WO2018070443A1 - Agent de traitement de fibre et étoffe non tissée perméable aux liquides le contenant - Google Patents

Agent de traitement de fibre et étoffe non tissée perméable aux liquides le contenant Download PDF

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Publication number
WO2018070443A1
WO2018070443A1 PCT/JP2017/036869 JP2017036869W WO2018070443A1 WO 2018070443 A1 WO2018070443 A1 WO 2018070443A1 JP 2017036869 W JP2017036869 W JP 2017036869W WO 2018070443 A1 WO2018070443 A1 WO 2018070443A1
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WIPO (PCT)
Prior art keywords
nonwoven fabric
carbon atoms
component
processing agent
fiber processing
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PCT/JP2017/036869
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English (en)
Japanese (ja)
Inventor
早織 田中
矢放　正広
一史 加藤
文明 山下
Original Assignee
旭化成株式会社
日華化学株式会社
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Application filed by 旭化成株式会社, 日華化学株式会社 filed Critical 旭化成株式会社
Priority to CN201780063373.5A priority Critical patent/CN109844214B/zh
Priority to JP2018545033A priority patent/JP7146641B2/ja
Publication of WO2018070443A1 publication Critical patent/WO2018070443A1/fr

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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00—Bandages or dressings; Absorbent pads
    • A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
    • A61F13/51—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the outer layers
    • A61F13/511—Topsheet, i.e. the permeable cover or layer facing the skin
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/144—Alcohols; Metal alcoholates
    • D06M13/148—Polyalcohols, e.g. glycerol or glucose
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/165—Ethers
    • D06M13/17—Polyoxyalkyleneglycol ethers
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53—Polyethers
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/647—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing polyether sequences

Definitions

  • the present invention relates to a fiber processing agent capable of imparting excellent wettability and repeated water permeability to a nonwoven fabric, a liquid-permeable nonwoven fabric containing the fiber processing agent, and a hygiene using the liquid-permeable nonwoven fabric Regarding materials.
  • Patent Document 1 proposes a polyolefin-based nonwoven fabric provided with a hydrophilic treating agent containing a specific polyether and a polyether-modified silicone.
  • a hydrophilic treating agent containing a specific polyether and a polyether-modified silicone containing a specific polyether and a polyether-modified silicone.
  • the problem to be solved by the present invention is composed of a fiber processing agent capable of improving the wettability and repeated water permeability of a nonwoven fabric, and a fiber provided with the fiber processing agent. Is to provide a non-woven fabric.
  • the present inventors have conducted intensive studies and repeated experiments.
  • the specific component (A) represented by the general formula (1) and the specific component represented by the general formula (2) ( In combination with B) the balance between hydrophilicity and hydrophobicity is maintained, the compatibility with the nonwoven fabric and the compatibility with body fluids such as urine are compatible, and the initial water permeability, wettability, and repeated water permeability are excellent.
  • the present inventors have found that a nonwoven fabric can be provided and have completed the present invention.
  • R 1 and R 3 are each independently a hydrogen atom, an alkyl group having 1 to 24 carbon atoms, an alkenyl group having 2 to 24 carbon atoms, an alkanoyl group having 2 to 24 carbon atoms, or 2 to 24 carbon atoms.
  • R 4 is an alkylene group having 1 to 12 carbon atoms, an alkenylene group having 2 to 12 carbon atoms, or an arylene group having 6 to 12 carbon atoms
  • X is a hydrogen atom or an anion
  • R 2 is an alkylene group having 1 to 12 carbon atoms, an alkenylene group having 2 to 12 carbon atoms, or an arylene group having 6 to 12 carbon atoms
  • 2 and A 3 are each independently an alkylene group having 2 to 4 carbon atoms
  • l is an integer of 0 or 1 to 1000
  • m is an integer of 0 or 1 to 1000
  • n Is an integer of 0 or 1-100.
  • the component (B) represented by; A fiber processing agent containing [2] The fiber processing agent according to [1], further including a polyether-modified silicone as the component (C).
  • the nonwoven fabric coated with the fiber processing agent according to the present invention is excellent in initial water permeability, wettability, and repeated water permeability. Therefore, sanitary materials such as sanitary napkins, incontinence pads, disposable diapers and other top sheets and second sheets are used. Or, for example, masks, warmers, tape base materials, patch base materials, emergency bandages, packaging materials, wipe products, medical gowns, bandages, clothing, skin care sheets, etc. It can be preferably used.
  • the fiber processing agent of this embodiment has the following general formula (1): HO— (A 1 O) p —H: General formula (1) ⁇ In the formula, A 1 is an alkylene group having 2 to 4 carbon atoms, and p is an integer of 1 to 3. ⁇ (A); and the following general formula (2) different from the component (A): R 1 —O— (A 2 O) 1 — ⁇ C (O) R 2 C (O) — (A 3 O) m ⁇ n —R 3 ...
  • R 1 and R 3 are each independently a hydrogen atom, an alkyl group having 1 to 24 carbon atoms, an alkenyl group having 2 to 24 carbon atoms, an alkanoyl group having 2 to 24 carbon atoms, or 2 to 24 carbon atoms.
  • R 4 is an alkylene group having 1 to 12 carbon atoms, an alkenylene group having 2 to 12 carbon atoms, or an arylene group having 6 to 12 carbon atoms
  • X is a hydrogen atom or an anion
  • R 2 is an alkylene group having 1 to 12 carbon atoms, an alkenylene group having 2 to 12 carbon atoms, or an arylene group having 6 to 12 carbon atoms
  • 2 and A 3 are each independently an alkylene group having 2 to 4 carbon atoms
  • l is an integer of 0 or 1 to 1000
  • m is an integer of 0 or 1 to 1000
  • l + n is 1 or more.
