WO2002026870A1 - Process for producing sheet-form sealing material - Google Patents

Process for producing sheet-form sealing material Download PDF

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Publication number
WO2002026870A1
WO2002026870A1 PCT/JP2001/006542 JP0106542W WO0226870A1 WO 2002026870 A1 WO2002026870 A1 WO 2002026870A1 JP 0106542 W JP0106542 W JP 0106542W WO 0226870 A1 WO0226870 A1 WO 0226870A1
Authority
WO
WIPO (PCT)
Prior art keywords
nonwoven fabric
sheet
binder
sealing material
rubber
Prior art date
Application number
PCT/JP2001/006542
Other languages
French (fr)
Japanese (ja)
Inventor
Takahito Nishida
Kenji Horii
Minoru Asahina
Tsuneshi Sano
Kiyohito Takata
Shinya Kurokawa
Original Assignee
Nippon Valqua Industries, Ltd.
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nippon Valqua Industries, Ltd. filed Critical Nippon Valqua Industries, Ltd.
Priority to AU2001276697A priority Critical patent/AU2001276697A1/en
Publication of WO2002026870A1 publication Critical patent/WO2002026870A1/en

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B15/00Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
    • B29B15/08Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
    • B29B15/10Coating or impregnating independently of the moulding or shaping step
    • B29B15/12Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B15/00Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
    • B29B15/08Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
    • B29B15/10Coating or impregnating independently of the moulding or shaping step
    • B29B15/12Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length
    • B29B15/122Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length with a matrix in liquid form, e.g. as melt, solution or latex
    • B29B15/125Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length with a matrix in liquid form, e.g. as melt, solution or latex by dipping
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B15/00Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
    • B29B15/08Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
    • B29B15/10Coating or impregnating independently of the moulding or shaping step
    • B29B15/12Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length
    • B29B15/122Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length with a matrix in liquid form, e.g. as melt, solution or latex
    • B29B15/127Coating or impregnating independently of the moulding or shaping step of reinforcements of indefinite length with a matrix in liquid form, e.g. as melt, solution or latex by spraying
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/10Materials in mouldable or extrudable form for sealing or packing joints or covers
    • C09K3/1025Materials in mouldable or extrudable form for sealing or packing joints or covers characterised by non-chemical features of one or more of its constituents
    • C09K3/1028Fibres
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/58Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
    • D04H1/587Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives characterised by the bonding agents used
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/58Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
    • D04H1/64Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives the bonding agent being applied in wet state, e.g. chemical agents in dispersions or solutions
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/693Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural or synthetic rubber, or derivatives thereof

Definitions

  • the present invention relates to a method for producing a sheet-like seal material, and more particularly, to a method for producing a sheet-like seal material, in which strength anisotropy is suppressed and gas sealability is improved.
  • the present invention relates to a method for producing a sheet-like sealing material excellent in quality.
  • gaskets are used for general industry, but the most versatile ones are mainly fibers and fillers and rubbers or rubbers. Examples include a jump sheet or a beater sheet composed of a resin and a resin.
  • the joint sheet is made of non-fiber such as stone or glass fiber, or aromatic polyamid fiber, or fibrillated aromatic poly.
  • Organic fibers such as amide fibers are used as base fibers, and rubber, resin, vulcanizing agents and other rubber chemicals as fillers and fillers are added and mixed.
  • a composition for forming an int sheet is prepared, and the composition is inserted between a pair of rolls composed of a heating roll and a cooling roll, and heated and rolled to form a joint sheet.
  • the composition is obtained by laminating the composition on the hot roll side and then peeling off the sheet-like material laminated on the hot roll.
  • a filler and rubber or resin are added to asbestos fiber or non-asbestos fiber in a beater, and these are stirred and uniformly dispersed in water. It is obtained by making paper with a paper machine.
  • the first problem with joint sheets is that the fibers that can be used in the manufacturing process are limited.
  • the wettability between the raw material, fiber, and rubber or resin is important, and if the wettability is poor, the sheet is formed at the time of sheet molding. Wrinkles and breaks occur.
  • Asbestos joint sheets are excellent products that can maintain excellent properties over a long period of time at high temperatures, can be used for various fluids at various temperatures, and have high versatility.
  • the use of asbestos fiber itself is restricted for safety and health reasons, and asbestos joint sheets are being replaced by other gaskets.
  • non-asbestos joint sheets can be used for a long time in actual equipment at high temperatures compared to asbestos joint sheets. Poor properties (also referred to as "long-term health") that maintain excellent properties such as strength, tensile strength, and elongation at break. This means that non-asbestos sheets are liable to harden due to the history of high-temperature air, and consequently are liable to break when used at high temperatures for a long period of time on actual equipment. I do.
  • the strength of the entire sheet is significantly increased by setting a high proportion of asbestos fibers, thereby increasing the strength of the asbestos fiber. It complements the strength 'anisotropy.
  • the fiber blending ratio cannot be set high, and the fiber anisotropy described above cannot be complemented by the fiber blended. For this reason, when stress is generated inside the gasket due to the hardening of the rubber during use of the actual machine at high temperature for a long period of time, the stress concentrates in the weaker direction or in the weaker portion, resulting in a lower result. It is presumed that cracking of the gasket is induced.
  • beater sheets have a problem in terms of airtightness.
  • beater sheets are used for liquid seals such as lubricating oil and fuel oil, and specifically for oil pumps and fuel pumps. .
  • it is not used for gaskets that require strict airtightness, such as gaseous fluids.
  • the gasket obtained by the beater sheet manufacturing method currently on the market conforms to “ASTMF 37 — B” and has a gasket surface pressure of 19.6 MPa and a nitrogen internal pressure of 0. 9 to 8 MPa Set, this filtrate and was measured fluid leakage amount of gas Ke Tsu DOO outer diameter or al, 6 3 1 0 -? 2 &'showed 111 3/3 (see Table 1). It is considered that the reason for the large amount of gas leakage is that some of the voids included in the sheet during the papermaking process are not removed during the manufacturing process but remain. Under actual conditions of use, the existence of leakage of gaseous fluid from the gasket is generally determined by the lithographic water foaming method.
  • the detection sensitivity of this water-foaming method is about 2 ⁇ 10 ” 4 Pa ⁇ m 3 Zs.
  • the beater sheet is generally used for detection of this water-foaming method.
  • the sealing performance of the beater sheet is low because it exhibits a leakage amount of 18 to 55 times the sensitivity, making it unsuitable as a sealing material for gaseous fluids. Therefore, a sealing performance that shows a leakage amount of 2 X 10 — 4 Pa ⁇ m 3 Z s or less is required.
  • Rubber material as an organic binder, rubber chemicals, and the above A binder mixture obtained by mixing a solvent or dispersion medium for rubber material or mixing a resin as an organic binder with the solvent or dispersion medium for resin. Is impregnated with (forcibly) expelling gas present in the nonwoven fabric into the nonwoven fabric made of the base fiber, and at least a part of the nonwoven fabric impregnated with the mixed solution is impregnated. The solvent or dispersion medium is volatilized and removed, and then the nonwoven fabric is heated and compressed to vulcanize the rubber material or to cure the resin to produce a sheet-like sealing material.
  • the present inventors have found that anisotropy is suppressed and that a sheet-like sealing material excellent in gas sealing properties and the like can be obtained, and the like, and the present invention has been completed.
  • JP-A-57-116709 describes that one or two or more nonwoven fabrics composed of hydrophobic short fibers such as tetron or nylon are laminated.
  • a packing for food machinery and the like which is formed by using a base material as a base material and impregnating the base material with a binder such as resin and rubber.
  • the packing for food machinery and appliances is formed by impregnating a base material with a binder such as resin or rubber and drying the base material as described above. It states that it is manufactured.
  • this patch is excellent in sealability and sanitary.
  • the impregnation step included in the publication is resin impregnation for the purpose of preventing fiber scattering and packing corrosion, it can be obtained by the method described in the publication.
  • packing, gas, gas, etc. are used as packing materials that severely restrict leakage. Inadequate sealing performance for liquids.
  • Japanese Patent Publication No. 8_30686 states that colloid particles of silicone resin or colloid particles of polytetrafluoroethylene resin and water
  • a water-dispersed emulsion without flammability and harmfulness due to volatilization is created, and a cotton-like body mainly composed of glass fiber is produced.
  • the moisture of the emulsion impregnated into the needle mat is evaporated.
  • a silicone resin or polytetrafluoroethylene resin and an acrylic-based primer are adhered to the entire inside of the needle mat, and the surface of the needle mat is adhered to the needle mat.
  • Paste release paper with acrylic adhesive Method for manufacturing a device for path tree rk material that have the indicated open.
  • the publication discloses that an emulsion of a water dispersion system is stored in an immersion tank, and the needle mat is continuously fed by a roller feeding device to the emulsion while being continuously fed thereto. It describes that the immersion is carried out for about 0 to 100 seconds so that the entire interior of the needle mat is impregnated with the emulsion.
  • the use of the above-mentioned water-dispersed emulsion makes it possible for the first time to impregnate the entire interior of the needle mat with the emulsion, thereby constituting the needle mat. Silicon resin or the surface of all glass fibers
  • the present invention is intended to solve the problems associated with the prior art as described above, and there is no limitation on the type of fiber to be blended, and the fiber can be used for a long time under a high temperature condition. It is intended to provide a method of manufacturing a sheet-like sealing material that can be used as a substitute for a point sheet and is suitably used for gas and liquid sealing. .
  • a first method for producing a sheet-like sealing material according to the present invention comprises: mixing a rubber material as an organic binder, a rubber chemical, and the rubber material solvent or dispersion medium;
  • the obtained binder mixed solution is impregnated into a nonwoven fabric made of a base fiber while expelling gas present inside the nonwoven fabric,
  • At least a part of the solvent or dispersion medium is volatilized and removed from the nonwoven fabric impregnated with the above mixed solution,
  • the nonwoven fabric is heated and compressed, and the rubber material is vulcanized to obtain a sheet-like sealing material.
  • the mixed solution of the binder is used in the form of a latex.
  • a resin as an organic binder is mixed with the resin solvent or the dispersion medium,
  • the obtained binder mixed solution is applied to a non-woven fabric made of the base fiber and the inside of the non-woven fabric.
  • At least a part of the solvent or dispersion medium is volatilized and removed from the non-woven fabric impregnated with the above mixed solution,
  • the nonwoven fabric is heated and compressed, and the resin is cured to obtain a sheet-like sealing material.
  • the base fiber is a non-asbestos fiber.
  • the nonwoven fabric is in a felt shape.
  • the binder-mixture liquid contains a filler.
  • the step of purging gas present inside the nonwoven fabric and impregnating with the binder mixed solution is performed by previously compressing the nonwoven fabric and then mixing the binder one mixed solution. Immersed in a non-woven fabric It is preferred to do this by compressing and then spontaneously restoring this in a binder mixture.
  • the step of driving out the gas present inside the nonwoven fabric and impregnating with the binder mixed solution is performed by spraying the binder mixed solution onto the nonwoven fabric under high pressure. It is preferable to do it.
  • the step of driving out the gas present inside the nonwoven fabric and impregnating the mixture with the binder is performed by placing the nonwoven fabric in a reduced-pressure container and reducing the pressure inside the container. It is preferable to do this by injecting a mixture of the nozzles.
  • FIG. 1 shows successive steps of nonwoven cloth compression, one-binder mixed liquid impregnation-nonwoven cloth, spontaneous restoration, and setting of adhesion amount, which are preferably used in one embodiment of the present invention.
  • FIG. 3 is a schematic explanatory view of a roll-conveying type impregnating machine that can perform this.
  • FIG. 2 shows the impregnation of a nonwoven fabric, a binder and a mixture in a binder mixture, which is preferably used in one embodiment of the present invention.
  • FIG. 4 is a schematic explanatory view of a belt transport type impregnating machine capable of continuously performing each operation of spontaneous non-woven fabric spontaneous restoration and adhesion amount setting.
  • FIG. 3 is a schematic explanatory view of a high-pressure spray impregnating machine preferably used in one embodiment of the present invention.
  • FIG. 4 is a diagram showing an embodiment in which a suction device is provided below the mesh base in the high-pressure spray impregnator shown in FIG.
  • a rubber material as an organic binder, a rubber chemical, and the rubber material solvent or dispersion medium are mixed.
  • the obtained binder mixed solution is impregnated into a nonwoven fabric made of a base fiber while expelling gas present inside the nonwoven fabric,
  • At least a part of the solvent or dispersion medium is volatilized and removed from the nonwoven fabric impregnated with the above mixed solution,
  • the nonwoven fabric is heated and compressed, and the rubber material is vulcanized to produce a sheet-like sealing material.
  • the resin as an organic binder is used as the binder mixture in the first production method;
  • the method is basically the same as the above-mentioned first production method, except that a mixed solvent and a dispersion medium are used, and the obtained binder mixture is used. That is, in the method for producing a sheet-like sealing material of the present invention, unlike the calendar roll production method which is a conventional method for producing a joint sheet, a nonwoven fabric is used as the base fiber. When impregnating the non-woven fabric with the binder mixture, the gas in the non-woven fabric is forcibly driven out, and the non-woven fabric filled with the non-woven fabric contains gas. It is unique in that it does not exist.
  • the above-mentioned organic mixture may be a rubber material or a resin, and may contain both of them. However, these organic binders contribute to improving the sealing performance of the sheet-like sealing material.
  • the binder mixture When the organic binder is a rubber material, the binder mixture contains a rubber chemical, a solvent or a dispersion medium for the rubber material in addition to the rubber material, and is further filled as necessary. Agents may be included. Also, when this organic binder is resin, In addition, the binder mixture contains a resin solvent or a dispersion medium in addition to the resin, and may further contain a filler if necessary.
  • Examples of the rubber material include natural rubber, isoprene rubber, butadiene rubber, styrene butadiene rubber, urethane rubber, chloroprene rubber, acrylonitrile butadiene rubber, butyl rubber, and ethylene rubber.
  • Examples include pyrene rubber, acryl rubber, silicone rubber, and fluorine rubber.
  • the resin examples include a urea-based resin, a melamine-based resin, a polyester-based resin, an epoxy-based resin, and a phenol-based resin.
  • one kind of the binder is not particularly limited, and one kind or a combination of two or more kinds may be used.
  • rubber chemicals conventionally known rubber chemicals can be widely used, for example, vulcanizing agents, vulcanizing aids, accelerators, anti-aging agents, and the like.
  • Agents, heat-sensitive gelling agents (thermosensitive agents), surfactants, etc. may be used.
  • thickener examples include synthetic alcohols such as polyvinyl alcohol, polyacrylic acid, polymethacrylic acid, and polyacrylamide. Molecules and their alginates; natural and semi-synthetic polymers such as casein, gelatin, and guar gum; and the like.
  • thermosensitive agent examples include, in addition to polyvinyl methyl ether, silicones, polyalkylene oxyside derivatives, and the like.
  • surfactant a wide variety of known surfactants such as anionic, nonionic, cationic and amphoteric can be used.For example, carbonates, sulfonates and the like can be used.
  • Surfactants such as phenol-based, sulfate-based, and phosphate-based surfactants; nonionic surfactants such as polyoxyethylene derivative-based and polyvalent alcohol-based derivatives; alkylamines And cationic surfactants such as salt and quaternary ammonium salt; and the like.
  • thermosensitive gelling agent is usually contained in an amount of 1 to 10 parts by weight, preferably 2 to 5 parts by weight, based on 100 parts by weight of the binder. This is desirable,
  • Such a surfactant is usually used in an amount of 0.2 to 5 parts by weight, preferably 0.4 to 4 parts by weight, based on 100 parts by weight of the solid content in the binder mixture. It is desirable that it be contained in parts.
  • the filler is used as needed, and contributes to the stress relaxation property of the sheet-like sealing material and the improvement of the sealing performance.
  • a filler specifically, for example, Inorganic powders such as luc, myric, clay, magnesium oxide, calcium carbonate and the like. In the present invention, these fillers are used alone or in combination of two or more.
  • the rubber material and Z or the resin are usually 5 to 4% in total. It is used in an amount of 0% by weight, preferably from 10 to 30% by weight. This noise If the rubber material and / or resin content is less than 5% by weight, it will not be possible to sufficiently cover the surface of the fibers constituting the nonwoven fabric and the surface of the filler used as necessary. Or, the voids inside the nonwoven fabric cannot be sufficiently filled with the binder mixture, and as a result, the seal of the sheet-like seal material is consequently lost. Performance may be degraded (see Table 1).
  • a filler is usually less than 80% by weight, preferably 5 to 80% by weight, in a total of 100% by weight of the solid content and nonwoven fabric in the binder mixture. Used in quantity. If the filler content exceeds 80% by weight, the amount of the binder for sufficiently covering the filler surface may be insufficient, and the sealing performance of the sheet-like sealing material may be reduced. You. If the filler content is less than 5% by weight, the effect of adding the filler, such as the stress relaxation property of the sheet-like sealing material and the improvement of the sealing performance, cannot be expected much.
  • a binder mixture containing such various components is used in a fluidized state, and may be in a latex state or a solution state.
  • a solution rubber solid rubber and solid rubber
  • solvent Material for example, liquid silicone rubber, liquid fluoro rubber, liquid rubber without solvent alone
  • rubber latex for example, liquid silicone rubber, liquid fluoro rubber, liquid rubber without solvent alone
  • solution resin for example, resin Used as emulsion.
  • binder mixtures may be used alone or in combination of two or more.
  • the method for preparing such a binder mixture is not particularly limited, and a conventionally known method may be employed.
  • Nonwoven fabric is a base material for sheet-like sealing materials and contributes to the improvement of its strength.
  • Such nonwoven fabric can be used in both asbestos-based and non-asbestos-based materials, and is useful for humans and the environment.
  • non-asbestos nonwoven fabrics are preferably used, and such non-asbestos nonwoven fabrics include, for example, p-aramid fiber, Fibers that have high strength at high temperatures, such as fluororesin fibers, carbon fibers, ceramic fibers, and mineral fibers, can be suitably used alone or in combination. .
  • non-woven fabrics there are various methods for producing such non-woven fabrics, such as wet, dry, span lace, snow pour, melt blown, needle punch, and state bond.
  • the type of nonwoven fabric used in the present invention is not limited to the present production method.
  • nonwoven fabric As properties of the obtained nonwoven fabric, it is preferable to use a needle punch felt shape, a wet-laid nonwoven fabric shape, or the like.
  • the above-mentioned nonwoven fabric which contributes to the improvement of the strength of the sheet-like sealing material is obtained by combining the solid content in the binder mixed solution with the nonwoven fabric Or a nonwoven fabric fiber) in a total amount of 100% by weight, usually in an amount of 5 to 80% by weight, preferably 10 to 70% by weight. If the content of the nonwoven fabric (or fiber) is less than 5% by weight, the sheet strength sufficient for practical use cannot be obtained, while if it exceeds 80% by weight, the content of the nonwoven fabric increases. As a result, the voids in the nonwoven fabric increase, the amount of the binder mixed liquid to be impregnated and filled in the voids becomes insufficient, and a sheet-like sealing material having sufficient sealing performance cannot be obtained. It tends to be.
  • Step 1 ⁇ Step of Preparing Binder Mixture (Step 1)>
  • the binder, the solvent or the dispersion medium for the binder, the filler optionally used, and the rubber as the binder are used.
  • rubber chemicals eg, vulcanizing agent, vulcanizing aid, accelerator, anti-aging agent, etc.
  • a thickener, a heat-sensitive gelling agent (heat-sensitive agent), a surfactant and the like may be added.
  • stirring and mixing are usually performed at normal temperature (20 to 30 ° C:) and normal pressure, and if necessary, heating to a temperature at which the components do not change chemically. You may do it.
  • Step 2 ⁇ Step of Impregnating Binder Mixture and Eliminating Gas (Step 2)>
  • the gas present inside the nonwoven fabric is forcibly expelled, and as described above.
  • the binder mixed solution obtained as described above is impregnated into a nonwoven fabric made of a base fiber.
  • the sheet-shaped sealing material has excellent sealing performance. In order to achieve this, it is necessary to completely replace and fill the voids present inside the nonwoven fabric with the binder mixture.
  • the gas usually air
  • the binder-mixture is removed. It is desirable that the step of impregnation is performed by any of the following methods (1) to (4).
  • a method in which a nonwoven fabric is placed in a reduced-pressure container, the inside of the container is reduced in pressure, and then a binder mixed solution is injected also referred to as a “reduced-pressure injection method or a reduced-pressure replacement method”. Is preferred.
  • the non-woven fabric is pre-pressurized and compressed to reduce the voids in which the gas is present, thereby extruding the gas to reduce and eliminate the voids.
  • the nonwoven fabric is immersed in the binder mixture and the pressure on the nonwoven is released in the binder mixture, and the nonwoven fabric returns to its original shape spontaneously. come .
  • the inside of the nonwoven fabric is in a negative pressure state, and the binder mixed solution is sucked into the nonwoven fabric and penetrates, so that the fiber gaps constituting the nonwoven fabric can be completely filled with the binder mixed solution.
  • the binder mixed solution sprayed at high pressure on the surface of the nonwoven fabric is depressurized and suctioned by the suction device provided on the back surface of the nonwoven fabric. Spraying and impregnating the liquid may be more efficient.
  • the method (1) is a method in which the voids inside the nonwoven fabric are replaced with a binder mixed solution under reduced pressure.
  • the inside of the container is kept under reduced pressure, the voids in the nonwoven fabric are reduced. Is also reduced in pressure.
  • the binder mixture is poured into the container under such reduced pressure, the binder mixture diffuses into the container under negative pressure and also penetrates into the voids in the non-woven fabric.
  • the fiber gap in the nonwoven fabric can be filled with the binder mixture.
  • Such a vacuum injection method II is effective, for example, when a non-woven fabric is relatively small in size, without requiring large-scale equipment.
  • the method (operation) (1) to (4) above may be performed only once to obtain the nonwoven fabric.
  • the impregnation amount of the binder mixed solution is insufficient, it is desirable to repeat the method a plurality of times to completely fill the interstices of the fibers constituting the nonwoven fabric with the binder mixed solution.
  • the binder mixed solution described above should be used. It is desirable to mix a surfactant into the binder mixture in the “Preparation process”.
  • the viscosity of the binder mixed solution is low, so that a part of the binder mixed solution impregnated in the nonwoven fabric may flow out, and voids may be generated inside the nonwoven fabric again.
  • the obtained binder mixed solution-impregnated nonwoven fabric is passed between a pair of rolls adjusted at a predetermined interval. Therefore, it is desirable to set (adjust) the adhesion amount (impregnation amount) of the binder mixture to a predetermined amount.
