WO2015198538A1 - Caoutchouc régénéré, son procédé de fabrication et courroie de transmission le comprenant - Google Patents

Caoutchouc régénéré, son procédé de fabrication et courroie de transmission le comprenant Download PDF

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Publication number
WO2015198538A1
WO2015198538A1 PCT/JP2015/002834 JP2015002834W WO2015198538A1 WO 2015198538 A1 WO2015198538 A1 WO 2015198538A1 JP 2015002834 W JP2015002834 W JP 2015002834W WO 2015198538 A1 WO2015198538 A1 WO 2015198538A1
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Prior art keywords
rubber
recycled
transmission belt
thermoplastic resin
mass
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PCT/JP2015/002834
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English (en)
Japanese (ja)
Inventor
公睦 大野
博之 橘
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バンドー化学株式会社
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Application filed by バンドー化学株式会社 filed Critical バンドー化学株式会社
Priority to CN201580033686.7A priority Critical patent/CN106536617A/zh
Priority to JP2016529010A priority patent/JPWO2015198538A1/ja
Publication of WO2015198538A1 publication Critical patent/WO2015198538A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
    • C08L23/32—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment by reaction with compounds containing phosphorus or sulfur
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16G—BELTS, CABLES, OR ROPES, PREDOMINANTLY USED FOR DRIVING PURPOSES; CHAINS; FITTINGS PREDOMINANTLY USED THEREFOR
    • F16G1/00—Driving-belts
    • F16G1/06—Driving-belts made of rubber
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16G—BELTS, CABLES, OR ROPES, PREDOMINANTLY USED FOR DRIVING PURPOSES; CHAINS; FITTINGS PREDOMINANTLY USED THEREFOR
    • F16G5/00—V-belts, i.e. belts of tapered cross-section
    • F16G5/04—V-belts, i.e. belts of tapered cross-section made of rubber
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/62—Plastics recycling; Rubber recycling

Definitions

  • the present invention relates to recycled rubber, a method for producing the same, and a transmission belt using the same.
  • Recycled rubber is made into a state where it can be molded again by applying chemical treatment or physical treatment to the crosslinked rubber of used rubber products.
  • the use of recycled rubber is extremely effective in reducing the material cost and manufacturing cost of rubber products.
  • Patent Document 1 a crosslinked rubber, the manufacturing method of the reclaimed rubber subjected to desulfurization treatment of conditions of temperature 180 ⁇ 350 ° C. and a shear stress 10 ⁇ 150kg / cm 2 is disclosed.
  • Patent Document 2 discloses a method for producing a reclaimed rubber in which a shearing stress is applied to a crosslinked rubber at a heating temperature equal to or higher than the regenerating temperature at which a break such as cross-linking between the rubber molecules occurs.
  • Patent Document 3 discloses a method for producing a reclaimed rubber in which a raw material powder of a crosslinked rubber and a diene rubber are mixed and a shear stress of a maximum shear rate of 300 / sec or more is applied thereto.
  • Patent Document 4 discloses a method for producing a recycled rubber in which a crosslinked rubber is subjected to a desulfurization treatment under conditions of a temperature of 220 to 350 ° C. and a shear stress of 10 to 150 kg / cm 2 .
  • the recycled rubber of the present invention contains a dispersion of a thermoplastic resin compounding material having a maximum particle size of 250 ⁇ m or less.
  • the method for producing a recycled rubber according to the present invention is to desulfurize a crosslinked rubber by applying a shear stress in the presence of a thermoplastic resin compounding material, and the processing temperature in the desulfurization treatment is set to the compounding temperature of the thermoplastic resin.
  • a temperature of 20 ° C. or more lower than the melting point of the material is set, and a recycled rubber containing a compounded material of a thermoplastic resin having a maximum particle size of 250 ⁇ m or less is obtained.
  • At least a part of the belt main body is made of a rubber composition using the recycled rubber of the present invention.
  • FIG. 1 is a perspective view of a piece of a wrapped V belt according to Embodiment 1.
  • FIG. It is the 1st explanatory view showing the manufacturing method of the wrapped V belt concerning an embodiment.
  • It is 2nd explanatory drawing which shows the manufacturing method of the wrapped V belt which concerns on embodiment.
  • It is 3rd explanatory drawing which shows the manufacturing method of the wrapped V belt which concerns on embodiment.
  • It is a 5th explanatory view showing a manufacturing method of a wrapped V belt concerning an embodiment.
  • It is a 7th explanatory view showing a manufacturing method of a wrapped V belt concerning an embodiment.
  • the recycled rubber according to Embodiment 1 is derived from a rubber composition containing sulfur-crosslinked ethylene propylene diene monomer (hereinafter referred to as “EPDM”), and has a high gel fraction of 50 to 85 mass%.
  • EPDM sulfur-crosslinked ethylene propylene diene monomer
  • the recycled rubber according to Embodiment 1 is derived from sulfur-crosslinked EPDM, and the gel fraction resulting from the sulfur crosslinking is as high as 50 to 85% by mass. Therefore, the rubber composition using the recycled rubber has high rubber elasticity.
  • tan ⁇ is low. Therefore, it is preferable that at least a part of the belt main body of the transmission belt that is bent repeatedly is constituted by the rubber composition using the recycled rubber according to the first embodiment.
  • the gel fraction of the reclaimed rubber according to Embodiment 1 is preferably 50% by mass or more, more preferably from the viewpoint of being easy to re-crosslink, suppressing deterioration of physical properties and obtaining excellent processability. Is 65% by mass or more, preferably 85% by mass or less, more preferably 80% by mass or less.