  • the component (B) represented by; Containing.
  • a 1 is an alkylene group having 2 to 4 carbon atoms
  • p is an integer of 1 to 3.
  • a 1 is an alkylene group having 2 to 4 carbon atoms, but an alkylene group having 3 to 4 carbon atoms is preferable and an alkylene group having 3 carbon atoms is more preferable from the viewpoints of wettability and repeated water permeability.
  • p represents the degree of polymerization of the alkyleneoxy group represented by (A 1 O) and is an integer of 1 to 3, preferably 1 to 2 and more preferably 1 from the viewpoints of wettability and repeated water permeability. preferable.
  • the component (A) is, for example, an alkylene glycol having 2 to 4 carbon atoms such as ethylene glycol, propylene glycol, butylene glycol, and the like, such as ethylene oxide, propylene oxide, butylene oxide, etc. at 80 to 200 ° C. under a base catalyst. It can be obtained by adding an alkylene oxide having 2 to 4 carbon atoms.
  • a base catalyst for example, potassium hydroxide, sodium hydroxide and the like can be used.
  • Commercially available ethylene glycol, propylene glycol, butylene glycol, diethylene glycol, dipropylene glycol, dibutylene glycol, triethylene glycol, tripropylene glycol, tributylene glycol, and the like may be used.
  • R 1 and R 3 are each independently a hydrogen atom, an alkyl group having 1 to 24 carbon atoms, an alkenyl group having 2 to 24 carbon atoms, an alkanoyl group having 2 to 24 carbon atoms, An alkenoyl group having 2 to 24 carbon atoms or —C (O) —R 4 —COOX (where R 4 represents an alkylene group having 1 to 12 carbon atoms, an alkenylene group having 2 to 12 carbon atoms, or an arylene having 6 to 12 carbon atoms) And X is a hydrogen atom or anion.) And R 2 is an alkylene group having 1 to 12 carbon atoms, an alkenylene group having 2 to 12 carbon atoms, or an arylene group having 6 to 12 carbon atoms.
  • a 2 and A 3 are each independently an alkylene group having 2 to 4 carbon atoms, l is 0 or an integer of 1 to 1000, m is 0 or an integer of 1 to 1000, n is 0 or an integer of 1 to 100. However, since l + n is 1 or more and component (B) is a compound different from component (A), in this specification, general formula (2) is obtained by removing general formula (1). To do.
  • any one of R 1 and R 3 is an alkyl group having 1 to 24 carbon atoms, an alkenyl group having 2 to 24 carbon atoms, an alkanoyl group having 2 to 24 carbon atoms, or An alkenoyl group having 2 to 24 carbon atoms is preferable.
  • the carbon number is preferably 8 to 22, and more preferably 12 to 18.
  • alkyl group, alkenyl group, alkanoyl group and alkenoyl group may be linear or branched.
  • a 2 and A 3 are, independently of each other, an alkylene group having 2 to 4 carbon atoms, but from the viewpoints of rewetting, repeated water permeability, and processing bath stability, they are alkylene groups having 2 to 3 carbon atoms. Is preferred. From the same viewpoint, the polyalkyleneoxy groups represented by (A 2 O) 1 and (A 3 O) m are an alkyleneoxy group having 2 carbon atoms (ethyleneoxy group) and an alkyleneoxy group having 3 carbon atoms. It is more preferable to use (propyleneoxy group) together.
  • the addition method may be block addition or random addition.
  • l and m represent the degree of polymerization of the polyalkyleneoxy group represented by (A 2 O) l and (A 3 O) m , respectively, l represents 0 or an integer from 1 to 1000, and m represents 0 Alternatively, it represents an integer of 1 to 1000, and l and m are preferably 10 to 200 from the viewpoints of rewetting and repeated water permeability.
  • the component (B) represented by the general formula (2) preferably has an average molecular weight of 100,000 or less from the viewpoint of ease of handling.
  • component (B) examples include polyalkylene glycol (B1), polyoxyalkylene alkyl ether (B2), alkyleneoxy group adduct (B3) of divalent carboxylic acid, esterified product (B4) thereof and the like. be able to.
  • Polyalkylene glycol (B1) can be obtained, for example, by adding an alkylene oxide to a divalent alcohol.
  • the polyoxyalkylene alkyl ether (B2) can be obtained, for example, by adding an alkylene oxide to a monovalent alcohol.
  • a base catalyst such as potassium hydroxide or sodium hydroxide may be used at 80 to 200 ° C.
  • Examples of the divalent alcohol include ethylene glycol, propylene glycol, butylene glycol and the like.
  • Examples of monohydric alcohols include alcohols having 1 to 24 carbon atoms. Such an alcohol may have a branch or a double bond.
  • As the alkylene oxide an alkylene oxide having 2 to 4 carbon atoms such as ethylene oxide, propylene oxide, butylene oxide can be used. When two or more types of alkylene oxide are used, the addition method may be a block or random.
  • the alkyleneoxy group adduct (B3) of a divalent carboxylic acid can be obtained, for example, by adding an alkylene oxide to a divalent carboxylic acid or by reacting a divalent carboxylic acid with a polyalkylene glycol.
  • the esterified product (B4) is, for example, the polyalkylene glycol (B1), the polyoxyalkylene alkyl ether (B2), and / or the alkyleneoxy group adduct (B3) of a divalent carboxylic acid obtained above.
  • Monovalent and / or divalent carboxylic acids can be obtained by reacting at about 100 to 300 ° C. according to a conventional method. This reaction may be non-catalytic or may use a catalyst such as sulfuric acid or paratoluenesulfonic acid.