  • the roll transfer type impregnating machine 10 shown in FIG. 1 is provided in the impregnating tank 3 in which the binder mixed liquid 2 is stored, and is provided outside the impregnating tank 3 in front of the impregnating tank 3. Delivery rolls 7 and 8, a compression roll 4 for guiding the delivered nonwoven fabric 1 into the impregnation tank 3 and compressing the same, and a non-woven fabric 1 provided outside the impregnation tank 3 and provided through the impregnation tank 3. A pair of squeezing and driving rolls 5 and 6 for adjusting the amount of the binder mixture are provided.
  • the nonwoven fabric 1 is guided into the impregnation tank 3 by the compression roll 4 through the discharge ports 7 and 8, and is mixed with the binder mixture 2 in the impregnation tank 3. While being immersed, the delivery rolls 7 and 8, the compression roll 4, and a pair of up-and-down squeezing drive rolls 5 and 6 hold and tension the tension of the compression roll 4. Compressed by receiving downward pressure at.
  • the nonwoven fabric tension, compression surface pressure, etc. at this time differ depending on the material, manufacturing method, condition, etc. of the nonwoven fabric, and are not determined unconditionally, but the elongation of the nonwoven fabric will be 1 to 5%.
  • High tension or compression Sometimes it is desirable to apply a load that can make the thickness 10 to 40% of the thickness of the original substrate.
  • Such conditions can be achieved by appropriately adjusting the rotational speed of these rolls and the mutual positional relationship of these rolls, and the non-woven fabric 1 on the compression rolls 4 can be formed.
  • the compression amount can be adjusted appropriately.
  • a belt-mesh transport impregnator 20 may be used.
  • the nonwoven fabric 1 compressed by the compression roll 4 in the impregnation tank 3 in this way is released from the pressure by the compression roll 4 after passing through the compression roll 4 and squeezed up and down.
  • the spontaneous restoration is performed in the process of moving toward the drive rolls 5 and 6, but in this spontaneous restoration process, the void in the nonwoven fabric 1 becomes negative pressure, and the binder mixed liquid in the impregnation layer is filled in the void.
  • the space between the fibers in the nonwoven fabric 1 that has been inhaled and spontaneously restored is filled with the binder mixed solution 2 (not shown).
  • the nonwoven fabric 1 in which all the inter-fiber spaces are filled with the binder mixed solution as described above is used as a set of squeezers provided outside the impregnation tank 3.
  • the amount of the binder mixture that is sandwiched (inserted) between the drive rolls 5 and 6 and impregnated and adhered to the nonwoven fabric 1 is adjusted to a predetermined range.
  • the binder mixed liquid For example, by installing a plurality of such belt-mesh transfer impregnating machines 20 in the vertical direction. You may.
  • one compression roll is shown.
  • the compression roll is also provided below the nonwoven cloth 1 so as to be paired with the compression roll 4.
  • the nonwoven fabric 1 may be compressed and pinched by a pair of compression rolls 4 and 4a.
  • a pair of upper and lower compression rolls may be provided in the impregnation tank 3 to repeat the “compression / opening-impregnation” of the nonwoven fabric to increase the impregnation efficiency. (Not shown).
  • a belt-conveying impregnator 20 schematically shown in FIG.
  • the above impregnation process can be automated by successively performing the operations of “impregnating the mixed solution of the binder and the nonwoven fabric spontaneously restoring and setting the adhesion amount”.
  • the belt transfer type impregnating machine 20 shown in FIG. 2 includes an impregnating tank 3 in which the binder mixture 2 is stored,
  • a compressed roll 4 for guiding the delivered nonwoven fabric 1 into the impregnation tank 3 and compressing the same.
  • a pair of upper and lower squeezing-drive rolls 5 and 6 are provided at the rear outside of the impregnation tank 3 and adjust the amount of the binder mixed liquid in the nonwoven fabric 1 that has passed through the impregnation tank 3.
  • the belt conveyor type impregnating machine 20 is provided with two conveyor belts 21 and 22 which may be in the form of an endless track mesh.
  • the upper conveyor belt 21 circulates around the upper delivery roll 25a, the compression roll 4, and the upper squeezing / driving roll 5, and the upper conveyance belt 21 and the upper squeezing roll 4a.
  • a spontaneous restoration roll 25 b is provided between the drive roll 5 and the drive roll 5.
  • the lower conveying belt 22 circulates around the lower feeding roll 26 a, the compression roll 4, and the lower squeezing / driving roll 6, and the lower squeezing / driving roll 6 and the lower sending roll 6 Auxiliary rolls 26c and 26b are provided between and 26a.
  • the inner surface of the upper transfer belt 21 is in circumferential contact with a part of the surface of the compression port 4, and is in circumferential contact with the compression roll 4.
  • the outer side surface of the upper transfer belt 21 and the outer side surface of the lower transfer belt 22 are in tight contact with each other.
  • the nonwoven fabric 1 is held between the upper and lower delivery rolls 25a and 26a by the upper and lower conveyor belts 21 and 22. While being compressed, it is guided into the impregnation tank 3 where the compression rolls 4 are present, is immersed in the binder mixed solution 2 in the impregnation tank 3, and is moved vertically below the compression belt 4 at the bottom of the compression belt 4. It is pinched and compressed by 1, 2 2.
  • the compression surface pressure, the compression amount of the nonwoven fabric 1 at the four compression rolls, and the compression time can be adjusted as described above. Can be adjusted appropriately as in the above example.
  • Nonwoven fabric 1 used If the impregnating machine 10 as shown in Fig. 1 is used, if the nonwoven fabric 1 is likely to be stretched, the upper and lower conveyor belts 21 and 22 are thus stretched. Non-woven fabric 1 will not be excessively stretched if it is transported by being sandwiched between non-woven fabrics, so that it can be used for a wide variety of non-woven fabrics with different base fiber types and their contents, tensile strengths, etc.
  • a root conveyor impregnator 20 can be used.
  • the high-pressure spray impregnating machine 30 schematically shown in FIG.
  • the binder mixed solution 1a is sprayed from above the nonwoven fabric 1 placed on the surface of the nonwoven fabric 1 below, and the relative positions of the nonwoven fabric 1 and the spray nozzle 32a are continuously measured. It is possible to automate the above-mentioned impregnation step by changing the impregnation step.
  • the nonwoven fabric 1 is placed on the mesh-shaped base 31, and the binder mixed solution is applied from above to the surface of the nonwoven fabric 1.
  • the binder mixture can be uniformly and sufficiently penetrated (impregnated) into the nonwoven fabric.
  • the conditions for efficiently impregnating the nonwoven fabric 1 with the binder mixed solution by the high-pressure spray method depend on the moving speed of the nonwoven fabric, the spraying time, the distance from the nozzle to the nonwoven fabric, and the like. Although it is not generally determined differently, for example, the above-mentioned conditions can be set so as to spray 10 to 50 times the required impregnation amount.
  • FIG. 4 shows an embodiment in which a suction device 33 is provided below the mesh base 31 in the high-pressure spray impregnator 30 shown in FIG.
  • a suction device 33 is provided below the mesh-shaped base 31 to reduce the pressure and suction of the gas and the like in the nonwoven fabric 1.
  • the penetration (impregnation) efficiency can be improved at any time.
  • the impregnating machine described in the above embodiment it is possible to uniformly and completely impregnate the inside of the nonwoven fabric with the binder mixed solution.
  • a sheet-like sealing material excellent in gas and liquid sealing properties and the like can be obtained, the present invention is not limited to such an embodiment using an impregnating machine, and is described above.
  • the method adopts “pre-compressed liquid spontaneous restoration method” 1, “liquid compression spontaneous restoration method” 2, “high-pressure spraying method” 3, “reduced pressure injection method, decompressed displacement method”, etc. It can be used favorably in the invention.
  • the binder mixed solution is impregnated inside the nonwoven fabric, and gas such as air existing in the voids inside the nonwoven fabric is forcibly and substantially completely displaced.
  • gas such as air existing in the voids inside the nonwoven fabric is forcibly and substantially completely displaced.
  • the impregnation process of the binder mixture and the gas expelling process (Simply referred to as the impregnation process.)
  • the solvent unnecessary for the final product, sheet-like sealing material or, a dispersion medium is contained.
  • the solvent or dispersion medium of the nonwoven fabric impregnated with the binder mixed solution is removed from the nonwoven fabric after the impregnation step before performing the drying step described below.
  • Removal of the solvent or dispersion medium takes place between 1 and 3 o'clock in a dryer set at 80 ° C or higher, preferably 80 ° C or higher and 100 ° C or lower.
  • the solvent or the dispersion medium may be volatilized and removed by heating the sheet for a while. If the sheet is dried at a high temperature exceeding 100 ° C, the solvent or dispersion medium in the nonwoven fabric may be rapidly vaporized and expanded, and voids may be generated inside the nonwoven fabric.
  • the drying step is performed at a temperature exceeding 100 ° C, the crosslinking of the rubber in the sheet and the curing of the resin are promoted before the following “forming step” is performed.
  • the effect of improving the airtightness by compression may not be sufficiently obtained. Also, when the sheet is dried at a temperature lower than 80 ° C, it takes a long time to completely volatilize and remove the solvent or the dispersion medium, which is inefficient.
  • the evaporation of the solvent or the dispersion medium mainly occurs on the sheet surface, and the solvent or the dispersion medium remaining inside the sheet moves to the surface, and is thereby generated by the cycle.
  • the solvent or dispersion medium is removed.
  • not only the solvent or dispersion medium but also the binder mixture inside the sheet itself may be guided to the sheet surface (also referred to as migration).
  • the rubber compounding ratio inside the sheet is reduced by the rubber compounding ratio near the sheet surface.
  • the obtained sheet-like sealing material does not show sufficiently excellent sealing performance and stress relaxation performance.
  • the "binder" Preparation of one liquid mixture ” In the step (Step 1), a heat-sensitive gelling agent (thermosensitive agent) is blended when preparing the binder mixture, and in this“ drying step ”, the solvent or dispersion medium drying temperature Heating at the following temperature, preferably at a temperature of 40 to 80 ° C, increases the viscosity of the binder mixture and reduces the flowability of solids. Is effective (also called “pre-drying process”).
  • the sheet After performing the pre-drying step in this way, as described above, the sheet is placed in a dryer set at a temperature of 80 ° C or more, preferably 80 to 100 ° C.
  • the solvent or the dispersion medium is volatilized and removed by heating, the resulting sheet-like sealing material has a uniform component content regardless of its location, such as inside or near the surface. There is a tendency to obtain a sheet-like sealing material that is excellent in both balance and stress relaxation.
  • heating in a moist and hot atmosphere is an effective method for suppressing migration.
  • the method it is possible to increase the viscosity of the binder mixed liquid inside the sheet and reduce the flowability of the solid content without involving the movement or volatilization of the solvent or the dispersion medium.
  • Heating in such a moist heat atmosphere is 100 to 150 ° C, preferably in a steam atmosphere at a temperature of 120 to 130 ° C (humidity: 80 to 100 ° C). %) By heating the sheet for about 5 to 20 minutes.
  • a "drying step” may be performed in which the sheet is heated in a dryer set as follows to volatilize and remove the solvent or the dispersing medium.
  • the airtightness of the sheet after the drying step is completed by pressing the dried product (sheet) obtained through the drying step under heating in the “forming step”.
  • cross-linking of the compounded rubber or curing of the resin is performed.
  • a hot press is usually used as a molding device.
  • the molding conditions vary depending on the composition of the components, etc., and are not generally determined. However, usually, the heating temperature is 120 to 250 ° (heating time: 3 to 15 minutes, compression surface pressure: 5 to 50 minutes). It is set appropriately within the range of 40 MPa.
  • the heating temperature is 150 to 250 ° (:, the heating time is 0.5 to 24 hours, and the heating may be performed under the dry heat or the wet heat.
  • free pressure is not applied, and freezing is often used.
  • rubber or resin as an organic binder is usually 5 to 40% by weight, preferably 10 to 40% by weight.
  • the base fiber constituting the nonwoven fabric is usually required in an amount of 5 to 80% by weight, preferably 10 to 70% by weight, and more preferably 10 to 50% by weight. Is contained in an amount of 0 to 80% by weight, particularly when a filler is incorporated, preferably 5 to 80% by weight, and more preferably 30 to 80% by weight. It is desirable that it be included in the amount of weight%.
  • the sheet-like sealing material obtained in this way can maintain excellent gas-sealing properties and liquid-sealing properties over a long period of time at high temperatures, and have a difference in the strength of the sealing material. There is no isotropic.
  • usable fibers are not limited, and a nonwoven fabric made of a wide variety of fibers can be used. That is, unlike the conventional method of producing a single piece of calender, in the present invention, the nonwoven fabric is impregnated with the binder mixed solution, and the gas inside the nonwoven fabric is completely removed, followed by drying and heating. Since heat-compression is performed, no shear stress is generated on the surface of the molded sheet-like sealing material, and the mixing conditions are such that the wettability between the fiber and the binder is poor. No wrinkles or breakage during molding.
  • the fibers that can be used in the production method there are no restrictions on the fibers that can be used in the production method, and it is possible to produce a sheet-like sealing material containing rubber or resin that does not contain p-aramid fibers. ing.
  • the sheet-like sealing material obtained by the manufacturing method of the present invention hardly hardens when used under high-temperature conditions, it can maintain excellent sealing performance and other properties over a long period of time and can maintain a long-term soundness. Excellent.
  • the sheet-like sealing material obtained by the production method of the present invention uses a non-woven fabric unlike conventional joint sheets and beater sheets.
  • the binder component is dispersed in the binder-mixture. . In the process of impregnating the nonwoven fabric with the binder mixed solution, drying and forming, one component of the binder inside the sealing material is maintained in a dispersed state.
  • the binder component exists in a discontinuous state inside the sealing material, when used under high-temperature conditions, even if the binder component hardens in the dispersed particles, This does not induce hardening and shrinkage of the sheet-like sealing material.
  • rubber latex or resin emulsion which is an aqueous dispersion system
  • any of solution rubber, liquid rubber, and solution resin can be used.
  • Nonwoven fabric is a material that originally contains a large number of voids. Therefore, it is possible to uniformly impregnate the inside of the nonwoven fabric with the binder mixed solution.
  • a highly airtight sheet-like seal material can be obtained by forming the binder mixed solution once impregnated while holding it inside the nonwoven fabric.
  • the method of measuring the “elongation at break after thermal history”, which indicates the degree of hardening of the sheet material used in the following examples and comparative examples, is as follows.
  • a 1.5 mm thick, 15 OX 25 mm strip test piece was prepared in consideration of application to the tensile test, and this was treated in heated air at 180 ° for 96 hours, and then used for gripping. Set the distance between the jigs to 100 mm and measure the elongation at break by performing a tensile test at a tensile speed of 5 mm Z minutes. The elongation at break (R ⁇ ) was calculated.
  • the tensile strength (according to JISR3453) of the obtained sheet-like sealing material is 20.8 MPa in the high-strength direction (vertical direction, a), and 20.8 MPa in the low-strength direction (horizontal direction, b).
  • the OMPa was 20.
  • the strength anisotropy (a / b) was 1.0.
  • the number of days until cracking when it was installed at 230 ° C in the actual machine line was more than 360 days.
  • the tensile strength of the obtained sheet-like sealing material is 25.3 MPa in the high-strength direction (vertical direction, a), 22.8 MPa in the low-strength direction (horizontal direction, b), and the strength anisotropy (aZ b) was 1.1.
  • cold seal resistance ASTM F 3 7 - compliant B surface pressure 1 9 6 MP a, nitrogen pressure 0 9 8 MP a...
  • ASTM F 3 7 - compliant B surface pressure 1 9 6 MP a, nitrogen pressure 0 9 8 MP a... Are, 7 5 E - 5 and (P a • m 3 Z s ) ,
  • the elongation at break (% (lower of the values in the vertical and horizontal directions)) after thermal history is 0.80%
  • the number of days until cracking occurred when it was installed at 230 ° C in the actual machine line was over 360 days.
  • the tensile strength (according to JISR3453) of the obtained sheet-like sealing material is 26.3 M in the high strength direction (vertical direction, a). In the low strength direction (transverse direction, b), Pa was 23. IMPa, and the strength anisotropy (aZb) was 1.1.
  • the elongation at break (% (lower of the values in the vertical and horizontal directions)) at break after thermal history is 3.00%.
  • the number of days until the occurrence of cracks when it was installed at 230 ° C in the actual machine line was more than 360 days.
  • Table 1 shows the amounts of each component and the test results. [Reference example 1]
  • the elongation at break after heat history (% (the lower of the values in the vertical and horizontal directions)) is 0.70%
  • the number of days until the occurrence of cracks when it was installed in the actual machine line and held at 230 was 180 days.
  • Table 1 shows the amounts of each component and the test results.
  • composition for forming a joint sheet having the following composition was prepared.
  • NBR 15.9% by weight Rubber chemicals 2.3% by weight Inorganic fillers (heavy coal, clay) 71.0% by weight Toluene 0.7 liter per 1 kg of the above mixture
  • the obtained composition was inserted between a hot roll kept at 130 ° C. and a cooling roll kept at 30 ° C. and rolled by heating. In this way, the composition was formed into a sheet-like viscous layer on the hot roll side. The sheet was peeled off from the heat roll with a doctor blade to obtain a 1.5 mm thick joint sheet.
  • the tensile strength of the obtained joint sheet is 42.7 MPa in the high strength direction (vertical direction, a), 17.1 MPa in the low strength direction (horizontal direction, b), and the strength anisotropy (a Z b) was 2.5.
  • the room temperature sealability (conforming to ASTMF 37-B.
  • the surface pressure is 19.6 MPa and the internal pressure of nitrogen is 0.98 MPa) is 3.1 E—4 (Pa • m 3 / s).
  • the elongation at break (% (lower of the values in the vertical and horizontal directions)) after thermal history is 0.25%
  • the number of days until the occurrence of cracks when it was installed in the actual machine line and held at 230 was 120 days.
  • composition for forming a joint sheet having the following composition was prepared.
  • a jump sheet was obtained in the same manner as in Comparative Example 1 except that the obtained composition was used.
  • the elongation at break (% (lower of the values in the vertical and horizontal directions)) at break after thermal history is 1.02%
  • the number of days until cracking when it was installed at 230 ° C in the actual machine line was more than 360 days.
  • Inorganic filler (creative) 59% by weight
  • the obtained composition was formed into a paper by a round-mesh paper machine, and then dried and pressed to obtain a bead sheet.
  • the tensile strength (according to JISR3453) of the obtained beef sheet is 36.2 MPa in the high-strength direction (vertical direction, a) and 36.2 MPa in the low-strength direction (lateral direction, b). 12.7 MPa and the strength anisotropy (a / b) was 2.9.
  • room temperature sealability (based on ASTMF 37-B. Surface pressure 19.6 MPa, The internal pressure of nitrogen 0.98 MPa) is 6.3 E-2 (P
  • Table 1 shows the amounts of each component and the test results.
  • the production method of the present invention does not limit the fiber type of the nonwoven fabric to be a nonwoven fabric.
  • organic fibers such as ceramic fibers, mineral fibers, PPS fibers and m-aramid fibers are used as the sole fiber type.
  • Sheet-like sealing materials, and sheet-like sealing materials in which PPS fibers and ceramic fibers were mixed, could also be manufactured.
  • the sheet-like sealing material obtained by the production method of the present invention shows the non-asbestos joint obtained by the conventional production method based on the result of “elongation at break after thermal history”. It can be seen that the degree of curing under high temperature conditions is reduced as compared with toseat.
  • the sealing performance of the sheet-shaped sealing material of the present invention is much lower than that of gas-sealing. It turns out that it has sufficient sealing performance.

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  • Gasket Seals (AREA)

Abstract

A process for producing a sheet-form sealing material which comprises: impregnating a nonwoven fabric with a liquid binder mixture comprising a rubber material or resin and a solvent or dispersion medium, while expelling the gas present in the nonwoven fabric; and heating and compressing the impregnated nonwoven fabric to vulcanize the rubber material or cure the resin. The impregnation is conducted, for example, by a method in which the nonwoven fabric which has been compressed is allowed to spontaneously recover its original shape in the liquid mixture. Alternatively, the impregnation may be conducted by the high-pressure spraying of the liquid mixture or by infiltration at a reduced pressure. Thus, a sheet-form sealing material reduced in strength anisotropy and excellent in gas-barrier properties, etc. is obtained.

Description

明 糸田 シー 卜状シール材の製造方法 技術分野 本発明は、 シー ト状シール材の製造方法に関 し、 さ ら に 詳し く は、 強度異方性が抑制さ れ、 かつガス シール性な ど に優れたシー ト状シール材の製造方法に関する 。  TECHNICAL FIELD The present invention relates to a method for producing a sheet-like seal material, and more particularly, to a method for producing a sheet-like seal material, in which strength anisotropy is suppressed and gas sealability is improved. The present invention relates to a method for producing a sheet-like sealing material excellent in quality.
背景技術 Background art
現在、 一般産業用 と して多種のガス ケ ッ ト が使用 さ れて いる が、 最も汎用性の高い も の と して、 主と して繊維お よ び充填剤 と、 ゴム あ る いは樹脂 とカゝ ら構成さ れてい る 、 ジ ョ ィ ン ト シ一 ト あ る いはビータ一シ一 ト が挙げ られる。  At present, various gaskets are used for general industry, but the most versatile ones are mainly fibers and fillers and rubbers or rubbers. Examples include a jump sheet or a beater sheet composed of a resin and a resin.
こ こで、 ジ ョ イ ン ト シー ト は、 石 帛、 ガ ラ ス繊維等の無 :繊維、 あ る いは芳香族ポ リ ア ミ ド繊維、 フ ィ ブリ ル化 し た芳香族ポ リ ア ミ ド繊維な ど の有機繊維を基材繊維 と し、 こ れに結合剤 と しての ゴム、 樹脂、 加硫剤な どのゴム薬品 およ び充填剤等を添加混鍊 してジ ョ イ ン ト シ一 ト形成用組 成物を調製 し、 こ の組成物を熱ロール と冷却 ロール とか ら なる 一対の ロール間に挿入 して加熱圧延 し、 ジ ョ イ ン ト シ 一 ト 成形用組成物 を熱 ロール側に積層 させ次いで熱ロール に積層 さ れた シー ト 状物 を剥離す る こ と に よ っ て得 ら れ る。 ま た、 ビー夕一シー ト は、 叩解機内 にて石綿繊維あ る い は非石綿繊維に充填剤およびゴム あ る い は樹脂を添加 し、 これ ら を攪拌 し水に均一分散さ せたのち抄造機で抄造する こ と によ っ て得 ら れる 。 Here, the joint sheet is made of non-fiber such as stone or glass fiber, or aromatic polyamid fiber, or fibrillated aromatic poly. Organic fibers such as amide fibers are used as base fibers, and rubber, resin, vulcanizing agents and other rubber chemicals as fillers and fillers are added and mixed. A composition for forming an int sheet is prepared, and the composition is inserted between a pair of rolls composed of a heating roll and a cooling roll, and heated and rolled to form a joint sheet. The composition is obtained by laminating the composition on the hot roll side and then peeling off the sheet-like material laminated on the hot roll. In addition, in the beating machine, a filler and rubber or resin are added to asbestos fiber or non-asbestos fiber in a beater, and these are stirred and uniformly dispersed in water. It is obtained by making paper with a paper machine.
