Classifications

• • D—TEXTILES; PAPER
  • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
  • D04H—MAKING 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
  • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
  • D04H1/40—Non-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
• • 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
  • D06M13/244—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 sulfur or phosphorus
  • D06M13/282—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 sulfur or phosphorus with compounds containing phosphorus
  • D06M13/285—Phosphines; Phosphine oxides; Phosphine sulfides; Phosphinic or phosphinous acids or derivatives thereof

Definitions

• the present invention relates to a fiber treatment agent, a water-permeable fiber to which it is attached, and a method for producing a nonwoven fabric.
• absorbent articles such as sanitary products such as disposable diapers and synthetic napkins are hydrophilic to various non-woven fabrics mainly composed of fibers (polyolefin fibers, polyester fibers, etc.) containing at least one thermoplastic resin. It has a structure formed by three layers in which a top sheet provided, a back sheet provided with water repellency, and a material made of cotton-like pulp or a polymer absorber are disposed between the top sheet and the back sheet. There are many cases. Liquids such as urine and body fluid pass through the top sheet and are absorbed by the absorber, but the top sheet has good water permeability, that is, until the liquid is completely absorbed by the internal absorber from the top sheet.
• Instant water permeability is required for a very short time.
• good card passage properties such as prevention of winding around the cylinder and generation of static electricity are required.
• the tow may be wound around the roller during the production of the fiber. However, if the winding occurs, the quality of the fiber is deteriorated and the yield is deteriorated.
• the fibers to which the treatment agent of Patent Document 1 or Patent Document 2 is applied have good instantaneous water permeability and liquid return prevention property of the nonwoven fabric, but the passability of the card process, which is one process of the nonwoven fabric processing, is not sufficient.
• the object of the present application is to impart excellent card passage properties, instantaneous water permeability and liquid return prevention properties to the fibers, and to prevent the occurrence of wrapping during fiber production and the instantaneous water permeability of the nonwoven fabric.
• Another object of the present invention is to provide a water-permeable fiber that is excellent in preventing liquid return and at the same time excellent in card passing properties, and a method for producing a nonwoven fabric that is excellent in instantaneous water permeability and liquid return preventing property.
• the present invention is a fiber treatment agent for short fibers, Essentially contains a compound (A) represented by the following general formula (1), a compound (B) represented by the following general formula (2) and a compound (C) represented by the following general formula (3),
• the weight ratio of the compound (C) to the nonvolatile content of the treating agent is 1 to 35% by weight
• the weight ratio (C / (A + B)) of the total of the compound (A) and the compound (B) to the compound (C) is 0.01 to 0.5
• the weight ratio of inorganic phosphoric acid is 3%.
• R 1 is a hydrocarbon group having 6 to 15 carbon atoms.
• R 1 may be linear or branched, and may be saturated or unsaturated.
• AO is an oxyalkylene group having 2 to 4 carbon atoms, m is an integer of 0 to 15.
• M 1 is an alkali metal, and M 2 is a hydrogen atom or an alkali metal.
• R 1 and R 2 are hydrocarbon groups having 6 to 15 carbon atoms.
• R 1 and R 2 may be linear or branched, and may be saturated or unsaturated.
• AO is an oxyalkylene group having 2 to 4 carbon atoms, m is an integer of 0 to 15.
• M 1 is an alkali metal, and (AO) m is 2 in the molecule. If there are two, they may be the same or different from each other (the number of carbons in R 1 ) (the number of carbons in R 2 is satisfied).
• R 1 and R 2 are hydrocarbon groups having 6 to 15 carbon atoms.
• R 1 and R 2 may be linear or branched, and may be saturated or unsaturated.
• AO is an oxyalkylene group having 2 to 4 carbon atoms
• m is an integer of 0 to 15.
• M 1 is an alkali metal
• M 2 is a hydrogen atom or an alkali metal
• Q is M 2 or R 2 O
• AO m
• Y is 1 or 2. If there are two or more M 2 or (AO) m in the molecule, they may be the same as each other may be different. (number of carbon atoms in R 1) ⁇ (R carbon number of 2) satisfies.)
• the weight ratio (A1 + B1 + C1) / (A2 + B2 + C2) to the total weight of the compound (C2) in which R 1 in 3) has 11 to 15 carbon atoms is preferably 1 to 20.
• the total of the compound (A), the compound (B), and the compound (C) in the nonvolatile content of the treatment agent is 60% by weight or more.
• a nonionic surfactant (D) is further included, and the nonionic surfactant (D) in the nonvolatile content of the treatment agent preferably has a weight ratio of 1 to 40% by weight.
• the nonionic surfactant (D) contains a compound (D3) which is an ester obtained by blocking at least one hydroxyl group of a polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester and a dicarboxylic acid with a fatty acid. It is preferable when used for synthetic fibers for producing nonwoven fabrics.
• the water-permeable fiber of the present invention is obtained by adhering the fiber treatment agent to a synthetic fiber for producing a nonwoven fabric.
• the manufacturing method of the nonwoven fabric of this invention includes the process of accumulating the said water-permeable fiber, producing a fiber web, and heat-processing the obtained fiber web.
• the fiber treatment agent of the present invention can impart excellent card passing properties, instantaneous water permeability and liquid return prevention properties to fibers, and can prevent the occurrence of winding during fiber production.
• the water-permeable fiber of the present invention is excellent in the non-woven fabric's instantaneous water permeability and liquid return prevention property, and at the same time, in card passing properties.
• the manufacturing method of the nonwoven fabric of this invention is excellent in instantaneous water permeability and liquid return prevention property.
• the fiber treatment agent of the present invention is a fiber treatment agent comprising a specific phosphoric acid compound, compound (A), compound (B), and compound (C) in a specific ratio, and an inorganic phosphoric acid amount being a certain amount or less. is there. Details will be described below.
• the compound (A) is a component that is essentially included in the fiber treatment agent of the present invention, and is a component that reduces friction between fibers and metal when wet and is excellent in instantaneous water permeability.
• the compound (A) is represented by the general formula (1).
• R 1 is a hydrocarbon group having 6 to 15 carbon atoms.
• R 1 may be linear or branched, and may be saturated or unsaturated.
• Examples of the hydrocarbon group include an alkyl group, an alkenyl group, and an aryl group.
• AO is an oxyalkylene group having 2 to 4 carbon atoms.
• M which is the number of repeating oxyalkylene units, is an integer from 0 to 15, preferably from 0 to 10, more preferably from 0 to 3, and when m is 0 and no polyoxyalkylene group is contained, This is particularly preferable from the viewpoint of low friction between metals.
• (AO) m is preferably a polyoxyalkylene group having 50 mol% or more of oxyethylene units as oxyalkylene units.
• M 1 is an alkali metal.
• the alkali metal include potassium, sodium, lithium and the like, and potassium or sodium is preferable from the viewpoint of availability.
