PA46, PA66, PA612, PAlOlO, PA1012, PA69, PAIl, PA12, PA1212, PA6T, PA6I, PA12T, PA12I, and PA12/6T and 12/61.
  • a homopolyamide resin composed of structural units having an average carbon number per one amide group of 8 to 15 or a copolymerized polyamide resin having an average carbon number per one amide group of 8 to 15 is preferable with a view to obtaining improved toughness and improved extrusion moldability.
  • polyamide include PA12, PAIl, PA1112 and PA1212.
  • polyesters obtained from dicarboxylic acids and aliphatic diols.
  • dicarboxylic acids include: aliphatic dicarboxylic acids each having 2 to 20 carbon atoms such as terephthalic acid, azelaic acid, sebacic acid, adipic acid, dodecanedicarboxylic acid and isophthalicacid; aromaticdicarboxylic acids suchas isophthalic acid and naphthalenedicarboxylic acid; and alicyclic dicarboxylic acids such as cyclohexanedicarboxylic acid. Each of them may be used alone, or two or more of them may be used as a mixture.
  • the aliphatic diols include ethylene glycol, propylene glycol, 1, 4-butanediol, trimethylene glycol, 1, 4-cyclohexanedimethanol, and hexamethylene glycol.
  • thermoplastic polyester examples include polyethylene terephthalate, polypropylene terephthalate, polybutylene terephthalate, polyhexamethylene terephthalate, polycyclohexylenedimethylene terephthalate, and polyethylene naphthalate.
  • polybutylene terephthalate having an appropriate mechanical strength or a copolyester composed of: a dicarboxylic acid component containing 60 mol% or more (preferably 70 mol% or more) of terephthalic acid, and dodecanedicarboxylic acid and/or isophthalic acid; and a 1, 4-butanediol component is particularly preferably used
  • the fluorine-basedresin is agenerallyknown fluorine resin which is composed of a thermoplastic resin alone or is formed as a result of copolymerization of thermoplastic resins, and is preferably a perfluoro-based copolymer.
  • a copolymer of tetrafluoroethylene and perfluoroalkyl vinyl ether examples include: a copolymer of tetrafluoroethylene and perfluoroalkyl vinyl ether; a copolymer of tetrafluoroethylene and hexafluoropropylene; a copolymer of tetrafluoroethylene and ethylene (ETFE); andatertiarycopolymeroftetrafluoroethylene, hexafluoropropylene, and perfluoroalkyl vinyl ether.
  • ETFE tetrafluoroethylene and ethylene
  • the vapor grown carbon fiber to be used is the same as used in above (A) .
  • the above resin composition contains the above heat-resistant resin and the above vapor grown carbon fiber.
  • the blending amount of the vapor grown carbon fiber is 10 mass % or less in the resin composition, preferably 2 to 8 mass %. If the blending amount exceeds 10 mass %, the stretching property of the resin composition deteriorates. Further, if the blending amount is too small, electroconductivity as desired cannot be obtained.
  • Mixing/kneading of the above components may be carried out in the same manner as described in the above (A) .
  • the resin composition of the present invention can be adapted to have a volume specific resistivity of 1 x 10 8 ⁇ cm or less, preferably 1 x 10 2 to 1 x 10 8 ⁇ cm, or more preferably 1 x 10 4 to 1 x 10 7 ⁇ cm by adjusting the physical properties and loadings of the vapor grown carbon fibers.
  • the resin composition of the present invention can suppress a reduction in breaking elongation due to the compounding of the above specific vapor grown carbon fibers as a conductive filler. Therefore, the resin composition can be said to be a material that brings together excellent conductivity and excellent elongation property.
  • A breaking elongation
  • B breaking elongation of the resin composition of the present invention prepared by compounding the resin with vapor grown carbon fibers
  • B a maintenance factor (B/A x 100 (%) ) of the breaking elongation of the conductive resin composition to the breaking elongationofthe resinalone canbe 80% ormore.
  • Thevalue reduces to about 20% when carbon black or a carbon nanotube is used as a conductive filler.
  • the composition of the present invention is suitable for producing a hollow molded product such as a tube molded product or a blow molded product, and is particularly suitable for producing a multi-layer hollow molded product through co-extrusion.