  • Examples of monovalent carboxylic acids include carboxylic acids having 1 to 24 carbon atoms. Such a carboxylic acid may have a branch or a double bond.
  • Examples of the divalent carboxylic acid include aromatic dicarboxylic acids such as terephthalic acid, isophthalic acid and phthalic acid, and aliphatic dicarboxylic acids such as 1,4-cyclohexanedicarboxylic acid, adipic acid, sebacic acid, maleic acid and succinic acid. Can be mentioned. Among these, from the viewpoints of wettability and repeated water permeability, aliphatic dicarboxylic acids are preferably used, and adipic acid and succinic acid are more preferably used.
  • the blending ratio of the component (A) is less than the lower limit value, the wettability tends to decrease, and when the blending ratio of the component (A) exceeds the upper limit value, the water permeability tends to decrease repeatedly.
  • a polyether-modified silicone may be further added to the fiber processing agent of the present embodiment as the component (C) for improving the initial water permeability (45-degree inclined flow length). It can.
  • the blending ratio of component (C) is preferably 5% by mass to 50% by mass with respect to the total amount of component (A) and component (B). % To 30% by mass is more preferable.
  • a commercially available polyether-modified silicone can be used as the component (C).
  • the polyether-modified silicone used as the component (C) is not particularly limited, but those having an HLB of 5 to 15 are preferably used from the viewpoints of rewetting, repeated water permeability, and 45 ° gradient flow length. Further, those having a viscosity of 50 to 10,000 cSt are preferably used.
  • the fiber processing agent of the present embodiment may contain other compounds depending on the desired purpose as long as the desired effect is not impaired. I do not care.
  • various surfactants as emulsifiers, softeners, smoothing agents, antistatic agents, and antifoaming agents can be appropriately contained.
  • the adhesion amount of the fiber processing agent varies depending on the intended use.
  • the total amount of the essential components A and B is 0.05% by weight to 1.50 with respect to the nonwoven fabric. It is preferable to apply so as to adhere by weight.
  • the amount of fiber processing agent mixed with component A, component B, component C, and other compounds is 0.10% by weight to 1% in a pure amount (pure amount) excluding a solvent for diluting the processing agent such as water.
  • a range of .50% by weight is preferable, and 0.15% to 1.20% by weight is more preferable. If it is less than 0.05% by weight, satisfactory water permeation performance cannot be obtained. On the other hand, if it exceeds 1.50% by weight, skin irritation or rash may occur.
  • the fiber processing agent When applying the fiber processing agent to the nonwoven fabric, it is also effective to directly apply each of the component (A), the component (B), and the component (C) or a mixture of these to the nonwoven fabric. However, it is preferable to mix in advance, dilute with a solvent such as water, and apply to the nonwoven fabric as an aqueous fiber processing agent solution.
  • the fiber processing agent of the present embodiment is obtained by mixing and homogenizing the component (A), the component (B), and optionally the component (C), and the other compound described above, preferably at a temperature equal to or higher than the melting point. be able to.
  • a known method such as a dipping method, a spraying method, or a coating method can be adopted, and after applying the fiber processing agent, it may be dried using a drying means such as hot air or a hot roll.
  • a drying means such as hot air or a hot roll.
  • the application amount of the aqueous fiber processing agent solution is small so as not to cause insufficient drying in the drying process accompanying the speeding up of the nonwoven fabric production facility.
  • the coating amount (% by weight) with respect to the nonwoven fabric is preferably 1.0% to 65% by weight, more preferably 3.0% to 60% by weight, and still more preferably 5.0% by weight in any of the application methods. % By weight to 50% by weight. If the amount is less than 1.0% by weight, uniform coating cannot be obtained. On the other hand, if the amount exceeds 65% by weight, the required drying capacity increases, the equipment cost increases, and insufficient drying may occur.
  • the concentration of the fiber processing agent to be applied is preferably 0.05% by weight to 100% by weight.
  • a coating method is generally used.
  • Known coating methods include kiss coaters and dies, but it is preferable to use a gravure application method because the fiber processing agent can be applied uniformly in the nonwoven fabric width direction.
  • the gravure roll handle may be a lattice type or a pyramid type, but is preferably a diagonal type in which the fiber processing agent hardly remains on the bottom of the gravure cell.
  • the cell volume is preferably 5 cm 3 / m 2 to 40 cm 3 / m 2 . If it is less than 5 cm ⁇ 3 > / m ⁇ 2 >, since the application amount is too small, uniform application of the fiber processing agent becomes difficult.
  • the cell depth of the gravure roll is preferably 10 ⁇ m to 80 ⁇ m, and the interval is preferably designed to be within the range of 80 mesh to 250 mesh so as to have the above cell volume.
  • the method for scraping off the liquid on the surface of the gravure roll may be a doctor blade method using a general doctor made of a hardened steel plate or a rubber roll method using a roll having a rubber surface.
  • the suppression pressure in the case of the doctor blade method is preferably 0.5 kg / cm to 1.0 kg / cm, more preferably 0.6 kg / cm to 0.8 kg / cm.
  • the suppression pressure is preferably 1.0 kg / cm or more and 5.0 kg / cm or less, more preferably 1.5 kg / cm or more and 3.5 kg / cm or less, within a rubber hardness range of 60 ° or more and 80 ° or less. preferable.
  • the restraining pressure is within the above range, the amount of application of the fiber processing agent is less varied since the nonwoven fabric can be uniformly restrained in the width direction.
  • the application method by the spray method is preferable because it can cope with the high speed of the equipment, can be applied efficiently, and it is easy to maintain the thickness of the nonwoven fabric.