• M 2 is a hydrogen atom or an alkali metal. Examples of the alkali metal include potassium, sodium, lithium and the like, and potassium or sodium is preferable from the viewpoint of availability.
• the compound (A1) is the instantaneous permeability
• the compound (A2) is excellent in reducing the fiber / metal friction when wet.
• the R 1 is more preferably 6 to 13 from the viewpoint of reducing the friction between fibers / metals when wet.
• compound (A) include, but are not limited to, monohexyl phosphate monopotassium salt, monohexyl phosphate dipotassium salt, monohexyl phosphate monosodium salt, monohexyl phosphate disodium salt, monooctyl phosphate monopotassium salt, mono Octyl phosphate dipotassium salt, monooctyl phosphate monosodium salt, monooctyl phosphate disodium salt, monodecyl phosphate monopotassium salt, monodecyl phosphate dipotassium salt, monodecyl phosphate monosodium salt, monodecyl phosphate disodium salt, monolauryl phosphate mono Potassium salt, monolauryl phosphate dipotassium salt, monolauryl phosphate monosodium salt, monolauryl phosphate Sodium salt, monotridecyl phosphate monopotassium salt, monotridecyl phosphate mono
• monooctyl phosphate monopotassium salt monooctyl phosphate dipotassium salt, monodecyl phosphate monopotassium salt, monodecyl phosphate dipotassium salt, monolauryl phosphate monopotassium salt, and monolauryl phosphate dipotassium salt are preferable.
• Compound (A) can be detected by 31 P-NMR method. About 30 mg of the measurement sample non-volatile content was weighed into an NMR sample tube having a diameter of 5 mm, dissolved by adding about 0.5 ml of heavy water (D 2 O) as a deuterated solvent, and 31 P-NMR measurement apparatus (manufactured by BRUKER) (AVANCE 400, 162 MHz). The peak of phosphorus element derived from the compound (A) is detected at +4 to -1 ppm.
• the peak of the phosphorus element derived from the compound (A), the compound (B) described later and the inorganic phosphoric acid described later is detected at +4 to ⁇ 1 ppm, but from the low magnetic field side, the inorganic phosphoric acid, the compound (A)
• the assignment is determined in the order of compound (B).
• the compound (B) is an essential component contained in the fiber treatment agent of the present invention. By using it together with the compound (A), the effect of optimizing the friction between the fiber and the metal when the compound (C) is wet is obtained. Has enhanced performance. Compound (B) has the performance of preventing liquid return.
• the compound (B) is represented by the general formula (2).
• R 1 and R 2 are hydrocarbon groups having 6 to 15 carbon atoms. R 1 and R 2 may be linear or branched, and may be saturated or unsaturated. Examples of the hydrocarbon group include an alkyl group, an alkenyl group, and an aryl group.
• the compound (B) obtained by phosphorylating two or more kinds of alcohols having different carbon numbers may have different R 1 and R 2 , in which case the carbon number of R 1 ) ⁇ (R 2 Of carbon).
• AO is an oxyalkylene group having 2 to 4 carbon atoms.
• M which is the number of repeating oxyalkylene units, is an integer from 0 to 15, preferably from 0 to 10, more preferably from 0 to 3, and when m is 0 and no polyoxyalkylene group is contained, from the viewpoint of card passage From the above, it is particularly preferable.
• (AO) m is preferably a polyoxyalkylene group having 50 mol% or more of oxyethylene units as oxyalkylene units. When two (AO) m are present in the molecule, they may be the same or different from each other.
• Compound (B) when classified into compound compound the carbon number of R 1 is 6 ⁇ 10 (B1) and the number of carbon atoms of R 1 is 11 ⁇ 15 (B2), the compound (B1) is the instantaneous permeability
• the compound (B2) is excellent in card passing property.
• the R 1 is more preferably 6 to 13 from the viewpoint of reducing the friction between fibers / metals when wet.
• M 1 is an alkali metal.
• the alkali metal include potassium, sodium, lithium and the like, and potassium or sodium is preferable from the viewpoint of availability.
• M 2 is a hydrogen atom or an alkali metal. Examples of the alkali metal include potassium, sodium, lithium and the like, and potassium or sodium is preferable from the viewpoint of availability.
• the compound (B) include, but are not limited to, dihexyl phosphate potassium salt, dihexyl phosphate sodium salt, dioctyl phosphate potassium salt, dioctyl phosphate sodium salt, didecyl phosphate potassium salt, didecyl phosphate sodium salt, dilauryl phosphate.
• Potassium salt dilauryl phosphate sodium salt, ditridecyl phosphate potassium salt, ditridecyl phosphate sodium salt, dipolyoxyethylene 3 mol addition octyl phosphate potassium salt, dipolyoxyethylene 3 mol addition hexyl phosphate potassium salt, dimyristyl phosphate potassium salt And dimyristyl phosphate sodium salt.
• dioctyl phosphate potassium salt, didecyl phosphate potassium salt, and dilauryl phosphate potassium salt are preferable.
• Compound (B) can be detected by the 31 P-NMR method in the same manner as compound (A).
• the peak of phosphorus element derived from the compound (B) is detected at +4 to -1 ppm.
• the peak of phosphorus element derived from compound (A), compound (B) and inorganic phosphoric acid is detected at +4 to -1 ppm, but from the low magnetic field side, inorganic phosphoric acid, compound (A), compound (B ) Is determined in the order.
• Compound (C) is a component that is essential in the fiber treatment agent of the present invention, and when applied to the fiber, The liquid return of the nonwoven fabric can be reduced, and the friction between fiber / metal when wet is an appropriate component. Since compound (C) is an appropriate component for friction between fiber and metal when wet, it can prevent wrapping around the drawing roller and slip during fiber production, and crimp in the crimping step. Is uniformly performed to reduce crimped spots. The reason why the friction between the fiber and the metal when the compound (C) is wet is not clear, but it is generally estimated as follows.
• a hydroxyl group or a site where the hydroxyl group is substituted with an alkali metal is ionically dissociated when wet, and the dissociated portion tends to be oriented on the metal surface, and the alkyl group site (R 1 in Formula 1 ) is oriented to a hydrophobic fiber.
• Compound (C) has two hydroxyl sites in the molecule or sites where hydroxyl groups are substituted with alkali metals, and is located at a distant position, so that the orientation tendency to the metal surface and fiber surface becomes stronger, so that the fiber / Lubrication between metals is appropriate.
• the compound (C) is represented by the general formula (3).
• R 1 and R 2 are hydrocarbon groups having 6 to 15 carbon atoms.
• R 1 and R 2 may be linear or branched, and may be saturated or unsaturated.
• AO is an oxyalkylene group having 2 to 4 carbon atoms, and m is an integer of 0 to 15.
• M 1 is an alkali metal.
• M 2 is a hydrogen atom or an alkali metal.
