WO2021251281A1 - Aqueous solution of synthetic fiber treatment agent, and method for manufacturing synthetic fibers - Google Patents

Aqueous solution of synthetic fiber treatment agent, and method for manufacturing synthetic fibers Download PDF

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Publication number
WO2021251281A1
WO2021251281A1 PCT/JP2021/021314 JP2021021314W WO2021251281A1 WO 2021251281 A1 WO2021251281 A1 WO 2021251281A1 JP 2021021314 W JP2021021314 W JP 2021021314W WO 2021251281 A1 WO2021251281 A1 WO 2021251281A1
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group
treatment agent
ester
aqueous solution
mass
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PCT/JP2021/021314
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French (fr)
Japanese (ja)
Inventor
卓 村上
英里 坪田
久典 村田
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竹本油脂株式会社
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Application filed by 竹本油脂株式会社 filed Critical 竹本油脂株式会社
Priority to CN202180002707.4A priority Critical patent/CN113728137B/en
Priority to KR1020227020898A priority patent/KR102460480B1/en
Priority to EP21821920.2A priority patent/EP4159913A4/en
Publication of WO2021251281A1 publication Critical patent/WO2021251281A1/en

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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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
    • D06M13/165Ethers
    • D06M13/17Polyoxyalkyleneglycol ethers
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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
    • D06M13/224Esters of carboxylic acids; Esters of carbonic acid

Definitions

  • the present invention comprises a step of adhering an aqueous solution of a synthetic fiber treatment agent having excellent retention of components on the fiber and excellent low temperature handleability, and an aqueous solution of the synthetic fiber treatment agent to the synthetic fiber. Regarding the manufacturing method of.
  • a treatment for adhering a synthetic fiber treatment agent to the surface of the filament yarn of the synthetic fiber is performed from the viewpoint of reducing friction and reducing fiber damage such as yarn breakage.
  • the form of the adhesion treatment is that when the treatment agent for synthetic fibers is diluted with water (emulsion refueling), the treatment agent for synthetic fibers is diluted with a diluent such as low-viscosity mineral oil or applied as it is without being diluted. There is a case (straight refueling).
  • Patent Document 1 discloses an emulsion containing a treatment agent for synthetic fibers containing a lauryl isostearate, a smoothing agent such as mineral oil, and a surfactant such as an oleyl alcohol EO adduct.
  • Patent Document 2 discloses an emulsion containing a treatment agent for synthetic fibers containing a glycerin ester compound, a branched ester compound and the like.
  • the present invention has been made in view of such circumstances, and an object thereof is to provide an aqueous solution of a treatment agent for synthetic fibers, which is excellent in retention of components in fibers and excellent in low temperature handling. Further, the present invention provides a method for producing a synthetic fiber, which comprises a step of adhering an aqueous solution of the treatment agent for synthetic fiber to the synthetic fiber.
  • the present inventors have contained a predetermined ester compound and a surfactant as a smoothing agent in the aqueous solution of the synthetic fiber treatment agent, and the temperature of the synthetic fiber treatment agent is 30 ° C. It has been found that it is correct and suitable that the kinematic viscosity has a predetermined range.
  • the aqueous solution of the synthetic fiber treatment agent for solving the above problems is an aqueous solution of the synthetic fiber treatment agent containing a smoothing agent, a nonionic surfactant, and an ionic surfactant, and the smoothing agent is used.
  • the ester A1 shown in Chemical formula 1 below and the ester A2 shown in Chemical formula 2 below are optionally contained, and the ester A1 is contained in the smoothing agent in a proportion of 40 to 100% by mass, and the ester is said. Assuming that the total content of A1 and the ester A2 is 100% by mass, the ester A1 is contained in a proportion of 50 to 100% by mass, and the kinematic viscosity of the synthetic fiber treatment agent at 30 ° C. is 40 to 150 mm 2. It is characterized by being / s.
  • R 1 Saturated hydrocarbon group having 7 to 23 carbon atoms or unsaturated hydrocarbon group having 7 to 23 carbon atoms
  • R 2 Saturated hydrocarbon group having 8 to 24 carbon atoms or unsaturated hydrocarbon group having 8 to 24 carbon atoms.
  • R 1 and R 2 has a branched chain structure.
  • R 3 Saturated hydrocarbon group having 7 to 23 carbon atoms or unsaturated hydrocarbon group having 7 to 23 carbon atoms
  • R 4 Saturated hydrocarbon group having 8 to 24 carbon atoms or unsaturated hydrocarbon group having 8 to 24 carbon atoms.
  • R 3 and R 4 have a linear structure.
  • the cooling cloud point of the aqueous liquid of the synthetic fiber treatment agent is preferably 10 ° C. or lower.
  • the aqueous solution of the synthetic fiber treatment agent further contains an antioxidant, and the total content of the smoothing agent, the nonionic surfactant, the ionic surfactant, and the antioxidant is 100% by mass. Then, it is preferable to contain the antioxidant in an amount of 0.01 to 0.5% by mass.
  • the aqueous solution of the synthetic fiber treatment agent has 7 to 17 carbon atoms in R 1 and 8 to 18 carbon atoms in R 2 and 7 to 7 carbon atoms in R 3 of the chemical compound 2.
  • the number of carbon atoms of 17, and R 4 is preferably a 8-18.
  • a method for producing a synthetic fiber for solving the above-mentioned problems is characterized by including a step of adhering an aqueous liquid of the treatment agent for synthetic fibers to the synthetic fiber.
  • the aqueous solution of the synthetic fiber treatment agent of the present invention is excellent in the retention of components in the fiber and also in the low temperature handling property.
  • the aqueous liquid of the present embodiment is composed of a smoothing agent, a nonionic surfactant, a synthetic fiber treatment agent containing an ionic surfactant (hereinafter referred to as a treatment agent), and water.
  • the treatment agent may further contain an antioxidant.
  • the smoothing agent used in this embodiment contains the ester A1 shown in Chemical formula 3 below.
  • R 1 Saturated hydrocarbon group having 7 to 23 carbon atoms or unsaturated hydrocarbon group having 7 to 23 carbon atoms
  • R 2 Saturated hydrocarbon group having 8 to 24 carbon atoms or unsaturated hydrocarbon group having 8 to 24 carbon atoms.
  • R 1 and R 2 has a branched chain structure.
  • One of these esters A1 may be used alone, or two or more thereof may be used in combination.
  • compounds having 7 to 17 carbon atoms in R 1 of Chemical formula 3 and 8 to 18 carbon atoms in R 2 are preferable. By defining it in such a range, it is possible to lower the cooling cloud point of the treating agent in particular and further improve the low temperature handling property of the aqueous liquid.
  • linear saturated hydrocarbon group constituting R 1 examples include heptyl group, octyl group, nonyl group, decyl group, undecyl group, dodecyl group, tridecylic group, tetradecyl group, pentadecyl group, hexadecyl group and heptadecyl.
  • examples thereof include a group, an octadecyl group, an icosyl group, a docosyl group, a tridecylic group and the like.
  • saturated hydrocarbon group having a branched chain structure constituting R 1 is, for example isoheptyl group, isooctyl group, an isononyl group, an isodecyl group, isoundecyl group, isododecyl group, an isotridecyl group, isotetradecyl group, iso-pentadecyl
  • saturated hydrocarbon group having a branched chain structure constituting R 1 is, for example isoheptyl group, isooctyl group, an isononyl group, an isodecyl group, isoundecyl group, isododecyl group, an isotridecyl group, isotetradecyl group, iso-pentadecyl
  • examples thereof include a group, an isohexadecyl group, an isoheptadecyl group, an isooctadecyl group,
  • the unsaturated hydrocarbon group constituting R 1 is an alkenyl group having one double bond as an unsaturated carbon bond, an alkazienyl group having two or more double bonds, an alkatienyl group, or the like. May be good. Further, it may be an alkynyl group having one triple bond as an unsaturated carbon bond, an alkadynyl group having two or more triple bonds, or the like.
  • linear unsaturated hydrocarbon group having one double bond in the hydrocarbon group include, for example, a heptenyl group, an octenyl group, a nonenyl group, a decenyl group, an undecenyl group, a dodecenyl group, a tridecenyl group, and a tetradecenyl group.
  • the unsaturated hydrocarbon group in the hydrocarbon group constituting R 1 has a branched chain structure having one double bond, for example isoheptenyl group, isooctenyl group, Isononeniru group, Isodeseniru group, Isoundeseniru group, isododecenyl Group, isotridecenyl group, isotetradecenyl group, isopentadecenyl group, isohexadecenyl group, isoheptadecenyl group, isooctadecenyl group, isoicosenyl group, isodococenyl group, isotricosenyl group, etc. Can be mentioned.
  • linear saturated hydrocarbon group constituting R 2 examples include an octyl group, a nonyl group, a decyl group, an undecyl group, a dodecyl group, a tridecylic group, a tetradecyl group, a pentadecyl group, a hexadecyl group, a heptadecyl group and an octadecyl group.
  • examples thereof include a group, an icosyl group, a docosyl group, a tridecylic group, a tetracosyl group and the like.
  • saturated hydrocarbon group having a branched chain structure constituting R 2 include an isooctyl group, an isononyl group, an isodecyl group, an isoundesyl group, an isododecyl group, an isotridecyl group, an isotetradecyl group, an isopentadecyl group and an iso.
  • Examples thereof include a hexadecyl group, an isoheptadecyl group, an isooctadecyl group, an isoicosyl group, an isodocosyl group, an isotricosyl group and an isotetracosyl group.
  • the unsaturated hydrocarbon group constituting R 2 is an alkenyl group having one double bond as an unsaturated carbon bond, an alkazienyl group having two or more double bonds, an alkatienyl group, or the like. May be good. Further, it may be an alkynyl group having one triple bond as an unsaturated carbon bond, an alkadynyl group having two or more triple bonds, or the like.
  • linear unsaturated hydrocarbon group having one double bond in the hydrocarbon group include, for example, an octenyl group, a nonenyl group, a decenyl group, an undecenyl group, a dodecenyl group, a tridecenyl group, a tetradecenyl group, and a pentadecenyl group.
  • the unsaturated hydrocarbon group in the hydrocarbon group constituting R 2 has a branched chain structure having one double bond, for example isooctenyl group, Isononeniru group, Isodeseniru group, Isoundeseniru group, isododecenyl group, Isotorideseniru Group, Isotetradecenyl group, Isopentadecenyl group, Isohexadecenyl group, Isoheptadecenyl group, Isooctadecenyl group, Isoicosenyl group, Isodococenyl group, Isotricosenyl group, Isotetracosenyl group The group etc. can be mentioned.
  • ester A1 examples include isotridecyl oleate, lauryl isosteleart, isooctyl octylate, octyl isooctylate, isotridecyl isosteleert, oleyl isosteert, icosyl isosteleert, and isotetraco. Examples include silole art.
  • the smoothing agent used in this embodiment optionally contains the ester A2 shown in Chemical formula 4 below.
  • R 3 Saturated hydrocarbon group having 7 to 23 carbon atoms or unsaturated hydrocarbon group having 7 to 23 carbon atoms
  • R 4 Saturated hydrocarbon group having 8 to 24 carbon atoms or unsaturated hydrocarbon group having 8 to 24 carbon atoms.
  • R 3 and R 4 have a linear structure.
  • These esters A2 may be used alone or in combination of two or more.
  • R 3 of Chemical formula 4 has 7 to 17 carbon atoms and R 4 has 8 to 18 carbon atoms.
  • saturated hydrocarbon group or unsaturated hydrocarbon group constituting R 3 or R 4 are those exemplified as the saturated hydrocarbon group or unsaturated hydrocarbon group constituting R 1 or R 2 of Chemical formula 3. , Linear ones can be mentioned.
  • ester A2 examples include oleyl octylate, lauryl oleart, stearyl elkhart, lauryl elkhart and the like.
  • the aqueous solution contains the ester A1 in a ratio of 50 to 100% by mass.
  • the aqueous solution preferably contains the ester A1 in a proportion of 60 to 100% by mass.
  • a smoothing agent other than the above may be used in combination.
  • known ones can be appropriately adopted.
  • Specific examples of the smoothing agent include (1) an ester compound of an aliphatic monoalcohol and an aliphatic monocarboxylic acid such as (1) butyl stealert, isobutyl laurate, and isohexacocil stealert, and an aliphatic monoalcohol having a carbon number of carbon atoms.