  • the innermost layer of the structure is preferably formed of the composition.
  • the same material as that for the innermost layer may be used for an outer layer or for, if the multi-layer structure has three or more layers, an intermediate layer of the structure.
  • the electroconductive thermoplastic resin composition of the present invention having a composition different from that of the innermost layer may be used therefor.
  • a thermoplastic resin composition compounded with no conductivity imparting material may also be used. Examples of the thermoplastic resin composition compounded with no conductivity impartingmaterial includepolyamide, polyester, and a fluorine-based resin.
  • Table 1 shows the compounding conditions for Examples
  • PCM30 co-rotating twin screw extruder manufactured by IKEGAIwasused. Kneadingwasperformedat atemperatureof280 0 C. ii) Thermosetting resin
  • a pressure kneader manufactured by Toshin Chemitech Co., Ltd. (having a kneading volume of 10 liters) was used.
  • the temperature was set to 60°C.
  • a copolymer of tetrafluoroethylene and ethylene (ETFE: manufactured by ASAHI GLASS CO., LTD., AfIon type COP-55AXT, melting point: 260 0 C) was used as a fluorine-based resin.
  • EFE tetrafluoroethylene and ethylene
  • a uniaxial extruder Laboplastomill manufactured by Toyo Seiki Seisaku-Sho, Ltd.
  • a cylindrical film molding die having a diameter of 10 cm and a thickness of 200 ⁇ m.
  • ADMFsolutionofpolyamicacid (havinga solidconcentration of 18.5% and a viscosity of 3,000 poise) , which had been obtained by using 4, 4 '-diaminodiphenyl ether as an aromatic diamine and pyromellitic dianhydride as an aromatic tetracarboxylic dianhydride, was used. A specific amount of vapor grown carbon fiber was added to the solution, and the resultant dispersion liquid was kneaded. Next, the resultant was cast into a cylindrical SUS, andthe wholewas treated at 140 0 C for 15minutes, 200 0 C for 20 minutes, 25O 0 C for 30 minutes, 300 0 C for 30 minutes, and350 0 C for 30minutes .
  • VGCF-S Vapor grown carbon fiber manufactured by SHOWA DENKO K.K.
  • the fiber was pulverized by means of a jet mill to have an adjusted average filament length of 5 ⁇ m (aspect ratio: 63) .
  • Carbon nanotube hollow carbon fibril
  • RMB 8515-00 A PEI master batchmanufacturedbyHyperionCatalysis (RMB 8515-00: containing 15mass% ofCNT) was used.
  • AKetjenBlack (KB) EC600JDmanufacturedbyLIONCORPORATION having a specific surface area of 800 mVg was used.
  • Breaking ratio of carbon fiber (%) The breaking ratio of carbon fiber filaments was determined from the following expression.
  • Breaking ratio of carbon fiber (%) ⁇ 1 - (Aspect ratio of carbon fiber in molded product of composition/Aspect ratio of carbon fibers before mixing and kneading) ⁇ x 100
  • Thermal conductivity was measured according to a hot-wire method by means of a quick thermal conductivity meter manufactured by Kyoto Electronic
  • a test sample used was obtained by laminating films so as to have a shape of 100 x 100 x 2 mm thick.
  • Table 2 shows the compounding conditions for the compositions of Examples andComparative Examples. Aresin and a conductive filler were melt-kneaded in accordance with Table 2, and the kneaded product was subjected to injection-molding, to thereby obtain a flat plate for measuring a volume specific resistance.
  • Table 2 also shows the volume specific resistance, presence or absence of an agglomerate, the breaking ratio, the thermal conductivity, the ten point average roughness, the outgas amount, and the amountofparticles fallingoffthe sample eachobtainedinExamples and Comparative Examples.
  • Fig.1 shows anpicture of scanningelectronmicroscope(at amagnificationof 2, 000) of the conductive resin composition obtained in Example 9.
  • PC Polycarbonate resin
  • m-PPE Modified polyphenylene ether resin
  • NORYL registered trademark 534 manufactured by GE Plastics
  • PCM30 manufacturedbyIKEGAI was used.
  • PC andm-PPE were kneadedat temperatures of 270 0 Cand260 0 C, respectively.