こ れ ら の シー ト は、 比較的安価であ る 、 大寸法品の生産 が容易であ る 、 各種形状への加工が容易であ る、 取扱が容 易であ る 、 比較的低締付力で も流体を シールする こ とがで き る等、 種々 の特長を有 してい る。 しカゝ しなが ら 、 こ れ ら ジ ョ イ ン ト シ一 ト ゃ ビー 夕 ー シー ト に も 問題点が存在す る。  These sheets are relatively inexpensive, easy to produce large size products, easy to process into various shapes, easy to handle, relatively low tightening It has various features, such as the ability to seal fluids with force. However, there are also problems with these jump-to-be-go seats.
ジ ョ イ ン ト シー ト の第一の問題点 と して、 製法上使用 で き る 繊維に制限があ る 。 ジ ョ イ ン ト シー ト の製造に際 して は、 原料であ る 、 繊維 と、 ゴム または樹脂 と の濡れ性が重 要であ り 、 その濡れ性が悪い と、 シー ト 成形時に シー ト に しわや破断が生 じ る。  The first problem with joint sheets is that the fibers that can be used in the manufacturing process are limited. In the production of a joint sheet, the wettability between the raw material, fiber, and rubber or resin is important, and if the wettability is poor, the sheet is formed at the time of sheet molding. Wrinkles and breaks occur.
現在、 ゴム あ る いは樹脂 と のぬれ性の良い石綿繊維を配 合 し た石綿ジ ョ イ ン ト シー ト と、 石綿繊維を含まない ノ ン アスベス ト ジ ョ イ ン ト シー ト (非石綿系ジ ョ イ ン ト シー ト) とが存在するが、 ゴム と の濡れ性に劣る と さ れてい る炭素 繊維等を単独で繊維種 と して用 いたジ ョ イ ン ト シ一 ト は極 めて少な く 、 上市さ れている ノ ンアスペス ト ジ ョ イ ン ト シ 一 ト の大部分には少量の p —ァ ラ ミ ド繊維が配合さ れてい る 。 使用可能な繊維種上の制限は、 ガス ケ ッ ト材の品質向 上を図る上で大きな制約 となっ ている。 第二の問題点 と して、 石綿繊維に対する使用規制が挙げ ら れる 。 石綿ジ ョ イ ン ト シー ト は、 高温下で長期に亘つ て 優れた特性 を保持でき る 、 種々 の温度の種々 の流体に対 し て使用 でき汎用 性が高い等、 優れた製品ではあ るが、 安全 衛生上石綿繊維 自 身の使用が制限さ れてお り 、 石綿ジ ョ イ ン ト シー ト は他のガスケ ッ トへ代替さ れつつ あ る。 At present, asbestos joint sheets that combine asbestos fibers with good wettability with rubber or resin, and non-asbestos joint sheets that do not contain asbestos fibers (non-asbestos) (Joint sheet), but the use of carbon fiber, etc., which is said to have poor wettability with rubber, as a fiber type alone, is extremely short. At the very least, most of the commercially available non-asbestos short sheets contain a small amount of p-aramid fiber. Restrictions on the types of fibers that can be used are a major constraint in improving the quality of gasket materials. The second problem is the regulation on the use of asbestos fibers. Asbestos joint sheets are excellent products that can maintain excellent properties over a long period of time at high temperatures, can be used for various fluids at various temperatures, and have high versatility. However, the use of asbestos fiber itself is restricted for safety and health reasons, and asbestos joint sheets are being replaced by other gaskets.
第三の問題点 と して、 ノ ンアスベス ト ジ ョ イ ン ト シー ト は、 石綿ジ ョ イ ン ト シー ト と比較 して、 高温下で実機にて 長期間使用 した場合に、 例えば、 シール性、 引張強度、 破 断時伸び率な ど の優れた性能が保持さ れる性質 ( 「長期健 全性」 と も 言 う 。 ) に劣る 。 こ れは ノ ンア ス ベス ト シー 卜 が高温空気履歴によ る硬化を起 こ しやす く 、 結果と して高 温下で長期間実機使用 し た場合に割れやす く なる こ と を意 味する。  The third problem is that non-asbestos joint sheets can be used for a long time in actual equipment at high temperatures compared to asbestos joint sheets. Poor properties (also referred to as "long-term health") that maintain excellent properties such as strength, tensile strength, and elongation at break. This means that non-asbestos sheets are liable to harden due to the history of high-temperature air, and consequently are liable to break when used at high temperatures for a long period of time on actual equipment. I do.
石綿ジ ョ イ ン ト シー ト の場合、 強度を担う 石綿繊維の配 合比率を高 く 設定する こ と に よ っ て、 配合さ れている ゴム や樹脂 自 身の硬化がシー ト 全体の硬化に与え る影響を軽減 する こ とができ る。 一方、 ノ ンアスベス ト ジ ョ イ ン ト シー 卜 の場合、 一般的に ; p — ァ ラ ミ ド繊維を強度向上剤 と して 配合 してい るが、 該繊維はぬれ性が悪 く p — ァ ラ ミ ド繊維 を多量に配合 し て も シー ト の強度は増加せずむ し ろその他 の特性および加工性が悪化する こ とが多 く 、 該繊維を多量 に配合する こ と は困難であ り 、 結果 と してゴムや樹脂 自 身 の硬化がシー 卜 全体の硬化へとつながる。 第四の問題点 と して、 ジ ョ イ ン ト シー ト では、 製法上シ 一 卜 の強度異方性を排除する こ とができない (表 1 参照) 。 これは力 レ ンダー ロールによ る圧縮加硫工程 を経る こ と に よ り 、 配合する繊維がほぼ一様に配向する ためであ る 。 In the case of asbestos joint sheets, by setting a high ratio of asbestos fibers that are responsible for strength, the curing of the compounded rubber and resin itself cures the entire sheet. The effect on the environment can be reduced. On the other hand, in the case of non-asbestos joint sheets, generally, p-aramid fiber is blended as a strength improver, but the fiber has poor wettability and the p-aramid fiber has poor wettability. Even if a large amount of the laminating fiber is blended, the strength of the sheet does not increase, but other properties and workability often deteriorate. Therefore, it is difficult to blend the fiber in a large amount. As a result, the curing of the rubber or resin itself leads to the curing of the entire sheet. As a fourth problem, in the case of a joint sheet, the strength anisotropy of the sheet cannot be excluded due to the manufacturing method (see Table 1). This is because the fibers to be blended are oriented almost uniformly by undergoing a compression vulcanization step using a force render roll.
石綿ジ ョ イ ン ト シ一 卜 の場合には、 石綿繊維の配合比率 を高 く 設定する こ と に よ っ てシー ト 全体の強度を著 し く 増 加さ せ、 こ れに よ り 上記の強度'異方性を補完する こ とがで さる。  In the case of asbestos joint sheets, the strength of the entire sheet is significantly increased by setting a high proportion of asbestos fibers, thereby increasing the strength of the asbestos fiber. It complements the strength 'anisotropy.
一方、 ノ ンアスベス ト ジ ョ イ ン ト シー ト の場合に は、 そ の繊維配合比率 を高 く 設定できず、 配合する繊維で前述 し た強度異方性を補完する こ とができない。 そのため、 長期 高温下での実機使用 にお いてゴム分の硬化に よ り ガス ケ ッ ト 内部に応力が発生 した際、 強度の弱い方向 あ る い はその 部分にその応力が集中 し、 結果 と してガス ケ ッ ト の割れが 誘発さ れる と推測される。  On the other hand, in the case of non-asbestos joint sheets, the fiber blending ratio cannot be set high, and the fiber anisotropy described above cannot be complemented by the fiber blended. For this reason, when stress is generated inside the gasket due to the hardening of the rubber during use of the actual machine at high temperature for a long period of time, the stress concentrates in the weaker direction or in the weaker portion, resulting in a lower result. It is presumed that cracking of the gasket is induced.
一方、 ビ一タ ーシー ト には気密性の点で問題があ る 。 一 般的 に ビーター シ一 ト は、 潤滑油や燃料油 と い っ た液体シ —ル用 と して使用 さ れ、 具体的にはオイ ルパ ンやフ ユ エル ポ ン プ等に使用 される 。 一方、 ガス性流体な ど、 厳 し い気 密性能 を要求 さ れる ガス ケ ッ ト と し て は使用 さ れて い な い。  On the other hand, bitter sheets have a problem in terms of airtightness. Generally, beater sheets are used for liquid seals such as lubricating oil and fuel oil, and specifically for oil pumps and fuel pumps. . On the other hand, it is not used for gaskets that require strict airtightness, such as gaseous fluids.
現在上市されてい る ビーター シー ト製法で得 られたガス ケ ッ ト につ レ て、 「 A S T M F 3 7 — B 」 に準拠 し、 ガ ス ケ ッ ト 面圧 1 9 . 6 M P a 、 窒素内圧 0 . 9 8 M P a に 設定 し、 ガス ケ ッ ト外径部か ら の流体漏洩量を測定 し た と こ ろ 、 6 . 3 ズ 1 0 —2 ? & ' 111 3 / 3 を示した (表 1 参照) 。 こ の よ う にガス漏洩量が多い のは、 抄造工程 において シー ト 中 に 内包さ れた空隙の一部が製造工程中 に除去さ れず残 存 して し ま う ため と考え ら れる 。 実使用条件下では、 一般 的に石験水発泡法にてガスケ ッ 卜 か ら のガス性流体の漏洩 の存否 を判断してお り 、 こ の石鹼水発泡法では、 実機 (ガ ス性流体用配管) フ ラ ンジ部に試験用 ガス ケ ッ ト を組付け、 ガス ケ ッ ト 外径側あ る い はフ ラ ン ジ間隙に石鹼水を塗布 し たのち 、 気泡発生の有無によ り 、 ガス性流体用配管の接続 部か ら ガス性流体が漏洩 してい る か否かを判断する 。 こ の 石鹼水発泡法での検出感度は、 約 2 X 1 0 "4 P a · m 3 Z s であ る 。 ビ一ターシー ト は、 一般的に、 こ の石鹼水発泡 法の検出感度の 1 8 〜 5 5 0 倍の漏洩量を示す こ とか ら 、 ビーター シー 卜 の シール性能は低 く 、 ガス性流体用 シール 材 と しては不適当であ る 。 ガス用 シール材 と しては 2 X 1 0 — 4 P a · m 3 Z s 以下の漏洩量 を示すシール性能が必要 であ る。 The gasket obtained by the beater sheet manufacturing method currently on the market conforms to “ASTMF 37 — B” and has a gasket surface pressure of 19.6 MPa and a nitrogen internal pressure of 0. 9 to 8 MPa Set, this filtrate and was measured fluid leakage amount of gas Ke Tsu DOO outer diameter or al, 6 3 1 0 -? 2 &'showed 111 3/3 (see Table 1). It is considered that the reason for the large amount of gas leakage is that some of the voids included in the sheet during the papermaking process are not removed during the manufacturing process but remain. Under actual conditions of use, the existence of leakage of gaseous fluid from the gasket is generally determined by the lithographic water foaming method. Attach a test gasket to the flange and apply stone water to the outside diameter of the gasket or to the gap between the flanges. Thus, it is determined whether the gaseous fluid is leaking from the connection of the gaseous fluid pipe. The detection sensitivity of this water-foaming method is about 2 × 10 ” 4 Pa · m 3 Zs. The beater sheet is generally used for detection of this water-foaming method. The sealing performance of the beater sheet is low because it exhibits a leakage amount of 18 to 55 times the sensitivity, making it unsuitable as a sealing material for gaseous fluids. Therefore, a sealing performance that shows a leakage amount of 2 X 10 — 4 Pa · m 3 Z s or less is required.
しか し なが ら こ れまでの と こ ろ 、 上記のよ う な ビー夕一 シー ト 製法で得 ら れ、 かつ優れたガス シール性能等を有す る シール材は知 られていない。  However, as of now, there is no known sealing material obtained by the above-mentioned beading sheet manufacturing method and having excellent gas sealing performance and the like.
そ.こ で本発明者 ら は、 上記問題点を解決すべ く 鋭意研究 を重ねた と こ ろ 、  Therefore, the present inventors have conducted intensive research to solve the above-mentioned problems.
有機系バイ ンダー と しての ゴム材 と、 ゴム薬品 と、 前記 ゴム材用 溶剤また は分散媒 と を混合する か、 あ る い は有機 系バイ ンダー と しての樹脂 と、 前記樹脂用溶剤または分散 媒 と を混合 して、 得 ら れたバイ ンダー混合液を、 基材繊維 か ら なる 不織布に、 該不織布内部に存在する気体を (強制 的に) 追い出す と と も に含浸さ せ、 上記混合液が含浸さ れ た不織布か ら 少な く と も一部の溶剤または分散媒を揮散 · 除去 し、 次いで こ の不織布を加熱圧縮 して、 上記ゴム材を 加硫させ、 あ る い は上記樹脂を硬化させてシー ト状シール 材を製造する と、 強度異方性が抑制さ れ、 かつガス シール 性な どに著 し く 優れたシー ト状シール材が得 ら れる こ と な どを見出 して本発明を完成する に至っ た。 Rubber material as an organic binder, rubber chemicals, and the above A binder mixture obtained by mixing a solvent or dispersion medium for rubber material or mixing a resin as an organic binder with the solvent or dispersion medium for resin. Is impregnated with (forcibly) expelling gas present in the nonwoven fabric into the nonwoven fabric made of the base fiber, and at least a part of the nonwoven fabric impregnated with the mixed solution is impregnated. The solvent or dispersion medium is volatilized and removed, and then the nonwoven fabric is heated and compressed to vulcanize the rubber material or to cure the resin to produce a sheet-like sealing material. The present inventors have found that anisotropy is suppressed and that a sheet-like sealing material excellent in gas sealing properties and the like can be obtained, and the like, and the present invention has been completed.
なお、 ① : 特開昭 5 7 — 1 1 6 9 7 0 号公報には、 テ ト ロ ン、 ナイ ロ ン等の疎水性短繊維よ り なる不織布を 1 枚ま たは 2 枚以上重ね合わせた も の を基材 と し、 これに樹脂、 ゴム等のバイ ンダーを含浸さ せて成型 した食品機械器具用 パ ッ キンが開示さ れてい る。 ま た、 該公報には、 上記の よ う に基材 に樹脂、 ゴム等のバイ ンダー を含浸さ せて乾燥さ せた も の を加圧成型 して、 上記食品機械器具用 パ ッ キン を 製造する こ と が記載さ れてい る 。 また該公報には、 こ のパ ツ キ ンは、 シール性に優れ、 かつ衛生的であ る 旨記載さ れ てい る 。 しか しなが ら 、 該公報に含まれる含浸工程 は、 繊 維飛散防止、 パ ッ キ ン腐食防止を 目 的 と した樹脂含浸であ る こ とか ら 、 該公報に記載の方法で得 ら れるパ ッ キンでは、 漏洩を厳格に制限するパ ツ キン材 と して用 いる には、 ガス、 液体等のシール性の点で不十分であ る。 (1): JP-A-57-116709 describes that one or two or more nonwoven fabrics composed of hydrophobic short fibers such as tetron or nylon are laminated. There is disclosed a packing for food machinery and the like, which is formed by using a base material as a base material and impregnating the base material with a binder such as resin and rubber. In addition, as disclosed in the publication, the packing for food machinery and appliances is formed by impregnating a base material with a binder such as resin or rubber and drying the base material as described above. It states that it is manufactured. The publication also states that this patch is excellent in sealability and sanitary. However, since the impregnation step included in the publication is resin impregnation for the purpose of preventing fiber scattering and packing corrosion, it can be obtained by the method described in the publication. In packing, gas, gas, etc. are used as packing materials that severely restrict leakage. Inadequate sealing performance for liquids.
ま た、 ② : 特公平 8 _ 3 0 8 6 号公報には、 水に シ リ コ ン樹脂の コ ロイ ド粒子又はポ リ テ ト ラ フ ロ ロエチ レ ン樹脂 の コ ロイ ド粒子 と アク リ ル系 プライ マ と を分散させる こ と に よ り 、 揮発に よ る発火性及び有害性の無い水分散系のェ マルジ ヨ ン を作成 し、 ガラス繊維を主体 とする綿状体を二 一 ド ルパ ンチ加工 してなる ニー ドルマ ツ 卜 の内部全体に前 記ェマルジ ヨ ン を含浸させた後、 前記ニー ドルマ ッ ト に含 浸 し た前記ェマルジ ョ ンの水分を蒸発さ せる こ と によ り 、 前記ニー ドルマ ツ 卜 の内部全体に シ リ コ ン樹脂又はポ リ テ ト ラ フ ロ ロ エチ レ ン樹脂 と ア ク リ ル系プライ マ と を付着さ せ、 前記ニー ドルマ ッ ト の表面にア ク リ ル系粘着剤付き の 剥離紙を貼着する 、 燃焼器具用パ ツ キ ン材の製造方法が開 示さ れてい る。 また、 該公報には、 水分散系のェマルジ ョ ンを浸漬槽に貯留 し、 前記ニー ドルマ ッ ト を ローラ送 り 装 置に よ っ て連続的に送 り なが ら 前記ェマルジ ョ ンに 2 0 〜 1 0 0 秒程度浸漬する こ と に よ り 、 該ニー ドルマ ツ 卜 の内 部全体に該ェマルジ ヨ ンを含浸さ せる こ とが記載さ れてい る。 また、 上記水分散系ェマルジ ョ ンを用 いる こ と によ り 、 該ニー ドルマ ツ ト の内部全体に該ェマルジ ョ ン を含浸させ る こ とが初めて可能 とな り 、 ニー ドルマ ツ 卜 を構成 して い る全てのガ ラ ス繊維の表面及び繊維間に シ リ コ ン樹脂又は In addition, ②: Japanese Patent Publication No. 8_30686 states that colloid particles of silicone resin or colloid particles of polytetrafluoroethylene resin and water By dispersing water-based primers, a water-dispersed emulsion without flammability and harmfulness due to volatilization is created, and a cotton-like body mainly composed of glass fiber is produced. By impregnating the entire interior of the rudder cut needle mat with the above-described emulsion, the moisture of the emulsion impregnated into the needle mat is evaporated. A silicone resin or polytetrafluoroethylene resin and an acrylic-based primer are adhered to the entire inside of the needle mat, and the surface of the needle mat is adhered to the needle mat. Paste release paper with acrylic adhesive, Method for manufacturing a device for path tree rk material that have the indicated open. Further, the publication discloses that an emulsion of a water dispersion system is stored in an immersion tank, and the needle mat is continuously fed by a roller feeding device to the emulsion while being continuously fed thereto. It describes that the immersion is carried out for about 0 to 100 seconds so that the entire interior of the needle mat is impregnated with the emulsion. In addition, the use of the above-mentioned water-dispersed emulsion makes it possible for the first time to impregnate the entire interior of the needle mat with the emulsion, thereby constituting the needle mat. Silicon resin or the surface of all glass fibers
P T F E 樹脂 を 付着 さ せる こ と がで き る 旨記載さ れて い る。 しか し なが ら 、 該公報に記載の方法に は圧縮成形工程 を 含んでお らず、 ノ° ッ キ ンの気密性は向上 してお らず、 該公 報 に 記載 の方法 に よ り 得 ら れる 燃焼器具用 パ ツ キ ン材で は、 ガス あ る いは液体シ一ル性な どの点で不十分であ る 。 発明の開示 It states that PTFE resin can be attached. However, the method described in the official gazette does not include a compression molding step, does not improve the airtightness of the knock-in, and is not described in the publication. The resulting packing material for combustion appliances is insufficient in terms of gas or liquid sealing properties. Disclosure of the invention
【発明の 目 的】  [Purpose of the invention]
本発明 は、 上記のよ う な従来技術に伴う 問題点を解決 し よ う とする も のであ っ て、 配合する繊維種に制限がな く 、 高温条件下で長期間使用 でき、 従来の ジ ョ イ ン ト シー ト の 代替品 と して使用 でき、 ガスや液体の シールに好適に使用 し う る 、 シー ト状シール材の製造方法を提供する こ と を 目 的 と してレ、る 。  The present invention is intended to solve the problems associated with the prior art as described above, and there is no limitation on the type of fiber to be blended, and the fiber can be used for a long time under a high temperature condition. It is intended to provide a method of manufacturing a sheet-like sealing material that can be used as a substitute for a point sheet and is suitably used for gas and liquid sealing. .
【発明の概要】  Summary of the Invention
本発明 に係る シー 卜状シール材の第 1 の製造方法は、 有機系バイ ンダー と しての ゴム材 と、 ゴム薬品 と、 前記 ゴム材用溶剤または分散媒 と を混合 し、  A first method for producing a sheet-like sealing material according to the present invention comprises: mixing a rubber material as an organic binder, a rubber chemical, and the rubber material solvent or dispersion medium;
得 ら れたバイ ンダー混合液を、 基材繊維か ら なる不織布 に、 該不織布内部に存在する気体を追い出すと と も に含浸 させ、  The obtained binder mixed solution is impregnated into a nonwoven fabric made of a base fiber while expelling gas present inside the nonwoven fabric,
上記混合液が含浸さ れた不織布か ら 少な く と も一部の溶 剤または分散媒を揮散 · 除去し、  At least a part of the solvent or dispersion medium is volatilized and removed from the nonwoven fabric impregnated with the above mixed solution,
次いで こ の不織布を加熱圧縮 して、 上記ゴム材を加硫さ せてシー 卜状シール材を得る こ と を特徴と している。 本発明に係る第 1 の製造方法にお いては、 前記バイ ンダ 一混合液が、 ラ テ ッ ク ス の形態で用 い ら れる こ とが好ま し い Then, the nonwoven fabric is heated and compressed, and the rubber material is vulcanized to obtain a sheet-like sealing material. In the first production method according to the present invention, it is preferable that the mixed solution of the binder is used in the form of a latex.