  • the spraying method may be a known spraying method by air compression or a method of directly compressing and spraying the aqueous fiber processing agent solution, but the rotor dampening method is preferred from the viewpoint of uniform application to the nonwoven fabric.
  • the rotor dampening method is a method in which a fiber processing agent aqueous solution is supplied onto a rotating rotor and the fiber processing agent aqueous solution is sprayed by using centrifugal force of rotor rotation.
  • the openings are limited so that the liquid particles of the fiber processing agent aqueous solution that is blown off by the rotation of the rotor in the application direction can be sprayed only on the nonwoven fabric side to be applied and can be uniformly applied in the width direction of the nonwoven fabric. It is possible to adjust the spray particle diameter according to the rotational speed of the rotor.
  • a rotor having a diameter of 40 mm to 100 mm is selected, and the nonwoven fabric surface to be applied and the center of the rotor so that the aqueous fiber processing agent solution can uniformly adhere in the width direction of the nonwoven fabric to be applied.
  • the rotors are preferably arranged in the width direction at an equal interval in the range of 60 mm to 220 mm to have two stages.
  • the point of applying uniformly is to make spray particles reach the inside of the nonwoven fabric to be applied, and the spray particle diameter is preferably 10 ⁇ m to 200 ⁇ m, more preferably 30 ⁇ m to 70 ⁇ m.
  • the surface tension of the aqueous fiber processing agent solution is important.
  • Spray particle diameter ( ⁇ m) ⁇ 100000 ⁇ ⁇ (surface tension (N / m)) ⁇ / (rotor diameter (mm) ⁇ rotor rotational speed (rpm)) Is calculated by
  • the temperature of the fiber processing agent aqueous solution in these coating methods is preferably 5 ° C. to 50 ° C., and more preferably 12 ° C. to 40 ° C. from the viewpoint of uniform dispersion and stability of the solution.
  • the viscosity of the aqueous fiber processing agent solution is preferably 0.5 mPa ⁇ s to 50 mPa ⁇ s, and more preferably 0.8 mPa ⁇ s to 20 mPa ⁇ s from the viewpoint of easier application. When the viscosity exceeds 50 mPa ⁇ s, the permeability of the aqueous fiber processing agent solution to the nonwoven fabric tends to be poor, and uniform application tends to be difficult.
  • a conventional drying method can be used for drying after the application of the aqueous fiber processing agent solution, and it is not particularly limited, and a known method using convection heat transfer, conduction heat transfer, radiant heat transfer, etc. is adopted.
  • Various drying methods such as a hot air circulation type, a hot air penetration type, an infrared heater type, a method of blowing hot air on both surfaces of the nonwoven fabric, and a method of introducing into a heated gas can be used.
  • the non-woven fabric of this embodiment is made of thermoplastic fibers, and may be a long-fiber non-woven fabric manufactured by a spunbond method or a short-fiber non-woven fabric manufactured by a card method or a wet papermaking method.
  • the fibers constituting the web are preferably long fibers produced by a spunbond method.
  • the long fiber means one having a fiber length of 55 mm or more.
  • the form of the thermoplastic fiber not only those having a round cross section, but also having a special cross section such as a flat cross section or a Y-shaped cross section, a hollow fiber or a crimped thread, can be used. It is not particularly limited.
  • the web may be a single layer, but may be laminated by spraying a web that is melt-spun by the melt blown method (M) on the web formed by the spunbond method (S).
  • M melt blown method
  • S spunbond method
  • the state of lamination may be laminated with SS, SSS, SSSS from the viewpoint of productivity, or may be laminated like SM, SMS, SMMS, SMSMS.
  • a method of joining the laminated webs a method of joining using an adhesive, a method of adhering with a low melting fiber or a composite fiber, a method of spraying a hot melt binder during web formation, a melt joining method, a needle punch, a water flow, etc. Any of the methods such as mechanical entanglement such as entanglement with hot air or joining with hot air may be used. However, it is preferable to join by partial thermocompression from the viewpoint of high-speed productivity.
  • the web can be bonded between heated embossed / flat rolls that can provide bonding points such as pinpoint, elliptical, diamond, and rectangular shapes.
  • the area ratio of thermocompression bonding in partial thermocompression bonding is preferably 5 to 40%, more preferably 5 to 25%, from the viewpoint of strength retention and flexibility.
  • a hot air from a viewpoint of maintaining the bulk of a nonwoven fabric and obtaining the cushioning texture preferred as a top sheet of sanitary materials. Any joining method using hot air can be used without particular limitation as long as it is a hot air circulation type, a hot air penetration type, or a method of wiping hot air on both surfaces of a nonwoven fabric.
  • thermoplastic resin constituting the thermoplastic fiber of the present embodiment examples include polyolefin resins such as polyethylene, polypropylene and copolymer polypropylene, and polyester resins such as polyethylene terephthalate, polybutylene terephthalate, polyethylene naphthalate and copolymer polyester.
  • Polyamide resins such as nylon-6, nylon-66, and copolymerized nylon
  • biodegradable resins such as polylactic acid, polybutylene succinate, and polyethylene succinate are not particularly limited.
  • polyolefin resins are preferred from the viewpoints of general use and convenience of recovery.
  • the fiber may be one type or a combination of two or more types of resins such as side-by-side and sheath core.
  • the average fineness of the nonwoven fabric fibers is preferably 0.45 dtex to 10.0 dtex, more preferably 0.55 dtex to 8.0 dtex, and still more preferably 0.86 dtex to 5.0 dtex. From the viewpoint of spinning stability, the average fineness is preferably 0.45 dtex or more, and from the viewpoint of the texture of the nonwoven fabric used for the sanitary material, it is preferably 10.0 dtex or less.