  • the recycled rubber according to Embodiment 1 includes a rubber component and other rubber compounding agents.
  • the content of the rubber component in the recycled rubber according to Embodiment 1 is preferably 30% by mass or more, more preferably 40% by mass or more, and preferably 70% by mass or less, more preferably 60% by mass or less. .
  • the content of EPDM in the rubber component of the recycled rubber according to Embodiment 1 is preferably 50% by mass or more, more preferably 70% by mass or more.
  • the content of EPDM in the rubber component of the recycled rubber is most preferably 100% by mass, that is, the rubber component of the recycled rubber is most preferably only EPDM.
  • Examples of rubber components other than EPDM that can be included in the recycled rubber according to Embodiment 1 include ethylene- ⁇ -olefin elastomers other than EPDM such as ethylene propylene rubber (EPM), natural rubber (NR), and the like. .
  • EPM ethylene propylene rubber
  • NR natural rubber
  • a rubber compounding agent contained in the recycled rubber according to Embodiment 1 for example, a reinforcing material such as carbon black, a softening agent, a processing aid, a vulcanization acceleration aid, and a crosslinking agent, which have been contained before the desulfurization treatment described later.
  • Agents, vulcanization accelerators, anti-aging agents and the like for example, a reinforcing material such as carbon black, a softening agent, a processing aid, a vulcanization acceleration aid, and a crosslinking agent, which have been contained before the desulfurization treatment described later.
  • the recycled rubber according to the first embodiment is blended with virgin rubber to be a base rubber material, or is used as it is as a base rubber material, and various rubber compounding agents including a crosslinking agent are blended therein.
  • a transmission belt It is used as a rubber composition constituting rubber products such as conveyor belts, tires and hoses. As described above, among these, it is particularly suitable for a transmission belt.
  • the recycled rubber according to Embodiment 1 can be obtained by taking out a crosslinked rubber (crosslinked rubber composition) from a used rubber product and desulfurizing the crosslinked rubber by a predetermined method.
  • the recycled rubber according to Embodiment 1 is obtained by previously pulverizing a crosslinked rubber containing sulfur-crosslinked EPDM into a powdery or granular form, and then applying the powdered or granular crosslinked rubber to a predetermined processing temperature. It is obtained by applying a shearing stress at desulfurization treatment.
  • the gel fraction of the recycled rubber can be controlled by a combination of conditions such as the processing temperature, shear stress, and processing time during the desulfurization process.
  • the regenerated rubber obtained by the desulfurization treatment in this way has a crosslinkable EPDM by cutting a part of the sulfur crosslinking point and the main chain of the EPDM, and the EPDM of the elastic rubber for the gel due to the remaining sulfur crosslinking.
  • the rubber composition using this the rubber elasticity is high and the tan ⁇ is low as compared with the case where only the virgin rubber is used.
  • examples of the used rubber product include a transmission belt, a conveyor belt, a tire, and a hose.
  • the average particle diameter of the powdery or granular crosslinked rubber is preferably 10 ⁇ m or more, more preferably 100 ⁇ m or more, and preferably 5 mm or less, more preferably 3 mm or less.
  • the treatment temperature of the desulfurization treatment is 150 to 250 ° C., and preferably 180 ° C. or more and preferably 230 ° C. or less from the viewpoint of the balance between the desulfurization and the remaining gel content.
  • the shear stress during the desulfurization treatment is preferably 0.981 MPa or more, more preferably 4 MPa or more, and preferably 20 MPa or less, more preferably 15 MPa or less, from the viewpoint of the balance between the desulfurization and the residual gel content. is there.
  • the desulfurization treatment as described above can be performed using known processing equipment such as a single-screw or twin-screw extruder.
  • the recycled rubber according to Embodiment 1 may contain a dispersion of a thermoplastic resin compounding material having a maximum particle size of 250 ⁇ m or less.
  • a rubber composition obtained from a recycled rubber containing a dispersion material of a thermoplastic resin having a maximum particle size of 250 ⁇ m or less has a low tan ⁇ , so that heat generation is suppressed even when it is repeatedly bent. It is suitable for application to rubber products that are repeatedly bent such as a transmission belt.
  • thermoplastic resin examples include blending materials such as polyamide resin (PA), polyethylene terephthalate resin (PET), and polypropylene resin (PP).
  • PA polyamide resin
  • PET polyethylene terephthalate resin
  • PP polypropylene resin
  • PA polyamide resin
  • the compounding material of the thermoplastic resin may be composed of a single type or a plurality of types.
  • the form of the blended material of the thermoplastic resin include powdery, granular, and fibrous forms. Of these, fibrous fibers, particularly short fibers having a fiber diameter of 10 to 30 ⁇ m and a fiber length of 1 to 5 mm are preferred.
  • the content of the compounding material of the thermoplastic resin in the recycled rubber is preferably 2% by mass or more, more preferably 8% by mass or more, and preferably 30% by mass or less, more preferably 20% by mass or less. Further, when producing a recycled rubber containing a thermoplastic resin having a maximum particle size of 250 ⁇ m or less, the treatment temperature in the desulfurization treatment is set to a temperature that is 20 ° C. or more lower than the melting point of the thermoplastic resin compounding material. Is preferred.
  • FIG. 1 shows a wrapped V-belt B (power transmission belt) according to the first embodiment.
  • the wrapped V belt B according to the first embodiment is used for, for example, an agricultural machine or an industrial machine.