• Q is M 2 or R 2 O (AO) m .
• Y is 1 or 2.
• the compound (C) obtained by phosphorylating two or more alcohols having different carbon numbers may have different R 1 and R 2 , in which case (carbon number of R 1 ) ⁇ (R 2 carbon number).
• Compound (C) when classified into compound compound the carbon number of R 1 is 6 ⁇ 10 (C1) and the number of carbon atoms of R 1 is 11 ⁇ 15 (C2), the compound (C1) is the instantaneous permeability And the compound (C2) has very excellent anti-return properties.
• the R 1 is more preferably 6 to 13 from the viewpoint of reducing the friction between fibers / metals when wet.
• the compound (C) include, but are not limited to, polyhexyl phosphate potassium salt, polyhexyl phosphate sodium salt, polyoctyl phosphate potassium salt, polyoctyl phosphate sodium salt, polydecyl phosphate potassium salt, polydecyl phosphate sodium salt , Polylauryl phosphate potassium salt, polylauryl phosphate sodium salt, polytridecyl phosphate potassium salt, polytridecyl phosphate sodium salt, polyoxyethylene 3 mol addition polyoctyl phosphate potassium salt, polyoxyethylene 3 mol addition polyoctyl phosphate sodium salt , Polymyristyl phosphate potassium salt, polymyristyl phosphate sodium salt and the like. Of these, polyoctyl phosphate potassium salt, polydecyl phosphate potassium salt, and polylauryl phosphate potassium salt are preferable.
• Compound (C) can be detected as follows. [ 31 P-NMR method] About 30 mg of the measurement sample non-volatile content was weighed into an NMR sample tube having a diameter of 5 mm, dissolved by adding about 0.5 ml of heavy water (D 2 O) as a deuterated solvent, and 31 P-NMR measurement apparatus (manufactured by BRUKER) (AVANCE 400, 162 MHz). The peak of phosphorus element derived from the compound (C) is detected at -5 to -15 ppm.
• 31 P-NMR method About 30 mg of the measurement sample non-volatile content was weighed into an NMR sample tube having a diameter of 5 mm, dissolved by adding about 0.5 ml of heavy water (D 2 O) as a deuterated solvent, and 31 P-NMR measurement apparatus (manufactured by BRUKER) (AVANCE 400, 162 MHz). The peak of phosphorus element derived from the compound (C) is detected at -5 to -15 ppm
• Nonionic surfactant (D) When the fiber treatment agent of the present invention further contains a nonionic surfactant (D), it is preferable because instantaneous water permeability and durable water permeability are improved.
• the nonionic surfactant (D) is not particularly limited, and examples of components that improve instantaneous water permeability include PEG ester (D1) and POE alkyl ether (D2). (D3) or (D4) etc. are mentioned as a component which improves durable water permeability.
• PEG means polyethylene glycol
• POE means polyoxyalkylene.
• Examples of the PEG ester (D1) include an ester of polyethylene glycol having a structure in which a hydroxyl group of PEG and a monovalent fatty acid are esterified (hereinafter referred to as PEG ester).
• the carbon number of the monovalent fatty acid is not particularly limited, but is preferably 4 to 24, more preferably 12 to 22, and still more preferably 16 to 20.
• the fatty acid may be saturated or unsaturated.
• the weight average molecular weight of PEG is not particularly limited, but is preferably 200 to 600.
• the weight average molecular weight of the PEG ester is not particularly limited, but is preferably 300 to 1000, more preferably 400 to 900, and still more preferably 500 to 800.
• PEG ester examples include, for example, PEG (200) monolaurate, PEG (200) dilaurate, PEG (300) monolaurate, PEG (300) dilaurate, PEG (400) monolaurate, PEG (400) Dilaurate, PEG (600) monolaurate, PEG (600) dilaurate, PEG (200) monooleate, PEG (200) geolate, PEG (300) monooleate, PEG (300) geolate, PEG (400) monooleate, PEG (400) Dioleate, PEG (600) monooleate, PEG (600) dioleate, PEG (200) monoisostearate, PEG (200) diisostearate, PEG (300) monoisostearate, PEG (300) diisostearate DOO, PEG (400) monoisostearate, PEG (400) diisostearate, PEG (400) diisostearate, PEG (600) mono
• the POE alkyl ether (D2) is an alkyl ether having a structure obtained by polyoxyethylation of a monovalent aliphatic alcohol (hereinafter referred to as POE alkyl ether).
• the carbon number of the monovalent aliphatic alcohol is not particularly limited, but is preferably 8 to 24, more preferably 10 to 20, and still more preferably 12 to 18.
• the average number of moles of ethylene oxide constituting one mole of polyoxyethylene group is not particularly limited, but is preferably 3 to 20 moles, more preferably 5 to 16 moles, and still more preferably 8 to 12 moles. If it is less than 3 mol or more than 20 mol, the instantaneous water permeability may be reduced.
• the weight average molecular weight of the POE alkyl ether (D2) is not particularly limited, but is preferably 240 to 1300, more preferably 350 to 1000, and still more preferably 450 to 700.
• Specific examples of the POE alkyl ether (D2) include POE octyl ether, POE ethylhexyl ether, POE decyl ether, POE lauryl ether, POE oleyl ether, POE stearyl ether, POE isostearyl ether, and the like.
• the compound (D3) which is an ester in which at least one hydroxyl group of a condensate of a polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester (hereinafter sometimes referred to as polyhydroxy ester) and a dicarboxylic acid is blocked with a fatty acid, is the present invention.
• polyhydroxy ester a polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester
• dicarboxylic acid is blocked with a fatty acid
• the polyglycerin fatty acid ester is a compound obtained by esterifying a glycerin condensate and a fatty acid.
• glycerin condensates include diglycerin, triglycerin, tetraglycerin, pentaglycerin, hexaglycerin, heptaglycerin, octaglycerin, nonaglycerin, decaglycerin, undecaneglycerin, tridecaglycerin, detradecaglycerin, pentadecaglycerin.
• the fatty acid may be saturated or unsaturated, may be linear, and may have a branch.
• saturated fatty acids include caproic acid, caprylic acid, capric acid, undecanoic acid, lauric acid, tridecanoic acid, myristic acid, pentadecanoic acid, palmitic acid, stearic acid, nonadecanoic acid, arachidic acid, behenic acid, serotic acid, montan An acid, a mellic acid etc. are mentioned.
• Examples of the unsaturated fatty acid include oleic acid, elaidic acid, erucic acid, linoleic acid, linolenic acid, and the like.
• Polyglycerin fatty acid ester is not particularly limited, for example, hexaglycerol monooleate, diglycerol monolaurate, diglycerol monooleate, tetraglycerol monolaurate, tetraglycerol monostearate, tetraglycerol distearate, Hexaglycerol monolaurate, hexaglycerol monomyristate, hexaglycerol monostearate, hexaglycerol distearate, hexaglycerol dioleate, decaglycerol tristearate and the like.