  • An ester compound of an (poly) oxyalkylene adduct to which 2 to 4 alkylene oxides have been added and an aliphatic monocarboxylic acid (2) 1,6-hexanediol didecanoate, trimethylolpropane monooleate monolaurate, Ester compounds of aliphatic polyhydric alcohols and aliphatic monocarboxylic acids such as sorbitan trioleate, sorbitan monooleart, sorbitan monosteert, glycerin monolaurate, (3) dilauryl adipate, diorail azelate, Aliphatic monoalcohols and ester compounds of aliphatic polyvalent carboxylic acids such as diisocetylthiodipropionate and bispolyoxyethylene lauryl ether adipate, and alkylene oxides having 2 to 4 carbon atoms are added to the aliphatic monoalcohols.
  • Aromatic monoalcohols and aliphatic monocarboxylic acids such as (4) benzyloleate, benzyllaurate and polyoxypropylene benzyl steaert, which are ester compounds of the (poly) oxyalkylene adduct and aliphatic polyvalent carboxylic acids.
  • an ester compound of an aliphatic monocarboxylic acid and a (poly) oxyalkylene adduct having an alkylene oxide having 2 to 4 carbon atoms added to an aromatic monoalcohol (5) bisphenol A dilaurate, polyoxyethylene bisphenol.
  • An ester compound of an aromatic polyvalent alcohol and an aliphatic monocarboxylic acid such as A dilaurate, a (poly) oxyalkylene adduct to which an alkylene oxide having 2 to 4 carbon atoms is added to the aromatic polyvalent alcohol, and an aliphatic monocarboxylic compound.
  • Aliphatic monoalcohols, ester compounds of aliphatic monoalcohols and aromatic polyvalent carboxylic acids such as (6) bis2-ethylhexylphthalate, diisostearylisophthalate, trioctyl remeritate, and aliphatic monoalcohols with acids.
  • the smoothing agent contains ester A1 in a proportion of 40 to 100% by mass. By defining in such a range, the effect of the present invention can be improved. Further, the smoothing agent preferably contains ester A1 in a proportion of 60 to 100% by mass. By defining it in such a range, it is possible to lower the cooling cloud point of the treating agent in particular, and further improve the low temperature handling property and the fluff suppressing effect in post-processing.
  • the content of the smoothing agent in the treatment agent is appropriately set, but is preferably 20 to 80% by mass, more preferably 30 to 70% by mass, and further preferably 40 to 60% by mass. By defining in such a range, the smoothness of the fiber can be improved.
  • nonionic surfactant used in this embodiment, known ones can be appropriately adopted.
  • the nonionic surfactant include (1) a compound obtained by adding an alkylene oxide having 2 to 4 carbon atoms to an organic acid, an organic alcohol, an organic amine and / or an organic amide, for example, a polyoxyethylene dilauric acid ester.
  • Ionic surfactant (2) Polyoxyalkylene sorbitan trioleate, polyoxyalkylene palm oil, polyoxyalkylene castor oil, polyoxyalkylene cured castor oil, polyoxyalkylene cured castor oil trioctanoate, polyoxyalkylene cured castor
  • Polyoxyalkylene polyvalent alcohol fatty acid ester type nonionic surfactant such as maleic acid ester, stearic acid ester, or oleic acid ester of oil
  • Alkylamide type nonionic such as stearate diethanolamide and diethanolamine monolauroamide. Examples thereof include a surface active agent, (4) a polyoxyalkylene fatty acid amide type nonionic surface active agent such as polyoxyethylene diethanolamine monooleylamide, polyoxyethylene laurylamine, and polyoxyethylene beef amine.
  • the content of the nonionic surfactant in the treatment agent is appropriately set, but is preferably 5 to 70% by mass, more preferably 15 to 60% by mass, and further preferably 25 to 55% by mass. By defining in such a range, the effect of the present invention and the stability of the aqueous liquid can be improved.
  • ionic surfactant used in this embodiment, known ones can be appropriately adopted.
  • ionic surfactants include anionic surfactants, cationic surfactants, and amphoteric surfactants. These components may be used alone or in combination of two or more.
  • anionic surfactant used in the present embodiment, known ones can be appropriately adopted.
  • the anionic surfactant include (1) phosphate esters of aliphatic alcohols such as (1) lauryl phosphate ester salt, cetyl phosphate ester salt, octyl phosphate ester salt, oleyl phosphate ester salt, and stearyl phosphate ester salt. Salt, (2) At least one selected from ethylene oxide and propylene oxide for aliphatic alcohols such as polyoxyethylene lauryl ether phosphate ester salt, polyoxyethylene oleyl ether phosphate ester salt, and polyoxyethylene stearyl ether phosphate ester salt.
  • Phosphate ester salt with alkylene oxide added (3) Lauryl sulfonate, myristyl sulfonate, cetyl sulfonate, oleyl sulfonate, stearyl sulfonate, tetradecane sulfonate, dodecylbenzene sulfonate , An aliphatic sulfonate such as a secondary alkyl sulfonic acid (C13 to 15) salt or an aromatic sulfonate, (4) Sulfate of an aliphatic alcohol such as a lauryl sulfate ester salt, an oleyl sulfate ester salt, and a stearyl sulfate ester salt.
  • An aliphatic sulfonate such as a secondary alkyl sulfonic acid (C13 to 15) salt or an aromatic sulfonate
  • Sulfate of an aliphatic alcohol
  • Ester salts (5) Polyoxyethylene lauryl ether sulfate ester salts, polyoxyalkylene (polyoxyethylene, polyoxypropylene) lauryl ether sulfate ester salts, polyoxyethylene oleyl ether sulfate ester salts, and other aliphatic alcohols with ethylene oxide and Sulfate ester salt with at least one alkylene oxide added selected from propylene oxide, (6) sesame oil fatty acid sulfate ester salt, sesame oil fatty acid sulfate ester salt, tall oil fatty acid sulfate ester salt, soybean oil fatty acid sulfate ester salt, rapeseed oil fatty acid sulfate Esters, palm oil fatty acid sulfates, pig fat fatty acid sulfates, beef fat fatty acid sulfates, whale oil fatty acid sulfates and other fatty acid sulfates, (7) castor oil sulf
  • Examples thereof include sulfate ester salts, (8) fatty acid salts such as laurate, oleate and stearate, and (9) sulfosuccinic acid ester salts of aliphatic alcohols such as dioctyl sulfosuccinate.
  • Examples of the counterion of the anionic surfactant include alkali metal salts such as potassium salt and sodium salt, and alkanolamine salts such as ammonium salt and triethanolamine.
  • cationic surfactant used in the present embodiment known ones can be appropriately adopted.
  • Specific examples of the cationic surfactant include lauryltrimethylammonium chloride, cetyltrimethylammonium chloride, stearyltrimethylammonium chloride, behenyltrimethylammonium chloride, didecyldimethylammonium chloride and the like.
  • amphoteric surfactant used in the present embodiment known amphoteric surfactants can be appropriately adopted.
  • specific examples of the amphoteric tenside include a betaine-type amphoteric tenside.
  • the content of the ionic surfactant in the treatment agent is appropriately set, but is preferably 1 to 20% by mass, more preferably 3 to 16% by mass, and further preferably 6 to 13% by mass. By being defined in such a range, the effect of the present invention, the stability of the aqueous liquid, or the antistatic property can be improved.
  • the aqueous liquid of the present embodiment preferably contains an antioxidant.
  • an antioxidant By containing an antioxidant, the retention of the component in the fiber can be further improved.
  • known antioxidants can be appropriately adopted. Specific examples of the antioxidant include (1) 1,3,5-tris (3', 5'-di-t-butyl-4-hydroxybenzyl) isocyanuric acid and 1,3,5-tris (4).
  • the aqueous solution preferably contains the antioxidant from 0.01 to 0. Contains 5% by mass.
  • the kinematic viscosity of the treatment agent at 30 ° C. is defined as 40 to 150 mm 2 / s. By defining in such a range, the effect of the present invention can be improved.
  • the content ratio of the treatment agent and water in the aqueous solution is not particularly limited. Assuming that the content ratio of the treating agent in the aqueous liquid is 100 parts by mass, the content ratio of water in the aqueous liquid is 30 parts by mass or less, preferably 5 to 30 parts by mass, and more preferably 5 to 20 parts by mass. .. By specifying such a blending ratio, the handleability of the aqueous liquid can be improved and the stability over time can be improved.
  • the cooling cloud point of the aqueous liquid is preferably 10 ° C. or lower, more preferably 8 ° C. or lower, and even more preferably 7 ° C. or lower.
  • the cooling cloud point indicates the temperature at which the prepared aqueous solution is gradually cooled from room temperature, the components are precipitated to form an opaque solution having turbidity, and then the temperature is gradually raised to eliminate the turbidity.
  • the synthetic fiber is produced through a step of adhering the aqueous liquid of the first embodiment or an emulsion obtained by further diluting the aqueous liquid with water to the synthetic fiber in, for example, a spinning or drawing step. ..
  • the aqueous liquid or emulsion attached to the synthetic fiber may evaporate the water content by a drying step.
  • polyester fiber such as polyethylene terephthalate, polypropylene terephthalate and polylactic acid ester
  • polyamide fiber such as nylon 6 and nylon 66
  • polyacrylic fibers such as polyacrylic and modal acrylic
  • polyolefin fibers such as polyethylene and polypropylene.
  • the amount of the treatment agent to be attached to the synthetic fiber is not particularly limited, but it is preferable to attach the treatment agent to the synthetic fiber at a ratio of 0.1 to 3% by mass (not containing water). With such a configuration, the effect of the present invention can be further improved.
  • the method of adhering the treatment agent is not particularly limited, and for example, a known method such as a roller refueling method, a guide refueling method using a measuring pump, a dip refueling method, or a spray refueling method can be adopted.
  • the aqueous liquid of the above embodiment contains a predetermined ester compound and a surfactant as a smoothing agent, and the kinematic viscosity of the treatment agent at 30 ° C. is configured to have a predetermined range. Therefore, the retention of the component in the fiber is excellent. In particular, since the components are well retained on the fiber surface, functions such as suppression of fluff and yarn breakage in post-processing can be sufficiently exhibited. In addition, it has the effect of being excellent in low temperature handling. In particular, it is excellent in low temperature handling in an environment below freezing point, and for example, it is possible to suppress coagulation of components during storage of an aqueous liquid and improve the stability of the aqueous liquid at a low temperature. In addition, after low-temperature storage, the stability during use can be improved.
  • the aqueous liquid of the present embodiment is usually used as an aqueous liquid such as a stabilizer, an antistatic agent, a binder, an ultraviolet absorber, etc. for maintaining the quality of the aqueous liquid, as long as the effect of the present invention is not impaired. Ingredients used may be further blended.
  • Test Category 1 Preparation of aqueous solution of synthetic fiber treatment agent
  • aqueous solution 50% of isotridecyloleate (A1-1) as a smoothing agent and 15% of ethylene oxide 25 mol addition (B-1) of cured castor oil as a nonionic surfactant.
  • B-1 isotridecyloleate
  • B-3 ethylene oxide 25 mol addition
  • B-3 random adduct
  • the treatment agent was 100 parts by mass
  • 11.11 parts by mass of ion-exchanged water was added and uniformly mixed to prepare the aqueous solution of Example 1 so that the water content in the aqueous solution was 10%.
  • Example 2 to 13 and Comparative Examples 1 to 4 Similar to the preparation of the aqueous liquid of Example 1, the components shown in Table 1 were used to prepare Examples 2 to 13 and Comparative Examples 1 to 4. Aqueous solution was prepared. In addition, in Table 1, the type of each component in the treatment agent is shown, and the compounding ratio (%) of each component when the component (treatment agent) other than water is 100% is shown. Further, the addition rate (parts) of water when the treatment agent is 100 parts is shown.
  • the types and contents of the smoothing agent, the types and contents of the nonionic surfactants, the types and contents of the ionic surfactants, and the types and contents of the antioxidants in the treatment agents of each example are shown in Table 1. It is as shown in the "smoothing agent” column, the “nonionic surfactant” column, the “ionic surfactant” column, and the “antioxidant” column, respectively.
  • the mass ratio of the content of the ester A1 in the smoothing agent is the mass ratio of the ester A1 in the "mass ratio: ester A1 / smoothing agent” column of Table 1, when the total content ratio of the ester A1 and the ester A2 is 100%.
  • the mass ratio of the content of is shown in the column of "mass ratio: ester A1 / (ester A1 + ester A2)" in Table 1.
  • the addition rate (part) of water is shown in the "water” column of Table 1.
  • the kinematic viscosity (mm 2 / s) of the treatment agent excluding water of the aqueous liquid of each example is shown in the column of "kinematic viscosity of the treatment agent at 30 ° C. (mm 2 / s)" in Table 1. ..
  • the operation of removing water (dehydration treatment) was performed by heat-treating the aqueous liquid at 105 ° C. for 2 hours.
  • the kinematic viscosity was determined by measuring the kinematic viscosity of the treatment agent after the dehydration treatment at 30 ° C. by the Canon Fenceke method.