  • the dimensions of the wrapped V-belt B according to the first embodiment are not particularly limited, and are, for example, a belt circumferential length of 700 to 5000 mm, a belt width of 16 to 17 mm, and a belt thickness of 8 to 10 mm.
  • the wrapped V-belt B according to the first embodiment is configured in a triple layer of a compression rubber layer 11 on the belt inner peripheral side (pulley contact side), an intermediate adhesive rubber layer 12 and a stretched rubber layer 13 on the belt outer peripheral side.
  • the belt body 10 having a trapezoidal cross-sectional shape is provided.
  • a core wire 14 is embedded in the adhesive rubber layer 12 so as to form a spiral having a pitch in the belt width direction.
  • the belt body 10 is entirely covered with a reinforcing cloth 15.
  • the compressed rubber layer 11, the adhesive rubber layer 12, and the stretch rubber layer 13 are all composed of a crosslinked rubber composition. At least one of the compressed rubber layer 11, the adhesive rubber layer 12, and the stretched rubber layer 13 is composed of a rubber composition that is cross-linked using the reclaimed rubber according to the first embodiment.
  • the rubber composition constituting the compressed rubber layer 11, the adhesive rubber layer 12, and the stretched rubber layer 13 is preferably made of the reclaimed rubber according to the first embodiment, and in that case, the same rubber is used. It may be a composition.
  • the rubber composition using the reclaimed rubber according to the first embodiment may use the reclaimed rubber according to the first embodiment as a base rubber material, and virgin rubber is blended as a rubber component to the base rubber. It may be used as a material.
  • the virgin rubber is preferably an ethylene- ⁇ -olefin elastomer, and more preferably EPDM.
  • the content of virgin rubber in the rubber component of the rubber composition is preferably 20% by mass or more, preferably 80% by mass or less, more preferably 60% by mass or less.
  • various rubber compounding agents are blended in addition to the rubber compounding agent contained in the recycled rubber according to the first embodiment.
  • rubber compounding agents include reinforcing materials such as carbon black, softeners, processing aids, vulcanization acceleration aids, crosslinking agents, vulcanization accelerators, and antiaging agents.
  • the reinforcing material may not be blended when the recycled rubber according to Embodiment 1 includes the reinforcing material.
  • the reinforcing material is preferably blended when the rubber composition containing the recycled rubber according to Embodiment 1 contains virgin rubber.
  • a reinforcing material for example, carbon black, channel black; furnace black such as SAF, ISAF, N-339, HAF, N-351, MAF, FEF, SRF, GPF, ECF, N-234; FT, MT, etc. Thermal black; acetylene black and the like.
  • Silica is also mentioned as a reinforcing agent.
  • the reinforcing agent may be composed of a single species or a plurality of species.
  • the content of the reinforcing material is preferably 30 to 80 parts by mass with respect to 100 parts by mass of the rubber component of the rubber composition, from the viewpoint of a balance between wear resistance and bending resistance.
  • the softener examples include petroleum softeners, mineral oil softeners such as paraffin wax, castor oil, cottonseed oil, sesame oil, rapeseed oil, soybean oil, palm oil, palm oil, fallen raw oil, waxy wax, rosin And vegetable oil-based softeners such as pine oil.
  • the softener may be composed of a single species or a plurality of species.
  • the content of the softening agent is, for example, 2 to 30 parts by mass with respect to 100 parts by mass of the rubber component of the rubber composition.
  • processing aids include stearic acid, polyethylene wax, and fatty acid metal salts.
  • the processing aid may be composed of a single species or a plurality of species.
  • the content of the processing aid is, for example, 0.1 to 3 parts by mass with respect to 100 parts by mass of the rubber component of the rubber composition.
  • the vulcanization acceleration aid examples include metal oxides such as magnesium oxide and zinc oxide (zinc white), metal carbonates, fatty acids and derivatives thereof.
  • the vulcanization acceleration aid may be composed of a single species or a plurality of species.
  • the content of the vulcanization acceleration aid is, for example, 0.5 to 8 parts by mass with respect to 100 parts by mass of the rubber component of the rubber composition.
  • crosslinking agent examples include sulfur and organic peroxides.
  • sulfur may be blended, an organic peroxide may be blended, or both of them may be used in combination.
  • the compounding amount of the crosslinking agent is, for example, 0.5 to 4.0 parts by mass with respect to 100 parts by mass of the rubber component of the rubber composition in the case of sulfur, and the rubber component 100 of the rubber composition in the case of an organic peroxide. For example, 0.5 to 8.0 parts by mass with respect to parts by mass.
  • organic peroxide examples include dialkyl peroxides such as dicumyl peroxide, peroxyesters such as t-butyl peroxyacetate, and ketone peroxides such as dicyclohexanone peroxide.
  • dialkyl peroxides such as dicumyl peroxide, peroxyesters such as t-butyl peroxyacetate, and ketone peroxides such as dicyclohexanone peroxide.
  • the organic peroxide may be a single species or a plurality of species.
  • the rubber composition When the crosslinking agent is sulfur, the rubber composition includes a gel component due to residual sulfur crosslinking and a sulfur bond derived from additional sulfur crosslinking.
  • the crosslinking agent is an organic peroxide, residual rubber crosslinking And a C—C bond derived from organic peroxide crosslinking. Therefore, by using the recycled rubber according to Embodiment 1, a rubber composition having more crosslinking points can be obtained as compared with a rubber composition using only EPDM virgin rubber.
  • the vulcanization accelerator examples include thiazole type (eg MBT, MBTS etc.), thiuram type (eg TT, TRA etc.), sulfenamide type (eg CZ etc.), dithiocarbamate type (eg BZ-P etc.) And the like.