本発明に係る シ一 卜状シール材の第 2 の製造方法は、 有機系バイ ンダー と しての樹脂 と、 前記樹脂用溶剤ま た は分散媒と を混合し、  In a second method for producing a sheet-like sealing material according to the present invention, a resin as an organic binder is mixed with the resin solvent or the dispersion medium,
得 ら れたバイ ンダー混合液を、 基材繊維か ら なる不織布 に、 該不織布内部に  The obtained binder mixed solution is applied to a non-woven fabric made of the base fiber and the inside of the non-woven fabric.
存在する気体を追い 出す と と も に含浸させ、 Expelling the existing gas and impregnating it,
上記混合液が含浸さ れた不織布か ら 少な く と も一部の溶 剤または分散媒を揮散 · 除去 し、  At least a part of the solvent or dispersion medium is volatilized and removed from the non-woven fabric impregnated with the above mixed solution,
次いで こ の不織布を加熱圧縮 して、 上記樹脂を硬化 さ せ てシー ト状シール材を得る こ と を特徴と している。  Subsequently, the nonwoven fabric is heated and compressed, and the resin is cured to obtain a sheet-like sealing material.
本発明に係る上記何れの シー 卜状シール材の製造方法に おいて も、 上記基材繊維が非石綿系繊維であ る こ とが好ま し レ 。  In any of the above-described methods for producing a sheet-like sealing material according to the present invention, it is preferable that the base fiber is a non-asbestos fiber.
本発明に係る上記何れの方法にお いて も、 上記不織布が フ ェル ト状であ る こ とが好ま し い。  In any of the above methods according to the present invention, it is preferable that the nonwoven fabric is in a felt shape.
本発明に係 る 上記何れの方法にお いて も、 上記バイ ンダ 一混合液が充填剤を含む こ とが好ま し い。  In any of the above methods according to the present invention, it is preferable that the binder-mixture liquid contains a filler.
本発明に係る 上記何れの方法において も、 不織布内部に 存在する気体を追い 出す と と も にバイ ンダー混合液を含浸 させる工程 を、 あ ら か じ め不織布を圧縮 した ま まバイ ンダ 一混合液中 に浸漬するか、 バイ ンダー混合液中で不織布を 圧縮 した上、 こ れをバイ ンダー混合液中 にて 自発復元さ せ る こ と に よ り 行な う こ とが好ま し い。 In any of the above methods according to the present invention, the step of purging gas present inside the nonwoven fabric and impregnating with the binder mixed solution is performed by previously compressing the nonwoven fabric and then mixing the binder one mixed solution. Immersed in a non-woven fabric It is preferred to do this by compressing and then spontaneously restoring this in a binder mixture.
本発明 に係 る 上記何れの方法において も 、 不織布内部 に 存在する気体を追い 出す と と も にバイ ンダー混合液を含浸 させる工程を、 バイ ンダー混合液を不織布に高圧噴霧する こ と によ り 行な う こ とが好ま し い。  In any of the above methods according to the present invention, the step of driving out the gas present inside the nonwoven fabric and impregnating with the binder mixed solution is performed by spraying the binder mixed solution onto the nonwoven fabric under high pressure. It is preferable to do it.
本発明 に係る 上記何れの方法において も 、 不織布内部に 存在する 気体を追い 出す と と も にパイ ンダー混合液を含浸 させる工程 を、 減圧容器に不織布を入れ容器内部を減圧下 に し たの ちノ イ ンダー混合液を注入する こ と に よ り 行な う こ とが好ま し い。  In any of the above methods according to the present invention, the step of driving out the gas present inside the nonwoven fabric and impregnating the mixture with the binder is performed by placing the nonwoven fabric in a reduced-pressure container and reducing the pressure inside the container. It is preferable to do this by injecting a mixture of the nozzles.
本発明 に係 る 上記 シー ト 状 シール材の 製造方法 に よ れ ば、 強度異方性がな く 、 配合する繊維種に制限がな く 、 高 温条件下でガス や液体 の シ一ル に長期間好適 に使用 し う る、 シー ト状シール材が得 ら れる。 図面の簡単な説明 図 1 は、 本発明の一実施態様で好ま し く 用 い られる 、 不 織布圧縮 一バイ ンダー混合液含浸ー不織布 自発復元—付着 量設定の各操作 を連続 して行 う こ とができ る ロール搬送式 含浸機の模式説明図であ る。  According to the method for producing a sheet-like sealing material according to the present invention, there is no strength anisotropy, there is no limitation on the type of fiber to be blended, and gas and liquid sealing can be performed under high temperature conditions. A sheet-like sealing material that can be suitably used for a long period is obtained. BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 shows successive steps of nonwoven cloth compression, one-binder mixed liquid impregnation-nonwoven cloth, spontaneous restoration, and setting of adhesion amount, which are preferably used in one embodiment of the present invention. FIG. 3 is a schematic explanatory view of a roll-conveying type impregnating machine that can perform this.
図 2 は、 本発明の一実施態様で好ま し く 用 い られる 、 バ ィ ンダー混合液中での不織布圧縮一バイ ング一混合液含浸 ー不織布 自発復元一付着量設定の各操作を連続して行 う こ と のできるベル ト搬送式含浸機の模式説明図である 。 FIG. 2 shows the impregnation of a nonwoven fabric, a binder and a mixture in a binder mixture, which is preferably used in one embodiment of the present invention. FIG. 4 is a schematic explanatory view of a belt transport type impregnating machine capable of continuously performing each operation of spontaneous non-woven fabric spontaneous restoration and adhesion amount setting.
図 3 は、 本発明の一実施態様で好ま し く 用 い られる 高圧 噴霧含浸機の模式説明図であ る。  FIG. 3 is a schematic explanatory view of a high-pressure spray impregnating machine preferably used in one embodiment of the present invention.
図 4 は、 図 3 に示す高圧噴霧含浸機において、 メ ッ シュ 状基台の下方に吸引装置を設けた態様を示す図であ る。  FIG. 4 is a diagram showing an embodiment in which a suction device is provided below the mesh base in the high-pressure spray impregnator shown in FIG.
【符号の説明】  [Explanation of symbols]
1 不織布  1 Non-woven fabric
1 a 、 2 バイ ンダー混合液  1a, 2 binder mixture
3 含浸槽  3 Impregnation tank
4 (上部) 圧縮ロール  4 (Upper) Compression roll
4 a (上部) 圧縮 ロ ール と対 と な る (下部) 圧縮 口 一ル  4a (Upper) Compression roll (lower) Combination with compression roll
5 , 6 絞 り · 駆動ロール  5, 6 Squeezing · Drive roll
7 , 8 送出 ロール  7, 8 Outgoing roll
1 0 ロール搬送式含浸機  10 Roll impregnation machine
2 0 ベル ト · メ ッ シュ搬送式含浸機  20 Belt mesh transport impregnator
2 1 , 2 2 搬送ベル ト  2 1, 2 2 Transfer belt
2 5 a , 2 6 a 上下送出 ロール  25 a, 26 a Vertical delivery roll
2 5 b 自発復元化ロール  2 5 b Spontaneous restoration role
2 6 b 、 2 6 c 補助ロール  26b, 26c auxiliary roll
3 0 高圧噴霧含浸機  30 High pressure spray impregnation machine
3 O A 高圧噴霧含浸機  3 O A high pressure spray impregnator
3 1 メ ッ シュ基台 3 2 a 噴霧ノ ズル 3 1 Mesh base 3 2a Spray nozzle
3 3 吸引装置  3 3 Suction device
発明を実施する ための最良の形態 BEST MODE FOR CARRYING OUT THE INVENTION
【発明の具体的説明】 DETAILED DESCRIPTION OF THE INVENTION
以下、 本発明 に係る シー ト状シール材の製造方法につ い て具体的 に説明する。  Hereinafter, the method for producing a sheet-like sealing material according to the present invention will be specifically described.
本発明 に係 る シー ト 状シール材の第 1 の製造方法では、 有機系バイ ンダー と してのゴム材 と、 ゴム薬品 と、 前記 ゴム材用溶剤または分散媒と を混合し、  In a first method for producing a sheet-like sealing material according to the present invention, a rubber material as an organic binder, a rubber chemical, and the rubber material solvent or dispersion medium are mixed.
得 ら れたバイ ンダー混合液を、 基材繊維か ら なる不織布 に、 該不織布内部に存在する気体を追い 出す と と も に含浸 させ、  The obtained binder mixed solution is impregnated into a nonwoven fabric made of a base fiber while expelling gas present inside the nonwoven fabric,
上記混合液が含浸さ れた不織布か ら 少な く と も一部の溶 剤または分散媒を揮散 · 除去し、  At least a part of the solvent or dispersion medium is volatilized and removed from the nonwoven fabric impregnated with the above mixed solution,
次いで こ の不織布を加熱圧縮 して、 上記ゴム材を加硫さ せてシー ト 状シール材を製造している。  Next, the nonwoven fabric is heated and compressed, and the rubber material is vulcanized to produce a sheet-like sealing material.
また、 本発明 に係る シー ト状シール材の第 2 の製造方法 では、 上記第 1 の製造方法にお ける上記バイ ンダー混合液 と して、 有機系バイ ンダー と しての樹脂 と、 該樹脂用 の溶 剤または分散媒 と を混合 し、 得 ら れたバイ ンダー混合液を 用 い る点以外は、 基本的には、 上記第 1 の製造方法 と 同様 であ る。 すなわち 、 本発明の シー ト状シール材の製造方法では、 従来の ジ ョ イ ン ト シ一 ト の製法であ る カ レ ンダ一ロール製 法と は異な り 、 基材繊維 と して、 不織布を用 いる点、 お よ び不織布にバイ ンダー混合液を含浸させる際に、 不織布中 の気体を強制的に追い 出 して、 ノ イ ンダ一混合液で満た さ れた不織布中 には気体が存在 しないよ う に している 点な ど に特徴があ り 、 こ の よ う に バイ ン ダー混合液 ( コ ン ノ\° ゥ ン ド) を不織布に含浸する と と も に気体を強制的に追出 した 後、 上記の よ う に不織布に含浸されているバイ ンダー混合 液中 の溶剤成分あ る いは分散媒を揮散除去 し、 次いで加熱 圧縮成形する こ と によ り 、 ガス、 液体に対する長期の シー ル性に著 し く 優れ、 かつ、 強度異方性のない シー ト状シ一 ル材が製造可能 となっ ている。 Further, in the second method for producing a sheet-like sealing material according to the present invention, the resin as an organic binder is used as the binder mixture in the first production method; The method is basically the same as the above-mentioned first production method, except that a mixed solvent and a dispersion medium are used, and the obtained binder mixture is used. That is, in the method for producing a sheet-like sealing material of the present invention, unlike the calendar roll production method which is a conventional method for producing a joint sheet, a nonwoven fabric is used as the base fiber. When impregnating the non-woven fabric with the binder mixture, the gas in the non-woven fabric is forcibly driven out, and the non-woven fabric filled with the non-woven fabric contains gas. It is unique in that it does not exist. In this way, impregnating the non-woven fabric with a binder mixture (container) and forcing gas into the non-woven fabric After being extruded, the solvent component or dispersion medium in the binder mixed solution impregnated in the non-woven fabric as described above is volatilized and removed, followed by heating and compression molding to obtain gas and liquid. Remarkably excellent long-term sealability against It is now possible to manufacture sheet-like seal materials without anisotropy.
以下、 上記バイ ンダー混合液、 不織布、 含浸方法な ど に ついて順次詳述する。  Hereinafter, the binder mixed solution, the nonwoven fabric, the impregnation method, and the like will be sequentially described in detail.
<バイ ンダー混合液 >  <Binder mixture>
ノ' ィ ンダー混合液には、 上記のよ う に含まれる有機系ノ イ ンダ一がゴム材の場合と樹脂の場合とがあ り 、 さ ら に は その両者が含まれていて も よ く 、 これ ら 有機系バイ ンダー は、 シー ト 状シール材のシ一ル性能向上に寄与する。  The above-mentioned organic mixture may be a rubber material or a resin, and may contain both of them. However, these organic binders contribute to improving the sealing performance of the sheet-like sealing material.
こ の有機系バイ ンダーがゴム材の場合には、 バイ ンダー 混合液には、 ゴム材の他、 ゴム薬品、 ゴム材用溶剤ま たは 分散媒が含まれ、 さ ら に必要に よ り 充填剤な どが含まれて いて も よ い。 また、 こ の有機系バイ ンダーが樹脂の場合に は、 バイ ンダー混合液に は、 樹脂の他、 樹脂用溶剤ま たは 分散媒が含まれ、 さ ら に必要によ り 充填剤な どが含まれて いて も よ い。 When the organic binder is a rubber material, the binder mixture contains a rubber chemical, a solvent or a dispersion medium for the rubber material in addition to the rubber material, and is further filled as necessary. Agents may be included. Also, when this organic binder is resin, In addition, the binder mixture contains a resin solvent or a dispersion medium in addition to the resin, and may further contain a filler if necessary.
ゴム材 と しては、 例え ば、 天然ゴム、 イ ソ プレンゴム、 ブタ ジエンゴム、 スチ レンブタ ジエンゴム、 ウ レタ ンゴム、 ク ロ ロ プ レ ンゴム、 ア ク リ ロニ ト リ ルブタ ジエンゴム、 ブ チルゴム、 エチ レ ンプロ ピ レ ンゴム、 ア ク リ ルゴム、 シ リ コ ンゴム、 フ ッ 素ゴムな どが挙げられる。  Examples of the rubber material include natural rubber, isoprene rubber, butadiene rubber, styrene butadiene rubber, urethane rubber, chloroprene rubber, acrylonitrile butadiene rubber, butyl rubber, and ethylene rubber. Examples include pyrene rubber, acryl rubber, silicone rubber, and fluorine rubber.
ま た、 樹脂 と しては、 例えば、 尿素系、 メ ラ ミ ン系、 ポ リ エステル系、 エポキシ系、 フ エ ノ ール系等が挙げられる。 本発明においては、 これ らバイ ンダ一の種類は特に制限さ れず、 また 1 種または 2 種以上組み合わせて用 いても よ い。  Examples of the resin include a urea-based resin, a melamine-based resin, a polyester-based resin, an epoxy-based resin, and a phenol-based resin. In the present invention, one kind of the binder is not particularly limited, and one kind or a combination of two or more kinds may be used.
上記ゴム薬品 と しては、 従来よ り 公知の も の を広 く 使用 でき、 例えば、 加硫剤、 加硫助剤、 促進剤、 老化防止剤等、 さ ら に必要 に よ り 、 増粘剤、 感熱ゲル化剤 (感熱剤) 、 界 面活性剤な どを用 いて も よ い。  As the above rubber chemicals, conventionally known rubber chemicals can be widely used, for example, vulcanizing agents, vulcanizing aids, accelerators, anti-aging agents, and the like. Agents, heat-sensitive gelling agents (thermosensitive agents), surfactants, etc. may be used.
増粘剤 と しては、 例え ば、 ポ リ ビエルアルコ ール系、 ポ リ ア ク リ ル酸系、 ポ リ メ タ ク リ ル酸系、 ポ リ ア ク リ ルア ミ ド 系等の合成高分子お よびその アルギ ン酸塩 ; カゼイ ン、 ゼラチン、 ク ァーガム等の天然、 半合成高分子 ; な どが挙 げ ら れる。  Examples of the thickener include synthetic alcohols such as polyvinyl alcohol, polyacrylic acid, polymethacrylic acid, and polyacrylamide. Molecules and their alginates; natural and semi-synthetic polymers such as casein, gelatin, and guar gum; and the like.
感熱ゲル化剤 (感熱剤) と しては、 例えば、 ポ リ ビ二ル メ チルエーテルの他、 シ リ コ ー ン系、 ポ リ アルキレ ンォキ シ ド誘導体系等が挙げ ら れる。 界面活性剤と しては、 ァニオ ン系、 ノ 二オン系、 カ チォ ン系、 両性な ど従来よ り 公知の も の を広 く 使用 でき、 例え ば、 カルボ ン酸塩系、 スルホン酸塩系、 硫酸塩系、 リ ン酸 塩系な どの ァニオ ン性界面活性剤 ; ポ リ ォキシエチ レ ン誘 導体系、 多価アルコ ール系誘導体等の ノ 二オ ン系界面活性 剤 ; アルキルア ミ ン塩系、 第 4 ア ンモニゥム塩系等のカ チ ォン性界面活性剤 ; 等が挙げ ら れる。 Examples of the heat-sensitive gelling agent (thermosensitive agent) include, in addition to polyvinyl methyl ether, silicones, polyalkylene oxyside derivatives, and the like. As the surfactant, a wide variety of known surfactants such as anionic, nonionic, cationic and amphoteric can be used.For example, carbonates, sulfonates and the like can be used. Surfactants such as phenol-based, sulfate-based, and phosphate-based surfactants; nonionic surfactants such as polyoxyethylene derivative-based and polyvalent alcohol-based derivatives; alkylamines And cationic surfactants such as salt and quaternary ammonium salt; and the like.
こ の よ う な感熱ゲル化剤 (感熱剤) は 、 ノ イ ンダー 1 0 0 重量部に対 して、 通常 1 〜 1 0 重量部、 好ま し く は 2 〜 5 重量部の量で含まれる こ とが望ま し い,  Such a thermosensitive gelling agent (thermosensitive agent) is usually contained in an amount of 1 to 10 parts by weight, preferably 2 to 5 parts by weight, based on 100 parts by weight of the binder. This is desirable,
ま た、 こ の よ う な界面活性剤は、 バィ ンダー混合液中 の 固形分 1 0 0 重量部に対して、 通常、 0 . 2 〜 5 重量部、 好ま し く は 0 . 4 ~ 4 重量部の量で含まれる こ とが望ま し い。  Such a surfactant is usually used in an amount of 0.2 to 5 parts by weight, preferably 0.4 to 4 parts by weight, based on 100 parts by weight of the solid content in the binder mixture. It is desirable that it be contained in parts.
充填剤は、 必要によ り 用 い ら れ、 シー 卜状シール材の応 力緩和特性およびシール性能向上等に寄与し、 このよ う な 充填剤 と して、 具体的に は、 例えば、 夕ルク 、 マイ 力 、 ク レー、 酸化マ グネ シウム、 炭酸カルシゥム等の無機粉体が 挙げ ら れる 。 本発明では、 これ ら 充填剤は、 1 種または 2 種以上組み合わせて用 い られる 。  The filler is used as needed, and contributes to the stress relaxation property of the sheet-like sealing material and the improvement of the sealing performance. As such a filler, specifically, for example, Inorganic powders such as luc, myric, clay, magnesium oxide, calcium carbonate and the like. In the present invention, these fillers are used alone or in combination of two or more.
本発明 にお いては、 上記ゴム材お よび Zまたは樹脂は、 バイ ンダー混合液中の固形分 と不織布 と の合計重量を 1 0 0 重量% と した場合に、 合計で、 通常、 5 〜 4 0 重量%、 好ま し く は 1 0 〜 3 0 重量% の量で用 い ら れる 。 こ の ノ ィ ンダ一 とな る ゴム材ぉよ び/または樹脂含量が 5 重量%未 満では、 不織布 を構成する繊維表面および必要によ り 用 い ら れる充填剤表面を十分に覆 う こ とができないか、 あ る い は不織布内部の空隙に十分にバイ ンダー混合液 (コ ンパ ゥ ン ド ) を充填する こ とができな く な り 、 結果 と してシー ト 状 シ ール材 の シ ール性能が低下す る こ と が あ る (表 1 参 照) 。 一方ゴム材お よ び Z ま たは樹脂含量が 4 ' 0 重量 % を 超え る と 、 得 ら れる シー ト 状シール材中 に含まれる 、 熱履 歴に よ る硬化や収縮が生 じやすい成分が過多 とな り 、 結果 と し てシー ト 状シール材 と して も熱履歴に よ る硬化、 割れ が生 じやす く な り 、 長期間優れたガス シール性、 液体シ一 ル性な どの特性が保持できに く く なる こ とがあ る。 In the present invention, when the total weight of the solid content in the binder mixed solution and the nonwoven fabric is 100% by weight, the rubber material and Z or the resin are usually 5 to 4% in total. It is used in an amount of 0% by weight, preferably from 10 to 30% by weight. This noise If the rubber material and / or resin content is less than 5% by weight, it will not be possible to sufficiently cover the surface of the fibers constituting the nonwoven fabric and the surface of the filler used as necessary. Or, the voids inside the nonwoven fabric cannot be sufficiently filled with the binder mixture, and as a result, the seal of the sheet-like seal material is consequently lost. Performance may be degraded (see Table 1). On the other hand, if the content of rubber and / or Z or resin exceeds 4'0% by weight, the components contained in the obtained sheet-like sealing material that are liable to undergo hardening or shrinkage due to heat history. As a result, even if a sheet-like sealing material is used, hardening and cracking due to heat history are likely to occur, and long-term excellent gas sealing properties, liquid sealing properties, etc. It may become difficult to maintain the characteristics.
充填剤を用 い る場合、 バィ ンダー混合液中の固形分 と不 織布 と の合計 1 0 0 重量% 中 に、 通常、 8 0 重量%以下、 好ま し く は 5 〜 8 0 重量% の量で用 い ら れる 。 こ の充填剤 含量が、 8 0 重量% を超える と、 充填剤表面を十分に覆 う ため のノ ィ ンダー量が不足 し、 シー ト状シ一ル材の シール 性能が低下する こ とがあ る。 なお、 こ の充填剤含量が 5 重 量% 未満では、 その添加効果であ る シー ト状シール材の応 力緩和特性お よびシール性能向上等はあ ま り 期待できな く なる 。  If a filler is used, it is usually less than 80% by weight, preferably 5 to 80% by weight, in a total of 100% by weight of the solid content and nonwoven fabric in the binder mixture. Used in quantity. If the filler content exceeds 80% by weight, the amount of the binder for sufficiently covering the filler surface may be insufficient, and the sealing performance of the sheet-like sealing material may be reduced. You. If the filler content is less than 5% by weight, the effect of adding the filler, such as the stress relaxation property of the sheet-like sealing material and the improvement of the sealing performance, cannot be expected much.
こ のよ う な種々 の成分を含むバイ ンダー混合液は、 流動 状態で使用 さ れ、 ラテ ッ ク ス状態、 溶液状態等が挙げ ら れ、 具体的には、 例えば、 溶液ゴム (固形ゴム と溶剤と の混合 物) 、 液状ゴム (例え ば、 液状シ リ コ ー ンゴム、 液状 フ ッ 素ゴムな どの よ う に、 溶剤な し の単体にて液状の ゴム) 、 ゴム ラ テ ッ ク ス、 溶液樹脂、 樹脂ェマルジ ヨ ン等と して使 用 さ れる 。 ま た、 これ ら バイ ンダー混合液は、 1 種ま たは 2 種以上の成分を組み合わせて使用 しても よい。 A binder mixture containing such various components is used in a fluidized state, and may be in a latex state or a solution state. Specifically, for example, a solution rubber (solid rubber and solid rubber) are used. Mixing with solvent Material), liquid rubber (for example, liquid silicone rubber, liquid fluoro rubber, liquid rubber without solvent alone), rubber latex, solution resin, resin Used as emulsion. These binder mixtures may be used alone or in combination of two or more.