  • the cooling cloud point of the aqueous liquid of each example is shown in the "cooling cloud point (° C.)" column of Table 1.
  • 10 mL of the aqueous solution of the treatment agent was collected in a test tube, cooled in a constant temperature bath at -10 ° C for 30 minutes, and then the thermometer was placed in the aqueous solution of the treatment agent and allowed to stand at room temperature of 20 ° C. It was placed and determined by measuring the temperature (° C) at which it was judged that there was no turbidity visually.
  • Test category 2 evaluation of aqueous solution
  • a predetermined amount of ion-exchanged water was further added to the aqueous liquid of each example obtained as described above, and the mixture was uniformly mixed to prepare an emulsion having a concentration of 10% of the treatment agent.
  • Chips of polyethylene terephthalate having an intrinsic viscosity of 0.64 and a titanium oxide content of 0.2% were dried by a conventional method and then spun at 295 ° C. using an extruder. After being discharged from the mouthpiece and cooled and solidified, the above emulsion was attached to the running yarn so as to be 1.0% as a treatment agent by a guide lubrication method using a measuring pump.
  • the yarn was focused by a guide, picked up by a pick-up roller heated to 90 ° C. at a speed of 1400 m / min, and then stretched 3.2 times between the pick-up roller and a stretching roller rotating at a speed of 4800 m / min.
  • a drawn yarn of 83.3 decitex (75 denier) 36 filaments was produced.
  • the retention of the component in the fiber was evaluated as fluff and yarn breakage in the post-processing.
  • the low temperature handling property of the aqueous liquid was evaluated by the following method. The results are shown in Table 1.
  • the "fluidity” shown in the following criteria means that the polybin containing the aqueous liquid is tilted sideways (90 °), and if a part of the aqueous liquid flows out of the container within 30 seconds, it is judged to be fluid.
  • the results are shown in the "Coagulability" column of Table 1.

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Abstract

The present invention addresses the problem of providing an aqueous solution of a synthetic fiber treatment agent that has excellent ingredient retention properties on fibers and that has excellent low-temperature handling properties. The present invention is an aqueous solution of a synthetic fiber treatment agent comprising a smoothing agent, a nonionic surfactant and an ionic surfactant, and is characterized by: the smoothing agent comprising a specific ester A1 and optionally a specific ester A2; the smoothing agent containing a ratio of 40-100 mass% of the ester A1; the ester A1 making up a ratio of 50-100 mass% when the total content ratio of the ester A1 and the ester A2 is 100 mass%; and the viscosity of the synthetic fiber treatment agent at 30°C being 40-150mm2/s.

Description

合成繊維用処理剤の水性液及び合成繊維の製造方法Aqueous solution of treatment agent for synthetic fibers and method for manufacturing synthetic fibers
 本発明は、繊維への成分の保持性に優れるとともに、低温ハンドリング性に優れる合成繊維用処理剤の水性液、及びかかる合成繊維用処理剤の水性液を合成繊維に付着させる工程を含む合成繊維の製造方法に関する。 The present invention comprises a step of adhering an aqueous solution of a synthetic fiber treatment agent having excellent retention of components on the fiber and excellent low temperature handleability, and an aqueous solution of the synthetic fiber treatment agent to the synthetic fiber. Regarding the manufacturing method of.
 一般に、合成繊維の紡糸工程において、摩擦を低減し、糸切れ等の繊維の損傷を低減させる観点から、合成繊維のフィラメント糸条の表面に合成繊維用処理剤を付着する処理が行われることがある。その付着処理の形態は、合成繊維用処理剤を水に希釈する場合(エマルション給油)と、合成繊維用処理剤を低粘度鉱物油等の希釈剤で希釈又は希釈せずそのままの状態で付与する場合(ストレート給油)がある。 Generally, in the synthetic fiber spinning process, a treatment for adhering a synthetic fiber treatment agent to the surface of the filament yarn of the synthetic fiber is performed from the viewpoint of reducing friction and reducing fiber damage such as yarn breakage. be. The form of the adhesion treatment is that when the treatment agent for synthetic fibers is diluted with water (emulsion refueling), the treatment agent for synthetic fibers is diluted with a diluent such as low-viscosity mineral oil or applied as it is without being diluted. There is a case (straight refueling).
 従来、特許文献1,2に開示される合成繊維用処理剤のエマルションが知られている。特許文献1は、ラウリルイソステアレート、鉱物油等の平滑剤、オレイルアルコールEO付加物等の界面活性剤を含む合成繊維用処理剤を含有するエマルションについて開示する。特許文献2は、グリセリンエステル化合物、分岐エステル化合物等を含む合成繊維用処理剤を含有するエマルションについて開示する。 Conventionally, emulsions of treatment agents for synthetic fibers disclosed in Patent Documents 1 and 2 are known. Patent Document 1 discloses an emulsion containing a treatment agent for synthetic fibers containing a lauryl isostearate, a smoothing agent such as mineral oil, and a surfactant such as an oleyl alcohol EO adduct. Patent Document 2 discloses an emulsion containing a treatment agent for synthetic fibers containing a glycerin ester compound, a branched ester compound and the like.
特開2006-70375号公報Japanese Unexamined Patent Publication No. 2006-70375 国際公開第2014/156318号International Publication No. 2014/156318
 ところが、これら従来の合成繊維用処理剤のエマルションでは、繊維への成分の保持性、及び低温でのハンドリング性が十分でなかった。 However, these conventional emulsions of synthetic fiber treatment agents do not have sufficient retention of components in fibers and handling at low temperatures.
 本発明は、こうした実情に鑑みてなされたものであり、その目的は、繊維への成分の保持性に優れるとともに、低温ハンドリング性に優れる合成繊維用処理剤の水性液を提供する処にある。また、この合成繊維用処理剤の水性液を合成繊維に付着させる工程を含む合成繊維の製造方法を提供する処にある。 The present invention has been made in view of such circumstances, and an object thereof is to provide an aqueous solution of a treatment agent for synthetic fibers, which is excellent in retention of components in fibers and excellent in low temperature handling. Further, the present invention provides a method for producing a synthetic fiber, which comprises a step of adhering an aqueous solution of the treatment agent for synthetic fiber to the synthetic fiber.
 本発明者らは、前記の課題を解決するべく研究した結果、合成繊維用処理剤の水性液において、平滑剤として所定のエステル化合物、界面活性剤を含み、合成繊維用処理剤の30℃の動粘度が所定の範囲を有することが正しく好適であることを見出した。 As a result of research to solve the above-mentioned problems, the present inventors have contained a predetermined ester compound and a surfactant as a smoothing agent in the aqueous solution of the synthetic fiber treatment agent, and the temperature of the synthetic fiber treatment agent is 30 ° C. It has been found that it is correct and suitable that the kinematic viscosity has a predetermined range.
 上記課題を解決するための合成繊維用処理剤の水性液は、平滑剤、非イオン界面活性剤、及びイオン界面活性剤を含有する合成繊維用処理剤の水性液であって、前記平滑剤が下記の化1で示されるエステルA1、及び任意選択で下記の化2で示されるエステルA2を含み、かつ前記平滑剤中に前記エステルA1を40~100質量%の割合で含有し、かつ前記エステルA1及び前記エステルA2の含有割合の合計を100質量%とすると、前記エステルA1を50~100質量%の割合で含有し、かつ前記合成繊維用処理剤の30℃の動粘度が40~150mm/sであることを特徴とする。 The aqueous solution of the synthetic fiber treatment agent for solving the above problems is an aqueous solution of the synthetic fiber treatment agent containing a smoothing agent, a nonionic surfactant, and an ionic surfactant, and the smoothing agent is used. The ester A1 shown in Chemical formula 1 below and the ester A2 shown in Chemical formula 2 below are optionally contained, and the ester A1 is contained in the smoothing agent in a proportion of 40 to 100% by mass, and the ester is said. Assuming that the total content of A1 and the ester A2 is 100% by mass, the ester A1 is contained in a proportion of 50 to 100% by mass, and the kinematic viscosity of the synthetic fiber treatment agent at 30 ° C. is 40 to 150 mm 2. It is characterized by being / s.
Figure JPOXMLDOC01-appb-C000003
Figure JPOXMLDOC01-appb-C000003
 (化1において、
 R:炭素数7~23の飽和炭化水素基、又は炭素数7~23の不飽和炭化水素基、
 R:炭素数8~24の飽和炭化水素基、又は炭素数8~24の不飽和炭化水素基。
(In Chemical formula 1
R 1 : Saturated hydrocarbon group having 7 to 23 carbon atoms or unsaturated hydrocarbon group having 7 to 23 carbon atoms,
R 2 : Saturated hydrocarbon group having 8 to 24 carbon atoms or unsaturated hydrocarbon group having 8 to 24 carbon atoms.
 但し、R、及びRの少なくとも1つが分岐鎖構造を有する。) However, at least one of R 1 and R 2 has a branched chain structure. )
Figure JPOXMLDOC01-appb-C000004
Figure JPOXMLDOC01-appb-C000004
 (化2において、
 R:炭素数7~23の飽和炭化水素基、又は炭素数7~23の不飽和炭化水素基、
 R:炭素数8~24の飽和炭化水素基、又は炭素数8~24の不飽和炭化水素基。
(In Chemical formula 2
R 3 : Saturated hydrocarbon group having 7 to 23 carbon atoms or unsaturated hydrocarbon group having 7 to 23 carbon atoms,
R 4 : Saturated hydrocarbon group having 8 to 24 carbon atoms or unsaturated hydrocarbon group having 8 to 24 carbon atoms.
 但し、R、及びRが直鎖構造を有する。)
 上記合成繊維用処理剤の水性液の冷却曇点は、10℃以下のものが好ましい。
However, R 3 and R 4 have a linear structure. )
The cooling cloud point of the aqueous liquid of the synthetic fiber treatment agent is preferably 10 ° C. or lower.
 上記合成繊維用処理剤の水性液は、さらに酸化防止剤を含有し、前記平滑剤、前記非イオン界面活性剤、前記イオン界面活性剤、及び前記酸化防止剤の含有割合の合計を100質量%とすると、前記酸化防止剤を0.01~0.5質量%で含有することが好ましい。 The aqueous solution of the synthetic fiber treatment agent further contains an antioxidant, and the total content of the smoothing agent, the nonionic surfactant, the ionic surfactant, and the antioxidant is 100% by mass. Then, it is preferable to contain the antioxidant in an amount of 0.01 to 0.5% by mass.
 上記合成繊維用処理剤の水性液は、前記化1のRの炭素数が7~17及びRの炭素数が8~18であり、かつ前記化2のRの炭素数が7~17及びRの炭素数が8~18であることが好ましい。 The aqueous solution of the synthetic fiber treatment agent has 7 to 17 carbon atoms in R 1 and 8 to 18 carbon atoms in R 2 and 7 to 7 carbon atoms in R 3 of the chemical compound 2. the number of carbon atoms of 17, and R 4 is preferably a 8-18.
 上記課題を解決するための合成繊維の製造方法は、前記合成繊維用処理剤の水性液を合成繊維に付着させる工程を含むことを特徴とする。 A method for producing a synthetic fiber for solving the above-mentioned problems is characterized by including a step of adhering an aqueous liquid of the treatment agent for synthetic fibers to the synthetic fiber.
 本発明の合成繊維用処理剤の水性液は、繊維への成分の保持性に優れるとともに、低温ハンドリング性に優れる。 The aqueous solution of the synthetic fiber treatment agent of the present invention is excellent in the retention of components in the fiber and also in the low temperature handling property.
 (第1実施形態)
 先ず、本発明に係る合成繊維用処理剤の水性液(以下、水性液ともいう)を具体化した第1実施形態について説明する。本実施形態の水性液は、平滑剤、非イオン界面活性剤、及びイオン界面活性剤を含有する合成繊維用処理剤(以下、処理剤という)と水とを含んで構成される。処理剤は、酸化防止剤をさらに含有してもよい。
(First Embodiment)
First, the first embodiment which embodies the aqueous solution (hereinafter, also referred to as an aqueous solution) of the synthetic fiber treatment agent according to the present invention will be described. The aqueous liquid of the present embodiment is composed of a smoothing agent, a nonionic surfactant, a synthetic fiber treatment agent containing an ionic surfactant (hereinafter referred to as a treatment agent), and water. The treatment agent may further contain an antioxidant.
 本実施形態に供される平滑剤は、下記の化3で示されるエステルA1を含む。 The smoothing agent used in this embodiment contains the ester A1 shown in Chemical formula 3 below.