  • the vulcanization accelerator may be composed of a single species or a plurality of species.
  • sulfur is used as the crosslinking agent, a vulcanization accelerator is preferably added. In that case, it is preferable to use a thiazole vulcanization accelerator and a thiuram vulcanization accelerator in combination.
  • the content of the vulcanization accelerator is, for example, 2 to 10 parts by mass with respect to 100 parts by mass of the rubber component of the rubber composition.
  • Antiaging agents include amine-based, quinoline-based, hydroquinone derivatives, phenol-based and phosphite-based agents.
  • the anti-aging agent may be composed of a single species or a plurality of species.
  • the content of the anti-aging agent is, for example, 0 to 8 parts by mass with respect to 100 parts by mass of the rubber component of the rubber composition.
  • layered silicates such as smectite group, vermulite group, kaolin group and the like may be blended.
  • the loss coefficient tan ⁇ at 100 ° C. in the line direction of the rubber composition using the recycled rubber according to Embodiment 1 is preferably 0.04 or more, more preferably 0.06 or more, and preferably 0. .15 or less, more preferably 0.12 or less.
  • the loss coefficient tan ⁇ is obtained based on JIS K6394.
  • the core wire 14 is composed of twisted yarns such as polyester fiber (PET), polyethylene naphthalate fiber (PEN), aramid fiber, vinylon fiber and the like.
  • PET polyester fiber
  • PEN polyethylene naphthalate fiber
  • aramid fiber vinylon fiber and the like.
  • an adhesive treatment for heating after being immersed in an RFL aqueous solution before molding and / or an adhesive treatment for drying after being immersed in rubber paste is performed.
  • the reinforcing cloth 15 is made of, for example, a woven fabric, a knitted fabric, a non-woven fabric, or the like formed of yarns such as cotton, polyamide fiber, polyester fiber, and aramid fiber.
  • the reinforcing cloth 15 is coated with rubber paste on the surface on the side of the belt main body 10 and / or an adhesive treatment in which it is immersed in an RFL aqueous solution and heated before molding. Adhesive treatment for drying is applied.
  • a rubber sheet 11 ′ for the compression rubber layer, a rubber sheet 12 ′ for the adhesive rubber layer, a rubber sheet 13 ′ for the stretch rubber layer, a twisted yarn 14 ′ for the core wire, and a cloth 15 ′ for the reinforcing cloth prepare.
  • those including the recycled rubber according to the first embodiment are the first embodiment.
  • An uncrosslinked rubber composition obtained by kneading the recycled rubber and the rubber compounding agent is obtained by processing into a sheet shape using a calender roll or the like.
  • the twisted yarn 14 ′ for the core wire and the fabric 15 ′ for the reinforcing fabric are subjected to adhesion treatment.
  • the rubber sheet 11 'for the compression rubber layer is wound around the mantle 21 a plurality of times, and the rubber sheet 12' for the adhesive rubber layer is wound thereon. Further, as shown in FIG. 2B, the twisted yarn 14 'is wound in a spiral shape. Further thereon, as shown in FIG. 2C, a rubber sheet 12 'for the adhesive rubber layer and a rubber sheet 13' for the stretch rubber layer are wound in order to produce a cylindrical laminated structure 10 '.
  • the cylindrical laminated structure 10 ′ is cut into a predetermined width on the mantle 21 and then removed from the mantle 21.
  • the annular laminated structure 10 ' is wound around a pair of pulleys with the rubber sheet 11' side for the compressed rubber layer facing outward and rotated.
  • the volume is adjusted by obliquely cutting both sides of the laminated portion of the sheet 11 ′ into a V shape.
  • the lapped annular laminated structure 10 ' is fitted into the groove 23 of the cylindrical mold 22, and it is placed in a vulcanizing can and heated and pressurized.
  • the rubber component of the annular laminated structure 10 ′ is cross-linked to form the belt main body 10
  • the twisted yarn 14 ′ is bonded and integrated to the belt main body 10 to form the core wire 14, and the cloth 15 ′ is the belt main body.
  • the wrapped V-belt B according to the first embodiment is manufactured by being bonded and integrated with 10 to form the reinforcing cloth 15.
  • examples of the used rubber product include a transmission belt, a conveyor belt, a tire, and a hose.
  • Examples of rubber components contained in the crosslinked rubber include natural rubber (NR), EPDM and EPM ethylene- ⁇ -olefin elastomers, chloroprene rubber (CR), hydrogenated nitrile rubber (H-NBR), and isoprene rubber (IR). Styrene butadiene rubber (SBR), butadiene rubber (BR), acrylonitrile butadiene rubber (NBR), butyl rubber (IIR) and the like.
  • the rubber component contained in the crosslinked rubber may be composed of a single species or a plurality of species.
  • the content of the rubber component in the crosslinked rubber is preferably 30% by mass or more, more preferably 40% by mass or more, and preferably 70% by mass or less, more preferably 60% by mass or less.
  • carbon black In addition to the crosslinked rubber, carbon black, a filler, an anti-aging agent, a plasticizer, and the like may be blended.
  • the rubber component is crosslinked, but it may be crosslinked by sulfur or by an organic peroxide.
  • the crosslinked rubber before the desulfurization treatment is preferably pulverized and powdery or granular from the viewpoint of efficiently performing the desulfurization treatment.