こ の よ う なバイ ンダー混合液の調製法は、 特に限定さ れ ず、 従来よ り 公知の方法を採用すればよい。  The method for preparing such a binder mixture is not particularly limited, and a conventionally known method may be employed.
<不織布 >  <Non-woven fabric>
不織布は、 シー ト 状シール材の基材であ り その強度向上 に寄与するが、 こ のよ う な不織布 と しては、 石綿系で も非 石綿系で も使用 でき、 人体 · 環境への安全性の見地を よ り 考慮する と好ま し く は非石綿系不織布が用 い ら れ、 こ の よ う な非石綿系不織布の う ち で も 、 例えば、 p — ァ ラ ミ ド繊 維、 フ ッ 素樹脂繊維、 炭素繊維、 セ ラ ミ'ッ ク繊維、 鉱物系 繊維な ど、 高温下での強度が高い繊維を、 単独ある い は複 数組み合わせて製作した ものが好適に使用 でき る。  Nonwoven fabric is a base material for sheet-like sealing materials and contributes to the improvement of its strength. Such nonwoven fabric can be used in both asbestos-based and non-asbestos-based materials, and is useful for humans and the environment. From the viewpoint of safety, non-asbestos nonwoven fabrics are preferably used, and such non-asbestos nonwoven fabrics include, for example, p-aramid fiber, Fibers that have high strength at high temperatures, such as fluororesin fibers, carbon fibers, ceramic fibers, and mineral fibers, can be suitably used alone or in combination. .
こ のよ う な不織布の製法には、 湿式、 乾式、 スパ ン レー ス、 スノ^ ンポ ン ド、 メ ル ト ブロ ー ン、 ニー ドルパンチ、 ス テ ツ チボ ン ド な どの種々 の製法があ る が、 本発明で用 い ら れる不織布の種類は本製法に制限される も のではない。  There are various methods for producing such non-woven fabrics, such as wet, dry, span lace, snow pour, melt blown, needle punch, and state bond. However, the type of nonwoven fabric used in the present invention is not limited to the present production method.
ま た得 ら れた不織布の性状 と しては、' ニー ドルパ ンチフ エル ト状、 湿式抄造不織布状な どが好ま し い。  Further, as properties of the obtained nonwoven fabric, it is preferable to use a needle punch felt shape, a wet-laid nonwoven fabric shape, or the like.
本発明では、 シー ト状シール材の強度向上に寄与する 上 記不織布は、 バイ ンダー混合液中 の固形分 と、 不織布 (あ る い は不織布用繊維) と の合計 1 0 0 重量% 中 に、 通常、 5 〜 8 0 重量%、 好ま し く は 1 0 〜 7 0 重量% の量で用 い ら れる。 こ の不織布 (あ る いは繊維) 含量が、 5 重量%未 満では、 実使用 に耐え う る シー ト 強度を得る こ とができず、 一方 8 0 重量 % を超え る と不織布含量が増大する に連れ て、 不織布中 の空隙が多 く な り 、 該空隙に含浸 · 充填すベ きバイ ンダー混合液量不足 とな り 、 十分な シール性能の シ 一 ト 状シール材が得 ら れな く なる傾向があ る。 In the present invention, the above-mentioned nonwoven fabric which contributes to the improvement of the strength of the sheet-like sealing material is obtained by combining the solid content in the binder mixed solution with the nonwoven fabric Or a nonwoven fabric fiber) in a total amount of 100% by weight, usually in an amount of 5 to 80% by weight, preferably 10 to 70% by weight. If the content of the nonwoven fabric (or fiber) is less than 5% by weight, the sheet strength sufficient for practical use cannot be obtained, while if it exceeds 80% by weight, the content of the nonwoven fabric increases. As a result, the voids in the nonwoven fabric increase, the amount of the binder mixed liquid to be impregnated and filled in the voids becomes insufficient, and a sheet-like sealing material having sufficient sealing performance cannot be obtained. It tends to be.
<バイ ンダー混合液の調製工程 (工程 1 ) > 本発明では、 上記バイ ンダー、 バイ ンダー用溶媒また は 分散媒、 および必要に よ り 用 い ら れる充填剤、 およびバイ ンダ一 と してゴム を使用する場合はゴム薬品 (例 : 加硫剤、 加硫助剤、 促進剤、 老化防止剤等) を攪拌容器に入れ、 均 一になる まで攪拌 · 混合 し、 バイ ンダー混合液 (コ ンパ ゥ ン ド ) を調製する 。 こ の際、 必要によ り 、 増粘剤、 感熱ゲ ル化剤 (感熱剤) 、 界面活性剤な ど を配合 して も よ い。 こ の よ う な攪拌 · 混合は、 通常、 常温 ( 2 0 〜 3 0 °C: ) 、 常 圧下に行われ、 必要によ り 、 配合成分が化学変化な ど生 じ ない程度の温度に加熱 して も よ い。  <Step of Preparing Binder Mixture (Step 1)> In the present invention, the binder, the solvent or the dispersion medium for the binder, the filler optionally used, and the rubber as the binder are used. When using rubber, put rubber chemicals (eg, vulcanizing agent, vulcanizing aid, accelerator, anti-aging agent, etc.) into a stirring vessel, stir and mix until uniform, and mix the binder mixture (Comparator). )). At this time, if necessary, a thickener, a heat-sensitive gelling agent (heat-sensitive agent), a surfactant and the like may be added. Such stirring and mixing are usually performed at normal temperature (20 to 30 ° C:) and normal pressure, and if necessary, heating to a temperature at which the components do not change chemically. You may do it.
<バイ ンダー混合液の含浸 と気体の追出 し工程 (工程 2 ) > 本発明では、 次いで、 該不織布内部に存在する気体を強 制的 に追 い出すと と も に、 上記の よ う に して得 られたバイ ンダー混合液を、 基材繊維か ら なる不織布に含浸させる 。  <Step of Impregnating Binder Mixture and Eliminating Gas (Step 2)> In the present invention, subsequently, the gas present inside the nonwoven fabric is forcibly expelled, and as described above. The binder mixed solution obtained as described above is impregnated into a nonwoven fabric made of a base fiber.
こ こで、 シー ト 状シール材に優れた シール性能を保有さ せる ため に は、 不織布内部に存在する空隙を完全にバイ ン ダー混合液にて置換し満たす必要があ る。 Here, the sheet-shaped sealing material has excellent sealing performance. In order to achieve this, it is necessary to completely replace and fill the voids present inside the nonwoven fabric with the binder mixture.
こ のよ う に該空隙を完全にバイ ンダー混合液で満たする ため に、 本発明では、 不織布内部に存在する気体 (通常空 気) を強制的 に追い出す と と も にバイ ンダ一混合液を含浸 させる工程 を、 下記①〜④の何れかに記載の方法で行 う こ とが望ま し い。  In order to completely fill the voids with the binder mixture in this way, in the present invention, the gas (usually air) present inside the nonwoven fabric is forcibly expelled and the binder-mixture is removed. It is desirable that the step of impregnation is performed by any of the following methods (1) to (4).
すなわち 、 ① : あ ら か じめ不織布を圧縮した状態でバイ ンダー混合液中 に浸漬 し、 これをバイ ンダー混合液中 にて 自発復元さ せる こ と に よ り 行 う 方法 ( 「事前圧縮液中 自 発 復元法」 と も言 う 。 ) ;  In other words, ①: A method in which the nonwoven fabric is compressed and immersed in a binder mixed solution, and then spontaneously restored in the binder mixed solution (“Pre-compressed liquid”). "Spontaneous restoration method".);
② : バイ ンダー混合液中で不織布を圧縮した上、 こ れを バイ ンダー混合液中 にて 自発復元させる こ と によ り 行な う 方法 (「液中圧縮 自発復元法」 と も言う 。) ;  ②: A method in which the nonwoven fabric is compressed in a binder mixed solution and then spontaneously restored in the binder mixed solution (also referred to as the “submerged compression spontaneous restoration method”). ;
③ : パイ ンダ一混合液を不織布に高圧噴霧する こ と によ り 行な う 方法 ( 「高圧噴霧法」 と も言う 。 ) ; あ る いは、 ③: A method in which a mixture of the binder and the non-woven fabric is sprayed onto the non-woven fabric by high pressure (also referred to as “high pressure spraying”);
④ : 減圧容器に不織布を入れ容器内部を減圧下に し たの ちバイ ンダー混合液を注入する こ と によ り 行な う方法 (「減 圧注入法、 減圧置換法」 と も言う 。 ) ; が好ま し い。 ④: A method in which a nonwoven fabric is placed in a reduced-pressure container, the inside of the container is reduced in pressure, and then a binder mixed solution is injected (also referred to as a “reduced-pressure injection method or a reduced-pressure replacement method”). Is preferred.
こ の①の方法 (事前圧縮液中 自発復元法) では、 不織布 を予め加圧 · 圧縮 して気体の存する空隙部を小さ く する こ とで気体を押出 し、 空隙部が低減 · 除去さ れた不織布 を、 パイ ンダー混合液中 に浸漬 し、 バイ ンダー混合液中で不織 布への加圧を開放する と、 不織布は原形状に 自発復元 して く る 。 こ の際、 不織布内部は負圧状態 とな り 、 不織布内 に バイ ンダー混合液が吸引 さ れて浸入 し、 不織布を構成する 繊維間隙 をバイ ン ダー混合液で完全 に満たす こ と がで き る。 In this method (pre-compressed liquid spontaneous recovery method), the non-woven fabric is pre-pressurized and compressed to reduce the voids in which the gas is present, thereby extruding the gas to reduce and eliminate the voids. The nonwoven fabric is immersed in the binder mixture and the pressure on the nonwoven is released in the binder mixture, and the nonwoven fabric returns to its original shape spontaneously. come . At this time, the inside of the nonwoven fabric is in a negative pressure state, and the binder mixed solution is sucked into the nonwoven fabric and penetrates, so that the fiber gaps constituting the nonwoven fabric can be completely filled with the binder mixed solution. You.
上記②の方法 (液中圧縮 自発復元法) では、 不織布をバ ィ ンダー混合液中 に浸漬 した状態で、 不織布の加圧 · 圧縮 と、 加圧開放に よ る不織布の 自発復元を行 う 点以外は、 上 記①の方法 と 同様であ る。  In method (2) above (compression in liquid spontaneous restoration method), the nonwoven fabric is immersed in a binder mixture, and the nonwoven fabric is pressurized and compressed, and the nonwoven fabric is spontaneously restored by pressure release. Other than the above, it is the same as the above method.
ま た、 ③の方法 (高圧噴霧法) では、 不織布表面に高圧 噴霧さ れたバイ ンダー混合液を、 不織布裏面に設けた吸引 装置によ り 減圧 · 吸引する よ う に して、 バイ ンダー混合液 の噴霧 · 含浸を効率化 して も よ い。  In the method (3) (high-pressure spray method), the binder mixed solution sprayed at high pressure on the surface of the nonwoven fabric is depressurized and suctioned by the suction device provided on the back surface of the nonwoven fabric. Spraying and impregnating the liquid may be more efficient.
ま た、 ④の方法 (減圧注入法) は、 減圧下にて不織布内 部の空隙 をバイ ンダー混合液に置換する方式であ り 、 容器 内を減圧下に保持する と 、 不織布内の空隙部 も減圧下 とな る。 その よ う な減圧下の容器内に、 バイ ンダー混合液を注 入する と 、 バイ ンダー混合液は、 負圧状態の容器内 に拡散 する と共に不織布内空隙部に も浸入 し、 結果的 に、 不織布 内繊維間隙 をバイ ンダー混合液で満たす こ とができ る 。 こ のよ う な減圧注入法④は、 例え ば、 不織布寸法が比較的小 さ い場合、 大型設備を必要とせず有効である。  In addition, the method (1) (vacuum injection method) is a method in which the voids inside the nonwoven fabric are replaced with a binder mixed solution under reduced pressure. When the inside of the container is kept under reduced pressure, the voids in the nonwoven fabric are reduced. Is also reduced in pressure. When the binder mixture is poured into the container under such reduced pressure, the binder mixture diffuses into the container under negative pressure and also penetrates into the voids in the non-woven fabric. The fiber gap in the nonwoven fabric can be filled with the binder mixture. Such a vacuum injection method II is effective, for example, when a non-woven fabric is relatively small in size, without requiring large-scale equipment.
なお、 本発明では、 圧縮さ れた不織布の復元方法は、 上 記の よ う に加圧開放に よ る 自発復元が好ま し いが強制的に 復元させて も よ い。 また、 不織布 とバイ ンダー混合液 とのな じ みに く さ あ る い はバイ ンダー混合液の粘度によ り 上記①〜④の方法 (操 作) を 1 回行 う だけでは不織布中へのバイ ンダー混合液の 含浸量が不十分であ る場合には、 該方法を複数回繰 り 返 し、 不織布を構成する繊維間隙をバイ ンダー混合液で完全に満 たすこ とが望ま し い。 In the present invention, as a method for restoring the compressed nonwoven fabric, as described above, spontaneous restoration by release of pressure is preferable, but restoration may be forcibly performed. In addition, depending on the compatibility between the nonwoven fabric and the binder mixture or the viscosity of the binder mixture, the method (operation) (1) to (4) above may be performed only once to obtain the nonwoven fabric. When the impregnation amount of the binder mixed solution is insufficient, it is desirable to repeat the method a plurality of times to completely fill the interstices of the fibers constituting the nonwoven fabric with the binder mixed solution.
また、 不織布にバイ ンダー混合液を含浸さ せよ う と して も、 不織布が撥水性を有 しバイ ンダー混合液をはじ く よ う な場合には、 あ ら 力 じ め上記 「バイ ンダー混合液の調製ェ 程」 にて、 バイ ンダー混合液に界面活性剤を配合してお く こ とが望ま し い。  Further, even if the nonwoven fabric is impregnated with the binder mixed solution, if the nonwoven fabric has water repellency and repels the binder mixed solution, the binder mixed solution described above should be used. It is desirable to mix a surfactant into the binder mixture in the “Preparation process”.
また、 バイ ンダー混合液の粘度が低 く 、 不織布に含浸さ せたバイ ンダー混合液の一部が流出 して し ま い、 不織布内 部に再度空隙が生 じ る場合があ る。 こ の よ う な場合に は、 上記 「バイ ンダー混合液の調製工程」 においてバイ ンダー 混合液に増粘剤を配合 し、 バイ ンダー混合液の流動性 を低 下させてお く こ とが望ま しい。  Further, the viscosity of the binder mixed solution is low, so that a part of the binder mixed solution impregnated in the nonwoven fabric may flow out, and voids may be generated inside the nonwoven fabric again. In such a case, it is desirable to mix a thickener with the binder mixture in the above-mentioned “binder mixture preparation step” to reduce the fluidity of the binder mixture. New
本発明では、 こ のよ う に不織布内部にバイ ンダー混合液 を含浸させた後、 得 ら れたバイ ンダー混合液含浸不織布を 所定間隔に調整さ れた一対の ロ ール間 に揷通させる こ と に よ っ て、 バイ ンダー混合液の付着量 (含浸量) を所定量に 設定 (調整) する こ とが望ま し い。  In the present invention, after the binder mixed solution is impregnated inside the nonwoven fabric as described above, the obtained binder mixed solution-impregnated nonwoven fabric is passed between a pair of rolls adjusted at a predetermined interval. Therefore, it is desirable to set (adjust) the adhesion amount (impregnation amount) of the binder mixture to a predetermined amount.
次に、 こ のよ う な 「バイ ンダー混合液の含浸と気体の追 出 し工程」 につ いて、 該工程で好適な各種含浸機を用 いた 態様を、 図面を参照 しつつ さ ら に詳説する。 Next, regarding such a “step of impregnating the binder mixture and purging out the gas”, various suitable impregnating machines were used in the step. Embodiments will be described in more detail with reference to the drawings.
<図 1 >  <Figure 1>
本発明では、 例えば、 上記②の方法を採用する場合には、 図 1 に模式的に示すロール搬送式含浸機 1 0 を用 いて、 「不 織布圧縮一 バイ ンダー混合液含浸ー不織布 自 発復元一 付着 量設定」 の各操作を連続 して行 う こ と に よ り 、 上記含浸ェ 程を 自動化する こ とが可能であ る。  In the present invention, for example, when the above-mentioned method (1) is adopted, a roll-conveying type impregnating machine 10 schematically shown in FIG. It is possible to automate the above-mentioned impregnation process by continuously performing each operation of “Restoration-adhesion amount setting”.
こ の図 1 に示すロール搬送式含浸機 1 0 は、 バイ ンダー 混合液 2 が貯留さ れる含浸槽 3 と、 含浸槽 3 の手前外部に 設け ら れ、 不織布 1 を含浸槽 3 に送 り 出す送出 ロール 7 , 8 と 、 送出 さ れた不織布 1 を含浸槽 3 内 に導いて圧縮する 圧縮 ロール 4 と、 含浸槽 3 の後方外部に設け ら れ、 含浸槽 3 を通過 し た不織布 1 中 のバイ ンダー混合液量を調整する 一対の絞 り · 駆動ロール 5 , 6 と を備えてい る 。  The roll transfer type impregnating machine 10 shown in FIG. 1 is provided in the impregnating tank 3 in which the binder mixed liquid 2 is stored, and is provided outside the impregnating tank 3 in front of the impregnating tank 3. Delivery rolls 7 and 8, a compression roll 4 for guiding the delivered nonwoven fabric 1 into the impregnation tank 3 and compressing the same, and a non-woven fabric 1 provided outside the impregnation tank 3 and provided through the impregnation tank 3. A pair of squeezing and driving rolls 5 and 6 for adjusting the amount of the binder mixture are provided.
こ の ロール搬送式含浸機 1 0 では、 不織布 1 は、 送出 口 ール 7 , 8 を経て、 圧縮ロール 4 にて含浸槽 3 内に導かれ、 該含浸槽 3 内のバイ ンダー混合液 2 に浸漬さ れる と共に、 送出 ロ ール 7 , 8 と圧縮ロール 4 と一対の上下絞 り ' 駆動 ロール 5 , 6 と に よ り 緊張状態で保持 · 張設さ れなが ら 、 圧縮 ロ ール 4 にて下方方向のに押圧を受ける こ と によ り 圧 縮される。  In the roll transport impregnating machine 10, the nonwoven fabric 1 is guided into the impregnation tank 3 by the compression roll 4 through the discharge ports 7 and 8, and is mixed with the binder mixture 2 in the impregnation tank 3. While being immersed, the delivery rolls 7 and 8, the compression roll 4, and a pair of up-and-down squeezing drive rolls 5 and 6 hold and tension the tension of the compression roll 4. Compressed by receiving downward pressure at.
こ の際の不織布張力、 圧縮面圧な どは、 不織布の材質、 製法、 状態な ど に も よ り 異な り 一概に決定さ れないが、 不 織布の伸びが 1 〜 5 %生ずる よ う な張力、 あ る いは、 圧縮 時に元の基材の厚みの 1 0 〜 4 0 % の厚さ にできる よ う な 荷重を加える こ とが望ま しい。 The nonwoven fabric tension, compression surface pressure, etc. at this time differ depending on the material, manufacturing method, condition, etc. of the nonwoven fabric, and are not determined unconditionally, but the elongation of the nonwoven fabric will be 1 to 5%. High tension or compression Sometimes it is desirable to apply a load that can make the thickness 10 to 40% of the thickness of the original substrate.
こ のよ う な条件は、 これ ら ロールの回転速度や こ れ ら 口 ールの相互の位置関係な ど を適宜調整する こ と によ り 達成 でき、 ま た圧縮ロール 4 での不織布 1 の圧縮量を適宜調整 する こ とができる。  Such conditions can be achieved by appropriately adjusting the rotational speed of these rolls and the mutual positional relationship of these rolls, and the non-woven fabric 1 on the compression rolls 4 can be formed. The compression amount can be adjusted appropriately.
(なお、 不織布 1 を こ の よ う な緊張状態に保持する と、 過度に伸びて し ま う よ う な場合には、 後述する 図 2 に示す (If non-woven fabric 1 is stretched excessively when held in such a tensioned state, as shown in FIG. 2 described later,
「ベル ト · メ ッ シュ搬送式含浸機」 2 0 を用 いればよ い。 ) こ のよ う に含浸槽 3 内の圧縮 ロール 4 にて圧縮さ れた不 織布 1 は、 該圧縮ロール 4 を通過後、 圧縮ロール 4 に よ る 圧力か ら 開放さ れ、 上下絞 り · 駆動 ロール 5 , 6 に 向かつ て移動する過程で 自発復元する が、 こ の 自発復元過程では 不織布 1 内空隙部は負圧とな り 、 該空隙部に含浸層内のバ ィ ンダー混合液 2 を吸入 し、 自発復元 し た不織布 1 内の繊 維間 はバイ ンダー混合液 2 で満た さ れる (図示せず) 。 こ のよ う にバイ ンダー混合液で全ての繊維間空隙部が満た さ れた不織布 1 は、 含浸槽 3 の外部に設け ら れた一組の絞 りA belt-mesh transport impregnator 20 may be used. The nonwoven fabric 1 compressed by the compression roll 4 in the impregnation tank 3 in this way is released from the pressure by the compression roll 4 after passing through the compression roll 4 and squeezed up and down. The spontaneous restoration is performed in the process of moving toward the drive rolls 5 and 6, but in this spontaneous restoration process, the void in the nonwoven fabric 1 becomes negative pressure, and the binder mixed liquid in the impregnation layer is filled in the void. The space between the fibers in the nonwoven fabric 1 that has been inhaled and spontaneously restored is filled with the binder mixed solution 2 (not shown). The nonwoven fabric 1 in which all the inter-fiber spaces are filled with the binder mixed solution as described above is used as a set of squeezers provided outside the impregnation tank 3.
• 駆動 ロ ール 5 , 6 に挟持 (挿通) さ れて、 不織布 1 に含 浸 · 付着 してい るバイ ンダー混合液量は所定の範囲に調整 される。 なお こ のよ う な 「ベル ト · メ ッ シュ搬送式含浸機」 2 0 を複数台縦方向に設置する な ど して、 複数回不織布の バイ ンダー混合液含浸処理を繰 り 返すよ う に しても よ い。 • The amount of the binder mixture that is sandwiched (inserted) between the drive rolls 5 and 6 and impregnated and adhered to the nonwoven fabric 1 is adjusted to a predetermined range. In order to repeat the process of impregnating the nonwoven fabric with the binder mixed liquid multiple times, for example, by installing a plurality of such belt-mesh transfer impregnating machines 20 in the vertical direction. You may.