  • the basis weight of the nonwoven fabric is preferably 8 g / m 2 to 80 g / m 2 , more preferably 10 g / m 2 to 40 g / m 2 or less, still more preferably 10 g / m 2 to 30 g / m 2 . If the basis weight is 8 g / m 2 or more, the nonwoven fabric used for the sanitary material is strong, and if it is 80 g / m 2 or less, the texture of the nonwoven fabric used for the sanitary material is satisfied. It tends to be difficult to give a thick impression.
  • the nonwoven fabric to which the fiber processing agent of the present embodiment is applied preferably has the following characteristics in order to absorb urine and body fluids without stagnation.
  • the repetitive water permeability that is an index of water permeability of the nonwoven fabric of the present embodiment is preferably 70% or more at the fourth time. Since diapers are not changed every urination, body fluids such as urine need to be passed through without stagnation in non-woven fabrics used for top sheets and second sheets, even for the second and third urination. There is. If the value of the fourth cycle water permeability is less than 70%, for example, when used for a top sheet or a second sheet of a disposable diaper, the water cannot be sufficiently passed to the urine after the second time, which causes urine leakage. there is a possibility.
  • the wettability as an index of water permeability of the nonwoven fabric of this embodiment is 0.5 g or less.
  • the wettability value exceeds 0.5 g, for example, when used as a surface material of a disposable diaper, after urination, when the surface material touches the skin, there is a very moist feeling and the usability is deteriorated. May cause rash.
  • the 45-degree inclined flow length serving as a water permeability index of the nonwoven fabric of the present embodiment is preferably 30 mm or less, more preferably 25 mm or less.
  • the 45-degree inclined flow length exceeds 30 mm, for example, when used for a surface material such as a disposable diaper, the liquid flow on the surface increases, and urine leakage is likely to occur.
  • the present invention will be specifically described by way of examples and comparative examples, but the present invention is not limited to the following examples.
  • the evaluation method of each characteristic is as follows, and the physical property of the obtained nonwoven fabric is shown in the following Table 2.
  • the flow direction in nonwoven fabric production is referred to as the MD direction, the direction perpendicular to that direction and the width direction as the CD direction.
  • Average fineness (dtex) A 1 cm square test piece was sampled by dividing the nonwoven fabric into 5 equal parts in the CD direction, 20 diameters of each fiber were measured with a microscope VHX-700F manufactured by Keyence, and the single yarn fineness was calculated from the average value.
  • Non-woven fabric weight (g / m 2 )
  • g / m 2 The weight per unit area was calculated as a basis weight (g / m 2 ).
  • Rewetting In order to make the characteristics of the absorber constant as the absorber, a test cloth is placed on three sheets of specific filter paper (GRADE: 989 manufactured by Ahlstrom). A 10 cm square plate with a hole of 25 mm in diameter (about 800 g) was placed on top of it, and physiological saline (amount 4.0 times the weight of the absorber) was dropped from the height of 25 mm above the center hole. And absorb. Next, the plate on the test cloth is removed, and a 3.5 kg weight (10 cm square) is placed on it for 3 minutes to stabilize the liquid distribution in the absorbent body.
  • GRADE 989 manufactured by Ahlstrom
  • the increase value (g) was defined as the wettability.
  • Extrusion was performed at a spinning temperature of 220 ° C. by a bond method, and the filament group was extruded toward a moving collection surface using a high-speed traction device using an air jet to prepare a long fiber web having an average fiber diameter of 2.8 dtex. Subsequently, the obtained long fiber web was flat roll and emboss roll at an upper and lower temperature of 135 ° C.
  • the filament group was extruded toward a moving collection surface using a high-speed traction device using an air jet to produce a long fiber web having an average fiber diameter of 2.3 dtex.
  • the obtained long fiber web was partially pressure-bonded to each other under the conditions of a vertical temperature of 135 ° C. and a pressure of 60 kg / cm, The line speed was adjusted so that the intended basis weight was 30 g / m 2 to obtain a long fiber nonwoven fabric (2).
  • Polypropylene (PP) resin having an MFR of 55 g / 10 min (measured at a temperature of 230 ° C. and a load of 2.16 kg according to JIS-K7210) is the first component, and the melt index (MI) is 26 g / 10 min (JIS-K7210).
  • the high-density polyethylene (HDPE) resin at a temperature of 190 ° C. and a load of 2.16 kg is used as the second component, the discharge amount of the first component is 0.54 g / min ⁇ hole, and the discharge amount of the second component is Extruded at a spinning temperature of 220 ° C.
  • the filament group was extruded toward the moving collection surface using a high-speed airflow traction device using an air jet to prepare an eccentric sheath-core type composite continuous fiber web having an average fiber diameter of 2.0 dtex.
  • the obtained long fiber web was partially pressure-bonded to each other under the conditions of an upper and lower temperature of 135 ° C. and a pressure of 60 kg / cm. The line speed was adjusted so that the intended basis weight was 15 g / m 2 to obtain a long fiber nonwoven fabric (4).
  • PP Polypropylene
  • MI is 26 g / 10 min
  • HDPE temperature High-density polyethylene
  • the first component discharge rate is 0.4 g / min ⁇ hole
  • the second component discharge rate is 0.4 g / Extruded at a spinning temperature of 220 ° C.
  • an eccentric sheath-core composite long fiber web having an average fiber diameter of 2.3 dtex was prepared by extrusion toward the moving collection surface. Subsequently, the obtained eccentric sheath-core type composite long fiber nonwoven web was subjected to a flat roll and an embossing roll at 100 ° C.