Figure JPOXMLDOC01-appb-C000005
Figure JPOXMLDOC01-appb-C000005
 (化3において、
 R:炭素数7~23の飽和炭化水素基、又は炭素数7~23の不飽和炭化水素基、
 R:炭素数8~24の飽和炭化水素基、又は炭素数8~24の不飽和炭化水素基。
(In Chemical Substance 3
R 1 : Saturated hydrocarbon group having 7 to 23 carbon atoms or unsaturated hydrocarbon group having 7 to 23 carbon atoms,
R 2 : Saturated hydrocarbon group having 8 to 24 carbon atoms or unsaturated hydrocarbon group having 8 to 24 carbon atoms.
 但し、R、及びRの少なくとも1つが分岐鎖構造を有する。)
 これらのエステルA1は、1種を単独で使用してもよく、2種以上を組み合わせて使用してもよい。これらの中でも化3のRの炭素数が7~17及びRの炭素数が8~18である化合物が好ましい。かかる範囲に規定することにより、特に処理剤の冷却曇点を下げ、水性液の低温ハンドリング性をより向上できる。
However, at least one of R 1 and R 2 has a branched chain structure. )
One of these esters A1 may be used alone, or two or more thereof may be used in combination. Among these, compounds having 7 to 17 carbon atoms in R 1 of Chemical formula 3 and 8 to 18 carbon atoms in R 2 are preferable. By defining it in such a range, it is possible to lower the cooling cloud point of the treating agent in particular and further improve the low temperature handling property of the aqueous liquid.
 Rを構成する直鎖の飽和炭化水素基の具体例としては、例えばヘプチル基、オクチル基、ノニル基、デシル基、ウンデシル基、ドデシル基、トリデシル基、テトラデシル基、ペンタデシル基、ヘキサデシル基、ヘプタデシル基、オクタデシル基、イコシル基、ドコシル基、トリコシル基等が挙げられる。 Specific examples of the linear saturated hydrocarbon group constituting R 1 include heptyl group, octyl group, nonyl group, decyl group, undecyl group, dodecyl group, tridecylic group, tetradecyl group, pentadecyl group, hexadecyl group and heptadecyl. Examples thereof include a group, an octadecyl group, an icosyl group, a docosyl group, a tridecylic group and the like.
 Rを構成する分岐鎖構造を有する飽和炭化水素基の具体例としては、例えばイソヘプチル基、イソオクチル基、イソノニル基、イソデシル基、イソウンデシル基、イソドデシル基、イソトリデシル基、イソテトラデシル基、イソペンタデシル基、イソヘキサデシル基、イソヘプタデシル基、イソオクタデシル基、イソイコシル基、イソドコシル基、イソトリコシル基等が挙げられる。 Specific examples of the saturated hydrocarbon group having a branched chain structure constituting R 1 is, for example isoheptyl group, isooctyl group, an isononyl group, an isodecyl group, isoundecyl group, isododecyl group, an isotridecyl group, isotetradecyl group, iso-pentadecyl Examples thereof include a group, an isohexadecyl group, an isoheptadecyl group, an isooctadecyl group, an isoicosyl group, an isodocosyl group, an isotricosyl group and the like.
 Rを構成する不飽和炭化水素基は、不飽和炭素結合として二重結合を1つ有するアルケニル基であっても、二重結合を2つ以上有するアルカジエニル基、アルカトリエニル基等であってもよい。また、不飽和炭素結合として三重結合を1つ有するアルキニル基であっても、三重結合を2つ以上有するアルカジイニル基等であってもよい。炭化水素基中に二重結合を1つ有する直鎖の不飽和炭化水素基の具体例としては、例えばヘプテニル基、オクテニル基、ノネニル基、デセニル基、ウンデセニル基、ドデセニル基、トリデセニル基、テトラデセニル基、ペンタデセニル基、ヘキサデセニル基、ヘプタデセニル基、オクタデセニル基、イコセニル基、ドコセニル基、トリコセニル基等が挙げられる。 The unsaturated hydrocarbon group constituting R 1 is an alkenyl group having one double bond as an unsaturated carbon bond, an alkazienyl group having two or more double bonds, an alkatienyl group, or the like. May be good. Further, it may be an alkynyl group having one triple bond as an unsaturated carbon bond, an alkadynyl group having two or more triple bonds, or the like. Specific examples of the linear unsaturated hydrocarbon group having one double bond in the hydrocarbon group include, for example, a heptenyl group, an octenyl group, a nonenyl group, a decenyl group, an undecenyl group, a dodecenyl group, a tridecenyl group, and a tetradecenyl group. , Pentadecenyl group, hexadecenyl group, heptadecenyl group, octadecenyl group, icosenyl group, docosenyl group, trichosenyl group and the like.
 Rを構成する炭化水素基中に二重結合を1つ有する分岐鎖構造を有する不飽和炭化水素基の具体例としては、例えばイソヘプテニル基、イソオクテニル基、イソノネニル基、イソデセニル基、イソウンデセニル基、イソドデセニル基、イソトリデセニル基、イソテトラデセニル基、イソペンタデセニル基、イソヘキサデセニル基、イソヘプタデセニル基、イソオクタデセニル基、イソイコセニル基、イソドコセニル基、イソトリコセニル基等が挙げられる。 Specific examples of the unsaturated hydrocarbon group in the hydrocarbon group constituting R 1 has a branched chain structure having one double bond, for example isoheptenyl group, isooctenyl group, Isononeniru group, Isodeseniru group, Isoundeseniru group, isododecenyl Group, isotridecenyl group, isotetradecenyl group, isopentadecenyl group, isohexadecenyl group, isoheptadecenyl group, isooctadecenyl group, isoicosenyl group, isodococenyl group, isotricosenyl group, etc. Can be mentioned.
 Rを構成する直鎖の飽和炭化水素基の具体例としては、例えばオクチル基、ノニル基、デシル基、ウンデシル基、ドデシル基、トリデシル基、テトラデシル基、ペンタデシル基、ヘキサデシル基、ヘプタデシル基、オクタデシル基、イコシル基、ドコシル基、トリコシル基、テトラコシル基等が挙げられる。 Specific examples of the linear saturated hydrocarbon group constituting R 2 include an octyl group, a nonyl group, a decyl group, an undecyl group, a dodecyl group, a tridecylic group, a tetradecyl group, a pentadecyl group, a hexadecyl group, a heptadecyl group and an octadecyl group. Examples thereof include a group, an icosyl group, a docosyl group, a tridecylic group, a tetracosyl group and the like.
 Rを構成する分岐鎖構造を有する飽和炭化水素基の具体例としては、例えばイソオクチル基、イソノニル基、イソデシル基、イソウンデシル基、イソドデシル基、イソトリデシル基、イソテトラデシル基、イソペンタデシル基、イソヘキサデシル基、イソヘプタデシル基、イソオクタデシル基、イソイコシル基、イソドコシル基、イソトリコシル基、イソテトラコシル基等が挙げられる。 Specific examples of the saturated hydrocarbon group having a branched chain structure constituting R 2 include an isooctyl group, an isononyl group, an isodecyl group, an isoundesyl group, an isododecyl group, an isotridecyl group, an isotetradecyl group, an isopentadecyl group and an iso. Examples thereof include a hexadecyl group, an isoheptadecyl group, an isooctadecyl group, an isoicosyl group, an isodocosyl group, an isotricosyl group and an isotetracosyl group.
 Rを構成する不飽和炭化水素基は、不飽和炭素結合として二重結合を1つ有するアルケニル基であっても、二重結合を2つ以上有するアルカジエニル基、アルカトリエニル基等であってもよい。また、不飽和炭素結合として三重結合を1つ有するアルキニル基であっても、三重結合を2つ以上有するアルカジイニル基等であってもよい。炭化水素基中に二重結合を1つ有する直鎖の不飽和炭化水素基の具体例としては、例えばオクテニル基、ノネニル基、デセニル基、ウンデセニル基、ドデセニル基、トリデセニル基、テトラデセニル基、ペンタデセニル基、ヘキサデセニル基、ヘプタデセニル基、オクタデセニル基、イコセニル基、ドコセニル基、トリコセニル基、テトラコセニル基等が挙げられる。 The unsaturated hydrocarbon group constituting R 2 is an alkenyl group having one double bond as an unsaturated carbon bond, an alkazienyl group having two or more double bonds, an alkatienyl group, or the like. May be good. Further, it may be an alkynyl group having one triple bond as an unsaturated carbon bond, an alkadynyl group having two or more triple bonds, or the like. Specific examples of the linear unsaturated hydrocarbon group having one double bond in the hydrocarbon group include, for example, an octenyl group, a nonenyl group, a decenyl group, an undecenyl group, a dodecenyl group, a tridecenyl group, a tetradecenyl group, and a pentadecenyl group. , Hexadecenyl group, heptadecenyl group, octadecenyl group, icosenyl group, docosenyl group, tricosenyl group, tetracosenyl group and the like.
 Rを構成する炭化水素基中に二重結合を1つ有する分岐鎖構造を有する不飽和炭化水素基の具体例としては、例えばイソオクテニル基、イソノネニル基、イソデセニル基、イソウンデセニル基、イソドデセニル基、イソトリデセニル基、イソテトラデセニル基、イソペンタデセニル基、イソヘキサデセニル基、イソヘプタデセニル基、イソオクタデセニル基、イソイコセニル基、イソドコセニル基、イソトリコセニル基、イソテトラコセニル基等が挙げられる。 Specific examples of the unsaturated hydrocarbon group in the hydrocarbon group constituting R 2 has a branched chain structure having one double bond, for example isooctenyl group, Isononeniru group, Isodeseniru group, Isoundeseniru group, isododecenyl group, Isotorideseniru Group, Isotetradecenyl group, Isopentadecenyl group, Isohexadecenyl group, Isoheptadecenyl group, Isooctadecenyl group, Isoicosenyl group, Isodococenyl group, Isotricosenyl group, Isotetracosenyl group The group etc. can be mentioned.
 エステルA1の具体例としては、例えばイソトリデシルオレアート、ラウリルイソステアラート、イソオクチルオクチラート、オクチルイソオクチラート、イソトリデシルイソステアラート、オレイルイソステアラート、イコシルイソステアラート、イソテトラコシルオレアート等が挙げられる。 Specific examples of the ester A1 include isotridecyl oleate, lauryl isosteleart, isooctyl octylate, octyl isooctylate, isotridecyl isosteleert, oleyl isosteert, icosyl isosteleert, and isotetraco. Examples include silole art.
 本実施形態に供される平滑剤は、任意選択で下記の化4で示されるエステルA2を含む。 The smoothing agent used in this embodiment optionally contains the ester A2 shown in Chemical formula 4 below.
Figure JPOXMLDOC01-appb-C000006
Figure JPOXMLDOC01-appb-C000006
 (化4において、
 R:炭素数7~23の飽和炭化水素基、又は炭素数7~23の不飽和炭化水素基、
 R:炭素数8~24の飽和炭化水素基、又は炭素数8~24の不飽和炭化水素基。
(In Chemical formula 4
R 3 : Saturated hydrocarbon group having 7 to 23 carbon atoms or unsaturated hydrocarbon group having 7 to 23 carbon atoms,
R 4 : Saturated hydrocarbon group having 8 to 24 carbon atoms or unsaturated hydrocarbon group having 8 to 24 carbon atoms.
 但し、R、及びRが直鎖構造を有する。)
 これらのエステルA2は、1種を単独で使用してもよく、2種以上を組み合わせて使用してもよい。これらの中でも化4のRの炭素数が7~17及びRの炭素数が8~18であることが好ましい。かかる範囲に規定することにより、特に処理剤の冷却曇点を下げ、水性液の低温ハンドリング性をより向上できる。
However, R 3 and R 4 have a linear structure. )
These esters A2 may be used alone or in combination of two or more. Among these, it is preferable that R 3 of Chemical formula 4 has 7 to 17 carbon atoms and R 4 has 8 to 18 carbon atoms. By defining it in such a range, it is possible to lower the cooling cloud point of the treating agent in particular and further improve the low temperature handling property of the aqueous liquid.
 R又はRを構成する飽和炭化水素基又は不飽和炭化水素基の具体例としては、化3のR又はRを構成する飽和炭化水素基又は不飽和炭化水素基として例示したもののうち、直鎖状のものが挙げられる。 Specific examples of the saturated hydrocarbon group or unsaturated hydrocarbon group constituting R 3 or R 4 are those exemplified as the saturated hydrocarbon group or unsaturated hydrocarbon group constituting R 1 or R 2 of Chemical formula 3. , Linear ones can be mentioned.
 エステルA2の具体例としては、例えばオレイルオクチラート、ラウリルオレアート、ステアリルエルカート、ラウリルエルカート等が挙げられる。 Specific examples of ester A2 include oleyl octylate, lauryl oleart, stearyl elkhart, lauryl elkhart and the like.