• the polyhydroxyester is structurally an ester of a polyoxyalkylene group-containing hydroxy fatty acid and a polyhydric alcohol, and two or more (preferably all) hydroxyl groups of the polyhydric alcohol are esterified. Therefore, the polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester is an ester having a plurality of hydroxyl groups.
• the polyoxyalkylene group-containing hydroxy fatty acid has a structure in which a polyoxyalkylene group is bonded to a fatty acid hydrocarbon group via an oxygen atom, and one end that is not bonded to the fatty acid hydrocarbon group of the polyoxyalkylene group is It is a hydroxyl group.
• the polyhydroxyester include an alkylene oxide adduct of an esterified product of a hydroxy fatty acid having 6 to 22 carbon atoms (preferably 12 to 22 carbon atoms) and a polyhydric alcohol.
• the number of added moles of alkylene oxide is preferably 80 or less, more preferably 5 to 30 per mole equivalent of hydroxyl group of the hydroxy fatty acid polyhydric alcohol ester. If the added mole number exceeds 80, the liquid return amount may increase, which is not preferable. In order to obtain high durable water permeability, it is important to adjust the balance between the hydrophilic group and the hydrophobic group.
• the proportion of ethylene oxide in the alkylene oxide is preferably 50 mol% or more, more preferably 80 mol% or more. If the ratio of ethylene oxide is less than 50 mol%, the hydrophobicity becomes strong and sufficient durable water permeability may not be obtained.
• the polyhydroxyester can be produced, for example, by esterifying a polyhydric alcohol and a hydroxy fatty acid (hydroxymonocarboxylic acid) under ordinary conditions to obtain an esterified product, and then subjecting the esterified product to an addition reaction with an alkylene oxide.
• the polyhydroxyester can be suitably produced also by using an oil and fat obtained from nature such as castor oil or a hardened castor oil obtained by adding hydrogen to this, and further subjecting it to an addition reaction with an alkylene oxide.
• the carboxyl group molar equivalent of hydroxy fatty acid per molar equivalent of hydroxyl group of polyhydric alcohol is preferably in the range of 0.5-1.
• the dicarboxylic acid preferably has 2 to 10 carbon atoms, more preferably 2 to 8 carbon atoms. If the carbon number of the dicarboxylic acid exceeds 10, sufficient hydrophilicity may not be imparted.
• dicarboxylic acids include oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, maleic acid, and phthalic acid.
• a carboxylic acid other than the dicarboxylic acid such as lauric acid, oleic acid, stearic acid, behenic acid and benzoic acid may be contained in an amount of 20% or less (preferably 10% or less).
• the carboxyl group molar equivalent of dicarboxylic acid per molar equivalent of hydroxyl group of polyhydroxyester is preferably in the range of 0.2 to 1, More preferred is 0.8.
• the esterification reaction may be performed under ordinary conditions and is not particularly limited.
• the compound (D3) is an ester in which at least one hydroxyl group is blocked with a fatty acid in the condensate of the polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester and dicarboxylic acid (hereinafter sometimes referred to as a condensate).
• Esters that are not sequestered with fatty acids have insufficient durable water permeability, and the viscosity of the compound increases with time, resulting in an increase in water-insoluble matter, so that the solution stability of the fiber treatment agent decreases.
• the carbon number of the fatty acid blocking at least one or more hydroxyl groups of the condensate can be used not only in the range of 10 to 22, but also in the range of 10 to 50.
• the number of carbon atoms of the fatty acid to be blocked is preferably 10 to 50, more preferably 12 to 36. Further, when the number of carbon atoms of the fatty acid is less than 10, the hydrophilicity becomes strong, and when it exceeds 50, the hydrophobicity becomes strong. Thus, when hydrophilicity and hydrophobicity are unbalanced, sufficient durable water permeability may not be obtained.
• fatty acids include lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, icosanoic acid, behenic acid, lignoceric acid, nervonic acid, serotic acid, montanic acid, melicic acid, lanolin fatty acid and the like.
• lanolin fatty acid having 12 to 36 carbon atoms which is a lanolin derivative obtained by purifying behenic acid or wool grease, is preferable.
• the carboxyl group molar equivalent of the fatty acid per molar equivalent of the hydroxyl group of the condensate is preferably in the range of 0.2 to 1, and more preferably 0.4 to 1. There are no particular limitations on the reaction conditions for esterification.
• the fiber treatment agent of the present invention further includes at least one compound (E) component selected from the following compound (E1), compound (E2) and compound (E3) from the viewpoint of imparting durable water permeability.
• Compound (E1) Polyoxyalkylene-modified silicone
• Compound (E2) At least one selected from sulfonates and sulfosuccinates
• Compound (E3) Quaternary ammonium salt type cationic surfactant, imidazolinium type cationic interface At least one selected from an activator, an alkylbetaine surfactant, an alkylimidazole-type betaine surfactant, and an amide group-containing betaine surfactant
• Compound (E1) is a polyoxyalkylene-modified silicone.
• dimethylsiloxane / methyl (polyoxyethylene) siloxane copolymer, dimethylsiloxane / methyl (polyoxypropylene) siloxane copolymer, dimethylsiloxane / methyl (polyoxyethylene / polyoxypropylene) siloxane copolymer Polymer, methyl (polyoxyethylene) polysiloxane copolymer, methyl (polyoxypropylene) polysiloxane copolymer, methyl (polyoxyethylene / polyoxypropylene) polysiloxane copolymer, methyl (polyoxyethylene / poly) And oxybutylene) polysiloxane copolymer.
• the content of Si element in the polyoxyalkylene-modified silicone (% by weight of Si element in the compound) is 5 to 40%.
• Si element content is more than 40%, the stability of the water-permeable fiber obtained by attaching the fiber treatment agent of the present invention is lowered, and the production cost is increased.
• Si element content is less than 5%, durable water permeability may not be obtained.
• the polyoxyalkylene group in the polyoxyalkylene-modified silicone include, for example, an oxyethylene group, an oxypropylene group, an oxybutylene group, a group obtained by polymerizing two or more monomers selected from these monomers, and the like. Can be mentioned.
• the order of addition thereof is not particularly limited, and the addition form may be either a block form or a random form.
• the proportion of oxyethylene groups in the entire polyoxyalkylene group is preferably 20% by weight or more, and if it is less than 20% by weight, water permeability may be lowered.
• the weight average molecular weight of the polyoxyalkylene-modified silicone is not particularly limited, but is preferably 1,000 to 100,000, and more preferably 2,000 to 80,000. When the weight average molecular weight is out of this range, the water permeability decreases, and this tendency is remarkable particularly when the weight average molecular weight is less than 1,000. In the present invention, these polyoxyalkylene-modified silicones can be used alone or in combination of two or more.