  • the discharge amount of the first component is 0.40 g / min ⁇ hole and the discharge amount of the second component (polyethylene) is 0.40 g.
  • a fiber having a total discharge rate of 0.8 g / min ⁇ hole and a ratio of the first component to the second component of 1: 1 was extruded at a spinning temperature of 220 ° C. by a spunbond method.
  • the extruded filament is stretched in the traction zone using the suction force of the moving collection surface, and then deposited on the moving collection surface through a diffuser, and a side-by-side type composite long fiber web having an average fiber diameter of 3.0 dtex.
  • the obtained side-by-side type composite long fiber web was bonded to each other with hot air having a hot air temperature of 142 ° C. and a hot air wind speed of 0.7 m / s, and a composite long fiber nonwoven fabric having a basis weight of 15 g / m 2 and a crimp number of 15 pieces / inch ( 6) was obtained.
  • PP Polypropylene
  • the filament group was extruded toward the moving collection surface using a high-speed airflow traction device using an air jet to prepare an eccentric sheath-core type composite long fiber web having an average fiber diameter of 2.8 dtex.
  • the fibers were bonded together with hot air having a hot air temperature of 120 ° C. and a hot air speed of 1.0 m / s to obtain a composite long fiber nonwoven fabric (7) having a basis weight of 20 g / m 2 and a crimp number of 25 pieces / inch.
  • HDPE High-density polyethylene
  • PET polyethylene terephthalate
  • MI solution viscosity ⁇ sp / c of 0.75 as the first component and an MI of 26 g / 10 min (measured according to JIS-K7210 at a temperature of 190 ° C. and a load of 2.16 kg).
  • the resin is the second component
  • the first component discharge rate is 0.50 g / min ⁇ hole
  • the second component discharge rate is 0.25 g / min ⁇ hole
  • the total discharge rate is 0.75 g / min ⁇ hole.
  • a fiber having a ratio of the first component to the second component of 2: 1 was extruded at a spinning temperature of 220 ° C. by a spunbond method.
  • the extruded filament is stretched in the traction zone by using the suction force of the moving collection surface, and then deposited on the moving collection surface through a diffuser to form an eccentric sheath-core composite with an average fiber diameter of 4.0 dtex.
  • a long fiber web was prepared.
  • the resulting eccentric sheath-core composite long fiber web was bonded to each other with hot air having a hot air temperature of 130 ° C. and a hot air speed of 0.7 m / s, and the composite length was 30 g / m 2 and the number of crimps was 13 pieces / inch.
  • a fiber nonwoven fabric (8) was obtained.
  • Component A-1 Propylene glycol manufactured by ADEKA Corporation was used.
  • Component A-2 Dipropylene glycol manufactured by ADEKA Corporation was used.
  • Component B-1 30 mol of propylene oxide and then 8 mol of ethylene oxide were added to propylene glycol according to a conventional method to obtain polyoxyalkylene glycol. Next, 1 mol of this polyoxyalkylene glycol was reacted with 1.5 mol of lauric acid to obtain Component B-1.
  • n is 0 in formula (2)
  • R 1 and R 3 are alkenoyl groups having 11 carbon atoms
  • (A 2 O) 1 is added to both ends of 31 mol of propylene oxide.
  • a compound in which 8 mol of ethylene oxide is added (l is 39), and in general formula (2), n is 0, and either R 1 or R 3 is an alkenoyl group having 11 carbon atoms , (A 2 O) l is a 1: 1 mixture with a compound in which a total of 8 mol of ethylene oxide is added to both ends of 31 mol of propylene oxide (l is 39).
  • Component B-2 50 mol of propylene oxide and then 15 mol of ethylene oxide were added to propylene glycol according to a conventional method to obtain polyoxyalkylene glycol. Next, 1 mol of this polyoxyalkylene glycol was reacted with 1.8 mol of stearic acid to obtain Component B-2.
  • n is 0, R 1 and R 3 are alkenoyl groups having 17 carbon atoms, and (A 2 O) 1 is added to both ends of 51 mol of propylene oxide.
  • Component B-3 30 mol of propylene oxide and then 8 mol of ethylene oxide were added to propylene glycol according to a conventional method to obtain polyoxyalkylene glycol. Subsequently, 3 mol of this polyoxyalkylene glycol was reacted with 2 mol of adipic acid. Next, this reaction product was reacted with 1 mol of lauric acid to obtain Component B-3.
  • Component B-3 in general formula (2), either R 1 or R 3 is an alkenoyl group having 11 carbon atoms, and (A 2 O) 1 is 8 mol in total at both ends of 31 mol of propylene oxide.
  • R 2 is an alkylene group having 4 carbon atoms
  • (A 3 O) m is added to both ends of 31 mol of propylene oxide for a total of 8 mol of ethylene oxide added.
  • a compound in which n is 2 and m is 39.
  • Component B-4 30 mol of propylene oxide and then 8 mol of ethylene oxide were added to propylene glycol according to a conventional method to obtain polyoxyalkylene glycol. Next, 5 mol of this polyoxyalkylene glycol was reacted with 4 mol of adipic acid to obtain Component B-4.
  • Component B-4 is a group (1) in which R 1 and R 3 are hydrogen and (A 2 O) 1 is a total of 8 moles of ethylene oxide added to both ends of 31 moles of propylene oxide. 39), R 2 is an alkylene group having 4 carbon atoms, and (A 3 O) m is a group in which 8 moles of ethylene oxide are added to both ends of 31 moles of propylene oxide (m is 39). , N is 4.
  • Component B-5 According to a conventional method, 24 mol of propylene oxide was added to lauryl alcohol to obtain Component B-5.
