WO2022210413A1 - 接着体および接着体の製造方法 - Google Patents

接着体および接着体の製造方法 Download PDF

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Publication number
WO2022210413A1
WO2022210413A1 PCT/JP2022/014626 JP2022014626W WO2022210413A1 WO 2022210413 A1 WO2022210413 A1 WO 2022210413A1 JP 2022014626 W JP2022014626 W JP 2022014626W WO 2022210413 A1 WO2022210413 A1 WO 2022210413A1
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WIPO (PCT)
Prior art keywords
adhesive
fluororubber
carbon dioxide
bonded
nonwoven fabric
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2022/014626
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English (en)
French (fr)
Japanese (ja)
Inventor
直樹 渡辺
善宏 瀬戸口
崇史 相澤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
National Institute of Advanced Industrial Science and Technology AIST
Valqua Ltd
Original Assignee
National Institute of Advanced Industrial Science and Technology AIST
Valqua Ltd
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Filing date
Publication date
Application filed by National Institute of Advanced Industrial Science and Technology AIST, Valqua Ltd filed Critical National Institute of Advanced Industrial Science and Technology AIST
Priority to JP2023511197A priority Critical patent/JP7679980B2/ja
Priority to US18/283,265 priority patent/US12565601B2/en
Priority to KR1020237030727A priority patent/KR20230163371A/ko
Publication of WO2022210413A1 publication Critical patent/WO2022210413A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C09J2400/266—Presence of textile or fabric in the pretreated surface to be joined
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2427/00—Presence of halogenated polymer
    • C09J2427/008—Presence of halogenated polymer in the pretreated surface to be joined

Definitions

  • One embodiment of the present invention relates to an adhesive body or a method for manufacturing an adhesive body.
  • Substrates such as non-woven fabrics, woven fabrics, fibers, porous membranes, and films may be used alone, but may also be used by laminating a plurality of the same substrates or other substrates. be.
  • the method of bonding substrates to each other using the adhesive has the advantage that the substrates can be easily bonded to each other. There is room for improvement in this regard, as contamination and contamination may occur from the adhesive part.
  • the method of bonding substrates by heat fusion has the advantage of being able to obtain a bonded body with high adhesive strength, but the degree of freedom in selecting substrates is limited in terms of heat resistance.
  • the shape and physical properties of the base material before fusion bonding specifically, the shape of voids, etc., that the base material had before fusion bonding, and the functional material contained in the base material before fusion bonding
  • the method of bonding substrates by heat-sealing has room for improvement in terms of energy cost.
  • One embodiment of the present invention is adhesion in which substrates are bonded to each other with sufficient adhesive strength using fluororubber without impairing the physical properties, shape, functions, etc. of the substrates before bonding. provide the body
  • a configuration example of the present invention is as follows.
  • the substrates are Fluorine containing at least one fluororubber selected from fluoroelastomers (FKM) and perfluoroelastomers (FFKM) and having a Mooney viscosity (ML1+10) at 121°C of 80 to 115 measured according to ASTM D 1646 An adhered body adhered via an adhesive layer obtained from a rubber composition.
  • FKM fluoroelastomers
  • FFKM perfluoroelastomers
  • the fluororubber composition is a fluororubber (A1) having a Mooney viscosity (ML1+10) of 40 to 150 at 121° C. measured according to ASTM D 1646;
  • a method for manufacturing an adhesive preparing a structure with an adhesive disposed between substrates; bonding the structure in the presence of liquid or gaseous carbon dioxide; including
  • the adhesive is an adhesive obtained from a fluororubber composition having a Mooney viscosity (ML1+10) at 121° C. of 80 to 115 measured according to ASTM D 1646.
  • a method for manufacturing an adhesive body is an adhesive obtained from a fluororubber composition having a Mooney viscosity (ML1+10) at 121° C. of 80 to 115 measured according to ASTM D 1646.
  • the step of introducing carbon dioxide into the pressure vessel comprises: A step of introducing liquid or gaseous carbon dioxide so that the pressure in the pressure vessel is 3 MPa or more, [7] The method for producing an adhesive body according to [7].
  • the fluororubber composition is a fluororubber (A1) having a Mooney viscosity (ML1+10) of 40 to 150 at 121° C. measured according to ASTM D 1646; Manufacture of the adhesive body according to any one of [6] to [9], which contains a fluororubber (A2) having a Mooney viscosity (ML1+10) at 121°C of 10 or more and less than 40 measured according to ASTM D 1646. Method.
  • the adhesive is the liquid or paste fluororubber composition, the dried liquid or paste fluororubber composition, or the fiber, nonwoven fabric or film obtained from the fluororubber composition.
  • the adhesive is A step of spinning the fluororubber composition, and Step B of cross-linking the fibers obtained in step A
  • sufficient adhesive strength (eg, peel strength 0.00) can be obtained using fluororubber without impairing the physical properties, shape, functions, etc. of the base material before adhesion. 3 N/10 mm or more) can provide an adhered body in which the substrates are adhered to each other.
  • the degree of freedom in selecting the base material is high, it is possible to obtain a bonded body using a desired base material without impairing its physical properties, shape, function, and the like.
  • the adhesive portion (adhesive layer) has excellent chemical resistance, and a bonded body that is less likely to be contaminated with foreign matter from the adhesive portion (adhesive layer) can be obtained.
  • the bonded body can be formed without applying heat from the outside, so that the bonded body can be obtained at low energy cost and in a simplified process. Furthermore, the resulting bonded body also has the advantage of being easy to secondary process. Also, according to an embodiment of the present invention, multiple bonds can be formed in a single process, so even if multiple bonds are required, low energy costs and a simplified process are possible. can obtain the desired bonded body.
  • FIG. 1 is a plan view schematically showing a laminate of a substrate and an adhesive used in Example 9.
  • FIG. 2 is a front view schematically showing a state in which the laminate of FIG. 1 is spirally wound around a rod or tubular member (state of the bonded body obtained in Example 9).
  • the substrates are made of at least one fluororubber selected from fluoroelastomers (FKM) and perfluoroelastomers (FFKM). and is bonded via an adhesive layer obtained from a fluororubber composition having a Mooney viscosity of 80 to 115.
  • FKM fluoroelastomers
  • FFKM perfluoroelastomers
  • Mooney viscosity in the present specification means Mooney viscosity (ML1+10) at 121° C. measured according to ASTM D 1646.
  • the bonded body may be a bonded body different from a so-called crimped body (hereinafter also referred to as "bonded body (I)”) in which base materials are bonded together without pressing them. It may be a so-called pressure-bonded body (hereinafter also referred to as “bonded body (II)").
  • the adhesive body (I) obtained by the present method (I) described below is usually subjected to a pressure (surface pressure) of about several hundred gf/cm 2 in the lamination direction of the substrates during bonding. It is different from a press-bonded body, which is usually subjected to a pressure of about 10 kgf/cm 2 or more in the lamination direction of the base material when being adhered.
  • This bonded body is a bonded body in which the substrates are sufficiently bonded together without substantially damaging the shape of the substrates before bonding (e.g., voids and fiber shapes of nonwoven fabrics, etc.).
  • the bonded body (I) is preferable, and the bonded body (II) is preferable from the viewpoint of superior adhesive strength between substrates.
  • the present adhesive body is an adhesive body bonded in the presence of liquid or gaseous carbon dioxide.
  • carbon dioxide plasticizes at least a portion of the fluororubber, resulting in an anchor effect, etc., which fixes the shape of the substrates while they are engaged with each other.
  • the bonded body (II) is a bonded body pressure-bonded in the presence of liquid or gaseous carbon dioxide, particularly in the presence of liquid, gas-liquid mixed state, or near-liquid carbon dioxide.
  • carbon dioxide in a state close to liquid specifically refers to carbon dioxide in a state with a density of 0.4 g/mL (approximately half the density of liquid carbon dioxide) or higher.
  • the bonded body is preferably bonded at a temperature lower than the temperature at which the fluororubber melts, preferably at a temperature of about 50° C. or less, and more preferably without applying heat from the outside.
  • various substrates can be used as the substrate in the present adhesive body, and even if a substrate subjected to functionalization treatment such as conventionally known surface treatment such as hydrophilic treatment is used, the function can be maintained. Since the bonded body is not damaged, there is a high degree of freedom in selecting the base material.
  • the bonded body when the bonded body can be made while taking advantage of the properties of the base material (e.g., function, voids of the nonwoven fabric, fiber shape), and the bonded body contains the following functional materials:
  • the bonded body even if the functional material is poor in heat resistance, the bonded body can take advantage of the functions and properties of the functional material.