• the compound (E2) is at least one selected from a sulfonate (compound (E2a)) and a sulfosuccinate (compound (E2b)).
• the sulfonate (compound (E2a)) is an octyl sulfonate, decyl sulfonate, lauryl sulfonate, myristyl sulfonate, cetyl sulfonate, stearyl sulfonate, or the like having 8 to 18 carbon atoms.
• alkyl sulfonic acid ester salts having an alkyl group having 8 to 12 carbon atoms, such as alkyl sulfonic acid ester salts, octyl benzene sulfonic acid salts, dodecyl benzene sulfonic acid salts and the like.
• Acid ester salts and alkylbenzene sulfonic acid ester salts having an alkyl group having 8 to 12 carbon atoms are preferred.
• 1 type (s) or 2 or more types may be used for a compound (E2a).
• the dialkylsulfosuccinate salt (compound (E2b)) is a dialkyl ester of succinic acid having a sulfonate group at the ⁇ -position.
• the number of carbon atoms of the alkyl group constituting the dialkyl ester may be distributed, and the alkyl group may be linear or branched, and may be saturated or unsaturated.
• the alkyl group preferably has 6 to 22 carbon atoms, more preferably 6 to 18 carbon atoms, still more preferably 8 to 18 carbon atoms, and particularly preferably 8 to 14 carbon atoms. If the alkyl group has less than 6 carbon atoms, the card passing property may decrease. On the other hand, if the alkyl group has more than 22 carbon atoms, the instantaneous water permeability may decrease.
• Examples of the compound (E2b) include dihexyl sulfosuccinate salt, di-2-ethylhexyl sulfosuccinate salt, dilauryl sulfosuccinate salt, dioctyl alkyl sulfosuccinate salt, ditridecyl sulfosuccinate salt, dimyristyl sulfone salt A succinate salt, a distearyl sulfosuccinate salt, etc. are mentioned. These dialkyl sulfosuccinate salts may be used alone or in combination of two or more.
• examples of the salt constituting it include alkali metal salts such as sodium salt and potassium salt, and alkanolamine salts such as monoethanolamine, diethanolamine and triethanolamine, among others.
• Alkali metal salts are preferable, and sodium salts and potassium salts are more preferable.
• a sodium salt and / or potassium salt is preferred because the liquid quickly penetrates into the fiber to which the fiber treating agent is adhered.
• Compound (E3) is a quaternary ammonium salt type cationic surfactant (compound (E3a)), an imidazolinium type cationic surfactant (compound (E3b)), an alkylbetaine surfactant (compound (E3c)), It is at least one selected from alkylimidazole-type betaine surfactant (compound (E3d)) and amide group-containing betaine surfactant (compound (E3e)).
• the quaternary ammonium salt type cationic surfactant (compound (E3a)) is not particularly limited.
• dioctyldimethylammonium chloride salt didecyldimethylammonium chloride salt, dilauryldimethylammonium chloride salt, distearyldimethyl Ammonium chloride salt, dicoconut alkyldimethylammonium chloride salt, di-cured tallow alkyldimethylammonium chloride salt, behenyltrimethylammonium chloride salt, dilauryldimethylammonium methosulfate salt, dilaurylmethylethylammonium etosulphate salt, distearyldimethylammonium methosulfate Salt, di (oleyloxyethyl) hydroxyethylmethylammonium methosulfate salt, di (stearin) Amidoethyl) hydroxyethyl methyl ammonium methyl
• dilauryl dimethyl ammonium chloride salt distearyl dimethyl ammonium chloride salt, and di-cured tallow alkyl dimethyl ammonium chloride salt are preferable.
• 1 type (s) or 2 or more types may be used for a compound (E3a).
• the imidazolinium-type cationic surfactant (compound (E3b)) is not particularly limited, but the substituent at the 2-position of the imidazolinium ring is an aliphatic hydrocarbon group having 11 to 21 carbon atoms, and an anionic group Is preferably an ionic residue selected from the group consisting of methyl sulfate ion, ethyl sulfate ion and dimethyl phosphate ion.
• imidazolinium type cationic surfactant examples include 1-hydroxyethyl-1-ethyl-2-laurylimidazolinium ethyl sulfate salt, 1-hydroxyethyl-1-ethyl-2-oleylimidazolinium ethyl sulfate salt, and the like.
• 1-hydroxyethyl-1-ethyl-2-oleylimidazolinium ethyl sulfate salt is preferable.
• 1 type (s) or 2 or more types may be used for a compound (E3b).
• the alkylbetaine surfactant (compound (E3c)) is not particularly limited, and examples thereof include lauryldimethylaminoacetic acid betaine, stearyldimethylaminoacetic acid betaine, lauryldimethylaminosulfopropylbetaine, and lauryldimethylhydroxysulfobetaine. Among these, stearyldimethylaminoacetic acid betaine is preferable. In addition, 1 type (s) or 2 or more types may be used for a compound (E3c).
• the alkylimidazole-type betaine surfactant (compound (E3d)) is not particularly limited.
• 2-lauryl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine 2-oleyl-N-carboxymethyl- Examples thereof include N-hydroxyethyl imidazolinium betaine.
• 2-lauryl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine is preferred.
• 1 type (s) or 2 or more types may be used for a compound (E3d).
• the amide group-containing betaine surfactant (compound (E3e)) is not particularly limited, and examples thereof include lauric acid amidopropyldimethylaminoacetic acid betaine, oleic acid amidopropyldimethylaminoacetic acid betaine, and stearic acid amidopropyldimethylaminoacetic acid betaine. Among these, betaine stearate amidopropyldimethylaminoacetate is preferable. In addition, 1 type (s) or 2 or more types may be used for a compound (E3e).
• the fiber treatment agent of the present invention may contain other surfactants other than those described above as long as the effects of the present invention are not impaired.
• Other surfactants include anionic surfactants other than the above compound (A), compound (B), compound (C) and compound (E2), nonionic surfactants other than the above nonionic surfactant (D), and cations.
• Surfactants and amphoteric surfactants include anionic surfactants other than the above compound (A), compound (B), compound (C) and compound (E2), nonionic surfactants other than the above nonionic surfactant (D), and cations.
• surfactants include, for example, alkylene oxide adducts of higher alkylamines such as octylamine, decylamine, laurylamine, myristylamine, palmitylamine, stearylamine; monolauric acid glyceride, monomyristic acid glyceride, monopalmitic acid Glycerides, monostearic glycerides, monooleic glycerides, polyglycerin stearates, polyglycerin laurates, sorbitan monolaurates, sorbitan monopalmitates, sorbitan monostearate, sorbitan monooleates, sorbitan trilaurates, sorbitan tripalmi And polyhydric alcohol fatty acid esters such as tate, sorbitan tristearate, sorbitan trioleate, and alkylene oxide adducts thereof. That.