  • Component B-5 in general formula (2), n is 0, R 1 and R 3 are alkyl groups having 12 carbon atoms, and (A 2 O) 1 is a group having 24 moles of propylene oxide (where l is 24).
  • glycerin concentrated glycerin for cosmetics manufactured by Miyoshi Oil Co., Ltd. was used.
  • glycerin condensate As the glycerin condensate, hexaglycerin monostearate (manufactured by Sakamoto Yakuhin Kogyo Co., Ltd., trade name: SY Glyster MS-5S) was used.
  • polyoxyalkylene castor oil ether As the polyoxyalkylene castor oil ether, polyoxyethylene (20) hydrogenated castor oil (trade name: NIKKOL HCO-20, manufactured by Nikko Chemical Co., Ltd.) was used.
  • Example 1 The component A-1: 25 parts by mass as the component (A), the component B-1: 55 parts by mass, and the component (C): 20 parts by mass as the component (B) were mixed uniformly at 30 ° C. A processing agent (1) was obtained. The blending ratio of each component is shown in Table 1 below.
  • Examples 2 to 10, Comparative Examples 1 to 7 The fiber processing of Examples 2 to 10 was carried out in the same manner as in Example 1 except that the blending ratio of Component (A), Component (B), Component (C), and other components was changed as shown in Table 1 below. Agents (2) to (10) and fiber finishing agents (Comparative 1) to (Comparative 7) of Comparative Examples 1 to 7 were obtained. The blending ratio of each component is shown in Table 1 below.
  • Example 11 In the nonwoven fabric (1), a 3% by weight aqueous solution of the fiber processing agent (1) of Example 1 is adjusted to a liquid temperature of 20 ° C., so that the coating amount becomes 10% by weight by the rotor dampening method. It applied to the nonwoven fabric, passed through an air-through dryer at 125 ° C., dried and wound up.
  • the rotor dampening apparatus used had a rotor diameter of 80 mm, and the rotors were arranged at intervals of 115 mm in the CD direction so that the distance between the rotor center and the nonwoven fabric to be applied was 180 mm. Further, the rotational speed of the rotor was adjusted so that the sprayed particle diameter of the fiber processing agent to be sprayed was 35 ⁇ m.
  • Table 2-1 Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 12 The fiber processing agent (2) of Example 2 was applied to the nonwoven fabric (1) in the same manner as in Example 11. Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 13 The fiber processing agent (3) of Example 3 was applied to the nonwoven fabric (1) in the same manner as in Example 11. Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 11 is the same as Example 11 except that the nonwoven fabric (1) was adjusted with a 5% by weight aqueous solution of the fiber processing agent (2) of Example 2 at a liquid temperature of 20 ° C. so that the coating amount was 10% by weight. It applied to the nonwoven fabric in the same manner. Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 15 To the nonwoven fabric (1), a 3.4 wt% aqueous solution of the fiber processing agent (4) of Example 4 is adjusted to a liquid temperature of 20 ° C. so that the coating amount is 30 wt%. It apply
  • Example 16 Example 11 except that the nonwoven fabric (1) was adjusted with a 10% by weight aqueous solution of the fiber processing agent (5) of Example 5 at a liquid temperature of 20 ° C. so that the coating amount was 10% by weight. It applied to the nonwoven fabric in the same manner. Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 17 In the production of the nonwoven fabric (1), a nonwoven fabric was obtained in the same manner except that the line speed was adjusted so that the basis weight was 8 g / m 2 . The obtained nonwoven fabric was subjected to corona treatment so that the wetting tension of the nonwoven fabric was 35 to 39 mN / m, and then a 0.34% by weight aqueous solution of the fiber processing agent (4) of Example 4 at a liquid temperature of 20 ° C. Other than the preparation, it was applied to the nonwoven fabric in the same manner as in Example 15. Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 18 In the production of the nonwoven fabric (1), a nonwoven fabric was obtained in the same manner except that the line speed was adjusted so that the basis weight was 15 g / m 2 . The obtained nonwoven fabric was applied to the nonwoven fabric in the same manner as in Example 15 except that a 1.67% by weight aqueous solution of the fiber processing agent (4) of Example 4 was adjusted at a liquid temperature of 20 ° C. Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 19 Example 11 except that the nonwoven fabric (2) was adjusted with a 10% by weight aqueous solution of the fiber processing agent (4) of Example 4 at a liquid temperature of 20 ° C. so that the coating amount was 10% by weight. It applied to the nonwoven fabric in the same manner. Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 20 A nonwoven fabric was produced in the same manner as in Example 19 except that the fiber processing agent (6) was used. Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 21 In the production of the nonwoven fabric (2), a nonwoven fabric was obtained in the same manner except that the line speed was adjusted so that the basis weight was 18 g / m 2 . The nonwoven fabric obtained was applied to the nonwoven fabric in the same manner as in Example 15 except that a 1.0% by weight aqueous solution of the fiber processing agent (7) of Example 7 was adjusted at a liquid temperature of 20 ° C. Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 22 In the production of the nonwoven fabric (1), a nonwoven fabric was obtained in the same manner except that the line speed was adjusted so that the basis weight was 15 g / m 2 . Moreover, the nonwoven fabric was produced by the method similar to Example 21 except having used the fiber processing agent (8). Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 23 The nonwoven fabric (3) was applied to the nonwoven fabric in the same manner as in Example 15 except that a 0.67% by weight aqueous solution of the fiber processing agent (7) was adjusted at a liquid temperature of 20 ° C. Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 24 A nonwoven fabric was produced in the same manner as in Example 23 except that the nonwoven fabric (4) was used. Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 25 A non-woven fabric was prepared in the same manner as in Example 11 except that the non-woven fabric (5) was adjusted with a 2% by weight aqueous solution of the fiber processing agent (7) at a liquid temperature of 20 ° C. and the coating amount was 10% by weight. Produced. Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 26 A fine nonwoven fabric was produced in the same manner as in Example 25 except that the nonwoven fabric (6) was used. Various measurement results of the obtained nonwoven fabric are shown in Table 2-1.