  • the shape and size of the adhesive body are not particularly limited, and may be appropriately selected according to the desired application.
  • Examples of the shape of the adhesive body include laminate, bag, ring, spiral, and tube (cylindrical).
  • the thickness of the adhesive body is also not particularly limited, and may be appropriately selected according to the intended use. It is above 30 mm, preferably 25 mm or less.
  • the present adhesive body can be suitably used in applications where substrates containing resin, carbon material, glass, metal, etc. have been used, and in particular, it can be suitably used in the medical field, electric equipment field, semiconductor field, etc. Specifically, it is suitably used as filters, various separators, clothing, and the like.
  • the adhesive body may contain one or more functional materials required for the application.
  • the functional materials include foodstuffs, drugs (medicine, agriculture, industry), dyes, adsorbents, deodorants, fragrances, insect repellents, electronic device materials, enzymes, and catalysts.
  • the adhesive body can be an adhesive body whose sustained release property or the like is controlled.
  • the adhesive layer is an adhesive layer obtained from the fluororubber composition.
  • the adhesive layer in the bonded body refers to a member that bonds between base materials, and is not necessarily limited to a layer (film), and includes a layer that exists only between fibers (a member that connects fibers). .
  • the thickness of the adhesive layer varies depending on the adhesive used when manufacturing the bonded body, it is usually 1 ⁇ m or more, preferably 3 ⁇ m or more, and usually 1 mm or less, preferably 200 ⁇ m or less.
  • the fluororubber composition which is a raw material for the adhesive layer, contains at least one fluororubber selected from fluoroelastomers (FKM) and perfluoroelastomers (FFKM), and has a Mooney viscosity of 80-115.
  • the fluororubber composition in the adhesive used in the present method described below preferably contains at least one fluororubber selected from fluoroelastomers (FKM) and perfluoroelastomers (FFKM).
  • the Mooney viscosity of the fluororubber composition is 80 or more, preferably 85 or more, more preferably 90 or more, and 115 or less, preferably 110 or less.
  • An adhesive layer or an adhesive obtained from a fluororubber composition having a Mooney viscosity within the above range can easily provide an adhered body in which substrates are adhered to each other with sufficient adhesive strength.
  • at least a portion of the fluororubber is plasticized by the carbon dioxide, resulting in an anchor effect or the like.
  • the fluorororubber composition having the Mooney viscosity within the above range has a high affinity with carbon dioxide, and is not plasticized by carbon dioxide. Therefore, it is considered that by using the composition, it is possible to easily obtain an adhered body in which the substrates are adhered to each other with sufficient adhesive strength.
  • the fluororubber composition having a Mooney viscosity within the above range is easy to spin, the shape of the obtained fluororubber fiber (nonwoven fabric) is difficult to change after spinning, and the fiber (average fiber diameter) has a desired shape (average fiber diameter) Non-woven fabric) can be easily formed.
  • the fluororubber (fluororubber composition) may be crosslinked, but the Mooney viscosity in this specification refers to the Mooney viscosity before the fluororubber (fluororubber composition) is crosslinked. Say things.
  • the fluororubber is at least one selected from fluoroelastomers (FKM) and perfluoroelastomers (FFKM). Among these, FKM is preferable because it is considered to be easily plasticized by carbon dioxide. In addition, FKM has excellent chemical resistance and heat resistance, as well as excellent resistance to stains, stains, oxidation, and ultraviolet rays.
  • the fluororubber contained in the fluororubber composition may be one type, or two or more types.
  • the fluororubber used in the fluororubber composition it is preferable to use a fluororubber such that the resulting fluororubber composition has a Mooney viscosity within the above range.
  • a fluororubber one or more fluororubbers having a Mooney viscosity within the above range may be used.
  • a fluororubber composition having a Mooney viscosity within the above range can be easily prepared, and When a fluororubber fiber or a fluororubber nonwoven fabric is used as an adhesive for producing a bonded body, it is easy to spin, and the shape of the obtained fluororubber fiber (nonwoven fabric) does not easily change after spinning, and the desired shape can be obtained.
  • (A2) is preferably included.
  • the weight-average molecular weight of the fluororubber measured by the gel permeation chromatography method is excellent in solubility in solvents when forming a liquid or paste fluororubber composition, and easily forms an adhesive layer with excellent mechanical strength. From the point of view of formation, it is preferably 1 ⁇ 10 3 or more, more preferably 1 ⁇ 10 4 or more, and preferably 5 ⁇ 10 7 or less, more preferably 1 ⁇ 10 7 or less.
  • the fluorine content in the fluorororubber is preferably 55% by mass or more, more preferably 62% by mass or more, particularly preferably 64% by mass or more, and preferably 80% by mass or less, more preferably 78% by mass or less. be.
  • the fluorine content can be measured/calculated by solid-state nuclear magnetic resonance (NMR), mass spectrometry (MS spectrum method), or the like.
  • the content of the fluororubber in the adhesive layer is preferably 20% by mass or more, more preferably 30% by mass or more, and particularly preferably 50% by mass or more, and the upper limit of the content is not particularly limited. When the layer does not contain fillers described below, it may be 100% by mass.
  • the content of the fluororubber contained in the fluororubber composition is, for example, 5% by mass or more, preferably 10% by mass or more, and is, for example, 100% by mass or less, preferably 80% by mass or less, more preferably 70% by mass. It is below. When the content of the fluororubber is within the above range, it is possible to easily obtain an adhesive layer in which the physical properties of the fluororubber, such as chemical resistance and heat resistance, are exhibited more effectively.
  • ⁇ FFKM FFKM is not particularly limited, but includes polymers that do not contain hydrogen atoms (carbon-hydrogen bonds) in the polymer main chain (excluding the terminal), specifically, tetrafluoroethylene (TFE) - perfluorovinyl ether system
  • TFE tetrafluoroethylene
  • Examples thereof include copolymers, and preferred are copolymers containing structural units derived from TFE, structural units derived from perfluorovinyl ether, and, if necessary, structural units derived from a monomer containing a crosslinking site.
  • perfluorovinyl ether examples include perfluoro(alkyl vinyl ether) and perfluoro(alkoxyalkyl vinyl ether).
  • perfluoro(alkyl vinyl ether) examples include compounds in which the number of carbon atoms in the alkyl group is, for example, 1 to 10. Specific examples include perfluoro(methyl vinyl ether), perfluoro(ethyl vinyl ether), perfluoro Fluoro(propyl vinyl ether) is mentioned, preferably perfluoro(methyl vinyl ether).
  • FFKM can be imparted with crosslinkability by including a structural unit derived from a monomer containing a crosslinkable site.
  • the cross-linking site means a site capable of cross-linking reaction, and includes, for example, a nitrile group, a halogen group (eg, I group, Br group), and a perfluorophenyl group.
  • cross-linking site monomers having a nitrile group as a cross-linking site include nitrile group-containing perfluorovinyl ethers.
  • cross-linking site-containing monomer having a halogen group as a cross-linking site examples include halogen group-containing perfluorovinyl ether. A substituted compound and the like can be mentioned.
  • the content of structural units derived from TFE is preferably 50.0 to 79.9 mol%
  • the content of structural units derived from perfluorovinyl ether is preferably 20.0 to 46.9 mol%
  • crosslinked The content of structural units derived from site-containing monomers is preferably 0.1 to 2.0 mol %.
  • FKM examples include fluoroelastomers other than the FFKM, and are not particularly limited, but specific examples include vinylidene fluoride-hexafluoropropylene-based polymer; vinylidene fluoride-hexafluoropropylene-tetrafluoroethylene-based polymer; Tetrafluoroethylene-propylene polymer; Vinylidene fluoride-propylene-tetrafluoroethylene polymer; Ethylene-tetrafluoroethylene-perfluoromethyl vinyl ether polymer; Vinylidene fluoride-tetrafluoroethylene-perfluoromethyl vinyl ether polymer and vinylidene fluoride-perfluoromethyl vinyl ether polymer.
  • the FKM may contain structural units derived from the crosslinkable site-containing monomer, as in the section for the FFKM.
  • the fluororubber composition may optionally contain conventionally known additives within a range that does not impair the effects of the present invention.
  • the additive include polymers other than the fluororubber (e.g., fluororesin), cross-linking agents, co-cross-linking agents, anti-aging agents, antioxidants, vulcanization accelerators, stabilizers, and silane coupling. agents, fillers (reinforcing agents), plasticizers, flame retardants, waxes, lubricants, solvents, surfactants, dispersants, charge control agents, viscosity control agents, and fiber forming agents. Only one kind of each of the additives may be used, or two or more kinds thereof may be used.