• the fiber treatment agent of the present invention includes a specific phosphoric acid compound in a specific ratio, thereby imparting excellent instantaneous water permeability and liquid return preventing property to the fiber, and preventing the occurrence of winding during fiber production. be able to.
• the fiber treatment agent of the present invention can also be expressed as a “water permeability imparting agent” capable of imparting water permeability to fibers.
• the fiber treatment agent of this invention is used suitably for the synthetic fiber for nonwoven fabric manufacture mentioned later.
• the weight ratio of the compound (C) in the non-volatile content of the treating agent is 1 to 35% by weight, preferably 2 to 30% by weight, more preferably 3 to 25% by weight, still more preferably 4 to 23% by weight, 5 to 20% by weight is particularly preferred. If it is less than 1% by weight, the liquid return preventing property is insufficient. If it exceeds 35% by weight, the card passing ability is insufficient.
• the weight ratio (C / (A + B)) of the total of the compound (A) and the compound (B) to the compound (C) is 0.01 to 0.5, and 0.02 to 0.45. Preferably, 0.03 to 0.4 is more preferable, 0.04 to 0.35 is more preferable, and 0.05 to 0.25 is particularly preferable. If it is less than 0.01, the liquid return preventing property is insufficient. If it exceeds 0.5, card permeability and instantaneous water permeability are insufficient.
• the total of the compound (A), the compound (B) and the compound (C) occupying the nonvolatile content of the treating agent is preferably more than 15% by weight, more preferably 25% by weight or more, and further preferably 60% by weight or more.
• the upper limit is preferably 100% by weight, more preferably 90% by weight, and still more preferably 80% by weight.
• the weight ratio of inorganic phosphoric acid is 3% by weight or less.
• the weight ratio of inorganic phosphoric acid to the entire nonvolatile content of the treatment agent is 3% by weight or less, preferably 2% by weight or less, more preferably 1% by weight or less, 0.5% Less than wt% is particularly preferred.
• a preferred lower limit is 0% by weight. If the inorganic phosphoric acid is more than 3% by weight, the friction between the fiber and the metal at the time of wetting becomes very high, and winding occurs during the fiber production. Also, the card passing property is deteriorated.
• the inorganic phosphoric acid is considered to be present as an alkali metal salt such as potassium or sodium in a part of or all of the hydroxyl group in the fiber treatment agent.
• Inorganic phosphoric acid can be detected by the 31 P-NMR method as in the case of the compound (A).
• the peak of phosphorus element derived from inorganic phosphoric acid is detected at +4 to -1 ppm.
• the peak of phosphorus element derived from compound (B), compound (A) and inorganic phosphoric acid is detected at +4 to ⁇ 1 ppm, but from the low magnetic field side, inorganic phosphoric acid, compound (A), compound (B ) Is determined in the order.
• the non-volatile content of the fiber treatment agent of the present invention means a component in the fiber treatment agent remaining on the fiber surface even after the heat drying step for removing moisture and the like, and the fiber treatment agent is heat treated at 105 ° C. It means a component that has been removed without volatilization when it reaches a constant weight after removing volatile components such as water and solvent.
• the weight ratio of the nonionic surfactant (D) in the nonvolatile content of the treatment agent is preferably 1 to 40% by weight, and preferably 3 to 35% by weight. % Is more preferable, 4 to 30% by weight is further preferable, and 5 to 25% by weight is particularly preferable. If the weight ratio of the nonionic surfactant (D) is less than 1% by weight, the instantaneous water permeability may be insufficient. On the other hand, when the weight ratio of the nonionic surfactant (D) is more than 40% by weight, there is a possibility that the friction between the fibers and the metal when wet is increased.
• the weight ratio of the compound (E) in the nonvolatile content of the treatment agent is preferably 3 to 30% by weight, more preferably 5 to 28% by weight. 7 to 27% by weight is more preferable, and 10 to 25% by weight is particularly preferable.
• the weight ratio of the compound (E) is less than 3% by weight, the durable water permeability may be insufficient.
• the weight ratio of the compound (E) is more than 30% by weight, the liquid returnability may be lowered or the roller may be wound.
• the weight ratio of the compound (E2) in the non-volatile content of the treatment agent is high, the possibility of occurrence of lowering of liquid return and roller wrapping increases. Therefore, the weight ratio of the compound (E2) is 5% by weight. Is preferably less than 4% by weight, more preferably less than 3% by weight, and particularly preferably 0% by weight.
• the weight ratio (A1 + B1 + C1) / (A2 + B2 + C2) to the total weight of the compound (C2) in which R 1 is 11 to 15 carbon atoms is preferably 1 to 20, more preferably 1.1 to 15.
• 2 to 10 is more preferable, and 1.5 to 5 is particularly preferable. If it is less than 1, the instantaneous water permeability may be reduced, and if it exceeds 20, friction between the fiber and metal when wet may not be appropriate, or the card passing property may be insufficient.
• the fiber treatment agent of the present invention may contain water and / or a solvent, if necessary, and preferably contains water.
• the water used in the present invention may be any of pure water, distilled water, purified water, soft water, ion exchange water, tap water and the like.
• the weight ratio of the non-volatile content in the fiber treatment agent when producing the fiber treatment agent is preferably 10 to 60% by weight, and particularly preferably 18 to 50% by weight.
• the fiber treatment agent of the present invention may further contain an antibacterial agent, an antioxidant, an antiseptic, a matting agent, a pigment, an antirust agent, an fragrance, an antifoaming agent and the like, if necessary.
• an antibacterial agent such as a sulfuric acid
• organic acids such as lactic acid and a citric acid, as pH adjustment.
• the method for producing the fiber treatment agent of the present invention a known method can be adopted.
• an aqueous solution of the compound (A), the compound (B) and the compound (C) is mixed with a nonionic surfactant (D) and / or the compound (E) as necessary, and the mixture is stirred at a temperature of about 70 ° C. .
• a fiber treatment agent having a nonvolatile content of 10 to 60% by weight can be obtained.
• the electrical conductivity of the fiber treatment agent of the present invention is preferably less than 1300 ⁇ S / cm, more preferably 1000 ⁇ S / cm or less, and even more preferably 800 ⁇ S / cm or less from the viewpoint of durable hydrophilicity.
• a preferred lower limit is 0 ⁇ S / cm.
• the water-permeable fiber of the present invention refers to a fiber composed of a synthetic fiber (fiber body) for producing a nonwoven fabric and the fiber treatment agent attached thereto, and is generally a short fiber cut to a predetermined length. .
• the adhesion rate of the non-volatile content of the fiber treatment agent is 0.1 to 2% by weight, preferably 0.3 to 1% by weight, based on the water-permeable fiber. When the adhesion rate is less than 0.1% by weight, the instantaneous water permeability of fibers and nonwoven fabrics and the antistatic property of the card may be insufficient.