なお、 上記例では、 圧縮ロールが 1 個の場合を示し たが、 本発明は こ の よ う な態様に限定さ れず、 例えば、 図 1 中、 付番 4 a で示すよ う に、 圧縮ロール 4 と対になる よ う に不 織布 1 の下方に も圧縮ロ ールを設けて、 一対の圧縮ロール 4 , 4 a にて不織布 1 を圧縮 · 挟持する よ う に して も よ い。 ま た、 上下 1 対の圧縮ロ ールを、 複数組含浸槽 3 内 に設け て不織布の 「圧縮 /開放—含浸」 を繰 り 返させ、 含浸効率 を上げる よ う に して も よ レ (図示せず) 。 In the above example, one compression roll is shown. The present invention is not limited to such an embodiment. For example, as shown by reference numeral 4a in FIG. 1, the compression roll is also provided below the nonwoven cloth 1 so as to be paired with the compression roll 4. The nonwoven fabric 1 may be compressed and pinched by a pair of compression rolls 4 and 4a. Alternatively, a pair of upper and lower compression rolls may be provided in the impregnation tank 3 to repeat the “compression / opening-impregnation” of the nonwoven fabric to increase the impregnation efficiency. (Not shown).
ぐ図 2 >  Figure 2>
また、 本発明では、 上記②の方法 (液中圧縮 自発復元法) を採用する場合には、 図 2 に模式的に示すベル ト搬送式含 浸機 2 0 を用 いて、 「不織布圧縮 一バイ ンダー混合液含浸 ー不織布 自 発復元一付着量設定」 の各操作を連続して行 う こ と によ り 、 上記含浸工程 を 自動化する こ とが可能であ る。  Further, in the present invention, when the above method (1) (compression in liquid spontaneous restoration method) is adopted, a belt-conveying impregnator 20 schematically shown in FIG. The above impregnation process can be automated by successively performing the operations of “impregnating the mixed solution of the binder and the nonwoven fabric spontaneously restoring and setting the adhesion amount”.
こ の図 2 に示すベル ト搬送式含浸機 2 0 は、 バイ ンダー 混合液 2 が貯留される含浸槽 3 と、  The belt transfer type impregnating machine 20 shown in FIG. 2 includes an impregnating tank 3 in which the binder mixture 2 is stored,
含浸槽 3 の手前外部に設け ら れ、 不織布 1 を含浸槽 3 に 送 り 出す上下送出 ロール 2 5 a 、 2 6 a と、  Upper and lower delivery rolls 25 a and 26 a that are provided outside the impregnation tank 3 and send out the nonwoven fabric 1 to the impregnation tank 3.
送出 さ れた不織布 1 を含浸槽 3 内に導き、 圧縮する圧縮 ロール 4 と、  A compressed roll 4 for guiding the delivered nonwoven fabric 1 into the impregnation tank 3 and compressing the same.
含浸槽 3 の後方外部に設け ら れ、 含浸槽 3 を通過 した不 織布 1 中 のバイ ンダー混合液量を調整する一対の上下絞 り - 駆動ロール 5 , 6 と を備えてレ る。  A pair of upper and lower squeezing-drive rolls 5 and 6 are provided at the rear outside of the impregnation tank 3 and adjust the amount of the binder mixed liquid in the nonwoven fabric 1 that has passed through the impregnation tank 3.
こ のベル ト搬送式含浸機 2 0 には、 無限軌道のメ ッ シュ 状で も よ い 2 本の搬送ベル ト 2 1 , 2 2 が架け渡さ れてお り 、 上部搬送ベル ト 2 1 は、 上部送出 ロール 2 5 a と、 圧 縮ロ ール 4 と、 上部絞 り · 駆動ロール 5 と の周 り を周回 し、 こ の圧縮ロール 4 と上部絞 り · 駆動ロール 5 と の間 には 自 発復元化ロール 2 5 b が設け ら れている。 The belt conveyor type impregnating machine 20 is provided with two conveyor belts 21 and 22 which may be in the form of an endless track mesh. The upper conveyor belt 21 circulates around the upper delivery roll 25a, the compression roll 4, and the upper squeezing / driving roll 5, and the upper conveyance belt 21 and the upper squeezing roll 4a. · A spontaneous restoration roll 25 b is provided between the drive roll 5 and the drive roll 5.
下部搬送ベル ト 2 2 は、 下部送出 ロール 2 6 a と 、 圧縮 ロール 4 と、 下部絞 り · 駆動ロ ール 6 の周 り を周回 し、 こ の下部絞 り · 駆動 ロール 6 と下部送出 ロール 2 6 a と の間 には、 補助 ロール 2 6 c 、 2 6 b が設け ら れてレゝる 。  The lower conveying belt 22 circulates around the lower feeding roll 26 a, the compression roll 4, and the lower squeezing / driving roll 6, and the lower squeezing / driving roll 6 and the lower sending roll 6 Auxiliary rolls 26c and 26b are provided between and 26a.
こ の よ う な構成のベル ト搬送式含浸機 2 0 では、 圧縮 口 ール 4 の一部表面に上部搬送ベル ト 2 1 の内側面が周接 し てお り 、 圧縮ロール 4 と周接する こ の上部搬送ベル ト 2 1 の外側面に、 さ ら に、 下部搬送ベル ト 2 2 の外側面が緊張 状態で周接 している。  In the belt transfer type impregnating machine 20 having such a configuration, the inner surface of the upper transfer belt 21 is in circumferential contact with a part of the surface of the compression port 4, and is in circumferential contact with the compression roll 4. The outer side surface of the upper transfer belt 21 and the outer side surface of the lower transfer belt 22 are in tight contact with each other.
こ の よ う な構成のベル ト搬送機含浸機 2 0 では、 不織布 1 は、 上下送出 ロ ール 2 5 a 、 2 6 a 間で上下搬送ベル ト 2 1 , 2 2 によ り 挟持 ' 案内さ れつつ、 圧縮ロール 4 の存 在する含浸槽 3 内 に導かれ、 該含浸槽 3 内のバイ ンダー混 合液 2 に浸漬さ れる と共に、 圧縮ベル ト 4 下部で、 上下搬 送ベル ト 2 1 , 2 2 で挟持 ' 圧縮さ れる 。 圧縮ロール 4 の 回転速度や下部搬送ベル ト 2 2 の張力な どを適宜調整する こ と に よ り 、 上記 と 同様に圧縮面圧、 圧縮ロール 4 部での 不織布 1 の圧縮量、 圧縮時間な どを上記例 と 同様に、 適宜 調整する こ とができる。  In the belt conveyor impregnating machine 20 having such a configuration, the nonwoven fabric 1 is held between the upper and lower delivery rolls 25a and 26a by the upper and lower conveyor belts 21 and 22. While being compressed, it is guided into the impregnation tank 3 where the compression rolls 4 are present, is immersed in the binder mixed solution 2 in the impregnation tank 3, and is moved vertically below the compression belt 4 at the bottom of the compression belt 4. It is pinched and compressed by 1, 2 2. By appropriately adjusting the rotation speed of the compression roll 4 and the tension of the lower conveyor belt 22, the compression surface pressure, the compression amount of the nonwoven fabric 1 at the four compression rolls, and the compression time can be adjusted as described above. Can be adjusted appropriately as in the above example.
用 い ら れる不織布 1 の強度特に引張強度があ ま り 高 く な く 、 図 1 に示すよ う な含浸機 1 0 を用 いたのでは、 不織布 1 が伸びて し ま う よ う な場合には、 こ のよ う に上下搬送べ ル 卜 2 1 , 2 2 間で挟持 して搬送すれば、 不織布 1 が過度 に伸びて し ま う こ とがないため、 基材繊維種及びその含量、 引張強度等の異なる広範な種類の不織布に対 して、 こ のべ ル ト搬送機含浸機 2 0 を使用する こ とができ る 。 Strength, especially tensile strength, of nonwoven fabric 1 used If the impregnating machine 10 as shown in Fig. 1 is used, if the nonwoven fabric 1 is likely to be stretched, the upper and lower conveyor belts 21 and 22 are thus stretched. Non-woven fabric 1 will not be excessively stretched if it is transported by being sandwiched between non-woven fabrics, so that it can be used for a wide variety of non-woven fabrics with different base fiber types and their contents, tensile strengths, etc. A root conveyor impregnator 20 can be used.
<図 3 >  <Figure 3>
また、 本発明では、 上記③の方法 (高圧噴霧法) を採用 する場合には、 図 3 に模式的に示す高圧噴霧含浸機 3 0 を 用 いて、 メ ッ シ ュ状の基台 3 1 上に載置さ れた不織布 1 の 上方か ら 、 その下方の不織布 1 の表面に、 バイ ンダー混合 液 1 a を噴霧する と共に、 不織布 1 と噴霧ノ ズル 3 2 a と の相対的位置を連続的に変化さ せる こ と に よ り 、 上記含浸 工程を 自動化する こ と が可能である。  In the present invention, when the method (3) (high-pressure spraying method) described above is adopted, the high-pressure spray impregnating machine 30 schematically shown in FIG. The binder mixed solution 1a is sprayed from above the nonwoven fabric 1 placed on the surface of the nonwoven fabric 1 below, and the relative positions of the nonwoven fabric 1 and the spray nozzle 32a are continuously measured. It is possible to automate the above-mentioned impregnation step by changing the impregnation step.
不織布 1 と 噴霧ノ ズル 3 2 a と の相対的位置を変化さ せ る には、 (ィ ) : 噴霧器ノ ズル 3 2 a の位置を固定しておき、 メ ッ シュ状基台 3 1 と共に、 その基台 3 1 上の不織布 1 を 移動させる か、 あ る レ は、 (口) : メ ッ シュ状基台 3 1 と、 その基台 3 1 上の不織布 1 と を固定 しておき、 噴霧器 ノ ズ ル 3 2 a を移動させる よ う に して も よ く 、 また、 (ハ) : 噴 霧器ノ ズル 3 2 a と不織布 1 と の両者を互い に相異な る方 向に移動させる よ う に して もよ い。  To change the relative position between the nonwoven fabric 1 and the spray nozzle 32 a: (a): The position of the spray nozzle 32 a is fixed, and together with the mesh base 31, The nonwoven fabric 1 on the base 31 is moved or there is a (mouth): The mesh base 31 and the nonwoven fabric 1 on the base 31 are fixed, and the atomizer is used. The nozzle 32a may be moved, and (c): both the atomizer nozzle 32a and the nonwoven fabric 1 may be moved in different directions from each other. You can do it.
こ のよ う に、 メ ッ シュ状基台 3 1 上に不織布 1 を載置 し、 その上方よ り 不織布 1 の表面に向けてバイ ンダー混合液を 噴霧する こ と に よ り 、 不織布内部に までバイ ンダー混合液 を均一かつ充分 に浸透 (含浸) させる こ とが可能であ る 。 As described above, the nonwoven fabric 1 is placed on the mesh-shaped base 31, and the binder mixed solution is applied from above to the surface of the nonwoven fabric 1. By spraying, the binder mixture can be uniformly and sufficiently penetrated (impregnated) into the nonwoven fabric.
こ の よ う に高圧噴霧法にて不織布 1 にバイ ンダー混合液 を効率よ く 含浸させる際の条件は、 不織布な どの移動速度、 噴霧時間、 ノ ズルか ら不織布までの距離な どによ り 異な り 一概に決定さ れないが、 例えば、 必要な含浸量の 1 0 〜 5 0 倍量噴霧す る よ う に 上記諸条件 を設定する こ と がで き る。  The conditions for efficiently impregnating the nonwoven fabric 1 with the binder mixed solution by the high-pressure spray method depend on the moving speed of the nonwoven fabric, the spraying time, the distance from the nozzle to the nonwoven fabric, and the like. Although it is not generally determined differently, for example, the above-mentioned conditions can be set so as to spray 10 to 50 times the required impregnation amount.
<図 4 >  <Fig. 4>
図 4 には、 図 3 に示す高圧噴霧含浸機 3 0 において、 メ ッ シュ状基台 3 1 の下方に吸引装置 3 3 を設けた態様が示 さ れてい る 。  FIG. 4 shows an embodiment in which a suction device 33 is provided below the mesh base 31 in the high-pressure spray impregnator 30 shown in FIG.
こ の図 4 に示すよ う に、 メ ッ シュ状基台 3 1 の下方に吸 引装置 3 3 を設けて不織布 1 内の気体な どを減圧 · 吸引す れば、 バイ ンダー混合液 1 の浸透 (含浸) 効率をい つ そ う 高める こ とができる。  As shown in FIG. 4, a suction device 33 is provided below the mesh-shaped base 31 to reduce the pressure and suction of the gas and the like in the nonwoven fabric 1. The penetration (impregnation) efficiency can be improved at any time.
こ れ ら の何れの含浸機 1 0 , 2 0 , 3 0 , 3 0 A を用 い る場合にお いて も、 ノ ィ ンダ一混合液 2 を不織布 1 内部に 均一に含浸する ため には、 バイ ンダー混合液を所定量以上 の量で不織布内部に含浸させたのち に、 図 1 、 図 2 に付番 5 , 6 で示すよ う に、 所定間隔に調整 した一対の ロール間 に揷通させる こ とが望ま しい。  Regardless of which of these impregnating machines 10, 20, 30, 30 A is used, in order to uniformly impregnate the inside of the nonwoven fabric 1 with the mixed liquid 1, After the binder mixture is impregnated into the nonwoven fabric in an amount equal to or greater than a predetermined amount, the liquid is passed between a pair of rolls adjusted to a predetermined interval as shown by reference numerals 5 and 6 in FIGS. 1 and 2. This is desirable.
上記実施態様に示す含浸機を用 いれば、 不織布内部まで 均一か つ完全 に バイ ンダー混合液を含浸 さ せ る こ と がで き、 ガス、 液体シール性等に優れたシ一 ト 状シール材を得 る こ と ができ る が、 本発明は、 こ のよ う な含浸機を用 い る 態様に限定さ れず、 前述 した 「事前圧縮液中 自発復元法」 ①、 「液中圧縮 自発復元法」 ②、 「高圧噴霧法」 ③、 「減圧 注入法、 減圧置換法」 ④な どを採用する も のである 限 り 、 本発明では好ま し く 用 い る こ とができ る。 By using the impregnating machine described in the above embodiment, it is possible to uniformly and completely impregnate the inside of the nonwoven fabric with the binder mixed solution. Although a sheet-like sealing material excellent in gas and liquid sealing properties and the like can be obtained, the present invention is not limited to such an embodiment using an impregnating machine, and is described above. As long as the method adopts “pre-compressed liquid spontaneous restoration method” ①, “liquid compression spontaneous restoration method” ②, “high-pressure spraying method” ③, “reduced pressure injection method, decompressed displacement method”, etc. It can be used favorably in the invention.
本発明では、 上記の よ う に して、 不織布内部に、 バイ ン ダー混合液を含浸さ せる と共に、 不織布内部空隙に存在す る空気等の気体を、 強制的かつ実質上完全に追い出 し、 不 織布内の空隙部をパィ ンダー混合液で置換 し満たし た後、 卞記 「乾燥工程」 にて、 シー ト を乾燥させ、 シー ト 状シー ル材を得てい る。  In the present invention, as described above, the binder mixed solution is impregnated inside the nonwoven fabric, and gas such as air existing in the voids inside the nonwoven fabric is forcibly and substantially completely displaced. After filling and filling the voids in the nonwoven cloth with the binder mixture, the sheet was dried in the "drying process" described by Byon to obtain a sheet-like seal material.
ぐ乾燥工程 (工程 3 ) >  Drying process (process 3)>
上記 「バイ ンダー混合液の含浸と気体の追出 し工程」 (単 に、 含浸工程 と も言 う 。 ) 終了後の不織布 には、 最終製品 であ る シー ト 状シール材には不要な溶媒または分散媒が含 まれてい る 。 こ の状態でゴム分の架橋あ る いは樹脂分の硬 化を行っ た場合、 シー ト 状シール材内に溶媒または分散媒 が残存 し、 シー ト状シール材に安定し たシ一ル性能を発揮 させる こ とができない。 そ こ で、 バイ ンダー混合液が含浸 さ れた不織布は、 下記乾燥工程 を行 う 前に含浸工程終了後 の不織布か ら 溶媒または分散媒を除去する 。  (The impregnation process of the binder mixture and the gas expelling process) (Simply referred to as the impregnation process.) For the nonwoven fabric after completion, the solvent unnecessary for the final product, sheet-like sealing material Or, a dispersion medium is contained. In this state, when the rubber component is crosslinked or the resin component is cured, the solvent or dispersion medium remains in the sheet-like sealing material, and the sealing performance is stable to the sheet-like sealing material. Cannot be demonstrated. The solvent or dispersion medium of the nonwoven fabric impregnated with the binder mixed solution is removed from the nonwoven fabric after the impregnation step before performing the drying step described below.
溶媒または分散媒の除去は、 8 0 °C以上、 望ま し く は 8 0 °C以上 1 0 0 °C以下に設定 した乾燥機内 にて、 1 〜 3 時 間程度、 シー ト を加熱する こ と によ り 、 溶媒または分散媒 を揮散 · 除去すればよ い。 1 0 0 °C を超え る高温下でシー 卜 の乾燥を行 う と、 不織布内の溶媒ま たは分散媒が急激に 気化、 膨張 し、 不織布内部に空隙を発生させる こ とがあ る。 また、 こ の よ う な 1 0 0 °C を超える温度で乾燥工程 を実施 する と、 下記 「成形工程」 を行 う 前に、 シー ト 中の ゴム の 架橋や、 樹脂の硬化が促進さ れる ため、 下記 「成形工程」 時には圧縮に よ る気密性向上効果が十分に得 ら れな い場合 があ る。 ま た 8 0 °C未満の温度にてシー ト を乾燥さ せた場 合、 溶媒または分散媒を完全に揮散 · 除去する ため に長時 間を要し非効率的であ る。 Removal of the solvent or dispersion medium takes place between 1 and 3 o'clock in a dryer set at 80 ° C or higher, preferably 80 ° C or higher and 100 ° C or lower. The solvent or the dispersion medium may be volatilized and removed by heating the sheet for a while. If the sheet is dried at a high temperature exceeding 100 ° C, the solvent or dispersion medium in the nonwoven fabric may be rapidly vaporized and expanded, and voids may be generated inside the nonwoven fabric. In addition, if the drying step is performed at a temperature exceeding 100 ° C, the crosslinking of the rubber in the sheet and the curing of the resin are promoted before the following “forming step” is performed. Therefore, at the time of the “forming step” described below, the effect of improving the airtightness by compression may not be sufficiently obtained. Also, when the sheet is dried at a temperature lower than 80 ° C, it takes a long time to completely volatilize and remove the solvent or the dispersion medium, which is inefficient.
なお、 溶媒または分散媒の蒸発は主にシー ト 表面にて生 じ、 これに伴っ てシー ト 内部に残存する溶媒または分散媒 が表面に移動 し、 こ のサイ クルによ っ てシー ト 中の溶媒ま たは分散媒が除去される 。 その際、 溶媒または分散媒のみ な らず、 シー ト 内部のバイ ンダー混合液自体がシー ト表面 に誘導さ れる こ とがあ る (マイ グ レー シ ョ ン ( migration ) と も言う 。 ) 。  The evaporation of the solvent or the dispersion medium mainly occurs on the sheet surface, and the solvent or the dispersion medium remaining inside the sheet moves to the surface, and is thereby generated by the cycle. The solvent or dispersion medium is removed. At that time, not only the solvent or dispersion medium but also the binder mixture inside the sheet itself may be guided to the sheet surface (also referred to as migration).
こ の よ う なマイ グレーシ ョ ンの生 じたシー 卜 に対 して、 下記 「成形工程」 を実施する こ と によ っ て、 シー ト 内部の ゴム配合比がシー 卜表面近傍の ゴム配合比に比 して少な く な り 、 得 ら れた シー ト状シール材が、 充分に優れた シール 性能および応力緩和性能を示さ ない こ とがあ る 。  By performing the following “molding process” on the sheet in which such migration has occurred, the rubber compounding ratio inside the sheet is reduced by the rubber compounding ratio near the sheet surface. In some cases, the obtained sheet-like sealing material does not show sufficiently excellent sealing performance and stress relaxation performance.
こ の よ う な場合には、 前述 し たよ う に、 前記 「バイ ンダ 一混合液の調製」 工程 (工程 1 ) にてバイ ンダー混合液調 製時に感熱ゲル化剤 (感熱剤) を配合 しておき、 こ の 「乾 燥工程」 にて、 溶媒または分散媒乾燥温度以下の温度、 好 ま し く は 4 0 〜 8 0 °C の温度にて加熱する こ と によ っ て、 バイ ンダー混合液の粘度を増加させ、 固形分の流動性を低 下させる こ とが有効であ る (「前乾燥工程」 と も言う ) 。 In such a case, as described above, the "binder" Preparation of one liquid mixture ”In the step (Step 1), a heat-sensitive gelling agent (thermosensitive agent) is blended when preparing the binder mixture, and in this“ drying step ”, the solvent or dispersion medium drying temperature Heating at the following temperature, preferably at a temperature of 40 to 80 ° C, increases the viscosity of the binder mixture and reduces the flowability of solids. Is effective (also called “pre-drying process”).
こ のよ う に前乾燥工程を行っ た後、 上記 した通 り 、 8 0 °C以上、 望ま し く は 8 0 で以上 1 0 0 °C以下に設定 し た乾 燥機内に てシー ト を加熱する こ と によ り 、 溶媒または分散 媒を揮散 · 除去する と、 得 られる シー ト状シール材の内部、 表面近傍な ど、 その部位に依 ら ず均一な成分含量を有 し、 シ一ル性、 応力緩和性共にバラ ンス よ く 優れたシー ト 状シ 一ル材が得 ら れる傾向があ る。  After performing the pre-drying step in this way, as described above, the sheet is placed in a dryer set at a temperature of 80 ° C or more, preferably 80 to 100 ° C. When the solvent or the dispersion medium is volatilized and removed by heating, the resulting sheet-like sealing material has a uniform component content regardless of its location, such as inside or near the surface. There is a tendency to obtain a sheet-like sealing material that is excellent in both balance and stress relaxation.