  • the average particle size of the powdery or granular crosslinked rubber is preferably 10 ⁇ m or more, more preferably 100 ⁇ m or more, still more preferably 200 ⁇ m or more, and preferably 5 mm or less, more preferably 3 mm or less.
  • thermoplastic resin examples include blending materials such as polyamide resin (PA), polyethylene terephthalate resin (PET), and polypropylene resin (PP).
  • PA polyamide resin
  • PET polyethylene terephthalate resin
  • PP polypropylene resin
  • PA polyamide resin
  • the compounding material of the thermoplastic resin may be composed of a single type or a plurality of types.
  • the form of the blended material of the thermoplastic resin include powdery, granular, and fibrous forms. Of these, fibrous fibers, particularly short fibers having a fiber diameter of 10 to 30 ⁇ m and a fiber length of 1 to 5 mm are preferred.
  • the compounding material of the thermoplastic resin is contained in the crosslinked rubber, that is, present in a place where the crosslinked rubber is pre-dispersed and compounded in the crosslinked rubber taken out from the used rubber product, whereby shearing is applied to the crosslinked rubber.
  • the content of the thermoplastic resin compounding material in the crosslinked rubber is preferably 2% by mass or more, more preferably 8% by mass or more, and preferably 20% by mass or less, more preferably 15% by mass or less. It is.
  • the compounding material of the thermoplastic resin is not contained in the crosslinked rubber, and may be present in a place where the crosslinked rubber is mixed with the crosslinked rubber during the desulfurization treatment and thereby shear is applied to the crosslinked rubber.
  • the desulfurization treatment in the method for producing recycled rubber according to Embodiment 2 is a physical treatment in which shearing stress is applied to the crosslinked rubber to cut or depolymerize the crosslinked portion.
  • examples of the desulfurization treatment method include a method of continuously desulfurizing the crosslinked rubber using a shear flow field reaction tank having a uniaxial or biaxial screw.
  • the process temperature in a desulfurization process is set to the temperature 20 degreeC or more lower than melting
  • the treatment temperature in the desulfurization treatment is the temperature of the object to be treated at the time of the desulfurization treatment.
  • It is the set temperature in the tank.
  • the melting point of the blended material of the thermoplastic resin is, for example, 225 to 235 ° C. in the case of nylon 6 and 260 to 270 ° C. in the case of nylon 66, and is a polyethylene terephthalate resin (PET).
  • PET polyethylene terephthalate resin
  • PP polypropylene resin
  • DSC differential scanning calorimeter
  • the treatment temperature in the desulfurization treatment is, for example, set to 205 ° C. or less in the case of a blended material of nylon 6 having a melting point of 225 ° C., and to 240 ° C. or less in the case of nylon 66 having a melting point of 260 ° C. Set.
  • the treatment temperature in the desulfurization treatment is preferably set to a temperature that is 30 ° C. or more lower than the melting point of the blended material of the thermoplastic resin blended with the crosslinked rubber, from the viewpoint of suppressing deterioration of physical properties in the obtained recycled rubber, 50 ° C.
  • the temperature is set to 20 ° C. or lower than the lowest melting point among these melting points.
  • the shear stress in the desulfurization treatment is preferably set to 1 MPa or more, more preferably set to 4 MPa or more from the viewpoint of appropriately performing the desulfurization treatment, and the effect of the blended material of the thermoplastic resin is diluted. From the viewpoint of regulating the operation, it is preferably set to 20 MPa or less, and more preferably set to 15 MPa or less.
  • thermoplastic resin compounding material includes the above-mentioned polyamide resins (PA) and the like, and examples of the form include powdery, granular, fibrous and the like.
  • PA polyamide resins
  • the other thermoplastic resin compounding material may be the same as or different from the thermoplastic resin compounding material contained in the crosslinked rubber.
  • the compounded material of the thermoplastic resin is cut by shearing in the desulfurization process and dispersed to be reduced in particle size.
  • the reclaimed rubber obtained after the desulfurization process the same rubber as the crosslinked rubber In the component, a compounding material of a thermoplastic resin having a maximum particle size of 250 ⁇ m or less is dispersed and contained.
  • a thermoplastic resin compounding material having a maximum particle size of more than 250 ⁇ m is no longer a foreign substance and may cause cracks.
  • the maximum particle size of the thermoplastic resin compounding material is preferably 230 ⁇ m or less, more preferably 205 ⁇ m or less, and even more preferably from the viewpoint of suppressing the occurrence of cracks at the interface of the thermoplastic resin compounding material in the obtained recycled rubber. It is 155 ⁇ m or less, more preferably 150 ⁇ m or less, preferably 5 ⁇ m or more, more preferably 20 ⁇ m or more, still more preferably 50 ⁇ m or more, and even more preferably 100 ⁇ m or more.
  • the maximum particle size of the thermoplastic resin compounding material in the recycled rubber can be controlled by the shear stress or the like in the desulfurization process. The maximum particle size of the thermoplastic resin compounding material can be measured by observing the surface of the obtained recycled rubber.
  • the content of the rubber component in the recycled rubber is preferably 30% by mass or more, more preferably 40% by mass or more, and preferably 70% by mass or less, more preferably 60% by mass or less.
  • the content of the thermoplastic resin compounding material in the recycled rubber is preferably 2% by mass or more, more preferably 8% by mass or more, and preferably 30% by mass or less, more preferably 20% by mass or less.
  • the processing temperature at the time of desulfurization treatment by applying a shear stress to the crosslinked rubber in the presence of the thermoplastic resin compounding material is set to be the same as that of the thermoplastic resin compounding material.