 水性液中において、エステルA1及びエステルA2の含有割合の合計を100質量%とすると、水性液は、エステルA1を50~100質量%の割合で含有する。かかる範囲に規定することにより、本発明の効果を向上できる。また、エステルA1及びエステルA2の含有割合の合計を100質量%とすると、水性液は、エステルA1を60~100質量%の割合で含有することが好ましい。かかる範囲に規定することにより、特に処理剤の冷却曇点を下げ、低温ハンドリング性をより向上できる。 Assuming that the total content of the ester A1 and the ester A2 in the aqueous solution is 100% by mass, the aqueous solution contains the ester A1 in a ratio of 50 to 100% by mass. By defining in such a range, the effect of the present invention can be improved. Further, assuming that the total content of the ester A1 and the ester A2 is 100% by mass, the aqueous solution preferably contains the ester A1 in a proportion of 60 to 100% by mass. By defining it in such a range, it is possible to lower the cooling cloud point of the treating agent in particular and further improve the low temperature handling property.
 本実施形態に供される平滑剤として、上記以外の平滑剤を併用してもよい。上記以外の平滑剤としては、公知のものを適宜採用できる。平滑剤の具体例としては、例えば(1)ブチルステアラート、イソブチルラウラート、イソヘキサコシルステアラート等の、脂肪族モノアルコールと脂肪族モノカルボン酸とのエステル化合物、脂肪族モノアルコールに炭素数2~4のアルキレンオキサイドを付加した(ポリ)オキシアルキレン付加物と脂肪族モノカルボン酸とのエステル化合物、(2)1,6-ヘキサンジオールジデカノアート、トリメチロールプロパンモノオレアートモノラウラート、ソルビタントリオレアート、ソルビタンモノオレアート、ソルビタンモノステアラート、グリセリンモノラウラート等の、脂肪族多価アルコールと脂肪族モノカルボン酸とのエステル化合物、(3)ジラウリルアジパート、ジオレイルアゼラート、ジイソセチルチオジプロピオナート、ビスポリオキシエチレンラウリルエーテルアジパート等の、脂肪族モノアルコールと脂肪族多価カルボン酸とのエステル化合物、脂肪族モノアルコールに炭素数2~4のアルキレンオキサイドを付加した(ポリ)オキシアルキレン付加物と脂肪族多価カルボン酸とのエステル化合物、(4)ベンジルオレアート、ベンジルラウラート及びポリオキシプロピレンベンジルステアラート等の、芳香族モノアルコールと脂肪族モノカルボン酸とのエステル化合物、芳香族モノアルコールに炭素数2~4のアルキレンオキサイドを付加した(ポリ)オキシアルキレン付加物と脂肪族モノカルボン酸とのエステル化合物、(5)ビスフェノールAジラウラート、ポリオキシエチレンビスフェノールAジラウラート等の、芳香族多価アルコールと脂肪族モノカルボン酸とのエステル化合物、芳香族多価アルコールに炭素数2~4のアルキレンオキサイドを付加した(ポリ)オキシアルキレン付加物と脂肪族モノカルボン酸とのエステル化合物、(6)ビス2-エチルヘキシルフタラート、ジイソステアリルイソフタラート、トリオクチルトリメリタート等の、脂肪族モノアルコールと芳香族多価カルボン酸とのエステル化合物、脂肪族モノアルコールに炭素数2~4のアルキレンオキサイドを付加した(ポリ)オキシアルキレン付加物と芳香族多価カルボン酸とのエステル化合物、(7)ヤシ油、ナタネ油、ヒマワリ油、大豆油、ヒマシ油、ゴマ油、魚油及び牛脂等の天然油脂等、(8)鉱物油等、処理剤に採用されている公知の平滑剤挙げられる。これらの平滑剤は、1種を単独で使用してもよく、2種以上を組み合わせて使用してもよい。 As the smoothing agent used in this embodiment, a smoothing agent other than the above may be used in combination. As the smoothing agent other than the above, known ones can be appropriately adopted. Specific examples of the smoothing agent include (1) an ester compound of an aliphatic monoalcohol and an aliphatic monocarboxylic acid such as (1) butyl stealert, isobutyl laurate, and isohexacocil stealert, and an aliphatic monoalcohol having a carbon number of carbon atoms. An ester compound of an (poly) oxyalkylene adduct to which 2 to 4 alkylene oxides have been added and an aliphatic monocarboxylic acid, (2) 1,6-hexanediol didecanoate, trimethylolpropane monooleate monolaurate, Ester compounds of aliphatic polyhydric alcohols and aliphatic monocarboxylic acids such as sorbitan trioleate, sorbitan monooleart, sorbitan monosteert, glycerin monolaurate, (3) dilauryl adipate, diorail azelate, Aliphatic monoalcohols and ester compounds of aliphatic polyvalent carboxylic acids such as diisocetylthiodipropionate and bispolyoxyethylene lauryl ether adipate, and alkylene oxides having 2 to 4 carbon atoms are added to the aliphatic monoalcohols. Aromatic monoalcohols and aliphatic monocarboxylic acids such as (4) benzyloleate, benzyllaurate and polyoxypropylene benzyl steaert, which are ester compounds of the (poly) oxyalkylene adduct and aliphatic polyvalent carboxylic acids. , And an ester compound of an aliphatic monocarboxylic acid and a (poly) oxyalkylene adduct having an alkylene oxide having 2 to 4 carbon atoms added to an aromatic monoalcohol, (5) bisphenol A dilaurate, polyoxyethylene bisphenol. An ester compound of an aromatic polyvalent alcohol and an aliphatic monocarboxylic acid such as A dilaurate, a (poly) oxyalkylene adduct to which an alkylene oxide having 2 to 4 carbon atoms is added to the aromatic polyvalent alcohol, and an aliphatic monocarboxylic compound. Aliphatic monoalcohols, ester compounds of aliphatic monoalcohols and aromatic polyvalent carboxylic acids, such as (6) bis2-ethylhexylphthalate, diisostearylisophthalate, trioctyl remeritate, and aliphatic monoalcohols with acids. Ester compound of (poly) oxyalkylene adduct added with alkylene oxide having 2 to 4 carbon atoms and aromatic polyvalent carboxylic acid, (7) palm oil, rapeseed oil, sunflower oil, soybean oil, sunflower oil, sesame oil , Natural fats and oils such as fish oil and beef fat, (8) mineral oil and the like, and known smoothing agents used as treatment agents. These smoothing agents may be used alone or in combination of two or more.
 平滑剤は、エステルA1を40~100質量%の割合で含有する。かかる範囲に規定することにより、本発明の効果を向上できる。また、平滑剤は、エステルA1を60~100質量%の割合で含有することが好ましい。かかる範囲に規定することにより、特に処理剤の冷却曇点を下げ、低温ハンドリング性及び後加工における毛羽抑制効果をより向上できる。 The smoothing agent contains ester A1 in a proportion of 40 to 100% by mass. By defining in such a range, the effect of the present invention can be improved. Further, the smoothing agent preferably contains ester A1 in a proportion of 60 to 100% by mass. By defining it in such a range, it is possible to lower the cooling cloud point of the treating agent in particular, and further improve the low temperature handling property and the fluff suppressing effect in post-processing.
 処理剤中の平滑剤の含有量は、適宜設定されるが、好ましくは20~80質量%、より好ましくは30~70質量%、さらに好ましくは40~60質量%である。かかる範囲に規定されることにより、繊維の平滑性を向上できる。 The content of the smoothing agent in the treatment agent is appropriately set, but is preferably 20 to 80% by mass, more preferably 30 to 70% by mass, and further preferably 40 to 60% by mass. By defining in such a range, the smoothness of the fiber can be improved.
 本実施形態に供される非イオン界面活性剤としては、公知のものを適宜採用できる。非イオン界面活性剤の具体例としては、例えば(1)有機酸、有機アルコール、有機アミン及び/又は有機アミドに炭素数2~4のアルキレンオキサイドを付加した化合物、例えばポリオキシエチレンジラウリン酸エステル、ポリオキシエチレンオレイン酸エステル、ポリオキシエチレンオレイン酸ジエステル、ポリオキシエチレンオクチルエーテル、ポリオキシエチレンラウリルエーテル、ポリオキシエチレンラウリルエーテルメチルエーテル、ポリオキシエチレンポリオキシプロピレンラウリルエーテル、ポリオキシプロピレンラウリルエーテルメチルエーテル、ポリオキシエチレンオレイルエーテル、ポリオキシブチレンオレイルエーテル、ポリオキシエチレンポリオキシプロピレンノニルエーテル、ポリオキシプロピレンノニルエーテル、ポリオキシエチレンポリオキシプロピレンオクチルエーテル、2-ヘキシルヘキサノールのエチレンオキサイド付加物、ポリオキシエチレン2-エチル-1-ヘキシルエーテル、ポリオキシエチレンドデシルエーテル、ポリオキシエチレントリデシルエーテル、ポリオキシエチレンラウリルアミノエーテル、ポリオキシエチレンラウロアミドエーテル、ポリオキシエチレントリスチレン化フェニルエーテル等のエーテル型非イオン界面活性剤、(2)ポリオキシアルキレンソルビタントリオレアート、ポリオキシアルキレンヤシ油、ポリオキシアルキレンヒマシ油、ポリオキシアルキレン硬化ヒマシ油、ポリオキシアルキレン硬化ヒマシ油トリオクタノアート、ポリオキシアルキレン硬化ヒマシ油のマレイン酸エステル、ステアリン酸エステル、又はオレイン酸エステル等のポリオキシアルキレン多価アルコール脂肪酸エステル型非イオン界面活性剤、(3)ステアリン酸ジエタノールアミド、ジエタノールアミンモノラウロアミド等のアルキルアミド型非イオン界面活性剤、(4)ポリオキシエチレンジエタノールアミンモノオレイルアミド、ポリオキシエチレンラウリルアミン、ポリオキシエチレン牛脂アミン等のポリオキシアルキレン脂肪酸アミド型非イオン界面活性剤等が挙げられる。 As the nonionic surfactant used in this embodiment, known ones can be appropriately adopted. Specific examples of the nonionic surfactant include (1) a compound obtained by adding an alkylene oxide having 2 to 4 carbon atoms to an organic acid, an organic alcohol, an organic amine and / or an organic amide, for example, a polyoxyethylene dilauric acid ester. , Polyoxyethylene oleic acid ester, polyoxyethylene oleic acid diester, polyoxyethylene octyl ether, polyoxyethylene lauryl ether, polyoxyethylene lauryl ether methyl ether, polyoxyethylene polyoxypropylene lauryl ether, polyoxypropylene lauryl ether methyl Ether, polyoxyethylene oleyl ether, polyoxybutylene oleyl ether, polyoxyethylene polyoxypropylene nonyl ether, polyoxypropylene nonyl ether, polyoxyethylene polyoxypropylene octyl ether, ethylene oxide adduct of 2-hexylhexanol, polyoxy Ether type non-ether type such as ethylene 2-ethyl-1-hexyl ether, polyoxyethylene dodecyl ether, polyoxyethylene tridecyl ether, polyoxyethylene laurylamino ether, polyoxyethylene lauroamide ether, polyoxyethylene tristyrene phenyl ether, etc. Ionic surfactant, (2) Polyoxyalkylene sorbitan trioleate, polyoxyalkylene palm oil, polyoxyalkylene castor oil, polyoxyalkylene cured castor oil, polyoxyalkylene cured castor oil trioctanoate, polyoxyalkylene cured castor Polyoxyalkylene polyvalent alcohol fatty acid ester type nonionic surfactant such as maleic acid ester, stearic acid ester, or oleic acid ester of oil, (3) Alkylamide type nonionic such as stearate diethanolamide and diethanolamine monolauroamide. Examples thereof include a surface active agent, (4) a polyoxyalkylene fatty acid amide type nonionic surface active agent such as polyoxyethylene diethanolamine monooleylamide, polyoxyethylene laurylamine, and polyoxyethylene beef amine.
 処理剤中の非イオン界面活性剤の含有量は、適宜設定されるが、好ましくは5~70質量%、より好ましくは15~60質量%、さらに好ましくは25~55質量%である。かかる範囲に規定されることにより、本発明の効果及び水性液の安定性を向上できる。 The content of the nonionic surfactant in the treatment agent is appropriately set, but is preferably 5 to 70% by mass, more preferably 15 to 60% by mass, and further preferably 25 to 55% by mass. By defining in such a range, the effect of the present invention and the stability of the aqueous liquid can be improved.
 本実施形態に供されるイオン界面活性剤としては、公知のものを適宜採用できる。イオン界面活性剤の例としては、アニオン界面活性剤、カチオン界面活性剤、両性界面活性剤が挙げられる。これらの成分は、1種を単独で使用してもよく、2種以上を組み合わせて使用してもよい。 As the ionic surfactant used in this embodiment, known ones can be appropriately adopted. Examples of ionic surfactants include anionic surfactants, cationic surfactants, and amphoteric surfactants. These components may be used alone or in combination of two or more.