  • the content of the fluororubber with respect to the total 100% by mass of the fluororubber and the other polymer in the fluororubber composition is 50% by mass or more. be.
  • the cross-linking agent may be appropriately selected depending on the fluororubber to be used. For example, when FKM is used, peroxide-based cross-linking agents, polyamine-based cross-linking agents, and polyol-based cross-linking agents may be mentioned, and FFKM is used.
  • cross-linking agents include peroxide-based cross-linking agents, bisphenol-based cross-linking agents, triazine-based cross-linking agents, oxazole-based cross-linking agents, imidazole-based cross-linking agents, and thiazole-based cross-linking agents.
  • the amount of the cross-linking agent used is preferably 0.1 parts by mass or more, more preferably 0.5 parts by mass or more, and preferably 30 parts by mass or less, more preferably 100 parts by mass of the fluororubber. It is 10 parts by mass or less.
  • Peroxide cross-linking agents include, for example, 2,5-dimethyl-2,5-di(t-butylperoxy)hexane, dicumyl peroxide, 2,4-dichlorobenzoyl peroxide, di-t-butylperoxide, oxide, t-butyldicumyl peroxide, benzoyl peroxide, 2,5-dimethyl-2,5-(t-butylperoxy)hexyne-3, 2,5-dimethyl-2,5-di(benzoylperoxy ) hexane, ⁇ , ⁇ '-bis(t-butylperoxy-m-isopropyl)benzene, t-butylperoxyisopropyl carbonate, p-chlorobenzoyl peroxide.
  • co-crosslinking agent a conventionally known co-crosslinking agent (crosslinking aid) can be used.
  • co-crosslinking agent examples include triallyl isocyanurate, triallyl cyanurate, triallyl formal, triallyl trimellitate, N,N'-m-phenylenebismaleimide, dipropargyl terephthalate, diallyl phthalate, and tetraallyl.
  • examples include compounds (polyfunctional monomers) capable of co-crosslinking by radicals such as terephthalamide, and among these, triallyl isocyanurate is preferable from the viewpoint of reactivity and heat resistance of the resulting adhesive layer. .
  • the amount of the co-crosslinking agent used relative to 100 parts by mass of the fluororubber is preferably 0.1 parts by mass or more, more preferably 0.5 parts by mass or more, and preferably 30 parts by mass or less. Preferably, it is 10 parts by mass or less.
  • the filler examples include functional fillers (eg, thermally conductive particles, conductive particles, insulating particles, reinforcing fibers), and specifically, carbon materials (eg, carbon black, nanocarbon , carbon nanotubes, graphite), silica, alumina, zinc oxide, titanium dioxide, clay, talc, diatomaceous earth, barium sulfate, silicate compounds (silicates, etc.), calcium carbonate, magnesium carbonate, calcium oxide, mica, aluminum hydroxide , metal (eg, silver) particles, and resin fine particles.
  • the shape of the filler is not particularly limited, and examples thereof include particulate and fibrous.
  • the content of the filler in the fluororubber composition is such that the physical properties of the fluororubber such as chemical resistance and heat resistance are exhibited, and the physical properties of the filler is preferably 0.1% by mass or more, more preferably 1% by mass or more, and preferably 80% by mass or less, more preferably 70% by mass or less.
  • the solvent is not particularly limited as long as it can dissolve or disperse the fluororubber. Benzene, sulfolane, methanol, ethanol, phenol, pyridine, propylene carbonate, acetonitrile, trichloroethane, hexafluoroisopropanol, diethyl ether, and fluorine-based solvents.
  • the amount of the solvent used is, for example, 0% by mass or more, preferably 10% by mass or more, more preferably 20% by mass or more, preferably 90% by mass or less, more preferably 100% by mass of the fluororubber composition. It is 80% by mass or less.
  • the number of substrates may be one, or two or more.
  • Two or more substrates are preferably used for the adhesive body (II).
  • one substrate for example, both ends of the substrate are in contact (e.g., a sheet-like substrate is rolled so that both ends are in contact), and both ends of the one substrate in contact
  • a laminated body in which an adhesive 2 is placed on a long base material 1 is spirally formed into a bar or tubular member 4 as shown in FIG.
  • a ring-shaped or tube-shaped (cylindrical) bonded body can be obtained.
  • two or more substrates are used, two or more kinds of substrates having different materials, shapes, etc. may be used, or two or more substrates having the same materials, shapes, etc. may be used.
  • the substrate is not particularly limited, and examples thereof include substrates containing at least one selected from resins, carbon materials, glass and metals.
  • the base material is selected from nonwoven fabrics, woven fabrics, porous membranes and fibers from the viewpoint that a bonded body having a desired shape in which the base materials are bonded together with sufficient adhesive strength can be easily obtained. At least one is preferably used, and at least one selected from nonwoven fabrics, woven fabrics and porous membranes is more preferably used.
  • the resin examples include, but are not limited to, fluorine-based resins, engineering plastics, and other plastics. Among these, fluorine-based resins and engineering plastics are preferred.
  • the fluorine-based resin is not particularly limited, and conventionally known fluorine-based resins can be used.
  • the fluororubber contained in the fluororubber composition and the fluororesin constituting the base material may be the same or different, but are preferably different. More preferably, the crystallinity of the system resin is higher than the crystallinity of the fluororubber contained in the fluororubber composition.
  • fluorine resin examples include polytetrafluoroethylene (PTFE), tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA), tetrafluoroethylene-hexafluoropropylene copolymer (FEP), ethylene-tetra fluoroethylene copolymer (ETFE), tetrafluoroethylene-hexafluoropropylene-perfluoroalkyl vinyl ether copolymer (EPE), fluoroethylene-vinyl ether copolymer (FEVE), poly(chlorotrifluoroethylene) (PCTFE), Ethylene-chlorotrifluoroethylene-copolymer (ECTFE), polyvinylidene fluoride (PVDF), polyvinyl fluoride (PVF), vinylidene fluoride-hexafluoropropylene copolymer (VDF-HFP copolymer), vinylidene fluoride -hexafluoro
  • the engineering plastics are not particularly limited, and conventionally known engineering plastics can be used. Specific examples thereof include polyphenylene sulfide resins (PPS), polysulfone resins, polyethersulfone resins, and polyether ether ketone resins.
  • PPS polyphenylene sulfide resins
  • polysulfone resins polysulfone resins
  • polyethersulfone resins polyether ether ketone resins
  • PEEK polyarylate resin, liquid crystal polymer, aromatic polyester resin, polyimide resin, polyamideimide resin, polyetherimide resin, aramid resin, polycarbonate resin, polyacetal resin, polyethylene terephthalate (PET) , polyester resins such as polybutylene terephthalate (PBT) and polycyclohexylene dimethyl terephthalate (PCT), polyphenylene ether resins, polyphenylene oxide resins, nylon 6, nylon 66, polyamide resins such as aromatic polyamides, (meth) Acrylic polymer, vinyl chloride polymer, vinylidene chloride polymer, polybenzazole resin (e.g. polybenzimidazole (PBI)), polyethylene (e.g. ultra high molecular weight polyethylene), polypropylene (e.g. ultra high molecular weight polypropylene) and other olefin resins.
  • PBT polybutylene terephthalate
  • PCT polycyclohexylene dimethyl terephthalate
  • the other plastics are not particularly limited as long as they are resins other than fluorine-based resins and engineering plastics, and conventionally known plastics can be used. Specifically, for example, polyvinyl chloride (PVC), polystyrene (PS), acrylonitrile-butadiene-styrene resin (ABS), polymethyl methacrylate resin (PMMA), phenol resin (straight phenol resin, various modified phenol resins including), melamine resin, epoxy resin and other thermosetting resins.
  • PVC polyvinyl chloride
  • PS polystyrene
  • ABS acrylonitrile-butadiene-styrene resin
  • PMMA polymethyl methacrylate resin
  • phenol resin straight phenol resin, various modified phenol resins including
  • melamine resin epoxy resin and other thermosetting resins.
  • the base material containing the resin may contain fibers such as carbon fiber and glass fiber, and other components such as additives described in the adhesive layer section.
  • the shape of the substrate containing the resin examples include fibers, porous membranes (including stretched porous membranes), nonwoven fabrics, woven fabrics, and films.