  • the sum of the average absolute value of the height of the five highest peaks and the average absolute value of the depth of the five deepest valleys which were measured in a direction of longitudinal magnificationfromthe averagelineofaroughness curve was calculated, by using a surface roughness meter "Surfcom" manufactured by TOKYO SEIMITSU with a cut-off wavelength of 2.5 mm, a measuring length of 5 mm and a measuring speed of 0.3 mm/s.
  • the heights of the lowest bottom to the fifth lowest bottom were v) Falling-off of particles
  • a flat plate sample of 100 mm x 100 mm x 2 mm was immersed in 500ml ofpurewater andanultrasonicwave of 40 KHzwas appliedthereto for 60 seconds. After that, the extracted pure water was sucked with a submerged particle counter, and the number of particles each having a particle size of 1 ⁇ m or more was measured, vi) Measurement of the outgas amount
  • the amounts of n-heptane and methylene chloride and the total amount of outgas were measuredbymeans of a headspace gas chromatogram in accordance with the method described in JP 2001-118222 A.
  • the measurement method is specifically described as follows.
  • the total outgas amount, the amount of methylene chloride, and the amount of n-heptane were calculated as follows.
  • Amount of methylene chloride (Peak area of methylene chloride) / (Peak area of n-octane/Mass of n-octane (g) ) x 1/ (Mass of sample (g) )
  • Amount of heptane ( ⁇ g/g) (Peak area of heptane)/ (Peak area of n-octane/Mass of n-octane (g) ) x 1/ (Mass of sample (g) )
  • Table 3 shows the compounding conditions for the compositions preparedinExamplesandComparativeExamples.
  • Aresinandaconductive filler weremeltedandkneadedinaccordancewiththe formulation shown in Table 3, and the kneadedproduct wasmolded into a film formeasuring a volume specific resistance.
  • PCM30 Aco-rotatingtwinscrewextruder (PCM30) manufacturedby IKEGAI was used.
  • a PBT elastomer, ETFE and PA12 were kneaded at 260 0 C (PBT elastomer), 280 0 C (ETFE) and 210 0 C (PA12) , respectively.
  • a sycap-type injectionmoldingmachine having a fastening force of 75 ton manufactured by Sumitomo Heavy Industries, Ltd. was used to mold a flat plate (measuring 100 x 100 x 2 mm thick) from each the PBT elastomer, ETFE, and PA12 at 270 0 C (PBT elastomer) , 290 0 C (ETFE) and 230 0 C (PA12), respectively.
  • Anelongationratio wascalculated as a ratio (B/A x 100 (%) ) of the tensile elongation (B) to the tensile elongation (A) of a resin compounded with no conductive filler.
  • a tube having an outer diameter of 5 mm, an inner diameter of 3 mm, an inner layer thickness of 1 mm, an outer layer thickness of 1 mm and a length of 30 cm was produced by subjecting the resin composition of Example 15 (temperature 220 0 C) for the inner layer and PA12 (temperature 220 0 C) for the outer layer to co-extrusion by means of a multi-layer tube extruder equipped with two uniaxial extruders manufactured by SOUKEN CO., LTD.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • 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

L’invention concerne une courroie sans raccord moulée à partir d‘une composition de résine contenant une résine résistante thermiquement d’une température de transition vitreuse supérieure ou égale à 100°C et/ou un point de fusion supérieur ou égal à 200°C et une fibre de carbone produite par la vapeur d’un diamètre de filament moyen compris entre 50 et 130 nm, où la résistivité en volume de la composition de résine entre dans la fourchette de 1 x 106 à 1 x 1013 Ωcm. La courroie est excellente en matière de durabilité, de résistance thermique et de lissé de surface, avec une résistance électrique stable, et peut être utilisée comme photorécepteur ou autre. De plus, en jouant sur la résistivité en volume de la composition de résine de 1 x 102 à 1 x 1018 Ωcm, on peut élaborer un plateau de support de tête magnétique pour lecteur de disque magnétique de faible coût et excellent en matière de résistance mécanique et de propriété antistatique sans fibres de carbone tombant de la surface. La composition de résine électroconductrice thermoplastique comprenant une résine thermoplastique et une fibre de carbone produite par la vapeur convient comme matériau de tube combustible dans les automobiles ou autre.