 本実施形態に供されるアニオン界面活性剤としては、公知のものを適宜採用できる。アニオン界面活性剤の具体例としては、例えば(1)ラウリルリン酸エステル塩、セチルリン酸エステル塩、オクチルリン酸エステル塩、オレイルリン酸エステル塩、ステアリルリン酸エステル塩等の脂肪族アルコールのリン酸エステル塩、(2)ポリオキシエチレンラウリルエーテルリン酸エステル塩、ポリオキシエチレンオレイルエーテルリン酸エステル塩、ポリオキシエチレンステアリルエーテルリン酸エステル塩等の脂肪族アルコールにエチレンオキサイド及びプロピレンオキサイドから選ばれる少なくとも一種のアルキレンオキサイドを付加したもののリン酸エステル塩、(3)ラウリルスルホン酸塩、ミリスチルスルホン酸塩、セチルスルホン酸塩、オレイルスルホン酸塩、ステアリルスルホン酸塩、テトラデカンスルホン酸塩、ドデシルベンゼンスルホン酸塩、2級アルキルスルホン酸(C13~15)塩等の脂肪族スルホン酸塩又は芳香族スルホン酸塩、(4)ラウリル硫酸エステル塩、オレイル硫酸エステル塩、ステアリル硫酸エステル塩等の脂肪族アルコールの硫酸エステル塩、(5)ポリオキシエチレンラウリルエーテル硫酸エステル塩、ポリオキシアルキレン(ポリオキシエチレン、ポリオキシプロピレン)ラウリルエーテル硫酸エステル塩、ポリオキシエチレンオレイルエーテル硫酸エステル塩等の脂肪族アルコールにエチレンオキサイド及びプロピレンオキサイドから選ばれる少なくとも一種のアルキレンオキサイドを付加したものの硫酸エステル塩、(6)ひまし油脂肪酸硫酸エステル塩、ごま油脂肪酸硫酸エステル塩、トール油脂肪酸硫酸エステル塩、大豆油脂肪酸硫酸エステル塩、なたね油脂肪酸硫酸エステル塩、パーム油脂肪酸硫酸エステル塩、豚脂脂肪酸硫酸エステル塩、牛脂脂肪酸硫酸エステル塩、鯨油脂肪酸硫酸エステル塩等の脂肪酸の硫酸エステル塩、(7)ひまし油の硫酸エステル塩、ごま油の硫酸エステル塩、トール油の硫酸エステル塩、大豆油の硫酸エステル塩、菜種油の硫酸エステル塩、パーム油の硫酸エステル塩、豚脂の硫酸エステル塩、牛脂の硫酸エステル塩、鯨油の硫酸エステル塩等の油脂の硫酸エステル塩、(8)ラウリン酸塩、オレイン酸塩、ステアリン酸塩等の脂肪酸塩、(9)ジオクチルスルホコハク酸塩等の脂肪族アルコールのスルホコハク酸エステル塩等が挙げられる。アニオン界面活性剤の対イオンとしては、例えばカリウム塩、ナトリウム塩等のアルカリ金属塩、アンモニウム塩、トリエタノールアミン等のアルカノールアミン塩等が挙げられる。 As the anionic surfactant used in the present embodiment, known ones can be appropriately adopted. Specific examples of the anionic surfactant include (1) phosphate esters of aliphatic alcohols such as (1) lauryl phosphate ester salt, cetyl phosphate ester salt, octyl phosphate ester salt, oleyl phosphate ester salt, and stearyl phosphate ester salt. Salt, (2) At least one selected from ethylene oxide and propylene oxide for aliphatic alcohols such as polyoxyethylene lauryl ether phosphate ester salt, polyoxyethylene oleyl ether phosphate ester salt, and polyoxyethylene stearyl ether phosphate ester salt. Phosphate ester salt with alkylene oxide added, (3) Lauryl sulfonate, myristyl sulfonate, cetyl sulfonate, oleyl sulfonate, stearyl sulfonate, tetradecane sulfonate, dodecylbenzene sulfonate , An aliphatic sulfonate such as a secondary alkyl sulfonic acid (C13 to 15) salt or an aromatic sulfonate, (4) Sulfate of an aliphatic alcohol such as a lauryl sulfate ester salt, an oleyl sulfate ester salt, and a stearyl sulfate ester salt. Ester salts, (5) Polyoxyethylene lauryl ether sulfate ester salts, polyoxyalkylene (polyoxyethylene, polyoxypropylene) lauryl ether sulfate ester salts, polyoxyethylene oleyl ether sulfate ester salts, and other aliphatic alcohols with ethylene oxide and Sulfate ester salt with at least one alkylene oxide added selected from propylene oxide, (6) sesame oil fatty acid sulfate ester salt, sesame oil fatty acid sulfate ester salt, tall oil fatty acid sulfate ester salt, soybean oil fatty acid sulfate ester salt, rapeseed oil fatty acid sulfate Esters, palm oil fatty acid sulfates, pig fat fatty acid sulfates, beef fat fatty acid sulfates, whale oil fatty acid sulfates and other fatty acid sulfates, (7) castor oil sulfates, sesame oil sulfates , Thor oil sulfate, soybean oil sulfate, rapeseed oil sulfate, palm oil sulfate, pork fat sulfate, beef fat sulfate, whale oil sulfate, etc. Examples thereof include sulfate ester salts, (8) fatty acid salts such as laurate, oleate and stearate, and (9) sulfosuccinic acid ester salts of aliphatic alcohols such as dioctyl sulfosuccinate. Examples of the counterion of the anionic surfactant include alkali metal salts such as potassium salt and sodium salt, and alkanolamine salts such as ammonium salt and triethanolamine.
 本実施形態に供されるカチオン界面活性剤としては、公知のものを適宜採用できる。カチオン界面活性剤の具体例としては、例えばラウリルトリメチルアンモニウムクロライド、セチルトリメチルアンモニウムクロライド、ステアリルトリメチルアンモニウムクロライド、ベヘニルトリメチルアンモニウムクロライド、ジデシルジメチルアンモニウムクロライド等が挙げられる。 As the cationic surfactant used in the present embodiment, known ones can be appropriately adopted. Specific examples of the cationic surfactant include lauryltrimethylammonium chloride, cetyltrimethylammonium chloride, stearyltrimethylammonium chloride, behenyltrimethylammonium chloride, didecyldimethylammonium chloride and the like.
 本実施形態に供される両性界面活性剤としては、公知のものを適宜採用できる。両性界面活性剤の具体例としては、例えばベタイン型両性界面活性剤等が挙げられる。 As the amphoteric surfactant used in the present embodiment, known amphoteric surfactants can be appropriately adopted. Specific examples of the amphoteric tenside include a betaine-type amphoteric tenside.
 処理剤中のイオン界面活性剤の含有量は、適宜設定されるが、好ましくは1~20質量%、より好ましくは3~16質量%、さらに好ましくは6~13質量%である。かかる範囲に規定されることにより、本発明の効果、水性液の安定性、又は帯電防止性を向上できる。 The content of the ionic surfactant in the treatment agent is appropriately set, but is preferably 1 to 20% by mass, more preferably 3 to 16% by mass, and further preferably 6 to 13% by mass. By being defined in such a range, the effect of the present invention, the stability of the aqueous liquid, or the antistatic property can be improved.
 本実施形態の水性液は、酸化防止剤を含有することが好ましい。酸化防止剤を含有することにより繊維への成分の保持性をより向上できる。本実施形態に供される酸化防止剤としては、公知のものを適宜採用できる。酸化防止剤の具体例としては、例えば(1)1,3,5-トリス(3’,5’-ジ-t-ブチル-4-ヒドロキシベンジル)イソシアヌル酸、1,3,5-トリス(4-t-ブチル-3-ヒドロキシ-2,6-ジメチルベンジル)イソシアヌル酸、1,3,5-トリメチル-2,4,6-トリス(3,5-ジ-t-ブチル-4-ヒドロキシベンジル)ベンゼン、2,2’-メチレン-ビス(4-メチル-6-t-ブチルフェノール)、1,1,3-トリス(2-メチル-4-ヒドロキシ-5-t-ブチルフェニル)ブタン、テトラキス[メチレン-3-(3’,5’-ジ-t-ブチル-4’-ヒドロキシフェニル)プロピオナート]メタン等のフェノール系酸化防止剤、(2)オクチルジフェニルホスファイト、トリスノニルフェニルホスファイト、テトラトリデシル-4,4’-ブチリデン-ビス-(2-t-ブチル-5-メチルフェノール)ジホスファイト等のホスファイト系酸化防止剤、(3)4,4’-チオビス-(6-t-ブチル-3-メチルフェノール)、ジラウリル-3,3’-チオジプロピオナート等のチオエーテル系酸化防止剤等が挙げられる。これらの酸化防止剤は、単独で使用してもよく、2種以上を組み合わせて使用してもよい。 The aqueous liquid of the present embodiment preferably contains an antioxidant. By containing an antioxidant, the retention of the component in the fiber can be further improved. As the antioxidant used in the present embodiment, known antioxidants can be appropriately adopted. Specific examples of the antioxidant include (1) 1,3,5-tris (3', 5'-di-t-butyl-4-hydroxybenzyl) isocyanuric acid and 1,3,5-tris (4). -T-butyl-3-hydroxy-2,6-dimethylbenzyl) isocyanuric acid, 1,3,5-trimethyl-2,4,6-tris (3,5-di-t-butyl-4-hydroxybenzyl) Benzene, 2,2'-methylene-bis (4-methyl-6-t-butylphenol), 1,1,3-tris (2-methyl-4-hydroxy-5-t-butylphenyl) butane, tetrakis [methylene] -3- (3', 5'-di-t-butyl-4'-hydroxyphenyl) propionate] Phenolic antioxidants such as methane, (2) Octyldiphenylphosphite, Trisnonylphenylphosphite, Tetratridecyl A phosphite-based antioxidant such as -4,4'-butylidene-bis- (2-t-butyl-5-methylphenol) diphosphite, (3) 4,4'-thiobis- (6-t-butyl-3). -Methylphenol), thioether-based antioxidants such as dilauryl-3,3'-thiodipropionate and the like can be mentioned. These antioxidants may be used alone or in combination of two or more.
 前記平滑剤、前記非イオン界面活性剤、前記イオン界面活性剤、及び前記酸化防止剤の含有割合の合計を100質量%とすると、水性液は、酸化防止剤を好ましくは0.01~0.5質量%含有する。かかる範囲に規定することにより繊維への成分の保持性をより向上できる。 Assuming that the total content of the smoothing agent, the nonionic surfactant, the ionic surfactant, and the antioxidant is 100% by mass, the aqueous solution preferably contains the antioxidant from 0.01 to 0. Contains 5% by mass. By defining in such a range, the retention of the component in the fiber can be further improved.
 前記処理剤の30℃の動粘度は、40~150mm/sに規定される。かかる範囲に規定することにより本発明の効果を向上できる。 The kinematic viscosity of the treatment agent at 30 ° C. is defined as 40 to 150 mm 2 / s. By defining in such a range, the effect of the present invention can be improved.
 水性液中の前記処理剤及び水の含有割合は、特に限定されない。水性液中の処理剤の含有割合を100質量部とすると、水性液中の水の含有割合は30質量部以下であり、好ましくは5~30質量部、より好ましくは5~20質量部である。かかる配合割合に規定することにより、水性液のハンドリング性を向上できるとともに、経時安定性を向上できる。 The content ratio of the treatment agent and water in the aqueous solution is not particularly limited. Assuming that the content ratio of the treating agent in the aqueous liquid is 100 parts by mass, the content ratio of water in the aqueous liquid is 30 parts by mass or less, preferably 5 to 30 parts by mass, and more preferably 5 to 20 parts by mass. .. By specifying such a blending ratio, the handleability of the aqueous liquid can be improved and the stability over time can be improved.
 前記水性液の冷却曇点は、10℃以下が好ましく、8℃以下がより好ましく、7℃以下がさらに好ましい。水性液の冷却曇点が10℃以下であると、本発明の効果、特に低温ハンドリング性及び後加工における毛羽抑制効果をより向上できる。なお、冷却曇点は、まず調製した水性液を常温から徐々に冷却し、成分を析出させて濁りのある不透明の溶液とした後、徐々に温度を上げ、濁りがなくなる時の温度を示す。 The cooling cloud point of the aqueous liquid is preferably 10 ° C. or lower, more preferably 8 ° C. or lower, and even more preferably 7 ° C. or lower. When the cooling cloud point of the aqueous liquid is 10 ° C. or lower, the effect of the present invention, particularly the low temperature handling property and the fluff suppressing effect in post-processing can be further improved. The cooling cloud point indicates the temperature at which the prepared aqueous solution is gradually cooled from room temperature, the components are precipitated to form an opaque solution having turbidity, and then the temperature is gradually raised to eliminate the turbidity.