  • the surface on the side in contact with the adhesive can be obtained from the viewpoint that a bonded body in which the base materials are bonded together with sufficient adhesive strength can be obtained. It is preferable to use a film roughened by a conventionally known method.
  • the base material to be bonded to the film is a base material through which carbon dioxide can pass, For example, fibers, porous membranes, non-woven fabrics or woven fabrics are preferred.
  • Examples of the substrate containing the carbon material include substrates containing carbon fibers, carbon nanotubes, and graphite sheets.
  • the shape of the substrate containing the carbon fiber is not particularly limited, and examples thereof include fiber, filament, cloth, felt, mat, paper, and prepreg.
  • Examples of the base material containing the glass include glass fiber, glass woven fabric, and glass non-woven fabric, and specific examples thereof include glass cloth, glass paper, glass mat, glass felt, and the resin on the surface thereof. A base material is mentioned.
  • Examples of the base material containing the metal include metal woven fabric, metal nonwoven fabric, and metal fiber (including wool-like metal).
  • Examples of the substrate containing the metal include substrates obtained by treating a support such as fibers, porous membranes, non-woven fabrics, and woven fabrics with a metal (e.g., substrates obtained by plating a support, and substrates obtained by may be deposited).
  • Examples of the metal include stainless steel, aluminum, aluminum alloys, nickel, nickel alloys, titanium, titanium alloys, copper, copper alloys, gold, gold alloys, silver, silver alloys, tantalum, tantalum alloys, chromium, chromium alloys, and molybdenum. , molybdenum alloys, tungsten, and tungsten alloys.
  • the base material has excellent mechanical strength, heat resistance, chemical resistance, weather resistance, and electrical insulation, and it is possible to easily obtain an adhesive body in which all the components constituting the adhesive body are fluorine components. Therefore, a substrate made of a fluororesin is preferable, and a substrate made of PTFE, PFA, or the like is more preferable. Fluorine components are non-adhesive and have a small coefficient of friction. However, according to one embodiment of the present invention, the substrates can be bonded to each other with sufficient adhesive strength even with such an adhesive made of a fluorine component. A bonded body having a desired shape can be easily obtained.
  • the nonwoven fabric, woven fabric, porous membrane, fiber (tube) and film (sheet) are not particularly limited, and conventionally known nonwoven fabric, woven fabric, porous membrane, fiber (tube) and film (sheet) can be used. can be done.
  • the base material may be a base material that has been subjected to functionalization treatment such as conventionally known surface treatment such as hydrophilic treatment. According to one embodiment of the present invention, even if a base material subjected to such a functionalization treatment is used, an adhesive body in which the function is not impaired can be obtained.
  • the average fiber diameter of the fibers constituting the nonwoven fabric or woven fabric and the fibers serving as the base material is preferably 0.01 ⁇ m or more, more preferably 0.1 ⁇ m or more, and still more preferably 0.5 ⁇ m or more. It is 100 ⁇ m or less, more preferably 50 ⁇ m or less, still more preferably 20 ⁇ m or less.
  • the average fiber diameter is within the above range, the mechanical strength is excellent, and a bonded body having a desired shape in which the substrates are bonded together with sufficient adhesive strength to prevent fraying of the fibers can be easily obtained.
  • the average fiber diameter in this specification is obtained by observing the fiber (group) to be measured with a scanning electron microscope (SEM) (magnification: for example, 2000 times), and randomly selecting 20 fibers from the obtained SEM image. , is an average value calculated based on the measurement results obtained by measuring the fiber diameter (major diameter) of each of these fibers.
  • SEM scanning electron microscope
  • the fiber diameter variation coefficient calculated by the following formula of the fibers constituting the nonwoven fabric or woven fabric and the fiber as the base material is preferably 0.7 or less, more preferably 0.01 to 0.5. .
  • the fiber diameter variation coefficient is within the above range, the fiber diameter is uniform, the mechanical strength is excellent, and the fiber fraying is prevented, and a bonded body having a desired shape in which the base materials are bonded with sufficient adhesive strength can be easily produced.
  • Fiber diameter variation coefficient standard deviation / average fiber diameter ("standard deviation" is the standard deviation of the fiber diameters of the 20 fibers.)
  • the fiber length of the fibers constituting the non-woven fabric or woven fabric and the fibers serving as the base material are not particularly limited, but are preferably 0.5 mm or more, more preferably 1 mm or more, and preferably 100 mm or less, more preferably 50 mm. It is below.
  • the stretched porous membrane is not particularly limited, and may be a uniaxially stretched porous membrane or a biaxially stretched porous membrane.
  • the porosity of the nonwoven fabric, woven fabric, or porous membrane is not particularly limited, but is, for example, 0.1% by volume or more, preferably 30% by volume or more, and for example, 95% by volume or less, preferably 90% by volume or less.
  • the nonwoven fabric, woven fabric or porous membrane preferably has a basis weight of 100 g/m 2 or less, more preferably 1 to 80 g/m 2 .
  • the thickness of the nonwoven fabric, woven fabric, porous membrane and film (sheet) is usually 5 ⁇ m or more, preferably 10 ⁇ m or more, and usually 1 mm or less, preferably 500 ⁇ m or less.
  • the nonwoven fabric, woven fabric, porous membrane, and film (sheet) may be composed of a single layer, or may be composed of two or more layers that are the same or different.
  • a method for manufacturing an adhesive body according to an embodiment of the present invention comprises: Step I of preparing a structure in which an adhesive is arranged between substrates; Step II of bonding the structure in the presence of liquid or gaseous carbon dioxide; including
  • the adhesive is an adhesive obtained from a fluororubber composition having a Mooney viscosity ML1+10 at 121° C. of 80 to 115 measured according to ASTM D 1646. According to the present method, the present bonded body can be produced.
  • step 1 of placing the structure obtained in step I into a pressure vessel;
  • Step 2 of introducing carbon dioxide into the pressure vessel having the structure obtained in Step 1.
  • the step 2 may be performed as a step substantially the same as the step II.
  • this method includes a step 4 of crimping (bonding by crimping) the base material.
  • the base material is preferably a base material made of a fluororesin, and in this case, the present method can also be said to be a novel processing method for a base material made of a fluororesin, which is difficult to process.
  • the bonded body can be produced in a short time at a low cost at a temperature of about 50° C. or less without applying high temperature heat to melt the resin constituting the base material. Since basically no carbon dioxide remains in the bonded body, it is excellent in safety, controllability and productivity, can easily obtain a clean bonded body, has excellent mechanical strength, and has sufficient bonding strength. It is possible to easily obtain an adherent having a desired shape in which base materials are adhered to each other. In particular, it is possible to obtain an adhesive body while maintaining the physical properties, shape, function, etc. of the base material.
  • the present method when manufacturing an adhesive body containing a functional material used according to the desired application, even if the functional material is poor in heat resistance, the function possessed by the functional material, it is possible to obtain an adhesive body that takes advantage of its properties.
  • the bonded body can be formed without pressing the substrates together, so that the bonded body can be obtained at low energy cost and in a simplified process.
  • the present method (I) by putting a plurality of the structures in the pressure vessel, it is possible to form a plurality of bonded bodies in a single process (step 2). It can be obtained at low energy costs and in a simplified process.
  • the carbon dioxide plasticizes the fluororubber in the adhesive, and by applying pressure in the plasticized state, the carbon dioxide becomes subcritical and further plasticizes. It is thought that this is because the shape of the substrates can be fixed in the meshed state, and the adhesion and bonding can be performed.
  • the adhesive used in this method is not particularly limited as long as it is an adhesive obtained from a fluororubber composition having a Mooney viscosity within the above range, and has the same composition as the fluororubber composition described in the section for the adhesive layer. preferably an object.
  • Specific examples of the adhesive include the liquid or paste fluororubber composition (the fluororubber composition itself is an adhesive), and the liquid or paste dried fluororubber composition (dry body itself). is an adhesive), fibers, nonwoven fabrics or films obtained from the fluororubber composition (fibers, nonwoven fabrics or films themselves are adhesives).
  • One type or two or more types of adhesives may be used in this method.
  • the liquid or paste fluororubber composition may contain a solvent capable of dispersing or dissolving the fluororubber.
  • the fluororubber composition may contain a solvent capable of dissolving the fluororubber. preferable.
  • the concentration of the fluororubber in the fluororubber composition containing the solvent is preferably 0.01% by mass or more, more preferably 0.5% by mass or more, and preferably 20% by mass or less, more preferably 10% by mass. It is below.