PCT/JP2005/019150 2004-10-12 2005-10-11 Composition de résine contenant une fibre de carbone produite par la vapeur et utilisation de celle-ci WO2006041186A1 (fr)

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JP2006137937A (ja) * 2004-10-12 2006-06-01 Showa Denko Kk シームレスベルト用樹脂組成物及びシームレスベルト
WO2011053621A1 (fr) * 2009-10-27 2011-05-05 E. I. Du Pont De Nemours And Company Compositions et articles pour utilisation devant résister à l'usure à haute température
CN102120826A (zh) * 2011-01-21 2011-07-13 南京工业大学 一种抗静电聚酰亚胺薄膜的制备方法
CN101813905B (zh) * 2009-02-05 2012-01-25 株式会社理光 电子照相用中间转印带以及电子照相装置
RU2509786C2 (ru) * 2012-05-03 2014-03-20 Федеральное государственное бюджетное учреждение науки Институт проблем нефти и газа Сибирского отделения Российской академии наук Способ получения полимерной композиции для труб
US9086664B2 (en) 2012-12-26 2015-07-21 Canon Kabushiki Kaisha Fixing device with a heat generating layer containing a high molecular compound and a carbon fiber, and an electrophotographic image forming apparatus containing the fixing device
US9158251B2 (en) 2013-08-30 2015-10-13 Canon Kabushiki Kaisha Film and image heating device using film
CN106739322A (zh) * 2016-12-06 2017-05-31 厦门长塑实业有限公司 一种低吸水率双向拉伸尼龙薄膜及其制备方法
CN107110405A (zh) * 2014-12-24 2017-08-29 株式会社可乐丽 药液运输用多层管及聚酰胺树脂组合物
US10763004B2 (en) 2014-03-12 2020-09-01 3M Innovative Properties Company Conductive polymeric material

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JP2006137937A (ja) * 2004-10-12 2006-06-01 Showa Denko Kk シームレスベルト用樹脂組成物及びシームレスベルト
CN101813905B (zh) * 2009-02-05 2012-01-25 株式会社理光 电子照相用中间转印带以及电子照相装置
WO2011053621A1 (fr) * 2009-10-27 2011-05-05 E. I. Du Pont De Nemours And Company Compositions et articles pour utilisation devant résister à l'usure à haute température
CN102120826A (zh) * 2011-01-21 2011-07-13 南京工业大学 一种抗静电聚酰亚胺薄膜的制备方法
CN102120826B (zh) * 2011-01-21 2012-09-19 南京工业大学 一种抗静电聚酰亚胺薄膜的制备方法
RU2509786C2 (ru) * 2012-05-03 2014-03-20 Федеральное государственное бюджетное учреждение науки Институт проблем нефти и газа Сибирского отделения Российской академии наук Способ получения полимерной композиции для труб
US9086664B2 (en) 2012-12-26 2015-07-21 Canon Kabushiki Kaisha Fixing device with a heat generating layer containing a high molecular compound and a carbon fiber, and an electrophotographic image forming apparatus containing the fixing device
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US9158251B2 (en) 2013-08-30 2015-10-13 Canon Kabushiki Kaisha Film and image heating device using film
US9658585B2 (en) 2013-08-30 2017-05-23 Canon Kabushiki Kaisha Film and image heating device using film
US10042298B2 (en) 2013-08-30 2018-08-07 Canon Kabushiki Kaisha Film and image heating device using film
US10763004B2 (en) 2014-03-12 2020-09-01 3M Innovative Properties Company Conductive polymeric material
CN107110405A (zh) * 2014-12-24 2017-08-29 株式会社可乐丽 药液运输用多层管及聚酰胺树脂组合物
EP3239579A1 (fr) 2014-12-24 2017-11-01 Kuraray Co., Ltd. Tube multicouche pour transporter un médicament liquide et composition de résine polyamide
US10906278B2 (en) 2014-12-24 2021-02-02 Kuraray Co., Ltd. Multilayered tube for transporting liquid medicine and polyamide resin composition
CN106739322A (zh) * 2016-12-06 2017-05-31 厦门长塑实业有限公司 一种低吸水率双向拉伸尼龙薄膜及其制备方法

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