  • Example 27 A nonwoven fabric was prepared in the same manner as in Example 11 except that a 10% by weight aqueous solution of the fiber processing agent (4) was prepared at a liquid temperature of 20 ° C. to the nonwoven fabric (7) and the coating amount was 5% by weight. Produced. Various measurement results of the obtained nonwoven fabric are shown in Table 2-2 below.
  • Example 28 The nonwoven fabric (8) was prepared in the same manner as in Example 11 except that a 6% by weight aqueous solution of the fiber processing agent (4) was prepared at a liquid temperature of 20 ° C. and the coating amount was 5% by weight. Produced. Various measurement results of the obtained nonwoven fabric are shown in Table 2-2 below.
  • Example 29 A 0.67% by weight aqueous solution of the fiber processing agent (4) is prepared on the nonwoven fabric (5) at a liquid temperature of 20 ° C., and is applied using a kiss roll ( ⁇ 400 mm) so that the coating amount becomes 30% by weight. And passed through a 130 ° C. cylinder dryer and wound up.
  • Table 2-2 Various measurement results of the obtained nonwoven fabric are shown in Table 2-2 below.
  • Example 30 The nonwoven fabric (1) was prepared in the same manner as in Example 11 except that a 5% by weight aqueous solution of the fiber processing agent (9) was prepared at a liquid temperature of 20 ° C. and the coating amount was 10% by weight. Was made. Various measurement results of the obtained nonwoven fabric are shown in Table 2-2 below.
  • Example 31 The nonwoven fabric (1) was prepared in Example 11 except that a 3% by weight aqueous solution of the fiber processing agent (10) of Example 10 was prepared at a liquid temperature of 20 ° C. and the coating amount was 10% by weight. A nonwoven fabric was produced in the same manner. Various measurement results of the obtained nonwoven fabric are shown in Table 2-2 below.
  • Comparative Example 11 To the nonwoven fabric (1), the fiber processing agent of Comparative Example 1 (Comparative (1)) was applied to the nonwoven fabric in the same manner as in Example 14. Various measurement results of the obtained nonwoven fabric are shown in Table 2-2 below.
  • Comparative Example 12 A nonwoven fabric was obtained in the same manner as in Comparative Example 11 except that the fiber processing agent of Comparative Example 2 (Comparative (2)) was used. Various measurement results of the obtained nonwoven fabric are shown in Table 2-2 below.
  • Comparative Example 13 A nonwoven fabric was obtained in the same manner as in Comparative Example 11 except that the fiber processing agent of Comparative Example 3 (Comparative (3)) was used. Various measurement results of the obtained nonwoven fabric are shown in Table 2-2 below.
  • Example 14 The nonwoven fabric (1) was applied to the nonwoven fabric in the same manner as in Example 15 except that the 1.67% by weight aqueous solution of the fiber processing agent of Comparative Example 4 (Comparative (4)) was prepared at a liquid temperature of 20 ° C. Various measurement results of the obtained nonwoven fabric are shown in Table 2-2 below.
  • Example 15 The nonwoven fabric (1) was applied to the nonwoven fabric in the same manner as in Example 15 except that the 1.0% by weight aqueous fiber processing agent (Comparative (5)) solution of Comparative Example 5 was prepared at a liquid temperature of 20 ° C. Various measurement results of the obtained nonwoven fabric are shown in Table 2-2 below.
  • Example 17 A nonwoven fabric was produced in the same manner as in Example 11 except that the fiber processing agent of Comparative Example 7 (Comparative (7)) was used. Various measurement results of the obtained nonwoven fabric are shown in Table 2-2 below.
  • the nonwoven fabric coated with the fiber processing agent according to the present invention is excellent in initial water permeability, wettability, and repeated water permeability. Therefore, sanitary materials such as sanitary napkins, incontinence pads, disposable diapers and other top sheets and second sheets are used. For example, or suitable for masks, body warmers, tape base materials, patch base materials, emergency bandages, packaging materials, wipe products, medical gowns, bandages, clothing, skin care sheets, etc. Is available.

Abstract

La présente invention concerne un agent de traitement de fibre destiné à améliorer les propriétés de réhumification et de perméabilité aux liquides répétée d'une étoffe non tissée, une étoffe non tissée perméable aux liquides comprenant des fibres auxquelles l'agent de traitement de fibre a été appliqué, et un matériau hygiénique utilisant l'étoffe non tissée perméable aux liquides. L'invention concerne un agent de traitement de fibre qui contient un composant (A) représenté par la formule générale (1) : HO-(A1O)p-H dans laquelle A1 représente un groupe alkylène contenant 2 à 4 atomes de carbone et p est un nombre entier de 1 à 3, et un composant (B), qui est différent du composant (A), représenté par la formule générale (2) : R1-O-(A2O)l-{C(O)R2C(O)-(A3O)m}n-R3 dans laquelle R1, R2, R3, A2, A3, l, m et n sont définis dans les revendications. L'invention concerne également une étoffe non tissée perméable aux liquides qui contient l'agent de traitement de fibre et un matériau hygiénique qui utilise l'étoffe non tissée perméable aux liquides.
PCT/JP2017/036869 2016-10-13 2017-10-11 Agent de traitement de fibre et étoffe non tissée perméable aux liquides le contenant WO2018070443A1 (fr)

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