ま た、 本発明では、 上記のよ う に感熱剤を配合した前乾 燥工程に代えて、 湿熱雰囲気下での加熱も マイ グレーシ ョ ンを抑制する有効な方法であ り 、 このよ う な方法によれば、 上記溶媒 または分散媒の移動、 揮散を伴わずにシー ト 内部 のバイ ン ダー混合液の粘度を上昇させ、 固形分の流動性を 低下させ る こ とができ る。 こ の よ う な湿熱雰囲気下での加 熱は、 1 0 0 〜 1 5 0 °C、 好ま し く は 1 2 0 〜 1 3 0 の 温度の水蒸気雰囲気下 (湿度 : 8 0 〜 1 0 0 % ) に、 5 〜 2 0 分程度、 シー ト を加熱する こ と によ り 行われる。  Further, in the present invention, instead of the pre-drying step in which the heat-sensitive agent is blended as described above, heating in a moist and hot atmosphere is an effective method for suppressing migration. According to the method, it is possible to increase the viscosity of the binder mixed liquid inside the sheet and reduce the flowability of the solid content without involving the movement or volatilization of the solvent or the dispersion medium. Heating in such a moist heat atmosphere is 100 to 150 ° C, preferably in a steam atmosphere at a temperature of 120 to 130 ° C (humidity: 80 to 100 ° C). %) By heating the sheet for about 5 to 20 minutes.
本発明では、 こ のよ う に湿熱雰囲気下の加熱を行っ た後、 上記の通 り 、 8 0 °C以上、 望ま し く は 8 0 °C以上 1 0 0 °C 以下に設定 した乾燥機内にて シー ト を加熱し溶媒または分 散媒を揮散 · 除去する 「乾燥工程」 を行っ ても よい。 In the present invention, after the heating under the moist heat atmosphere, as described above, at least 80 ° C, preferably at least 80 ° C, and at least 100 ° C. A "drying step" may be performed in which the sheet is heated in a dryer set as follows to volatilize and remove the solvent or the dispersing medium.
<成形工程 (工程 4 ) >  <Molding process (process 4)>
本発明では、 上記乾燥工程 を経て得 ら れた乾燥物 ( シー ト) を、 こ の 「成形工程」 にて加熱下に加圧する こ と に よ り 、 乾燥工程終了後の シー ト の気密性を向上させる と と も に、 配合 し たゴム分の架橋あ る いは樹脂分の硬化を行 う 。  In the present invention, the airtightness of the sheet after the drying step is completed by pressing the dried product (sheet) obtained through the drying step under heating in the “forming step”. In addition to improving the rubber composition, cross-linking of the compounded rubber or curing of the resin is performed.
成形装置 と しては、 通常、 ホ ッ ト プレスが使用 さ れる。 成形条件は、 配合成分組成な どによ り 異な り 一概に決定 さ れないが、 通常、 加熱温度 1 2 0 〜 2 5 0 ° (:、 加熱時間 3〜 1 5 分間、 圧縮面圧 5〜 4 0 M P a の範囲内で適宜設 定さ れる 。  A hot press is usually used as a molding device. The molding conditions vary depending on the composition of the components, etc., and are not generally determined. However, usually, the heating temperature is 120 to 250 ° (heating time: 3 to 15 minutes, compression surface pressure: 5 to 50 minutes). It is set appropriately within the range of 40 MPa.
なお、 ホ ッ ト プレス に よ る加硫あ る いは硬化が不十分な 場合、 乾熱、 湿熱下にて二次加熱を行え ば、 上記ゴム加硫 ある いは樹脂硬化を い つ そ う 効果的に促進させる こ と がで き る 。 こ のよ う な二次加熱は、 下記の よ う な条件で行われ る。  If vulcanization or curing by hot pressing is insufficient, secondary heating under dry or moist heat can be used to cure the rubber or resin. It can be effectively promoted. Such secondary heating is performed under the following conditions.
すなわ ち 、 通常、 加熱温度 1 5 0 〜 2 5 0 ° (:、 加熱時間 0 . 5〜 2 4 時間、 乾熱下、 あ る いは湿熱下に保持すれば よ い。 なお、 二次加硫の際に は、 通常では、 面圧は印可せ ずフ リ ーべ一キ ングを採用する こ とが多い。  That is, usually, the heating temperature is 150 to 250 ° (:, the heating time is 0.5 to 24 hours, and the heating may be performed under the dry heat or the wet heat. In the case of vulcanization, usually, free pressure is not applied, and freezing is often used.
こ のよ う に して得 ら れたシー 卜状シール材には、 有機系 バイ ンダー と してのゴム材ま たは樹脂は、 通常 5〜 4 0 重 量%、 好ま し く は 1 0 〜 3 0 重量% の量で、 不織布を構成 してい る基材繊維は、 通常 5 〜 8 0 重量% 、 好ま し く は 1 0 〜 7 0 重量%、 さ ら に好ま し く は 1 0 〜 5 0 重量% の量で、 必要によ り 含有さ れる充填剤は、 0 〜 8 0 重量% の量で、 特に充填剤を配合する場合には、 好ま し く は 5 〜 8 0 重量%、 さ ら には 3 0 〜 8 0 重量%の量で含 まれてレ る こ とが望ま しい。 In the sheet-like sealing material thus obtained, rubber or resin as an organic binder is usually 5 to 40% by weight, preferably 10 to 40% by weight. In the amount of ~ 30% by weight, The base fiber constituting the nonwoven fabric is usually required in an amount of 5 to 80% by weight, preferably 10 to 70% by weight, and more preferably 10 to 50% by weight. Is contained in an amount of 0 to 80% by weight, particularly when a filler is incorporated, preferably 5 to 80% by weight, and more preferably 30 to 80% by weight. It is desirable that it be included in the amount of weight%.
こ の よ う に して得 ら れたシー ト 状シール材は、 高温下で 長期間 に亘つ て、 優れたガス シール性、 液体シ一ル性を維 持でき、 かつ シール材の強度異方性がない。  The sheet-like sealing material obtained in this way can maintain excellent gas-sealing properties and liquid-sealing properties over a long period of time at high temperatures, and have a difference in the strength of the sealing material. There is no isotropic.
【発明の効果】  【The invention's effect】
本発明に係る シー ト 状シール材の製造方法に よれば、 下 記のよ う な効果が得 ら れる。  According to the method for manufacturing a sheet-like sealing material of the present invention, the following effects can be obtained.
( 1 ) 本発明の シー ト状シール材の製造方法では、 使用 で き る繊維に制限がな く 、 広範な種類の繊維か ら なる不織布 を使用 でき る 。 すなわち 、 従来のカ レ ンダ一 口 一ル製法 と は異な り 、 本発明では不織布にバイ ンダー混合液を含浸す る と共に不織布内部の気体を完全に除去させたのち 、 乾燥 させ、 加熱あ る いは加熱圧縮 してい る ため、 成形さ れたシ 一 ト 状シール材の表面に剪断応力 を生 じ る こ とがな く 、 繊 維 とパイ ンダ一 と の濡れ性に劣る配合条件であ っ て も、 成 形時に しわや破断を生 じ る こ とがない。 こ のため、 製法上 使用 でき る繊維に制限がな く 、 p — ァ ラ ミ ド繊維を ま つ た く 含まない ゴム あ る い は樹脂を含む シー 卜 状シール材の製 造が可能 となっ ている。 ( 2 ) 本発明の製造方法によ り 得 ら れる シー ト状シール材 は、 高温条件下での使用 によ る硬化が小さ いため、 長期間 優れたシール性能等の性能を保持でき長期健全性に優れて い る。 本発明の製造方法に よ り 得 ら れる シー ト状シール材 は、 従来の ジ ョ イ ン ト シ一 卜や ビーターシー 卜 と は異な り 、 不織布を用 いてお り 、 これによ つ て、 強度因子であ る 繊維 間の絡み合い を あ ら か じめ付与する こ とができ る ため、 繊 維配合比率を低 く 設定 して も、 ゴムや樹脂自 身の硬化がシ 一 卜 の硬化に与える影響を軽減する こ とが可能 とな っ てい る。 また、 ノ イ ンダ一 と してゴム ラテ ッ ク ス あ る いは樹脂 ェマルジ ョ ン を単独あ る いは複数使用 し た場合、 バイ ンダ ―混合液中 にバイ ンダー成分が分散 して存在する。 こ のバ ィ ンダー混合液を不織布に含浸させ、 乾燥お よび成形する 工程 において、 シール材の内部に あ るバイ ンダ一成分は分 散状態の ま ま保持されてい る。 換言すれば、 バイ ンダー成 分はシ一ル材内部に非連続な状態で存在する ため、 高温条 件下で使用 した場合、 バイ ンダー成分の分散粒子内での硬 化が生 じて も 、 こ れがシ一 ト状シール材の硬化および収縮 を誘発 しない。 また、 本製法に は水分散系であ る ゴム ラテ ッ ク ス あ る い は樹脂ェマルジ ヨ ン以外に も、 溶液ゴム、 液 状ゴム、 溶液樹脂のいずれも用 いる こ とができ る。 (1) In the method for producing a sheet-like sealing material of the present invention, usable fibers are not limited, and a nonwoven fabric made of a wide variety of fibers can be used. That is, unlike the conventional method of producing a single piece of calender, in the present invention, the nonwoven fabric is impregnated with the binder mixed solution, and the gas inside the nonwoven fabric is completely removed, followed by drying and heating. Since heat-compression is performed, no shear stress is generated on the surface of the molded sheet-like sealing material, and the mixing conditions are such that the wettability between the fiber and the binder is poor. No wrinkles or breakage during molding. For this reason, there are no restrictions on the fibers that can be used in the production method, and it is possible to produce a sheet-like sealing material containing rubber or resin that does not contain p-aramid fibers. ing. (2) Since the sheet-like sealing material obtained by the manufacturing method of the present invention hardly hardens when used under high-temperature conditions, it can maintain excellent sealing performance and other properties over a long period of time and can maintain a long-term soundness. Excellent. The sheet-like sealing material obtained by the production method of the present invention uses a non-woven fabric unlike conventional joint sheets and beater sheets. Since the entanglement between fibers, which is a strength factor, can be imparted in advance, even if the mixing ratio of fibers is set to a low value, the curing of rubber or resin itself will cure the sheet. It is possible to reduce the impact. Also, when rubber latex or resin emulsion is used alone or plurally as a binder, the binder component is dispersed in the binder-mixture. . In the process of impregnating the nonwoven fabric with the binder mixed solution, drying and forming, one component of the binder inside the sealing material is maintained in a dispersed state. In other words, since the binder component exists in a discontinuous state inside the sealing material, when used under high-temperature conditions, even if the binder component hardens in the dispersed particles, This does not induce hardening and shrinkage of the sheet-like sealing material. Further, in the present production method, in addition to rubber latex or resin emulsion which is an aqueous dispersion system, any of solution rubber, liquid rubber, and solution resin can be used.
( 3 ) 本発明 に係る シー ト 状シール材の製造方法では、 高 温使用下での割れの一因であ る シー 卜 の強度異方性を低 く する こ とが可能であ る 。 これは、 あ ら か じめ繊維を不織布 の状態に成形 した も の を シール材形成用 の不織布 と し て使 用 してお り 、 不織布の段階にて繊維に配向性がないためで ¾る。 (3) In the method for producing a sheet-like sealing material according to the present invention, it is possible to reduce the strength anisotropy of the sheet, which is one of the causes of cracking at a high temperature. This is a pre-fabricated non-woven fabric This is used as a non-woven fabric for forming a sealing material, and the fibers are not oriented at the stage of the non-woven fabric.
( 4) 本製法によ る シー ト 状シール材は、 気密性に優れて いる 。 不織布は元来空隙を多数含有する材料であ るが、 そ のため不織布内部までバイ ンダー混合液を均一に含浸さ せ る こ とが可能であ る。 一度含浸させたバイ ンダー混合液を 不織布内部に保持させたま ま成形する こ と に よ っ て、 高気 密性シー ト状シ一ル材が得 ら れる。  (4) The sheet-like sealing material produced by this method has excellent airtightness. Nonwoven fabric is a material that originally contains a large number of voids. Therefore, it is possible to uniformly impregnate the inside of the nonwoven fabric with the binder mixed solution. A highly airtight sheet-like seal material can be obtained by forming the binder mixed solution once impregnated while holding it inside the nonwoven fabric.
【実施例】  【Example】
以下、 本発明について、 実施例に基づいて さ ら に具体的 に説明するが、 本発明は、 こ の よ う な実施例によ り 何 ら 制 限さ れる も のではない。  Hereinafter, the present invention will be described more specifically with reference to Examples, but the present invention is not limited to such Examples.
なお、 以下の実施例、 比較例な どで用 いた シー ト材の硬 化の程度 を表す 「熱履歴後の破断時伸び率」 の測定法は以 下の通 り 。  The method of measuring the “elongation at break after thermal history”, which indicates the degree of hardening of the sheet material used in the following examples and comparative examples, is as follows.
<熱履歴後の破断時伸び率 > シー ト 材の硬化の程度を表す数値 と して、 所定条件にお ける 熱履歴後の引張試験によ る破断時伸び率を測定した。  <Elongation at break after heat history> The elongation at break by a tensile test after heat history under predetermined conditions was measured as a numerical value indicating the degree of hardening of the sheet material.
引張試験への適用 を考慮 して厚さ 1 . 5 m m、 1 5 O X 2 5 m m短冊状の試験片を作製 し、 これを 1 8 0 の加熱 空気内で 9 6 時間処理 したのち 、 つかみ用治具間距離を 1 0 0 m m に設定 し 、 引張速度 5 m m Z分にて引張試験を行 う こ と に よ っ て破断時伸び量を測定 し、 以下の式によ り 破 断時伸び率 ( R τ) を算出 した。 A 1.5 mm thick, 15 OX 25 mm strip test piece was prepared in consideration of application to the tensile test, and this was treated in heated air at 180 ° for 96 hours, and then used for gripping. Set the distance between the jigs to 100 mm and measure the elongation at break by performing a tensile test at a tensile speed of 5 mm Z minutes. The elongation at break (Rτ) was calculated.
R τ = D L - 1 0 0 ( % )  R τ = D L-1 0 0 (%)
R τ: 破断時伸び率 (% )  R τ: Elongation at break (%)
D L: 破断時の引張治具間寸法 ( m m ) D L : Dimension between tension jigs at break (mm)
【実施例 1 】  [Example 1]
N B R ラ テ ッ ク ス を固形分重量にて 1 6 k g 、 炭酸カル シゥム 3 2 k g 、 粉末状硫黄 0 . 2 k g 、 粉末状亜鉛華 0 . 2 k g , 界面活性剤を 固形分重量にて 1 . 3 k g 、 感熱剤 を固形分重量にて 0 . 4 k g 、 増粘剤を固形分重量にて 0 . 3 k g を混合 し水 3 2 . 5 リ ツ トルで希釈する こ と によ り 、 バイ ンダ一混合液を調製 した。  16 kg of NBR latex, 32 kg of calcium carbonate, 0.2 kg of powdered sulfur, 0.2 kg of powdered zinc white, 0.2 kg of powdered solid, and surfactant of 1 kg by solid weight By mixing 3 kg, 0.4 kg of the heat sensitive agent by solid weight and 0.3 kg of the thickener by solid weight, and diluting with 32.5 liters of water, A binder-mixture was prepared.
ピ ッ チ系炭素繊維を用 い製造したニー ドルパ ンチフ ェル ト 1 3 k g を あ ら か じ め圧縮 した状態で上記バイ ンダー混 合液に浸漬さ せ、 バイ ンダー混合液浸漬中 に 発復元さ せ 含浸さ せた。 含浸操作を 3 回繰 り 返して実施し、 全バイ ン ダ一混合液を含浸さ せた。  13 kg of needle punch made using pitch-based carbon fiber is pre-compressed and immersed in the above-mentioned binder mixed solution, and is restored during immersion in the binder mixed solution. Soaked and impregnated. The impregnation operation was repeated three times to impregnate the mixed solution of all the binders.
これを電気炉内 に設置 し、 5 0 °Cで 3 0 分、 9 0 で 9 0 分間加熱 した。 次いで、 これを、 1 5 0 °C に設定したプ レス加硫機にて面圧 1 6 M P a にて 1 0 分間圧縮してシー ト状シール材を製造した。  This was placed in an electric furnace and heated at 50 ° C for 30 minutes and at 90 for 90 minutes. Next, this was compressed with a press vulcanizer set at 150 ° C at a surface pressure of 16 MPa for 10 minutes to produce a sheet-like sealing material.
得 ら れた シー ト状シール材の引張強 さ ( J I S R 3 4 5 3 準拠) は、 高強度方向 (縦方向、 a ) では 2 0 . 8 M P a 、 低強度方向 (横方向、 b ) では 2 0 . O M P a と な り 、 強度異方性 ( a ノ b ) は 1 . 0 とな っ た。 また、 常温 シール性 ( A S T M F 3 7 — B に準拠。 面圧 1 9 . 6 M P a 、 窒素内圧 0 . 9 8 M P a ) は、 9 . 1 E - 5 ( = 9 . 1 X 1 0 —5) ( P a · m 3 / s ) とな り 、 熱履歴後の破断時 伸び率 ( % (縦横方向の値の う ち 低い方の値) ) は、 0 . 9 9 % と な り 、 The tensile strength (according to JISR3453) of the obtained sheet-like sealing material is 20.8 MPa in the high-strength direction (vertical direction, a), and 20.8 MPa in the low-strength direction (horizontal direction, b). The OMPa was 20. The strength anisotropy (a / b) was 1.0. Also at room temperature Sealing performance (according to ASTMF 37 — B. Surface pressure 19.6 MPa, nitrogen internal pressure 0.98 MPa) is 9.1 E-5 (= 9.1 X 10 —5) (P a · m 3 / s), and the elongation at break (% (lower of the values in the vertical and horizontal directions)) at break after thermal history is 0.99%.
実機ライ ン に組み込み 2 3 0 °Cで保持した場合の割れ発 生までの 日 数は、 3 6 0 日 以上となっ た。  The number of days until cracking when it was installed at 230 ° C in the actual machine line was more than 360 days.
各成分の配合量および試験結果を表 1 に'併せて示す。 【実施例 2 】  The amounts of each component and the test results are shown in Table 1. [Example 2]
N B R ラテ ッ ク ス を固形分重量にて 1 6 k g 、 炭酸カル シゥム 3 2 k g 、 粉末状硫黄 0 . 2 k g 、 粉末状亜鉛華 0 . 2 k g , 界面活性剤を固形分重量にて 1 . 3 k g 、 感熱剤 を固形分重量にて 0 . 4 k g 、 増粘剤を固形分重量にて 0 . 3 k g を混合 し水 3 2 . 5 リ ッ トルで希釈する こ と に よ り 、 バイ ンダ一混合液を調製した。  16 kg of NBR latex in solid content, 32 kg of calcium carbonate, 0.2 kg of powdered sulfur, 0.2 kg of powdered zinc white, and surfactant of 1.2 kg in solid content. By mixing 3 kg, the heat-sensitive agent in a solid weight of 0.4 kg and the thickener in a solid weight of 0.3 kg, and diluting with 32.5 liters of water, A mixed solution was prepared.
ピ ッ チ系炭素繊維を用 い製造 した二一 ドルパ ンチフ ェル ト 2 2 k g を あ ら か じめ圧縮 した状態で上記バイ ンダー混 合液に浸漬さ せ、 バイ ンダー混合液浸漬中で 自発復元させ 全バイ ンダー混合液を含浸させた。  21 kg of 21 dollar punch made using pitch-based carbon fiber is immersed in the above-mentioned binder mixed liquid in a state of being compressed in advance and spontaneously immersed in the binder mixed liquid It was reconstituted and impregnated with all the binder mixture.
こ れを電気炉内 に設置 し、 5 0 °Cで 3 0 分、 9 0 °Cで 9 0 分間加熱 し た。 これを、 1 5 0 °C に設定 したプレス加硫 機にて面圧 1 6 M P a にて 1 0 分間圧縮 してシー ト状シー ル材を製造し た。  This was placed in an electric furnace and heated at 50 ° C for 30 minutes and at 90 ° C for 90 minutes. This was compressed with a press vulcanizer set at 150 ° C at a surface pressure of 16 MPa for 10 minutes to produce a sheet-like seal material.
得 ら れた シー ト状シール材の引張強さ ( J I S R 3 4 5 3 準拠) は、 高強度方向 (縦方向、 a ) では 2 5 . 3 M P a 、 低強度方向 (横方向、 b ) では 2 2 . 8 M P a と な り 、 強度異方性 ( a Z b ) は 1 . 1 となっ た。 ま た、 常温 シール性 ( A S T M F 3 7 — B に準拠。 面圧 1 9 . 6 M P a 、 窒素内圧 0 . 9 8 M P a ) は、 7 5 E - 5 ( P a • m 3 Z s ) とな り 、 The tensile strength of the obtained sheet-like sealing material (JISR 34 53) is 25.3 MPa in the high-strength direction (vertical direction, a), 22.8 MPa in the low-strength direction (horizontal direction, b), and the strength anisotropy (aZ b) was 1.1. Also, cold seal resistance (ASTM F 3 7 - compliant B surface pressure 1 9 6 MP a, nitrogen pressure 0 9 8 MP a... ) Are, 7 5 E - 5 and (P a • m 3 Z s ) ,
熱履歴後の破断時伸び率 (% (縦横方向の値の う ち 低い 方の値) ) は、 0 . 8 0 % とな り 、  The elongation at break (% (lower of the values in the vertical and horizontal directions)) after thermal history is 0.80%,
実機 ライ ン に組み込み 2 3 0 °Cで保持 した場合の割れ発 生までの 日 数は、 3 6 0 日 以上となっ た。  The number of days until cracking occurred when it was installed at 230 ° C in the actual machine line was over 360 days.
各成分の配合量および試験結果を表 1 に併せて示す。 【実施例 3 】  Table 1 shows the amounts of each component and the test results. [Embodiment 3]
N B R ラ テ ッ ク ス を固形分重量にて 1 6 k g 、 炭酸カ ル シゥム 9 6 k g 、 粉末状硫黄 0 . 2 k g 、 粉末状亜鉛華 0 . 2 k g , 界面活性剤を 固形分重量にて 1 k g 、 感熱剤を 固 形分重量にて 0 . 4 k g 、 増粘剤を固形分重量にて 0 . 5 k g を混合 し水 9 6 . 5 リ ツ トルで希釈する こ と によ り 、 バイ ンダー混合液を調製した。  16 kg of NBR latex by solid weight, 96 kg of calcium carbonate, 0.2 kg of powdered sulfur, 0.2 kg of powdered zinc white, surfactant by weight of solid content By mixing 1 kg, the heat-sensitive agent in a solid content of 0.4 kg and the thickener in a solid content of 0.5 kg, and diluting with 96.5 liters of water, A binder mixture was prepared.