• the fiber length of the water-permeable fiber of the present invention is preferably 2 to 100 mm, more preferably 10 to 64 mm, still more preferably 20 to 60 mm, and particularly preferably 31 to 55 mm. If the fiber length is less than 2 mm or more than 100 mm, the card passing property may be deteriorated.
• the thickness of the water-permeable fiber of the present invention is generally expressed in units of decitex (hereinafter expressed as dtex), preferably 0.7 to 4.0 dtex, more preferably 0.8 to 3.0 dtex, 0.9 to 2.0 dtex is more preferable, and 1.0 to 1.5 dtex is particularly preferable. If it is less than 0.7 dtex, the card passing property may be lowered. If it exceeds 4.0 dtex, the converging property is lowered, so that the card passing property may be lowered.
• Synthetic fibers for producing nonwoven fabric include, for example, polyolefin fibers, polyester fibers, nylon fibers, polyvinyl chloride fibers, composite fibers composed of two or more types of thermoplastic resins, etc.
• polyolefin resin / polyolefin resin for example, high density polyethylene / polypropylene, linear high density polyethylene / polypropylene, low density polyethylene / polypropylene, binary copolymer of propylene and other ⁇ -olefin or ternary Examples include copolymer / polypropylene, linear high-density polyethylene / high-density polyethylene, and low-density polyethylene / high-density polyethylene.
• polyolefin resin / polyester resin for example, polypropylene / polyethylene terephthalate, high-density polyethylene / polyethylene terephthalate, linear high-density polyethylene / polyethylene terephthalate, and low-density polyethylene / polyethylene terephthalate.
• polyester-type resin / polyester-type resin copolymer polyester / polyethylene terephthalate etc. are mentioned, for example.
• the fiber which consists of polyamide-type resin / polyester-type resin, polyolefin-type resin / polyamide-type resin etc. can be illustrated.
• the synthetic fiber for nonwoven fabric production before the fiber treatment agent is attached can also be referred to as a hydrophobic synthetic fiber.
• synthetic fibers for producing nonwoven fabrics fiber bodies
• polyolefin fibers including polyolefin fibers and polyolefin fibers
• the fiber treatment agent of the present invention is suitable for synthetic fibers for producing nonwoven fabrics such as composite fibers) and polyester fibers (complex fibers including polyester fibers and polyester fibers).
• Examples of the cross-sectional structure of the fiber include a sheath-core type, a parallel-type, an eccentric sheath-core type, a multilayer type, a radiation type, and a sea-island type.
• the sheath includes eccentricity.
• a core type or a parallel type is preferred.
• the cross-sectional shape can be a circular shape or an irregular shape. In the case of an irregular shape, for example, a flat shape, a polygonal shape such as a triangle to an octagon, a T shape, a hollow shape, a multileaf shape, and the like can be used.
• the fiber treatment agent of the present invention may be adhered to the fiber body without being diluted as it is, and diluted with water or the like to a concentration such that the weight ratio of the entire nonvolatile content becomes 0.5 to 5% by weight. You may make it adhere to a main body.
• the step of attaching the fiber treatment agent to the fiber body may be any of a spinning process, a stretching process, a crimping process, and the like of the fiber body.
• the means for attaching the fiber treatment agent of the present invention to the fiber main body is not particularly limited, and means such as roller lubrication, nozzle spray lubrication, and dip lubrication may be used.
• a method for obtaining a desired adhesion amount more uniformly and efficiently may be employed in accordance with the fiber manufacturing process and its characteristics.
• a method of drying the fiber to which the fiber treatment agent is applied a method of drying with hot air and infrared rays, a method of drying by contacting with a heat source, or the like may be used.
• Method for producing nonwoven fabric As a manufacturing method of a nonwoven fabric, a well-known method is employable without particular limitation. Short fibers or long fibers can be used as the raw fiber. Examples of the web forming method in which the raw fibers are short fibers include a dry method such as a card method and an airlaid method, and a wet method such as a papermaking method. Examples of the web forming method in which the raw fibers are long fibers include a spunbond method, a melt blow method, and a flash spinning method. Examples of the interfiber bonding method include a chemical bond method, a thermal bond method, a needle punch method, a spunlace method, and a stitch bond method.
• the method for producing a nonwoven fabric of the present invention preferably includes a step of producing a fiber web by passing the water-permeable fibers (for example, short fibers) of the present invention through a card machine or the like and heat-treating the obtained fiber web. That is, the fiber treatment agent of the present invention is particularly suitably used when it has a step of heat-treating the fiber web in the production of the nonwoven fabric.
• the method for bonding the fiber web by heat treatment include heat fusion methods such as thermocompression bonding using a heating roll or ultrasonic waves, heat fusion using heated air, and a thermocompression bonding (point bonding) method.
• heat-bonding the fiber web in the case of a sheath-core type composite fiber using a high melting point resin for the core and a low melting point resin for the sheath, heat treatment is performed near the melting point of the low melting point resin.
• thermal bonding of the fiber intersection can be easily performed.
• a method for producing a nonwoven fabric including a step of thermally bonding a method of integrating short-fibers provided with a fiber treatment agent into a web through a card machine or the like by heat-treating and integrating them as described above, an airlaid method
• a method of blending with the water-permeable fibers (short fibers) of the present invention when laminating pulp or the like, and joining them by heat treatment as described above is also included.
• a fiber molded body obtained by a spunbond method, a melt blow method, a flash spinning method, or the like is subjected to heat treatment with a heated roll or heated air or the like to which the fiber treatment agent of the present invention is attached, or a heated roll
• a method of manufacturing a nonwoven fabric by attaching the fiber treatment agent of the present invention to a material heat-treated with heated air or the like is also included.
• a composite fiber resin is spun, then the spun composite long fiber filament is cooled with a cooling fluid, and tension is applied to the filament with drawn air to obtain the desired fineness. Thereafter, the spun filament is collected on a collection belt and subjected to a bonding treatment to obtain a spunbonded nonwoven fabric.
• the joining means include thermocompression bonding using a heating roll or ultrasonic waves, thermal fusion using heated air, and a thermocompression bonding (point bonding) method.
• a method for applying the fiber treatment agent of the present invention to the obtained spunbonded nonwoven fabric it can be performed by a gravure method, a flexo method, a roll coating method such as a gate roll method, a spray coating method, etc.
• the amount is not particularly limited as long as the amount can be adjusted for each side.
• a drying method of the nonwoven fabric provided with the fiber treatment agent a method of drying by hot air and infrared rays, a method of drying by contacting with a heat source, or the like may be used.
• examples of the liquid that exhibits water permeability include urine, soft stool, mud stool, watery stool, blood, body fluid, and exudate.