  • a bonded body can be obtained while maintaining the shape of the adhesive used and the base material. It is preferable to use a fiber or nonwoven fabric obtained from a rubber composition, and use a substrate selected from nonwoven fabrics, woven fabrics and porous membranes as the substrate. By using such an adhesive and a base material, it is possible to obtain a fully porous bonded body in which the entirety of the bonded body is porous.
  • the average fiber diameter of the fibers used as the adhesive or the fibers constituting the nonwoven fabric is preferably 0.1 ⁇ m or more, more preferably 0.5 ⁇ m or more, and preferably 5 ⁇ m or less, more preferably 3 ⁇ m or less.
  • the fiber length of the fiber as the adhesive or the fiber constituting the nonwoven fabric is not particularly limited, but is preferably 0.1 mm or more, more preferably 0.5 mm or more, still more preferably 1 mm or more, and preferably 1000 mm or less. It is preferably 100 mm or less, more preferably 50 mm or less.
  • the porosity of the nonwoven fabric as the adhesive is not particularly limited, it is, for example, 0.1% by volume or more, preferably 30% by volume or more, and for example, 95% by volume or less, preferably 90% by volume or less.
  • the nonwoven fabric used as the adhesive preferably has a basis weight of 100 g/m 2 or less, more preferably 1 to 80 g/m 2 .
  • the thickness of the non-woven fabric or film used as the adhesive may be appropriately selected, and is usually 1 ⁇ m or more, preferably 3 ⁇ m or more, and usually 1 mm or less, preferably 200 ⁇ m or less.
  • the nonwoven fabric used as the adhesive may be composed of a single layer or composed of two or more layers having different materials and fiber diameters.
  • the fiber or non-woven fabric as the adhesive is preferably produced by a method including step A of spinning the fluororubber composition.
  • Step A examples include an electrospinning method, a melt spinning method, a melt electrospinning method, and a spunbond method (melt blowing method).
  • the electrospinning method and the melt spinning method are preferable.
  • a fiber having a desired shape can be easily spun, a fiber having a small fiber diameter can be obtained, and a nonwoven fabric or the like obtained using the fiber tends to have a high porosity and a high specific surface area.
  • the electrospinning method is particularly preferred.
  • the process A is performed by an electrospinning method, the obtained fibers may be formed on a collector, and in this case, a nonwoven fabric is formed on the collector. Therefore, one aspect of Step A is also a method for producing a nonwoven fabric.
  • a step of forming fibers by an electrospinning method or the like and a step of accumulating the formed fibers into a sheet to form a nonwoven fabric are performed at the same time.
  • the formed fibers are used, and the wet papermaking method, water punch method, chemical bond method, thermal bond method, spunbond method, needle punch method, stitch bond method, etc.
  • a step of forming a nonwoven fabric by accumulating in a sheet form may be performed.
  • a fluororubber composition containing a solvent is preferably used when forming fibers or non-woven fabrics by electrospinning.
  • the fiber-forming agent is preferably an organic polymer having high solubility in a solvent.
  • Acrylamide, cellulose, polyvinyl alcohol is preferred.
  • the amount used depends on the viscosity of the solvent and the solubility in the solvent. and is, for example, 15% by mass or less, preferably 10% by mass or less.
  • Conditions for electrospinning include, for example, the following conditions.
  • the applied voltage (voltage applied between the spinning nozzle and the fiber collection collector) is preferably 1 kV or higher, more preferably 5 kV or higher, still more preferably 10 kV or higher, preferably 100 kV or lower, more preferably 50 kV or lower, and even more preferably. 40 kV or less.
  • the spinning distance (the distance between the spinning nozzle and the fiber collecting collector) is preferably 5-30 cm.
  • the discharge rate of the fluororubber composition is preferably 0.01 to 3 ml/min.
  • the tip diameter (outer diameter) of the spinning nozzle used for electrospinning is preferably 0.1 mm or more, more preferably 0.2 mm or more, and preferably 2.0 mm or less, more preferably 1.6 mm or less.
  • the spinning atmosphere does not have to be particularly controlled, but it is preferable that the relative humidity is, for example, 10 to 50% and the temperature is, for example, 10 to 35°C.
  • a rotating collector or a flat collector can be used as the fiber collection collector.
  • the fibers ejected from the spinning nozzle are wound around the drum by rotating the drum, and a nonwoven fabric in which the fibers are oriented in a certain direction can be obtained.
  • the rotation speed of the rotating collector is, for example, 50 to 5,000 revolutions/minute.
  • a non-woven fabric made of non-oriented fibers can be obtained by using a flat fiber collection collector.
  • Melt spinning can be carried out, for example, by melting the fluororubber composition with heat, extruding it from a spinneret (nozzle) to make it fibrous, and then cooling it.
  • a specific method of melt spinning is not particularly limited, and a known method can be used depending on the raw material to be used.
  • ⁇ Process B When manufacturing the fiber or nonwoven fabric as the adhesive, only the step A may be performed, but the fiber shape (porous shape, nonwoven shape) obtained in step A can be maintained for a long period of time, It is preferable to carry out the step B of cross-linking the fibers obtained in the step A from the viewpoint that fibers having improved tensile properties such as tensile strength and tensile modulus can be easily obtained.
  • a fiber or nonwoven fabric containing at least one selected from crosslinked FKM and crosslinked FFKM can be obtained.
  • the step B includes a step of irradiating the fiber or nonwoven fabric obtained in the step A with radiation (radiation cross-linking), and a step of heating the fiber or nonwoven fabric obtained in the step A (thermal cross-linking). ), etc.
  • the cross-linking treatment is possible in a short time, and the fiber shape (porous shape, non-woven fabric shape) obtained in the step A can be easily maintained.
  • Crosslinking is preferred.
  • the fibers obtained in step A may be fibers immediately after being extruded from the nozzle or the like, or may be fibers (non-woven fabric) after being accumulated on a collector or the like.
  • Examples of the radiation include X-rays, gamma rays, electron beams, proton beams, neutron beams, heavy particle beams, alpha rays, and beta rays. Among these, electron beams are preferred.
  • One type of radiation may be used alone, or two or more types may be used.
  • the method of radiation crosslinking may be performed by a conventionally known method, and the conditions for electron beam irradiation include, for example, the following conditions.
  • the electron beam can be irradiated so that the absorbed dose is preferably 5 kGy or more, more preferably 10 kGy or more, still more preferably 20 kGy or more, preferably 500 kGy or less, more preferably 300 kGy or less, and further preferably 150 kGy or less. desirable.
  • the absorption dose is such that, for example, when a fiber or nonwoven fabric adhesive is used as described above, a bonded body having an adhesive layer having a shape that maintains the shape of the fiber or nonwoven fabric can be easily obtained.
  • it is preferably 30 to 100 kGy, and it is possible to easily obtain a bonded body having an adhesive layer having a shape that maintains the shape of the fiber or nonwoven fabric, and to easily obtain a bonded body having excellent bonding strength. It is preferably 30 to 70 kGy from the viewpoint of being able to When irradiating with radiation, the cross-linking reaction is unlikely to be inhibited, and a fiber or nonwoven fabric having excellent mechanical properties can be easily obtained. is preferred.
  • the heating conditions for the thermal cross-linking may be set according to the composition of the fluororubber composition to be used.
  • the step I is not particularly limited as long as it is a step of preparing a structure in which an adhesive is arranged between substrates, and when forming this structure, depending on the desired use, One or more functional materials may be used. Examples of the functional material include materials similar to the functional materials described in the section of the adhesive body.
  • the method of disposing the adhesive between the substrates is not particularly limited, but for example, Adhesives such as fibers (including linear adhesives), woven fabrics and non-woven fabrics (including grid-like adhesives), films (including spherical, particle, and dot-like adhesives) are prepared from the fluororubber composition. and disposing the adhesive between substrates; Substrates are immersed in liquid or paste adhesives, or liquid or paste adhesives are applied onto substrates in desired shapes (e.g., film, line, dot, grid). , A method of arranging the adhesive between the substrates (before or after placing the adhesive between the substrates, the adhesive is dried if necessary). may be used); is mentioned.
  • Adhesives such as fibers (including linear adhesives), woven fabrics and non-woven fabrics (including grid-like adhesives), films (including spherical, particle, and dot-like adhesives) are prepared from the fluororubber composition. and disposing the adhesive between substrates; Substrates are immersed in liquid or paste adhesives
  • two or more base materials may be laminated via the adhesive, and both ends of one base material are in contact (eg, sheet The substrate may be rolled up so that both ends are in contact with each other), and the adhesive may be placed between both ends of the one substrate that is in contact, as shown in FIG.