  • the temperature is set to 20 ° C. or more lower than the melting point, and a recycled rubber containing a thermoplastic resin compounding material having a maximum particle size of 250 ⁇ m or less is dispersed and contained. Therefore, the rubber composition obtained from the recycled rubber obtained has a low tan ⁇ as shown in the test evaluation 2 of the following examples, so that heat generation is suppressed even when it is repeatedly bent.
  • a recycled rubber suitable for application to a rubber product that undergoes repeated bending, such as a transmission belt, can be produced.
  • the blended material of thermoplastic resin such as short fibers contained in the raw material crosslinked rubber is usually separated as a foreign substance by sieving or an air floating table.
  • the blended material of the thermoplastic resin contributes to the reduction in tan ⁇ in the rubber composition using the obtained recycled rubber.
  • the recycled rubber obtained by the production method of Embodiment 2 may have the same configuration as the recycled rubber according to Embodiment 1, that is, derived from a rubber composition containing a sulfur-crosslinked ethylene propylene diene monomer. And the gel fraction may be 50 to 85% by mass.
  • the reclaimed rubber obtained by the production method of Embodiment 2 is blended with the same or different virgin rubber as contained in the reclaimed rubber to form a base rubber material as in Embodiment 1, or as it is with the base rubber material as it is. Then, a rubber compounding agent containing a crosslinking agent is compounded, and for example, a rubber constituting a rubber product such as a transmission belt such as a wrapped V belt B shown in FIG. 1 in Embodiment 1, a conveyor belt, a tire, a hose, etc. Used as a composition.
  • the recycled rubber obtained by the production method of Embodiment 2 has a low tan ⁇ rubber composition using the rubber, so that heat generation can be suppressed even when it is repeatedly bent. Therefore, it is preferable that at least a part of the belt body of the transmission belt bent repeatedly is constituted by the rubber composition using the recycled rubber obtained by the manufacturing method of Embodiment 2.
  • the storage elastic modulus E ′ at 25 ° C. in the line direction of the rubber composition using the recycled rubber obtained by the production method of Embodiment 2 is preferably 12 MPa or more, more preferably 15 MPa or more, Preferably it is 70 MPa or less, More preferably, it is 40 MPa or less.
  • the storage elastic modulus E ′ at 100 ° C. is preferably 8 MPa or more, more preferably 10 MPa or more, and preferably 50 MPa or less, more preferably 30 MPa or less.
  • the storage elastic modulus E ′ at 120 ° C. is preferably 7 MPa or more, more preferably 9 MPa or more, and preferably 50 MPa or less, more preferably 25 MPa or less.
  • the loss factor tan ⁇ at 25 ° C. in the row direction of the recycled rubber obtained by the production method of Embodiment 2 is preferably 0.06 or more, more preferably 0.08 or more, and preferably 0.20. Below, more preferably 0.18 or less.
  • the loss coefficient tan ⁇ at 100 ° C. is preferably 0.04 or more, more preferably 0.06 or more, and preferably 0.15 or less, more preferably 0.12 or less.
  • the loss coefficient tan ⁇ at 120 ° C. is preferably 0.04 or more, more preferably 0.06 or more, and preferably 0.14 or less, more preferably 0.11 or less.
  • the storage elastic modulus E ′ and the loss coefficient tan ⁇ are obtained based on JIS K6394.
  • a recycled rubber 1 having a gel fraction of 70% by mass at a treatment temperature of 200 ° C. and a screw rotation speed of 400 rpm (shear stress of 7 MPa) was obtained.
  • a recycled rubber 2 having a gel fraction of 52% by mass was obtained at a treatment temperature of 220 ° C. and a screw rotation speed of 400 rpm (shear stress of 8 MPa).
  • a recycled rubber 3 having a gel fraction of 45% by mass was obtained at a treatment temperature of 260 ° C. and a screw rotation speed of 600 rpm (shear stress of 11 MPa).
  • the gel fraction was determined by the toluene swelling method described above.
  • Example 1-1 For 200 parts by mass of recycled rubber 1 (100 parts by mass of EPDM as a rubber component), 1 part by mass of stearic acid (manufactured by NOF Corporation, trade name: bead stearic acid Tsubaki), zinc oxide (manufactured by Sakai Chemical Industry Co., Ltd.) Product name: 5 parts by mass of zinc oxide (3 types), softener (made by Idemitsu Kosan Co., Ltd., product name: Diana Process PW-90), 20 parts by mass, sulfur (oil treated sulfur by Karuizawa Smelter), 3 parts by mass, 2 parts by weight of a sulfur accelerator (trade name: Noxeller TET-G manufactured by Ouchi Shinsei Chemical Co., Ltd.) and 1 part by weight of a thiazole vulcanization accelerator (trade name: Noxeller DM-P manufactured by Ouchi Shinsei Chemical Co., Ltd.) An uncrosslinked rubber composition obtained by kneading was designated as Example 1-1.
  • Example 1-2 For 200 parts by mass of recycled rubber 1 (100 parts by mass of EPDM as a rubber component), 1 part by mass of stearic acid, 5 parts by mass of zinc oxide, 20 parts by mass of softening agent, organic peroxide (manufactured by NOF Corporation) Product name: Perbutyl P-40 Purity 40% by mass) An uncrosslinked rubber composition obtained by blending and kneading 8 parts by mass (active ingredient 3.2 parts by mass) was defined as Example 1-2.
  • Example 1-3 An uncrosslinked rubber composition having the same structure as in Example 1 except that the recycled rubber 2 was used was designated as Example 1-3.