 (第2実施形態)
 次に、本発明による合成繊維の製造方法を具体化した第2実施形態を説明する。本実施形態の合成繊維の製造方法では、第1実施形態の水性液又は水性液をさらに水で希釈したエマルションを例えば紡糸、延伸工程等において合成繊維に付着させる工程を経て合成繊維が製造される。合成繊維に付着させた水性液又はエマルションは、乾燥工程により水分を蒸発させてもよい。製造する合成繊維の具体例としては、特に制限はなく、例えば(1)ポリエチレンテレフタラート、ポリプロピレンテレフタラート、ポリ乳酸エステル等のポリエステル系繊維、(2)ナイロン6、ナイロン66等のポリアミド系繊維、(3)ポリアクリル、モダアクリル等のポリアクリル系繊維、(4)ポリエチレン、ポリプロピレン等のポリオレフィン系繊維等が挙げられる。
(Second Embodiment)
Next, a second embodiment embodying the method for producing a synthetic fiber according to the present invention will be described. In the method for producing a synthetic fiber of the present embodiment, the synthetic fiber is produced through a step of adhering the aqueous liquid of the first embodiment or an emulsion obtained by further diluting the aqueous liquid with water to the synthetic fiber in, for example, a spinning or drawing step. .. The aqueous liquid or emulsion attached to the synthetic fiber may evaporate the water content by a drying step. Specific examples of the synthetic fiber to be produced are not particularly limited, and for example, (1) polyester fiber such as polyethylene terephthalate, polypropylene terephthalate and polylactic acid ester, (2) polyamide fiber such as nylon 6 and nylon 66, and the like. Examples thereof include polyacrylic fibers such as polyacrylic and modal acrylic, and (4) polyolefin fibers such as polyethylene and polypropylene.
 処理剤を合成繊維に付着させる量に特に制限はないが、処理剤を合成繊維に対し0.1~3質量%(水を含まない)の割合となるよう付着させることが好ましい。かかる構成により、本発明の効果をより向上できる。また、処理剤を付着させる方法は、特に制限はなく、例えばローラー給油法、計量ポンプを用いたガイド給油法、浸漬給油法、スプレー給油法等の公知の方法を採用できる。 The amount of the treatment agent to be attached to the synthetic fiber is not particularly limited, but it is preferable to attach the treatment agent to the synthetic fiber at a ratio of 0.1 to 3% by mass (not containing water). With such a configuration, the effect of the present invention can be further improved. Further, the method of adhering the treatment agent is not particularly limited, and for example, a known method such as a roller refueling method, a guide refueling method using a measuring pump, a dip refueling method, or a spray refueling method can be adopted.
 上記実施形態の水性液、合成繊維の製造方法、及び合成繊維によれば、以下のような効果を得ることができる。 According to the aqueous solution of the above embodiment, the method for producing synthetic fiber, and the synthetic fiber, the following effects can be obtained.
 (1)上記実施形態の水性液は、平滑剤として所定のエステル化合物及び界面活性剤を含み、処理剤の30℃の動粘度が所定の範囲を有するように構成した。したがって、繊維への成分の保持性に優れる。特に成分が繊維表面に良好に保持されるため、後加工における毛羽、断糸の抑制等の機能を十分に発揮することができる。また、低温ハンドリング性に優れるという効果が生ずる。特に氷点下の環境下における低温ハンドリング性に優れ、例えば水性液の保管時における成分の凝固を抑制し、低温での水性液の安定性を向上できる。また、低温保管後、使用時における復元性も向上できる。 (1) The aqueous liquid of the above embodiment contains a predetermined ester compound and a surfactant as a smoothing agent, and the kinematic viscosity of the treatment agent at 30 ° C. is configured to have a predetermined range. Therefore, the retention of the component in the fiber is excellent. In particular, since the components are well retained on the fiber surface, functions such as suppression of fluff and yarn breakage in post-processing can be sufficiently exhibited. In addition, it has the effect of being excellent in low temperature handling. In particular, it is excellent in low temperature handling in an environment below freezing point, and for example, it is possible to suppress coagulation of components during storage of an aqueous liquid and improve the stability of the aqueous liquid at a low temperature. In addition, after low-temperature storage, the stability during use can be improved.
 (2)上記実施形態の合成繊維では、成分の保持性に優れる水性液により処理剤が繊維に付着されるため、後加工における毛羽、断糸を抑制できる。 (2) In the synthetic fiber of the above embodiment, since the treatment agent is attached to the fiber by an aqueous liquid having excellent retention of components, fluffing and yarn breakage in post-processing can be suppressed.
 なお、上記実施形態は以下のように変更してもよい。 The above embodiment may be changed as follows.
 ・本実施形態の水性液には、本発明の効果を阻害しない範囲内において、水性液の品質保持のための安定化剤や制電剤、つなぎ剤、紫外線吸収剤等の水性液に通常に用いられる成分をさらに配合してもよい。 -The aqueous liquid of the present embodiment is usually used as an aqueous liquid such as a stabilizer, an antistatic agent, a binder, an ultraviolet absorber, etc. for maintaining the quality of the aqueous liquid, as long as the effect of the present invention is not impaired. Ingredients used may be further blended.
 以下、本発明の構成及び効果をより具体的に説明するため、実施例等を挙げるが、本発明がこれらの実施例に限定されるというものではない。尚、以下の実施例及び比較例の説明において、部は質量部を、また%は質量%を意味する。 Hereinafter, examples and the like will be given in order to more specifically explain the configuration and effect of the present invention, but the present invention is not limited to these examples. In the following Examples and Comparative Examples, "parts" means "parts by mass" and "%" means "% by mass".
 試験区分1(合成繊維用処理剤の水性液の調製)
 ・水性液(実施例1)の調製
 平滑剤としてイソトリデシルオレアート(A1-1)を50%、非イオン界面活性剤として硬化ひまし油のエチレンオキサイド25モル付加物(B-1)を15%、オレイン酸のエチレンオキサイド15モル付加物(B-2)を15%、ラウリルアルコールのエチレンオキサイド8モル・プロピレンオキサイド2モルのランダム付加物(B-3)を10%、イオン界面活性剤としてポリオキシエチレン(2モル)ラウリルエーテルのリン酸エステルとカリウムとの塩を4.9%(C-1)、2級アルキルスルホン酸ナトリウム(炭素数13-15)(C-2)を4%、オレイン酸カリウム(C-3)を1%、酸化防止剤として1,1,3-トリス(2-メチル-4-ヒドロキシ-5-t-ブチルフェニル)ブタン(D-1)を0.1%を均一混合し、処理剤としての混合物を得た。
Test Category 1 (Preparation of aqueous solution of synthetic fiber treatment agent)
Preparation of aqueous solution (Example 1) 50% of isotridecyloleate (A1-1) as a smoothing agent and 15% of ethylene oxide 25 mol addition (B-1) of cured castor oil as a nonionic surfactant. , 15 mol of ethylene oxide 15 mol adduct (B-2) of oleic acid, 10% of random adduct (B-3) of 8 mol of ethylene oxide and 2 mol of propylene oxide of lauryl alcohol, poly as an ionic surfactant. Salt of oxyethylene (2 mol) lauryl ether phosphate ester and potassium 4.9% (C-1), secondary sodium alkyl sulfonate (13-15 carbon atoms) (C-2) 4%, Potassium oleate (C-3) 1%, antioxidant 1,1,3-tris (2-methyl-4-hydroxy-5-t-butylphenyl) butane (D-1) 0.1% Was uniformly mixed to obtain a mixture as a treatment agent.
 さらに、前記処理剤を100質量部としたとき11.11質量部のイオン交換水を加えて均一混合し、水性液中における水分が10%となるように実施例1の水性液を調製した。 Further, when the treatment agent was 100 parts by mass, 11.11 parts by mass of ion-exchanged water was added and uniformly mixed to prepare the aqueous solution of Example 1 so that the water content in the aqueous solution was 10%.
 ・水性液(実施例2~13及び比較例1~4)の調製
 実施例1の水性液の調製と同様に、表1に示される成分を用いて実施例2~13及び比較例1~4の水性液を調製した。なお、表1においては、処理剤中における各成分の種類を示すとともに、水以外の成分(処理剤)を100%とした場合の各成分の配合比率(%)を示す。また、処理剤を100部とした場合の水の添加率(部)を示す。
-Preparation of aqueous liquids (Examples 2 to 13 and Comparative Examples 1 to 4) Similar to the preparation of the aqueous liquid of Example 1, the components shown in Table 1 were used to prepare Examples 2 to 13 and Comparative Examples 1 to 4. Aqueous solution was prepared. In addition, in Table 1, the type of each component in the treatment agent is shown, and the compounding ratio (%) of each component when the component (treatment agent) other than water is 100% is shown. Further, the addition rate (parts) of water when the treatment agent is 100 parts is shown.
 各例の処理剤中における平滑剤の種類と含有量、非イオン界面活性剤の種類と含有量、イオン界面活性剤の種類と含有量、酸化防止剤の種類と含有量は、表1の「平滑剤」欄、「非イオン界面活性剤」欄、「イオン界面活性剤」欄、「酸化防止剤」欄にそれぞれ示すとおりである。また、平滑剤中におけるエステルA1の含有量の質量比は、表1の「質量比:エステルA1/平滑剤」欄、エステルA1及びエステルA2の含有割合の合計を100%とした場合のエステルA1の含有量の質量比は、表1の「質量比:エステルA1/(エステルA1+エステルA2)」欄に示す。水の添加率(部)は、表1の「水」欄に示す。 The types and contents of the smoothing agent, the types and contents of the nonionic surfactants, the types and contents of the ionic surfactants, and the types and contents of the antioxidants in the treatment agents of each example are shown in Table 1. It is as shown in the "smoothing agent" column, the "nonionic surfactant" column, the "ionic surfactant" column, and the "antioxidant" column, respectively. The mass ratio of the content of the ester A1 in the smoothing agent is the mass ratio of the ester A1 in the "mass ratio: ester A1 / smoothing agent" column of Table 1, when the total content ratio of the ester A1 and the ester A2 is 100%. The mass ratio of the content of is shown in the column of "mass ratio: ester A1 / (ester A1 + ester A2)" in Table 1. The addition rate (part) of water is shown in the "water" column of Table 1.
 また、各例の水性液の水を除いた処理剤の30℃における動粘度(mm/s)は、表1の「処理剤の30℃における動粘度(mm/s)」欄に示す。なお、水を除く操作(脱水処理)は、水性液を105℃で2時間熱処理することにより行った。動粘度は、脱水処理後の処理剤の30℃での動粘度をキャノンフェンスケ法により測定することにより求めた。 The kinematic viscosity (mm 2 / s) of the treatment agent excluding water of the aqueous liquid of each example is shown in the column of "kinematic viscosity of the treatment agent at 30 ° C. (mm 2 / s)" in Table 1. .. The operation of removing water (dehydration treatment) was performed by heat-treating the aqueous liquid at 105 ° C. for 2 hours. The kinematic viscosity was determined by measuring the kinematic viscosity of the treatment agent after the dehydration treatment at 30 ° C. by the Canon Fenceke method.
 また、各例の水性液の冷却曇点は、表1の「冷却曇点(℃)」欄に示す。なお、冷却曇点は、処理剤の水性液を試験管に10mL採取し、-10℃の恒温槽で30分冷却した後に、温度計を処理剤の水性液に入れ20℃の室温条件で静置し、目視にて濁りが無いと判断した温度(℃)を測定することにより求めた。 The cooling cloud point of the aqueous liquid of each example is shown in the "cooling cloud point (° C.)" column of Table 1. For the cooling cloud point, 10 mL of the aqueous solution of the treatment agent was collected in a test tube, cooled in a constant temperature bath at -10 ° C for 30 minutes, and then the thermometer was placed in the aqueous solution of the treatment agent and allowed to stand at room temperature of 20 ° C. It was placed and determined by measuring the temperature (° C) at which it was judged that there was no turbidity visually.