  • a laminate in which the adhesive 2 is placed on the material 1 may be spirally wound around a rod or cylindrical member 4 as shown in FIG. 2 is bonded between the substrate surface of the substrate 1 on the adhesive 2 side in the laminate of FIG. 1 and the substrate surface on the side opposite to the adhesive 2 side of the laminate It is a laminated portion of base material/adhesive (adhesive layer)/base material arranged so that agent 2 comes.).
  • the base material and the adhesive may be wound around an auxiliary member such as a rod, if necessary.
  • the structure is formed by bonding one base material and the adhesive in the presence of liquid or gaseous carbon dioxide to form a preliminary body, and then the obtained preliminary body and the It may be a step of arranging the preform and a desired base material to be adhered to each other using the adhesive, if necessary, so that the adhesive is placed between the base materials.
  • the structure when used in the present method (I), the structure is temporarily fixed by a temporary fixing means so that the substrate and the adhesive are in contact with each other in order to maintain the state of the structure.
  • a temporary fixing means include clips, springs, tapes, staples, screws, nails, needles, rubber bands, binding bands, weights, and magnets.
  • the step 1 is not particularly limited as long as it is a step of putting the structure obtained in the step I into a pressure vessel.
  • the structure may be placed in a pressure vessel, and multiple structures may be placed in the pressure vessel.
  • the pressure vessel is not particularly limited as long as it can withstand the pressure of the carbon dioxide introduced in step 2.
  • the pressure vessel may have any size as long as it corresponds to the bonded body to be formed.
  • Examples of the pressure vessel include a vessel including a carbon dioxide inlet, a valve for adjusting the amount of carbon dioxide introduced, a carbon dioxide outlet, and a valve for controlling the discharge.
  • the step 2 is not particularly limited as long as it is a step of introducing carbon dioxide into the pressure vessel having the structure obtained in the step 1, and it is preferable to introduce liquid or gaseous carbon dioxide. Through this step 2, an adhesive body is formed.
  • the carbon dioxide to be introduced subcritical or supercritical carbon dioxide may be used. It is preferable not to use carbon dioxide in a critical or supercritical state.
  • Carbon is desirably introduced into the pressure vessel so that the pressure of carbon dioxide in the pressure vessel is preferably 3 MPa or higher, more preferably 4 MPa or higher, and still more preferably 5 MPa or higher.
  • step 2 it is preferable not to press by pressing means.
  • the surface pressure (pressure in the lamination direction of the base material) during bonding in step 2 may be appropriately selected according to the type of base material to be used, the amount of adhesive, the desired shape of the bonded body, etc., but is preferably It is 10 gf/cm 2 or more, more preferably 100 gf/cm 2 or more, preferably 1000 gf/cm 2 or less, more preferably 500 gf/cm 2 or less.
  • the surface pressure is within the above range, it is possible to easily form a bonded body in which the substrates are sufficiently bonded to each other without substantially damaging the shape of the substrates before bonding (e.g., the voids and fiber shapes of nonwoven fabrics, etc.). can be formed into
  • step 2 it is believed that the fluororubber in the adhesive can be melted due to the phenomenon of melting point depression caused by impregnation of the fluororubber with carbon dioxide, and the bonded body can be formed without heating. Therefore, in step 2, the function of the base material is not impaired, the degree of freedom in selecting the base material is high, and further, in the case of forming an adhesive body containing a functional material, even if the functional material is a material with poor heat resistance. , From the point of view of being able to make an adhesive body that takes advantage of the functions and properties of the functional material, the temperature is below the temperature at which the fluororubber melts, preferably at a temperature of about 50 ° C.
  • the temperature in step 2 is generally 0° C. or higher, preferably 20° C. or higher, and generally 40° C. or lower, preferably 30° C. or lower.
  • the time of step 2 may be appropriately selected according to the type and amount of the base material and adhesive used, but is preferably 0.2 seconds or longer, more preferably 1 second or longer. is 15 minutes or less, more preferably 5 minutes or less.
  • Step 3 If a temporary fixing means is used in step I, the temporary fixing means is usually removed after step 2 is performed.
  • the obtained bonded body is further subjected to secondary processing for bonding to another base material. be able to.
  • the step 4 is a step of crimping (bonding by crimping) the substrates as the step II, that is, the substrates in the structure obtained in the step I are bonded together in the presence of liquid or gaseous carbon dioxide. There is no particular limitation as long as it is a process of crimping under pressure.
  • the fluororubber can be rapidly plasticized, and an adhesive body having excellent adhesive strength can be easily obtained.
  • it is preferably carbon dioxide in a state close to liquid.
  • carbon dioxide in a subcritical or supercritical state may be used, but the pressing force can be reduced, and crimping can be performed without using a device having a heating mechanism. Therefore, it is preferred that no subcritical or supercritical carbon dioxide is present.
  • the fluororubber in the adhesive is impregnated with carbon dioxide, and the fluororubber can be plasticized. body can be manufactured. Therefore, in step 4, the function of the base material is not impaired, the degree of freedom in selecting the base material is high, and further, in the case of forming an adhesive body containing a functional material, even if the functional material is a material with poor heat resistance.
  • the temperature is below the temperature at which the fluororubber melts, preferably at a temperature of about 50 ° C.
  • the temperature during pressure bonding in step 4 is generally 0° C. or higher, preferably 20° C. or higher, and generally 40° C. or lower, preferably 30° C. or lower.
  • step 4 is preferably performed by introducing liquid or gaseous carbon dioxide into the system.
  • the order of introducing the structure and carbon dioxide into the system is not particularly limited.
  • the structure is introduced into a system filled with carbon dioxide. Although it may be introduced, it is preferable to introduce carbon dioxide into the system into which the structure has been introduced.
  • liquid carbon dioxide is introduced, the compression step for liquefaction can be omitted compared to the case where gaseous carbon dioxide is introduced, and therefore the bonded body can be produced in a short time.
  • gaseous carbon dioxide when gaseous carbon dioxide is introduced, the process is easier than when liquid carbon dioxide is introduced.
  • the introduced carbon dioxide may be pressurized to liquefy the carbon dioxide. In this case, it is not necessary to liquefy all of the introduced carbon dioxide, and at least a portion may be liquefied.
  • the amount of carbon dioxide to be introduced is not particularly limited. Carbon dioxide is introduced to a concentration of 0.4 g/mL (approximately half the density of liquid carbon dioxide) or more.
  • the pressure of carbon dioxide introduced into the system is It is desirable to introduce carbon dioxide to a pressure of preferably 3 MPa or higher, more preferably 4 MPa or higher, and even more preferably 5 MPa or higher.
  • the surface pressure during crimping in step 4 may be appropriately selected according to the type and amount of the base material to be used, the shape of the desired bonded body, etc., but is preferably 4 MPa or more, more preferably 5 MPa or more, and the upper limit is is not particularly limited, but is, for example, 50 MPa or less.
  • the surface pressure is the sum of the pressure of carbon dioxide introduced into the system and the press pressure (the pressure of carbon dioxide introduced into the system when the pressure is not pressed).
  • the crimping time in step 4 may be appropriately selected according to the type and amount of the base material and adhesive to be used, the surface pressure and temperature during crimping, and is preferably 0.2 seconds or more, more preferably 1 second. Seconds or more, preferably 15 minutes or less, more preferably 5 minutes or less.
  • Step 4 may be performed in a closed vessel capable of reducing the volume, or may be performed using an open press apparatus.
  • the sealed container is, for example, a member that has a part for introducing liquid or gaseous carbon dioxide into the sealed space and a part for discharging carbon dioxide, and that can press the base material by reducing the volume of the sealed container such as a piston.
  • the object to be processed can be spot-processed without using a large processing container that covers the entire substrate to be processed. or a method of pressing with a roller instead of a piston, the bonded body can be manufactured continuously.
  • the bonded body obtained after performing the step 4 and further another base material are pressure-bonded. Subsequent processing can also be performed.
  • FKM1 (Daiel G901H, manufactured by Daikin Industries, Ltd.) was measured according to ASTM D 1646 so that the total concentration of FKM was 20% by mass in methyl ethyl ketone (special grade, manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.). Mooney viscosity at 121°C (ML1+10): 135) 70 mass% and FKM2 (Dai-El G902, manufactured by Daikin Industries, Ltd., Mooney viscosity (ML1+10) at 121°C measured according to ASTM D 1646 (ML1+10): 21) 30 mass % was dissolved to prepare a fluororubber composition. The obtained fluororubber composition had a Mooney viscosity (ML1+10) of 96 at 121° C. measured according to ASTM D 1646.