  • Example 1-4 50 parts by mass of virgin rubber (trade name: EP33 manufactured by JSR) of EPDM is blended with 100 parts by mass of recycled rubber 1 (EPDM 50 parts by mass of rubber component), and 100 parts by mass of rubber component contained therein,
  • EPDM 50 parts by mass of rubber component 100 parts by mass of recycled rubber 1
  • HAF carbon black trade name: SEAST 3 manufactured by Tokai Carbon Co., Ltd.
  • stearic acid 1 part by mass of stearic acid
  • 5 parts by mass of zinc oxide 20 parts by mass of a softening agent
  • 3 parts by mass of sulfur and thiuram-based vulcanization
  • An uncrosslinked rubber composition obtained by blending 2 parts by mass of an accelerator and 1 part by mass of a thiazole vulcanization accelerator and kneading was designated as Example 1-4.
  • Comparative Example 1-1 A non-crosslinked rubber composition having the same structure as in Example 1 except that the recycled rubber 3 was used was designated as Comparative Example 1-1.
  • Comparative Example 1-2 A non-crosslinked rubber composition having the same structure as in Example 2 except that the recycled rubber 3 was used was designated as Comparative Example 1-2.
  • the rubber compositions of Examples 1-1, 1-3, and 1-4 and Comparative Example 1-1 are sulfur cross-linked systems, the rubber compositions obtained by cross-linking these are residual The gel content due to sulfur cross-linking and the sulfur bond derived from the additional sulfur cross-linking are provided.
  • the rubber compositions of Example 1-2 and Comparative Example 1-2 are organic peroxide crosslinking systems, the rubber composition obtained by crosslinking them has a gel content due to residual sulfur crosslinking. And a C—C bond derived from organic peroxide crosslinking.
  • FIG. 3 shows a pulley layout of the belt running test machine 30.
  • the belt running test machine 30 includes a driving pulley 31 having a pulley diameter of 80 mm and a driven pulley 32 having a pulley diameter of 80 mm provided below the driving pulley 31.
  • the driven pulley 32 is configured to be movable up and down, and by suspending a weight (dead weight) from the driven pulley 32, the driven pulley 32 and the wrapped V-belt B wound around the driven pulley 32 can be loaded with tension. Has been.
  • the belt life was evaluated as a relative value with the belt running time until crack occurrence in Comparative Example 1-1 as 100. Further, the belt temperature during belt running was measured using a non-contact type surface thermometer, and the maximum value of the temperature difference from the ambient temperature was determined.
  • Test evaluation results The test results are shown in Table 1.
  • Example 1-3 of the sulfur crosslinking system using the regenerated rubber 2 having a gel fraction of 52% by mass higher than that of the regenerated rubber 3 tan ⁇ is lower than that in the case of Comparative Example 1-1 (0. 125), and the heat generation during running of the belt was small (+ 29 ° C.), and the belt life was also long (142).
  • Example 1-1 of the sulfur cross-linking system using the regenerated rubber 1 having a gel fraction of 70% by mass higher than that of the regenerated rubber 2 tan ⁇ is much lower than in the case of Example 1-2.
  • the heat generation during belt running was smaller (+ 25 ° C.), and the belt life was longer (149).
  • Example 1-2 of the organic peroxide cross-linking system using the regenerated rubber 1 having a gel fraction of 70% by mass tan ⁇ is much lower than that in Example 1-1 (0.
  • the heat generation during running of the belt was much smaller (+ 21 ° C.), and the belt life was even longer (168).
  • Example 1-4 of the sulfur crosslinking system in which recycled rubber 2 and EPDM virgin rubber were blended tan ⁇ was low (0.119) as compared with Comparative Examples 1-1 and 1-2. Also, the heat generated during belt running was small (+ 28 ° C.), and the belt life was also long (152).
  • Recycled rubbers 1 and 2 used in the rubber compositions of Examples 1-1 to 1-4 were obtained by desulfurization treatment of sulfur-crosslinked EPDM, but achieved performance superior to that of using EPDM virgin rubber. can do.
  • the crosslinked rubber After the crosslinked rubber is pulverized to an average particle size of 400 ⁇ m, it is put into a twin screw extruder (manufactured by Nippon Steel Works, model number: TEX30 ⁇ , screw diameter: 30 mm, screw length: 1785 mm), and the processing temperature is the melting point of nylon 66 short fiber.
  • Example 2-1 The recycled rubber of Example 2-1 was cut using a cutter, and observed using a microscope (Keyence Co., Ltd., model number: VHX2000) by magnifying three portions of the cross section by 200 times, as shown in FIG. Such a form was seen, and when the outer diameter (maximum outer diameter) of the largest nylon short fiber was measured by the measurement mode, it was 148 ⁇ m. Moreover, it was 62 mass% when the gel fraction was calculated
  • Example 2-2 A recycled rubber obtained in the same manner as in Example 2-1 except that the screw was rotated at 400 rpm (shear stress: 8 MPa) and subjected to desulfurization treatment by applying shear stress to the crosslinked rubber was obtained as Example 2-2. It was.
  • Example 2-2 For the recycled rubber of Example 2-2, the maximum outer diameter of the nylon short fiber was measured in the same manner as in Example 2-1, and it was 202 ⁇ m. Moreover, the gel fraction was 68 mass%.
  • Example 2-3 Except that the treatment temperature was 230 ° C., which is 30 ° C. lower than the melting point of nylon 66 short fiber, 230 ° C., and the screw rotation speed was 600 rpm (shear stress: 12 MPa), and the desulfurization treatment was performed by applying shear stress to the crosslinked rubber.