• Applications of the nonwoven fabric of the present invention include disposable diapers for infants, disposable diapers for nursing care, sanitary products, bandages, bandages, disinfecting cloths, surgical tapes, pet excretion sheets, fragrance absorbent cores, liquid insect repellents, etc. Examples include daily use applications such as liquid absorbent cores and cleaning cloths, and food-related applications such as coffee filters and draining sheets.
• an organic phosphoric acid compound which is a mixture of compound (A), compound (B), compound (C) and inorganic phosphoric acid, was produced as follows. 250 g of POE (3) octyl ether was charged into a 1 liter flask, and 55 g of phosphoric anhydride (corresponding to 0.4 mol as P 2 O 5 with respect to 1 mol of POE (3) octyl ether) was gradually added while stirring. The mixture was stirred for 3 hours while maintaining 80 ° C. A slightly brown transparent unneutralized product was obtained.
• Examples 2 to 7 In the same manner as in Example 1, fiber treating agents of Examples 2 to 7, which are mixtures of the compounds (A) to (C) and inorganic phosphoric acid shown in Table 1, were obtained.
• Examples 8 to 16 In the same manner as in Example 1, after obtaining a mixture of the compounds (A) to (C) and inorganic phosphoric acid shown in Table 1, the compound (D) or the compound (E) shown in Table 1 was mixed. 8 to 16 fiber treatment agents were obtained.
• Comparative Example 1 250 g of POE (3) octyl ether was charged into a 1 liter flask, and 55 g of phosphoric anhydride was gradually added while stirring, and the mixture was stirred for 3 hours while maintaining 80 ° C.
• compound (C) is 50% by weight with respect to the whole non-volatile content of the yellow translucent paste
• inorganic phosphoric acid is 4% by weight with respect to the whole non-volatile content of the yellow translucent paste.
• the fiber treatment agents of Examples 1 to 16 and Comparative Examples 1 to 7 having a non-volatile content in the entire fiber treatment agent of 25% by weight were prepared.
• the obtained fiber treating agents were each diluted with warm water of about 60 ° C. so that the weight ratio of non-volatile content was 0.9% by weight to obtain a diluted solution.
• 150 g of a diluted solution of each fiber treatment agent was attached to 300 g of the fiber main body by the dip oiling method, so that the non-volatile content of the fiber treatment agent attached to the water-permeable fiber was 0.45% by weight.
• the fiber body was a polypropylene (core) -polyethylene (sheath) based composite fiber to which no fiber treatment agent was attached, and had a single fiber fineness of 2.2 Dtex and a fiber length of 38 mm.
• the fibers to which the diluted solutions of the respective fiber treatment agents were adhered were placed in a hot air dryer at 80 ° C. for 2 hours, and then allowed to stand at room temperature for 8 hours or more to dry, thereby obtaining water-permeable fibers.
• the obtained water-permeable fibers were respectively passed through a fiber opening process and a card process using a card testing machine, and webs having a basis weight of 25 g / m 2 were produced.
• physical properties antistatic property, winding of cylinder, presence / absence of scum, number of neps
• the obtained web was heat-treated at 135 ° C. in an air-through hot air circulating dryer to fix the web to obtain a nonwoven fabric.
• the physical property instant water permeability, liquid return prevention property
• a durable water permeability evaluation result is shown to the durable water permeability of the following (4) nonwoven fabrics.
• Cotton-making process evaluation As a substitute evaluation with roller wrapping during the cotton-making process, the friction between the fibers and the metal when wet was measured. It has been confirmed that the lower the friction between the fiber and metal when wet, the lower the wrapping in the cotton making process. In the following evaluation method, it has been empirically obtained that winding is reduced in the cotton-making process if it is 40 g or less. Therefore, the fiber / metal friction during wetting was 40 g or less, and the index was evaluated as “good”, and the result was accepted.
• Friction between fiber / metal when wet 40 g or less
• Friction between fiber / metal when wet is more than 40 g (Measurement method of friction between fiber / metal when wet)
• Degreased polyester multifilament (total 167 dtex, 48 pieces) is wound around a friction body (3 cm diameter satin pin) with a contact angle of 450 °, and a 20 g load is applied to the tip. While the emulsion of the fiber treatment agent was dropped, it was pulled at a speed of 3 cm / min, and the frictional force (unit: g) at that time was measured.
• the temperature condition in that case is 20 degreeC.
• the scum adhered to the roller was observed after carding 200 g of the sample water permeable fiber under the conditions of 30 ° C. and 70% RH, and the presence or absence of scum generation was evaluated. 5 ... Scum is not seen 4 ... Scum is few 3 ... Scum is seen 2 ... Scum is seen much 1 ... Scum is seen very much If it is 4 or more, it can be put to practical use. (2-4) Number of Nep Using a card tester, the number of Nep was determined by visual judgment of a web obtained by carding 40 g of the sample water permeable fiber under the condition of 30 ° C. ⁇ 70% RH. The smaller the nep, the better the evaluation. 5 ... Nep is not seen 4 ... Nep is few 3 ... Nep is seen 2 ... Nep is seen a lot 1 ... Nep is seen a lot If it is 4 or more, it can be put to practical use.
• the disappearance time of physiological saline was measured at 20 locations by the instantaneous water permeability test method of the nonwoven fabric, and the number of disappearance time less than 5 seconds was determined. displayed. If this number is 18 or more, the durable water permeability is good. The same operation is repeated for the nonwoven fabric subjected to the test. In this repeated test, it is better that the number of disappearances of the physiological saline (the number of places where the disappearance time is less than 5 seconds) is large even if the number of times is repeated. In Example 12, the first time was 20, the second time was 3, and the third time was 0.
• Example 13 the first time was 20, the second time was 10, and the third time was 2.
• Example 14 the first time was 20, the second time was 5, and the third time was 0.
• the results of Examples 1 to 11 and Comparative Examples 1 to 7 were all zero at the first time.
• Examples 12 to 14 not only solved the problem of the present application, but also proved to have good durable water permeability.
• (5) Liquid return prevention property of nonwoven fabric Place a nonwoven fabric (10 cm x 10 cm) on a commercially available paper diaper, place a cylinder with an inner diameter of 60 mm on it, inject 100 ml of physiological saline into the cylinder, and pass through the nonwoven fabric into the paper diaper. Absorbed.
• each component in Table 1 is as follows.
• the fiber treatment agents of Examples 1 to 16 contain the compound (A), the compound (B), and the compound (C), and the weight ratio of the compound (C) is 1 to 35. %
• the weight ratio (C / (A + B)) of the compound (A) and the compound (B) to the compound (C) is 0.01 to 0.5
• the weight ratio of the inorganic phosphoric acid is In order to satisfy 3% by weight or less, the fiber-to-metal friction when wet is low, so that the cotton-permeable property is excellent, and the water-permeable fiber to which the treatment agent is applied has excellent card permeability and instant water permeability.
• the problem of the present application could be solved.

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