  • fluororubber fibers are directly spun (uncrosslinked fluororubber nonwoven fabric) on a collector to which aluminum foil is attached under the following conditions. formed).
  • the obtained non-crosslinked fluororubber non-woven fabric was observed by SEM (S-3400N, manufactured by Hitachi High-Technologies Corporation, the same device was used for the following SEM), and the fibers constituting the non-woven fabric had a fiber shape. I confirmed that The thickness of the obtained crosslinked fluororubber nonwoven fabric was 20 ⁇ m, and the average fiber diameter of the fibers constituting the uncrosslinked fluororubber nonwoven fabric was about 1 ⁇ m.
  • An adhesive layer A was produced by peeling off the obtained non-crosslinked fluororubber nonwoven fabric from the aluminum foil.
  • the obtained crosslinked fluororubber nonwoven fabric was observed with an SEM image, and it was confirmed that the fibers constituting the nonwoven fabric had a fibrous shape.
  • the thickness of the obtained crosslinked fluororubber nonwoven fabric was 20 ⁇ m, and the average fiber diameter of the fibers constituting the crosslinked fluororubber nonwoven fabric was about 1 ⁇ m.
  • An adhesive layer B was produced by cutting the obtained crosslinked fluororubber nonwoven fabric into a 5 mm ⁇ 20 mm square.
  • a fluororubber composition was prepared in the same manner as in Preparation Example 1, except that the amount of FKM1 used was changed to 80% by mass and the amount of FKM2 used was changed to 20% by mass.
  • the obtained fluororubber composition had a Mooney viscosity (ML1+10) of 109 at 121° C. measured according to ASTM D 1646.
  • a crosslinked fluororubber nonwoven fabric was produced in the same manner as in Production Example 2, except that the obtained fluororubber composition was used.
  • a fluororubber composition was prepared in the same manner as in Preparation Example 1, except that the amount of FKM1 used was changed to 90% by mass and the amount of FKM2 used was changed to 10% by mass.
  • the obtained fluororubber composition had a Mooney viscosity (ML1+10) of 120 at 121° C. measured according to ASTM D 1646.
  • a crosslinked fluororubber nonwoven fabric was produced in the same manner as in Production Example 2, except that the obtained fluororubber composition was used.
  • An adhesive layer D was produced by cutting the obtained crosslinked fluororubber nonwoven fabric into a 5 mm ⁇ 20 mm square.
  • a fluororubber composition was prepared in the same manner as in Preparation Example 1, except that the amount of FKM1 used was changed to 50% by mass and the amount of FKM2 used was changed to 50% by mass.
  • the obtained fluororubber composition had a Mooney viscosity (ML1+10) of 69 at 121° C. measured according to ASTM D 1646.
  • a crosslinked fluororubber nonwoven fabric was produced in the same manner as in Production Example 2, except that the obtained fluororubber composition was used.
  • An adhesive layer E was produced by cutting the obtained crosslinked fluororubber nonwoven fabric into a 5 mm ⁇ 20 mm square.
  • a fluororubber nonwoven fabric was produced in the same manner as in Production Example 1, except that the amount of FKM1 used was changed to 60% by mass and the amount of FKM2 used was changed to 40% by mass.
  • the obtained fluororubber composition had a Mooney viscosity (ML1+10) of 86 at 121° C. measured according to ASTM D 1646.
  • An adhesive layer F was produced by cutting the obtained fluororubber nonwoven fabric into a 5 mm ⁇ 20 mm square.
  • Adhesive layer A prepared in Production Example 1 (5 mm ⁇ adhesive layer A 20 mm square) was temporarily fixed with a clip at the overlapping portion of the three laminates.
  • the temporarily fixed laminate was placed in a pressure vessel having a pressure gauge, a carbon dioxide inlet and a carbon dioxide outlet, and then gaseous carbon dioxide was slowly introduced into the pressure vessel over 1 minute (final After the pressure in the pressure vessel: 5 MPa), carbon dioxide was immediately discharged, and the clip was removed to produce an adhesive body.
  • two nonwoven fabrics made of hydrophilically treated PTFE nanofibers were adhered with sufficient strength.
  • Example 2 In Example 1, instead of two nonwoven fabrics made of PTFE nanofibers hydrophilically treated with PVA, one nonwoven fabric made of PTFE nanofibers hydrophilically treated with PVA and PTFE nanofibers not hydrophilically treated A bonded body was produced in the same manner as in Example 1, except that one sheet of nonwoven fabric (manufactured by ZEUS Industrial Products, Inc., basis weight: 40 g/m 2 , 30 mm square) was used. In the resulting adhesive body, the non-woven fabric made of hydrophilically treated PTFE nanofibers and the non-woven fabric made of non-hydrophilically treated PTFE nanofibers adhered with sufficient strength.
  • one sheet of nonwoven fabric manufactured by ZEUS Industrial Products, Inc., basis weight: 40 g/m 2 , 30 mm square
  • Example 3 In Example 1, instead of the two nonwoven fabrics made of PTFE nanofibers that were hydrophilically treated with PVA, nonwoven fabrics made of PTFE nanofibers that were not hydrophilically treated (manufactured by ZEUS Industrial Products, Inc., basis weight: 40 g/m 2 , A bonded body was produced in the same manner as in Example 1, except that two sheets of 30 mm square) were used. In the resulting adhesive body, two non-woven fabrics composed of PTFE nanofibers that were not hydrophilically treated were adhered with sufficient strength.
  • Example 4 The adhesive layer A (adhesion A layer A cut into 10 mm ⁇ 10 mm squares) was placed on the SUS plate. Next, a magnet was placed on the portion where the three non-woven fabrics made of PTFE nanofibers were not in contact with the SUS plate, and the laminate was temporarily fixed by magnetic force. The temporarily fixed laminate was put in a pressure vessel having a pressure gauge, a carbon dioxide introduction part and a carbon dioxide discharge part together with the SUS plate, and then gaseous carbon dioxide was slowly put into the pressure vessel over 1 minute ( After the final pressure in the pressure vessel: 5 MPa), carbon dioxide was immediately discharged, and the SUS plate and the magnet were removed to produce an adhesive body. In the resulting adhesive body, two nonwoven fabrics made of hydrophilically treated PTFE nanofibers were adhered with sufficient strength.
  • Adhesive layer A prepared in Preparation Example 1 (adhesive layer A was cut into 25 mm ⁇ 10 mm squares), so that the stacking direction is parallel to gravity. . After that, a weight having an outer diameter of ⁇ 19.5 mm and a weight of 94.7 g was placed on the overlapping portion of the three laminates. Next, gaseous carbon dioxide was slowly introduced into the pressure vessel over a period of 1 minute (final pressure in the pressure vessel: 5 MPa), and then the carbon dioxide was immediately discharged, and the weight was removed to obtain an adhesive body. was made. In the resulting adhesive body, two nonwoven fabrics made of hydrophilically treated PTFE nanofibers were adhered with sufficient strength.
  • Example 6 The adhesive layer A (adhesion Layer A cut into 10 mm ⁇ 10 mm squares) was placed. Next, the 10 mm square portion of the non-woven fabric made of PTFE nanofibers on the side opposite to the side on which the adhesive layer A is arranged is rolled so that it overlaps with the adhesive layer A, and the portion where the three pieces overlap is attached to a jig (precision compression spring (manufactured by Samini Co., Ltd.), free length: 10 mm, spring constant: a fixing jig with a built-in spring of 0.209 N / mm) is temporarily fixed in a state of being tightened until the spring length becomes 5 mm. , to form a ring-shaped laminate.
  • a jig precision compression spring (manufactured by Samini Co., Ltd.), free length: 10 mm, spring constant: a fixing jig with a built-in spring of 0.209 N / mm
  • a bonded body was produced in the same manner as in Example 1, except that the formed ring-shaped laminate was placed in a pressure vessel having a pressure gauge, a carbon dioxide inlet and a carbon dioxide outlet.
  • the resulting adhesive body was a ring-shaped adhesive body in which both ends of a sheet of nonwoven fabric made of hydrophilically treated PTFE nanofibers were bonded with sufficient strength.
  • Example 7 An adhesive body was produced in the same manner as in Example 1, except that the adhesive layer B produced in Production Example 2 was used instead of the adhesive layer A in Example 1. In the resulting adhesive body, two nonwoven fabrics made of hydrophilically treated PTFE nanofibers were adhered with sufficient strength.