  • a recycled rubber obtained in the same manner as in Example 2-1 was designated as Example 2-3.
  • Example 2-3 For the recycled rubber of Example 2-3, the maximum outer diameter of the nylon short fiber was measured in the same manner as in Example 2-1, and was found to be 151 ⁇ m. Moreover, the gel fraction was 55 mass%.
  • Example 2-4 Example 2-1 except that the crosslinked rubber was subjected to a desulfurization treatment at a treatment temperature of 200 ° C., which is 60 ° C. lower than the melting point of nylon 66 short fiber, 260 ° C., and a screw rotation speed of 200 rpm (shear stress: 6 MPa). Recycled rubber obtained in the same manner as in Example 2-4 was used.
  • Example 2-4 For the recycled rubber of Example 2-4, the maximum outer diameter of the nylon short fiber was measured in the same manner as in Example 2-1, and it was 227 ⁇ m. Moreover, the gel fraction was 75 mass%.
  • Example 2-5 Except that the treatment temperature was 240 ° C., which is 20 ° C. lower than the melting point of nylon 66 short fiber of 260 ° C., and the screw rotation speed was 600 rpm (shear stress: 13 MPa). A recycled rubber obtained in the same manner as in Example 2-1 was designated as Example 2-5.
  • Example 2-5 For the recycled rubber of Example 2-5, the maximum outer diameter of the nylon short fiber was measured in the same manner as in Example 2-1, and it was 155 ⁇ m. Moreover, the gel fraction was 51 mass%.
  • the gel fraction of the recycled rubber of Comparative Example 2-1 was 78% by mass.
  • the maximum outer diameter of the nylon short fiber was measured in the same manner as in Example 2-1, and it was 147 ⁇ m. Moreover, the gel fraction was 46 mass%.
  • the maximum outer diameter of the nylon short fiber was measured in the same manner as in Example 2-1, and it was 311 ⁇ m. Moreover, the gel fraction was 83 mass%.
  • Example 2-4 The treatment temperature was 250 ° C., which is 10 ° C. lower than the melting point of nylon 66 short fiber, 260 ° C., and the rotational speed of the screw was 100 rpm (shear stress: 4 MPa).
  • a recycled rubber obtained in the same manner as in Example 2-1 was designated as Comparative Example 2-4.
  • the maximum outer diameter of the nylon short fiber was measured in the same manner as in Example 2-1, and it was 302 ⁇ m. Moreover, the gel fraction was 70 mass%.
  • ⁇ Dynamic viscoelasticity test> For the uncrosslinked rubber compositions using the reclaimed rubbers of Examples 2-1 to 2-5 and Comparative Examples 2-1 to 2-4, a sheet-like rubber sheet was molded and vulcanized, based on JIS K6394.
  • the storage elastic modulus E ′ and the loss coefficient tan ⁇ were measured at 25 ° C., 100 ° C., and 120 ° C. in the linear direction, with a vibration frequency of 10 Hz and a dynamic strain of 1.0%.
  • Test evaluation results The test results are shown in Tables 4 and 5.
  • Examples 2-1 to 2-5 containing Nylon 66 short fibers and Comparative Examples 2-3 to 2-4 were compared with Comparative Example 2-1 containing no Nylon 66 short fibers.
  • the storage elastic modulus E ′ is high, the loss coefficient tan ⁇ is low, and the belt durability is excellent.
  • Comparative Example 2-2 only the storage elastic modulus E ′ at 25 ° C. is lower than that of Comparative Example 2-1, but otherwise, the storage elastic modulus E ′ is higher than that of Comparative Example 2-1, and the loss. It can be seen that the coefficient tan ⁇ is low and the belt durability is excellent.
  • Comparative Example 2-1 does not contain nylon 66 short fibers, and therefore has a relatively low storage elastic modulus and a high tan ⁇ . As a result, it is presumed that heat generation during bending is large and deterioration proceeds greatly.
  • Examples 2-1 to 2-5 have better belt durability than Comparative Examples 2-1 to 2-4.
  • the present invention is useful in the technical field of recycled rubber, a method for producing the same, and a transmission belt using the same.

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Abstract

L'invention concerne un caoutchouc régénéré qui contient un matériau de résine thermoplastique dispersé dans celui-ci, ce matériau ayant un diamètre maximal de particules égal ou inférieur à 250 µm.
PCT/JP2015/002834 2014-06-25 2015-06-04 Caoutchouc régénéré, son procédé de fabrication et courroie de transmission le comprenant WO2015198538A1 (fr)

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JP2016529010A JPWO2015198538A1 (ja) 2014-06-25 2015-06-04 再生ゴム及びその製造方法、並びにそれを用いた伝動ベルト

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JP2017223361A (ja) * 2016-06-14 2017-12-21 三ツ星ベルト株式会社 ラップドｖベルト、及びラップドｖベルトの製造方法

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WO2017145866A1 (fr) * 2016-02-24 2017-08-31 横浜ゴム株式会社 Composition de caoutchouc pour adhésifs, procédé de collage pour caoutchoucs et bande transporteuse
CN107602965A (zh) * 2017-09-21 2018-01-19 如皋市嘉好热熔胶有限公司 一种轮胎再生胶及其制备方法
CN109721863A (zh) * 2019-01-23 2019-05-07 保定华月胶带有限公司 阻燃再生胶在阻燃输送带中的应用
JP6777835B1 (ja) * 2019-06-07 2020-10-28 バンドー化学株式会社 大型ｖベルト

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