次いで、 p — ァ ラ ミ ド繊維を用 い製造 したニー ドルパ ン チフ ェル ト 8 k g を用 いた以外は、 実施例 1 と 同様に して、 含浸工程、 乾燥工程お よび成型工程を行い、 シー ト 状シー ル材を製造 した。  Next, the impregnation step, the drying step, and the molding step were performed in the same manner as in Example 1 except that 8 kg of the needle punch made using p-aramid fiber was used. Manufacture of sheet-like seal material.
得 ら れた シー ト状シール材の引張強さ ( J I S R 3 4 5 3 準拠) は、 高強度方向 (縦方向、 a ) では 2 6 . 3 M P a 、 低強度方向 (横方向、 b ) では 2 3 . I M P a と な り 、 強度異方性 ( a Z b ) は 1 . 1 となっ た。 また、 常温 シール性 ( A S T M F 3 7 — B に準拠。 面圧 1 9 . 6 M P a 、 窒素内圧 0 . 9 8 M P a ) は、 8 . 4 E - 5 ( P a • m 3 / s ) と な り 、 The tensile strength (according to JISR3453) of the obtained sheet-like sealing material is 26.3 M in the high strength direction (vertical direction, a). In the low strength direction (transverse direction, b), Pa was 23. IMPa, and the strength anisotropy (aZb) was 1.1. The room-temperature sealability (conforming to ASTMF 37 — B. Surface pressure: 19.6 MPa, nitrogen internal pressure: 0.98 MPa) is 8.4 E-5 (Pa • m 3 / s). ,
熱履歴後の破断時伸び率 (% (縦横方向の値の う ち低い 方の値) ) は、 3 . 0 0 % とな り 、  The elongation at break (% (lower of the values in the vertical and horizontal directions)) at break after thermal history is 3.00%.
実機 ライ ンに組み込み 2 3 0 °Cで保持した場合の割れ発 生までの 日 数は、 3 6 0 日 以上 となっ た。  The number of days until the occurrence of cracks when it was installed at 230 ° C in the actual machine line was more than 360 days.
各成分の配合量および試験結果を表 1 に併せて示す。 【参考例 1 】  Table 1 shows the amounts of each component and the test results. [Reference example 1]
N B R ラテ ッ ク ス を固形分重量にて 3 k g 、 炭酸カ ルシ ゥム 9 6 k g 、 粉末状硫黄 0 . 1 k g 、 粉末状亜鉛華 0 . 1 k g 、 界面活性剤を固形分重量にて 0 . 4 k g 、 感熱剤 を 固形分重量にて 0 . 1 6 k g 、 増粘剤を固形分重量にて 0 . 2 k g を混合 し水 9 6 . 5 リ ッ トルで希釈する こ と に よ り 、 バイ ンダー混合液を調製した。  3 kg of NBR latex by solid weight, 96 kg of calcium carbonate, 0.1 kg of powdered sulfur, 0.1 kg of powdered zinc white, 0.1 kg of surfactant by solid weight By mixing 4 kg, 0.16 kg of the heat sensitive agent by solid weight and 0.2 kg of the thickener by solid weight, and diluting with 96.5 liters of water. A binder mixture was prepared.
次いで、 p — ァ ラ ミ ド繊維を用 い製造 したニー ド ルパ ン チフ ェル ト 7 . 5 k g を用 いた以外は、 実施例 1 と 同様に して、 含浸工程、 乾燥工程およ び成型工程 を行い、 シー ト 状シール材を製造した。 ' 得 ら れたシー ト 状シール材の引張強さ ( J I S R 3 4 5 3 準拠) は、 高強度方向 (縦方向、 a ) では 7 . 5 M P a 、 低強度方向 (横方向、 b ) では 7 . 2 M P a とな り 、 強度異方性 ( a / b ) は 1 . 0 となっ た。 ま た、 常温シー ル性 ( A S T M F 3 7 — B に準拠。 面圧 1 9 . 6 M P a 、 窒素内圧 0 . 9 8 M P a ) は、 2 . 5 E - 3 ( P a · m 3 Z s ) とな り 、 Next, the impregnation step, the drying step, and the molding were carried out in the same manner as in Example 1 except that 7.5 kg of the needle pan carbonate produced using p-aramid fiber was used. The process was performed to produce a sheet-like sealing material. '' The tensile strength of the obtained sheet-like sealing material (according to JISR3453) is 7.5 MPa in the high-strength direction (vertical direction, a) and 7.5 MPa in the low-strength direction (horizontal direction, b). 7.2 MPa, The strength anisotropy (a / b) was 1.0. Also, cold seal resistance (ASTM F 3 7 - compliant B surface pressure 1 9 6 MP a, nitrogen pressure 0 9 8 MP a... ) Is, 2 5 E -. 3 ( P a · m 3 Z s )
熱履歴後の破断時伸び率 ( % (縦横方向の値の う ち低い 方の値) ) は、 0 . 7 0 % とな り 、  The elongation at break after heat history (% (the lower of the values in the vertical and horizontal directions)) is 0.70%,
実機ライ ン に組み込み 2 3 0 でで保持 した場合の割れ発 生までの 日 数は、 1 8 0 日 となっ た。  The number of days until the occurrence of cracks when it was installed in the actual machine line and held at 230 was 180 days.
各成分の配合量および試験結果を表 1 に併せて示す。  Table 1 shows the amounts of each component and the test results.
【比較例 1 】  [Comparative Example 1]
以下の組成を有する ジ ョ イ ン ト シ一 卜 形成用組成物を調 製した。  A composition for forming a joint sheet having the following composition was prepared.
フ ィ ブリ ル化 し た芳香族ア ミ ド繊維 1 0 . 8 重量%10.8% by weight of fibrillated aromatic amide fiber
N B R 1 5 . 9 重量% ゴム薬品 2 . 3 重量% 無機充填剤 (重炭、 ク レー) 7 1 . 0 重量% トルエ ン 上記混合物 1 k g に対 して 0 . 7 リ ッ トル の割合 NBR 15.9% by weight Rubber chemicals 2.3% by weight Inorganic fillers (heavy coal, clay) 71.0% by weight Toluene 0.7 liter per 1 kg of the above mixture
得 ら れた組成物を 1 3 0 °C に保たれた熱ロ ールと 3 0 °C に保たれた冷却 ロール と の間 に挿入 して加熱圧延 した。 こ のよ う にする と、 該組成物は熱 ロール側に シー ト状に粘層 さ れた。 こ の シー ト状物 を熱 ロールか ら ド ク ターブレー ド によ り 剥離 して厚さ 1 . 5 m mのジ ョ イ ン ト シー ト を得た。  The obtained composition was inserted between a hot roll kept at 130 ° C. and a cooling roll kept at 30 ° C. and rolled by heating. In this way, the composition was formed into a sheet-like viscous layer on the hot roll side. The sheet was peeled off from the heat roll with a doctor blade to obtain a 1.5 mm thick joint sheet.
得 ら れた ジ ョ イ ン ト シー ト の引張強さ ( J I S R 3 4 5 3 準拠) は、 高強度方向 (縦方向、 a ) では 4 2 . 7 M P a 、 低強度方向 (横方向、 b ) では 1 7 . 1 M P a とな り 、 強度異方性 ( a Z b ) は 2 . 5 となっ た。 また、 常温 シール性 ( A S T M F 3 7 — B に準拠。 面圧 1 9 . 6 M P a 、 窒素内圧 0 . 9 8 M P a ) は、 3 . 1 E — 4 ( P a • m 3 / s ) とな り 、 The tensile strength of the obtained joint sheet (JISR 34 53 compliant) is 42.7 MPa in the high strength direction (vertical direction, a), 17.1 MPa in the low strength direction (horizontal direction, b), and the strength anisotropy (a Z b) was 2.5. In addition, the room temperature sealability (conforming to ASTMF 37-B. The surface pressure is 19.6 MPa and the internal pressure of nitrogen is 0.98 MPa) is 3.1 E—4 (Pa • m 3 / s). ,
熱履歴後の破断時伸び率 ( % (縦横方向の値の う ち 低い 方の値) ) は、 0 . 2 5 % とな り 、  The elongation at break (% (lower of the values in the vertical and horizontal directions)) after thermal history is 0.25%,
実機ラ イ ン に組み込み 2 3 0 で保持した場合の割れ発 生までの 日 数は、 1 2 0 日 となっ た。  The number of days until the occurrence of cracks when it was installed in the actual machine line and held at 230 was 120 days.
各成分の配合量および試験結果を表 1 に併せて示す。 【比較例 2 】  Table 1 shows the amounts of each component and the test results. [Comparative Example 2]
以下の組成を有する ジ ョ イ ン ト シ一 ト形成用組成物を調 製した。  A composition for forming a joint sheet having the following composition was prepared.
石綿繊維 7 5 . 3 重量% 75.3% by weight asbestos fiber
S B R 1 2 . 5 重量% SBR 12.5% by weight
ゴム薬品 3 . 2 重量% Rubber chemicals 3.2% by weight
無機充填剤 (ク レ一 ) 9 . 0 重暈% Inorganic filler (Cream) 9.0 Deep halo%
ト ルエ ン 上記混合物 1 k g に対して 0 . 7 リ ッ ト ルの割合 Toluene 0.7 liters per 1 kg of the above mixture
得 ら れた上記組成物を用 いた以外は、 比較例 1 と 同様に してジ ョ イ ン ト シ一 卜 を得た。  A jump sheet was obtained in the same manner as in Comparative Example 1 except that the obtained composition was used.
得 ら れたジ ョ イ ン ト シー ト の 引張強さ ( J I S R 3 4 The tensile strength of the obtained joint sheet (JISR 34
5 3 準拠) は、 高強度方向 (縦方向、 a ) では 8 2 . 4 M P a 、 低強度方向 (横方向、 b ) では 3 0 . 6 M P a とな り 、 強度異方性 ( a / b ) は 2 . 7 となっ た。 また、 常温 シ一ル性 ( A S T M F 3 7 — B に準拠。 面圧 1 9 . 6 M P a 、 窒素内圧 0 . 9 8 M P a ) は、 1 . 7 E — 3 ( P a • m 3 / s ) とな り 、 5 3 compliant) is 82.4 M in the high strength direction (vertical direction, a) P a was 30.6 MPa in the low strength direction (lateral direction, b), and the strength anisotropy (a / b) was 2.7. In addition, room temperature sealability (based on ASTMF 37 — B. Surface pressure of 19.6 MPa, internal pressure of nitrogen 0.98 MPa) is 1.7 E — 3 (Pa • m 3 / s )
熱履歴後の破断時伸び率 (% (縦横方向の値の う ち 低い 方の値) ) は、 1 . 0 2 % とな り 、  The elongation at break (% (lower of the values in the vertical and horizontal directions)) at break after thermal history is 1.02%,
実機ライ ン に組み込み 2 3 0 °Cで保持 した場合の割れ発 生までの 日 数は、 3 6 0 日 以上となっ た。  The number of days until cracking when it was installed at 230 ° C in the actual machine line was more than 360 days.
各成分の配合量および試験結果を表 1 に併せて示す。 【比較例 3 】  Table 1 shows the amounts of each component and the test results. [Comparative Example 3]
以下の組成を有する 水分散ス ラ リ ーを調製した。  An aqueous dispersion slurry having the following composition was prepared.
セ ラ ミ ッ ク繊維 1 4 重量% Ceramic fiber 14% by weight
セルロース繊維 5 重量% Cellulose fiber 5% by weight
ロ ッ ク ウール繊維 1 4 重量% Rock wool fiber 14% by weight
無機充填剤 (ク レ一 ) 5 9 重量% Inorganic filler (creative) 59% by weight
N B R ラテ ッ ク ス 8 重量% NBR Latex 8% by weight
得 ら れた組成物を丸網式抄造機にて抄造し、 次いで乾燥 およびプレスする こ と によ り ビー夕ーシー ト を得た。  The obtained composition was formed into a paper by a round-mesh paper machine, and then dried and pressed to obtain a bead sheet.
得 ら れた ビー夕一シー ト の引張強さ ( J I S R 3 4 5 3 準拠) は、 高強度方向 (縦方向、 a ) では 3 6 . 2 M P a 、 低強度方向 (横方向、 b ) では 1 2 . 7 M P a とな り 、 強度異方性 ( a / b ) は 2 . 9 となっ た。 また、 常温シー ル性 ( A S T M F 3 7 — B に準拠。 面圧 1 9 . 6 M P a , 窒素内圧 0 . 9 8 M P a ) は、 6 . 3 E - 2 ( P a · mThe tensile strength (according to JISR3453) of the obtained beef sheet is 36.2 MPa in the high-strength direction (vertical direction, a) and 36.2 MPa in the low-strength direction (lateral direction, b). 12.7 MPa and the strength anisotropy (a / b) was 2.9. In addition, room temperature sealability (based on ASTMF 37-B. Surface pressure 19.6 MPa, The internal pressure of nitrogen 0.98 MPa) is 6.3 E-2 (P
/ s ) となっ た。 / s).
各成分の配合量および試験結果を表 1 に併せて示す。 Table 1 shows the amounts of each component and the test results.
Figure imgf000045_0001
Figure imgf000045_0001
上記実施例、 参考例、 比較例を見れば、 本発明の製造方 法では、 不織布 となる不織布の繊維種に制限がない こ とが 分か る。 From the above Examples, Reference Examples and Comparative Examples, it can be seen that the production method of the present invention does not limit the fiber type of the nonwoven fabric to be a nonwoven fabric.
( a ) 本発明の製造方法によれば、 p — ァ ラ ミ ド繊維の みな らず、 カ レ ンダー ロール性能に よ る ジ ョ イ ン ト シー ト では通常困難と さ れてい る炭素繊維あ る い はガ ラス繊維を 唯一の繊維種 とする シー ト状シール材も製造可能と な っ て いる 。  (a) According to the production method of the present invention, not only p-aramid fiber but also carbon fiber fiber, which is usually difficult in a joint sheet due to calendar roll performance, is used. Alternatively, sheet-like sealing materials using glass fiber as the only fiber type can be manufactured.
ま た、 本発明の製造方法によれば、 上記繊維の他、 セ ラ ミ ッ ク繊維、 鉱物系繊維、 P P S 繊維や m— ァ ラ ミ ド繊維 等の有機系繊維を唯一の繊維種とする シー ト 状シール材、 およ び P P S 繊維 とセ ラ ミ ッ ク繊維を混合 したシー ト 状シ 一ル材も製造可能であ っ た。  Further, according to the production method of the present invention, in addition to the above-mentioned fibers, organic fibers such as ceramic fibers, mineral fibers, PPS fibers and m-aramid fibers are used as the sole fiber type. Sheet-like sealing materials, and sheet-like sealing materials in which PPS fibers and ceramic fibers were mixed, could also be manufactured.
( b ) 本発明の製造方法によ り 得 ら れる シー ト状シール 材は、 「熱履歴後の破断時伸び率」 の結果か ら 、 従来の製 法に よ る ノ ンアスベス ト ジ ョ イ ン ト シー ト と比較 して、 高 温条件下にお ける硬化の程度が軽減さ れてい る こ と が分か る。  (b) The sheet-like sealing material obtained by the production method of the present invention shows the non-asbestos joint obtained by the conventional production method based on the result of “elongation at break after thermal history”. It can be seen that the degree of curing under high temperature conditions is reduced as compared with toseat.
( c ) 本発明の製造方法によれば、 シー ト状シール材の 強度異方性の改善さ れたシー ト状シール材が得 ら れる こ と が分かる。  (c) It can be seen that according to the production method of the present invention, a sheet-like sealing material having improved strength anisotropy of the sheet-like sealing material can be obtained.
常態下の 引張強さ ( J I S R 3 4 5 3 に準拠) にお い て縦方 向 の値 a を横方向 の値 b で割 っ た も の ( a/b ) を 強度異方性 とする と、 二次元的に極めて高い等方性を有 し ている こ と力 s分かる。 In the tensile strength under normal conditions (based on JISR 3453), the value (a / b) obtained by dividing the value a in the vertical direction by the value b in the horizontal direction is defined as the strength anisotropy. Has a very high two-dimensional isotropy I understand the power.
( d ) 本発明の製造方法によ り 高気密性シー ト状シール 材を製造可能であ る こ とが分かる。  (d) It can be seen that a highly airtight sheet-like sealing material can be manufactured by the manufacturing method of the present invention.
従来法で得 ら れ る ビー 夕 ー シー 卜 の シール性能 に 比 し て、 本案の シー ト 状シール材の シール性能はいずれも 、 ガ ス シールを 目 的 と したシー ト状シール材 と して十分な シー ル性能を有してい る こ とが分かる。  Compared to the sealing performance of the bead sheet obtained by the conventional method, the sealing performance of the sheet-shaped sealing material of the present invention is much lower than that of gas-sealing. It turns out that it has sufficient sealing performance.

Claims

請 求 の 範 囲 The scope of the claims
1 .  1.
有機系バイ ンダー と しての ゴム材 と、 ゴム薬品 と、 前記 ゴム材用 の溶剤または分散媒 と を混合 し、  A rubber material as an organic binder, a rubber chemical, and a solvent or a dispersion medium for the rubber material are mixed,
得 ら れたバイ ンダー混合液を、 基材繊維か ら なる不織布 に、 該不織布内部に存在する気体を追い 出す と と も に含浸 させ、  The obtained binder mixed solution is impregnated into a nonwoven fabric made of a base fiber while expelling gas present inside the nonwoven fabric,
上記混合液が含浸さ れた不織布か ら 少な く と も一部の溶 剤または分散媒を揮散 · 除去し、  At least a part of the solvent or dispersion medium is volatilized and removed from the nonwoven fabric impregnated with the above mixed solution,
次いで こ の不織布を加熱圧縮して、 上記ゴム材を加硫さ せて シー ト 状シール材を得る こ と を特徴とする シ一 ト状シ 一ル材の製造方法。  Then, the nonwoven fabric is heated and compressed, and the rubber material is vulcanized to obtain a sheet-like seal material. A method for producing a sheet-like seal material.
2 .  2.
前記バイ ンダー混合液が、 ラテ ッ ク ス の形態で用 い ら れ る こ と を特徴 とする請求の範囲第 1 項に記載の シー ト 状シ 一ル材の製造方法。  2. The method for producing a sheet-like sealing material according to claim 1, wherein the binder mixed solution is used in the form of a latex.
3 ·  3 ·
有機系バイ ンダー と し ての樹脂と、 前記樹脂用溶剤また は分散媒 と を混合 し、  A resin as an organic binder is mixed with the solvent for a resin or a dispersion medium,
得 ら れたバイ ンダー混合液を、 基材繊維か ら なる不織布 に、 該不織布内部に  The obtained binder mixed solution is applied to a non-woven fabric made of the base fiber and the inside of the non-woven fabric.
存在する気体を追い出すと と も に含浸させ、 Expelling the existing gas and impregnating it,
上記混合液が含浸さ れた不織布か ら 少な く と も一部の溶 剤または分散媒を揮散 · 除去し、 At least a part of the non-woven fabric impregnated with the above mixture Volatilizes and removes the agent or dispersion medium,
次いで こ の不織布を加熱圧縮 して、 上記樹脂を硬化 さ せ てシー ト 状シール材を得る こ と を特徴 とする シー ト 状シー ル材の製造方法。  Then, the nonwoven fabric is heated and compressed, and the resin is cured to obtain a sheet-like sealing material. A method for producing a sheet-like sealing material.
4 .  Four .
基材繊維が非石綿系繊維であ る こ と を特徴 とする請求の 範囲第 1 項または第 3 項に記載の方法。  4. The method according to claim 1, wherein the base fiber is a non-asbestos fiber.
5 .  Five .
不織布がフ ェル 卜状であ る こ と を特徴 とする請求の範囲 第 1 項〜第 4 項のいずれかに記載の方法。  The method according to any one of claims 1 to 4, wherein the nonwoven fabric is in the form of a felt.
6 .  6.
バイ ンダー混合液が充填剤を含む こ と を特徴 とする請求 の範囲第 1 項〜第 5 項のいずれかに記載の方法。  The method according to any one of claims 1 to 5, wherein the binder mixture contains a filler.
7 .  7.
不織布内部に存在する気体を追い出すと と も にパイ ンダ 一混合液を含浸させる工程を、 あ ら か じめ不織布を圧縮 し た ま まバイ ンダー混合液中 に浸潰するか、 バィ ンダー混合 液中で不織布を圧縮し た上、 こ れをバイ ンダー混合液中 に て 自発復元さ せる こ と によ り 行な う こ と を特徴 とする請求 の範囲第 1 項〜第 6 項のいずれかに記載の方法。  The process of expelling the gas present inside the non-woven fabric and impregnating it with the binder-mixture is carried out by immersing the non-woven fabric in the binder mixture while compressing the non-woven fabric in advance, or by using a binder mixture. The method according to any one of claims 1 to 6, wherein the non-woven fabric is compressed in a binder mixture and spontaneously restored in a binder mixture. The method described in.
8 .  8.
不織布内部に存在する気体を追い 出す と と も にバイ ンダ 一混合液を含浸さ せる 工程 を、 バイ ンダー混合液を不織布 に高圧噴霧する こ と に よ り 行な う こ と を特徴とする請求の 範囲第 1 項〜第 6 項のいずれかに記載の方法。 Claims: The step of expelling gas present inside the nonwoven fabric and impregnating it with a binder mixture by spraying the binder mixture onto the nonwoven fabric under high pressure. of 7. The method according to any of paragraphs 1 to 6.
9 . 9.
不織布内部に存在する気体を追い出すと と も にバイ ンダ 一混合液を含浸さ せる 工程 を、 減圧容器に不織布を入れ容 器内部を減圧下に したのちバイ ンダー混合液を注入する こ と によ り 行な う こ と を特徴とする請求の範囲第 1 項〜第 6 項のいずれかに記載の方法。  The process of expelling the gas present inside the nonwoven fabric and impregnating it with the binder mixture is carried out by putting the nonwoven fabric in a vacuum container, reducing the pressure inside the container, and then injecting the binder mixture. The method according to any one of claims 1 to 6, wherein the method is performed.
PCT/JP2001/006542 2000-09-28 2001-07-30 Process for producing sheet-form sealing material WO2002026870A1 (en)

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JP2007092904A (en) * 2005-09-29 2007-04-12 Nichias Corp Sheet gasket and its manufacturing method
CN105121706B (en) * 2013-11-13 2018-04-06 日东电工株式会社 Anti-corrosion piece and its manufacture method

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JPS6364704A (en) * 1986-09-04 1988-03-23 Sumitomo Electric Ind Ltd Continuous resin-impregnating equipment for fiber bundle
JPS63159018A (en) * 1986-12-24 1988-07-01 Takuma Sogo Kenkyusho:Kk Device for varnish impregnation
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