  • Example 8 An adhesive body was produced in the same manner as in Example 1, except that the adhesive layer F produced in Production Example 6 was used instead of the adhesive layer A. In the resulting adhesive body, two nonwoven fabrics made of hydrophilically treated PTFE nanofibers were adhered with sufficient strength.
  • Example 9 The adhesive layer A prepared in Preparation Example 1 (adhesive layer A of 300 mm
  • the laminate with the adhesive 2) in FIG. 1 is placed in a ⁇ 6 mm SUS tube (cylindrical member) so that the length of the laminated portion 3 in FIG. 2 is 5 mm. , was spirally wound as shown in FIG.
  • a SUS tube with a spirally wound laminate is placed in a pressure vessel having a pressure gauge, a carbon dioxide inlet and a carbon dioxide outlet, and then gaseous carbon dioxide is slowly introduced into the pressure vessel for 1 minute. Immediately after the pressure inside the pressure vessel was 5 MPa, carbon dioxide was immediately discharged, and the SUS tube was pulled out to produce an adhesive body.
  • the obtained bonded body was tubular (cylindrical), and the nonwoven fabric made of PTFE nanofibers was bonded with sufficient strength at the bonding portion (substrate/adhesive layer/substrate laminated portion 3 in FIG. 2).
  • the average peel strength in Table 1 below is the measured value of the peel strength of the laminated portion 3 of base material/adhesive (adhesive layer)/base material in FIG.
  • Example 7 An attempt was made to produce an adhesive body in the same manner as in Example 7, except that carbon dioxide was not introduced.
  • the two non-woven fabrics made of hydrophilically treated PTFE nanofibers did not adhere. In other words, a desired bonded body could not be produced.
  • ⁇ Peel strength test> As the mechanical properties of the resulting bonded body, a universal tensile tester (EZ-test, manufactured by Shimadzu Corporation) was used to tear the bonded body in the bonding direction at a rate of 1 mm / s (perpendicular to the bonding surface The average peel strength (N/10 mm) of the adhesive was measured at a displacement of 5 to 10 mm (5 to 10 seconds after tearing) when a tensile load was applied to the adhesive.
  • EZ-test manufactured by Shimadzu Corporation
  • Example 10 After forming an uncrosslinked fluororubber nonwoven fabric in the same manner as in Production Example 1, the uncrosslinked fluororubber nonwoven fabric was exposed to an electron beam (EB) using an EB apparatus (manufactured by Iwasaki Electric Co., Ltd., CB250/30/20mA). After irradiation, the obtained crosslinked fluororubber nonwoven fabric was peeled off from the aluminum foil and cut into 5 mm x 20 mm squares to prepare adhesive layers. During this irradiation, the electron beam was irradiated at room temperature (21° C.) under N 2 so that the absorbed dose was 30, 40, 50, 60, 70, 80 or 100 kGy.
  • EB electron beam
  • An adhesive layer was placed between two nonwoven fabrics made of PTFE nanofibers (manufactured by ZEUS Industrial Products, Inc., basis weight: 24 g/m 2 ). lightly pressed by hand. The pressed laminate was placed in a pressure vessel with a pressure gauge, carbon dioxide inlet and carbon dioxide outlet, and the pressure vessel was then slowly charged with gaseous carbon dioxide over 1 minute (final pressure After the pressure in the container: 6 MPa), carbon dioxide was immediately discharged to produce an adhesive body. Using the produced adhesive body, the average peel strength was measured in the same manner as described above. Table 2 shows the results.
  • Example 11 A base material was produced by punching two sheets of nonwoven fabric (manufactured by ZEUS Industrial Products, Inc., basis weight: 24 g/m 2 ) made of PTFE nanofibers with an average fiber diameter of 900 nm into a circular shape of ⁇ 19. Further, an adhesive was produced by punching the crosslinked fluororubber nonwoven fabric produced in Production Example 2 into a ⁇ 19 circle.
  • a piston a sealable container having a carbon dioxide introduction part and a carbon dioxide discharge part (diameter: ⁇ 20 mm, container described in JP 2018-099885 A), the obtained base material, the obtained adhesive, the obtained Put the laminated body so that the base materials are in this order, introduce carbon dioxide equivalent to the vapor pressure of carbon dioxide (cylinder pressure: 6 MPa) at room temperature (25 ° C.), and lower the piston.
  • cylinder pressure 6 MPa
  • the two substrates were crimped with an adhesive (crosslinked fluororubber nonwoven fabric).
  • Example 12 A bonded body (crimped body) was produced in the same manner as in Example 11, except that the crosslinked fluororubber nonwoven fabric produced in Production Example 3 was used in place of the crosslinked fluororubber nonwoven fabric produced in Production Example 2. did. The average peel strength was measured in the same manner as described above using the resulting bonded body (press bonded body). Table 3 shows the results.
  • Example 11 a bonded body (press-bonded body) was produced in the same manner as in Example 11, except that carbon dioxide was not introduced. In the resulting adhered body (press-bonded body), the substrate and the adhesive (crosslinked fluororubber nonwoven fabric) did not adhere. In other words, a desired bonded body (press-bonded body) could not be produced.
  • a bonded body (crimped body) was produced in the same manner as in Example 11, except that the crosslinked fluororubber nonwoven fabric produced in Production Example 4 was used in place of the crosslinked fluororubber nonwoven fabric produced in Production Example 2. did.
  • the resulting bonded body (press-bonded body) has insufficient adhesion between the base material and the adhesive (crosslinked fluororubber nonwoven fabric) (average peel strength: less than 0.3 N/10 mm), and the base material and the adhesive are peeled off. have done. In other words, a desired bonded body (press-bonded body) could not be produced.
  • a bonded body (crimped body) was produced in the same manner as in Example 11, except that the crosslinked fluororubber nonwoven fabric produced in Production Example 5 was used in place of the crosslinked fluororubber nonwoven fabric produced in Production Example 2. did.
  • the resulting bonded body (press-bonded body) has insufficient adhesion between the base material and the adhesive (crosslinked fluororubber nonwoven fabric) (average peel strength: less than 0.3 N/10 mm), and the base material and the adhesive are peeled off. have done. In other words, a desired bonded body (press-bonded body) could not be produced.
  • base material 2 adhesive 3: base material/adhesive (adhesive layer)/laminated part of base material 4: bar or cylindrical member

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Mechanical Engineering (AREA)
  • Laminated Bodies (AREA)
  • Adhesives Or Adhesive Processes (AREA)
PCT/JP2022/014626 2021-03-31 2022-03-25 接着体および接着体の製造方法 Ceased WO2022210413A1 (ja)

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US18/283,265 US12565601B2 (en) 2021-03-31 2022-03-25 Bonded object, and method for manufacturing bonded object
KR1020237030727A KR20230163371A (ko) 2021-03-31 2022-03-25 접착체 및 접착체의 제조 방법

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5959909A (ja) * 1982-09-29 1984-04-05 Daikin Ind Ltd ゴム弾性フイラメント
JPH01108246A (ja) * 1987-10-21 1989-04-25 Asahi Chem Ind Co Ltd 加硫接着用フツ素ゴム組成物
JP2018099885A (ja) * 2016-12-20 2018-06-28 国立研究開発法人産業技術総合研究所 二酸化炭素による樹脂の接着方法、その接着物及び樹脂の接着装置
WO2021020147A1 (ja) * 2019-08-01 2021-02-04 株式会社バルカー 圧着体およびその製造方法

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002283517A (ja) 2001-03-27 2002-10-03 Daikin Ind Ltd フッ素樹脂積層シート
JP5607442B2 (ja) * 2010-07-09 2014-10-15 スリーエム イノベイティブ プロパティズ カンパニー フルオロポリマー系粘接着性組成物
JP2022540646A (ja) * 2019-07-17 2022-09-16 ソルベイ スペシャルティ ポリマーズ イタリー エス．ピー．エー． ポリアミドとフルオロエラストマーとを含む複合材料

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5959909A (ja) * 1982-09-29 1984-04-05 Daikin Ind Ltd ゴム弾性フイラメント
JPH01108246A (ja) * 1987-10-21 1989-04-25 Asahi Chem Ind Co Ltd 加硫接着用フツ素ゴム組成物
JP2018099885A (ja) * 2016-12-20 2018-06-28 国立研究開発法人産業技術総合研究所 二酸化炭素による樹脂の接着方法、その接着物及び樹脂の接着装置
WO2021020147A1 (ja) * 2019-08-01 2021-02-04 株式会社バルカー 圧着体およびその製造方法

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