Figure JPOXMLDOC01-appb-T000007
Figure JPOXMLDOC01-appb-T000007
 表1において、
 A1-1:イソトリデシルオレアート
 A1-2:ラウリルイソステアラート
 A1-3:イソオクチルオクチラート
 A1-4:オクチルイソオクチラート
 A1-5:イソトリデシルイソステアラート
 A1-6:オレイルイソステアラート
 A1-7:イコシルイソステアラート
 A1-8:イソテトラコシルオレアート
 A2-1:オレイルオクチラート
 A2-2:ラウリルオレアート
 A2-3:ステアリルエルカート
 A2-4:ラウリルエルカート
 a-1:なたね油
 a-2:鉱物油(100レッドウッド秒、30℃)
 a-3:イソブチルラウラート
 a-4:イソヘキサコシルステアラート
 B-1:硬化ひまし油のエチレンオキサイド25モル付加物
 B-2:オレイン酸のエチレンオキサイド15モル付加物
 B-3:ラウリルアルコールのエチレンオキサイド8モル・プロピレンオキサイド2モルのランダム付加物
 B-4:オレイルアルコールのエチレンオキサイド20モル付加物
 B-5:2-ヘキシルヘキサノールのエチレンオキサイド3モル付加物
 B-6:ステアリン酸ジエタノールアミド
 C-1:ポリオキシエチレン(2モル:エチレンオキサイドの付加モル数を示す。)ラウリルエーテルのリン酸エステルとカリウムとの塩
 C-2:2級アルキルスルホン酸ナトリウム(炭素数13-15)
 C-3:オレイン酸カリウム
 C-4:ラウリルリン酸エステルカリウム塩
 C-5:ラウリルスルホン酸ナトリウム塩
 D-1:1,1,3-トリス(2-メチル-4-ヒドロキシ-5-t-ブチルフェニル)ブタン
 D-2:1,3,5-トリス(4-t-ブチル-3-ヒドロキシ-2,6-ジメチルベンジル)イソシアヌル酸
 を示す。
In Table 1,
A1-1: Isotridecyl oleart A1-2: Lauryl isosteleart A1-3: Isooctyl octylate A1-4: Octyl isooctilate A1-5: Isotridecyl isosteleert A1-6: Oleyl isostele Alert A1-7: Icosyl Isoste Alert A1-8: Isotetracosyl Oleart A2-1: Oleyl Octilato A2-2: Lauryl Oleart A2-3: Stearyl Elkart A2-4: Lauryl Elkart a-1 : Rapeseed oil a-2: Mineral oil (100 redwood seconds, 30 ° C)
a-3: Isobutyllaurate a-4: Isohexacosyl stealert B-1: 25 mol adduct of ethylene oxide of hardened castor oil B-2: 15 mol adduct of ethylene oxide of oleic acid B-3: Ethylene oxide of lauryl alcohol Random adduct of 8 mol of oxide and 2 mol of propylene oxide B-4: 20 mol of ethylene oxide adduct of oleyl alcohol B-5: 3 mol of ethylene oxide adduct of 2-hexylhexanol B-6: Diethanolamide stearate C- 1: Polyoxyethylene (2 mol: indicates the number of adducts of ethylene oxide) Salt of lauryl ether phosphate ester and potassium C-2: Sodium secondary alkyl sulfonate (13-15 carbon atoms)
C-3: Potassium oleate C-4: Potassium lauryl phosphate C-5: Sodium lauryl sulfonic acid D-1: 1,1,3-Tris (2-methyl-4-hydroxy-5-t- Butylphenyl) butane D-2: 1,3,5-tris (4-t-butyl-3-hydroxy-2,6-dimethylbenzyl) isocyanuric acid.
 試験区分2(水性液の評価)
 ・延伸糸の製造
 上記のように得られた各例の水性液に、さらに所定量のイオン交換水を添加し、均一混合して、処理剤の濃度10%のエマルションを調製した。固有粘度0.64、酸化チタン含有量0.2%のポリエチレンテレフタラートのチップを常法により乾燥した後、エクストルーダーを用いて295℃で紡糸した。口金から吐出して冷却固化した後、走行糸条に前記のエマルションを、計量ポンプを用いたガイド給油法にて、走行糸条に対し処理剤として1.0%となるよう付着させた。その後、ガイドで集束させて、90℃に加熱した引き取りローラーにより1400m/分の速度で引き取り、ついで引き取りローラーと4800m/分の速度で回転する延伸ローラーとの間で3.2倍に延伸し、83.3デシテックス(75デニール)36フィラメントの延伸糸を製造した。製造した延伸糸を用いて、繊維への成分の保持性を後加工での毛羽・断糸として評価した。また、水性液の低温ハンドリング性を次の方法で評価した。結果を表1に示す。
Test category 2 (evaluation of aqueous solution)
-Production of drawn yarn A predetermined amount of ion-exchanged water was further added to the aqueous liquid of each example obtained as described above, and the mixture was uniformly mixed to prepare an emulsion having a concentration of 10% of the treatment agent. Chips of polyethylene terephthalate having an intrinsic viscosity of 0.64 and a titanium oxide content of 0.2% were dried by a conventional method and then spun at 295 ° C. using an extruder. After being discharged from the mouthpiece and cooled and solidified, the above emulsion was attached to the running yarn so as to be 1.0% as a treatment agent by a guide lubrication method using a measuring pump. Then, the yarn was focused by a guide, picked up by a pick-up roller heated to 90 ° C. at a speed of 1400 m / min, and then stretched 3.2 times between the pick-up roller and a stretching roller rotating at a speed of 4800 m / min. A drawn yarn of 83.3 decitex (75 denier) 36 filaments was produced. Using the produced drawn yarn, the retention of the component in the fiber was evaluated as fluff and yarn breakage in the post-processing. In addition, the low temperature handling property of the aqueous liquid was evaluated by the following method. The results are shown in Table 1.
 ・後加工毛羽の評価
 上記方法で得た延伸糸のパッケージを、整経機を模したミニチュア整経機に10本仕立て、25℃×65%RHの雰囲気下で糸速度600m/分で24時間巻き取った。
・ Evaluation of post-processed fluff 10 pieces of the drawn yarn package obtained by the above method are made into a miniature warp machine imitating a warp machine, and the yarn speed is 600 m / min for 24 hours in an atmosphere of 25 ° C × 65% RH. I rolled it up.
 ・毛羽の評価
 このときの巻き取り直前に、毛羽計数装置(東レエンジニアリング社製の商品名DT-105)にて毛羽数を4時間測定し、以下の評価基準で後加工毛羽を評価した。結果を表1の「後工程毛羽」欄に示す。
-Evaluation of fluff Immediately before winding at this time, the number of fluff was measured for 4 hours with a fluff counting device (trade name DT-105 manufactured by Toray Engineering Co., Ltd.), and post-processed fluff was evaluated according to the following evaluation criteria. The results are shown in the "Post-process fluff" column of Table 1.
 ◎◎(優れる):4時間での毛羽の数が0~2個の場合
 ◎(良好):4時間での毛羽の数が3~5個の場合
 ○(可):4時間での毛羽の数が6~9個の場合
 ×(不良):4時間での毛羽の数が10個以上の場合
 ・後加工断糸の評価
 毛羽の評価と同様の方法にて24時間巻き取った。24時間の巻き取り時に断糸した回数を測定し、以下の評価基準で後加工断糸を評価した。結果を表1の「後工程断糸」欄に示す。
◎ ◎ (excellent): When the number of fluff in 4 hours is 0 to 2 ◎ (Good): When the number of fluff in 4 hours is 3 to 5 ○ (Yes): When the number of fluff in 4 hours When the number is 6 to 9 × (defective): When the number of fluffs in 4 hours is 10 or more ・ Evaluation of post-processing yarn breakage Winding was performed for 24 hours by the same method as the evaluation of fluff. The number of yarn breaks during winding for 24 hours was measured, and post-processed yarn breaks were evaluated according to the following evaluation criteria. The results are shown in the "Post-process thread break" column of Table 1.
 ・断糸の評価
 ◎◎(優れる):24時間での断糸回数が0回の場合
 ◎(良好):24時間での断糸回数が1~2回の場合
 ○(可):24時間での断糸回数が3~4回の場合
 ×(不良):24時間での断糸回数が5回以上の場合
 ・低温ハンドリング性
 水性液の低温ハンドリング性を凝固性及び復元性として評価した。凝固性及び復元性は、以下の方法で求めた。
・ Evaluation of thread breakage ◎ ◎ (excellent): When the number of thread breaks in 24 hours is 0 ◎ (Good): When the number of thread breaks in 24 hours is 1 to 2 ○ (possible): In 24 hours When the number of thread breaks is 3 to 4 times × (defective): When the number of thread breaks in 24 hours is 5 times or more ・ Low temperature handling property The low temperature handling property of the aqueous solution was evaluated as coagulation property and restorability. Coagulability and stability were determined by the following methods.
 ・凝固性の評価
 30℃まで加温し、撹拌均一化させた水性液を容量100mLのふた付きポリビン(内径45mm)に60mL入れ、容器を密閉した。設定温度を-5℃にしたインキュベーターに水性液を入れたポリビンを3日静置した。静置後、水性液の外観を目視判定し、以下の基準により凝固性を評価した。下記基準に示される「流動性」とは水性液を入れたポリビンを横(90°)に傾け、30秒以内に水性液の一部が容器外へ流れ出た場合、流動性ありと判断した。結果を表1の「凝固性」欄に示す。
-Evaluation of coagulability 60 mL of an aqueous solution heated to 30 ° C. and stirred and homogenized was placed in a polybin with a lid (inner diameter 45 mm) having a capacity of 100 mL, and the container was sealed. A polybin containing an aqueous solution was allowed to stand in an incubator at a set temperature of −5 ° C. for 3 days. After standing, the appearance of the aqueous solution was visually judged, and the coagulation property was evaluated according to the following criteria. The "fluidity" shown in the following criteria means that the polybin containing the aqueous liquid is tilted sideways (90 °), and if a part of the aqueous liquid flows out of the container within 30 seconds, it is judged to be fluid. The results are shown in the "Coagulability" column of Table 1.
 ◎◎(優れる):外観に曇り、濁りはなく、流動性がある場合
 ◎(良好):外観に曇り、濁りがあり、一部固化している場合
 ○(可):外観に曇り、濁りがあり、大半が固化している場合
 ×(不良):完全に凝固しており、流動性がない場合
 ・復元性の評価
 凝固性評価で用いた水性液の入ったポリビンを-5℃のインキュベーターから取り出し、設定温度を10℃にしたインキュベーターに3時間静置した。その後の水性液の外観を目視判定し、以下の基準により復元性を評価した。なお、下記基準に示される「流動性」の判断基準は、凝固性欄に示される基準と同様である。結果を表1の「復元性」欄に示す。
◎ ◎ (excellent): If the appearance is not cloudy or turbid and has fluidity ◎ (Good): If the appearance is cloudy or turbid and partially solidified ○ (possible): The appearance is cloudy or turbid Yes, most of them are solidified × (Defective): Completely coagulated and have no fluidity ・ Evaluation of resilience Polybin containing the aqueous solution used in the coagulation evaluation was taken from the incubator at -5 ° C. It was taken out and allowed to stand in an incubator at a set temperature of 10 ° C. for 3 hours. After that, the appearance of the aqueous solution was visually judged, and the stability was evaluated according to the following criteria. The criteria for determining "fluidity" shown in the following criteria are the same as those shown in the coagulation column. The results are shown in the "Stability" column of Table 1.
 ◎◎(優れる):外観に曇り、濁りはなく、流動性がある場合
 ◎(良好):外観に曇り、濁りがあり、一部固化している場合
 ○(可):外観に曇り、濁りがあり、大半が固化している場合
 ×(不良):完全に凝固しており、流動性がない場合
 表1の結果からも明らかなように、各実施例の水性液は、後加工での毛羽・断糸、低温ハンドリング性の評価がいずれも可以上の評価であった。本発明によれば、繊維への成分の保持性に優れるとともに、低温ハンドリング性に優れる水性液を得ることができる。
◎ ◎ (excellent): If the appearance is not cloudy or turbid and has fluidity ◎ (Good): If the appearance is cloudy or turbid and partially solidified ○ (possible): The appearance is cloudy or turbid Yes, most of them are solidified × (Defective): Completely solidified and have no fluidity As is clear from the results in Table 1, the aqueous solution of each example is fluffed in post-processing. -Evaluation of thread breakage and low temperature handleability was the above evaluation. According to the present invention, it is possible to obtain an aqueous liquid having excellent retention of components on fibers and excellent low temperature handling.

Claims (5)

  1.  平滑剤、非イオン界面活性剤、及びイオン界面活性剤を含有する合成繊維用処理剤の水性液であって、前記平滑剤が下記の化1で示されるエステルA1、及び任意選択で下記の化2で示されるエステルA2を含み、かつ前記平滑剤中に前記エステルA1を40~100質量%の割合で含有し、かつ前記エステルA1及び前記エステルA2の含有割合の合計を100質量%とすると、前記エステルA1を50~100質量%の割合で含有し、かつ前記合成繊維用処理剤の30℃の動粘度が40~150mm/sであり、前記合成繊維用処理剤の含有割合を100質量部とすると水の含有割合が30質量部以下であることを特徴とする合成繊維用処理剤の水性液。
    Figure JPOXMLDOC01-appb-C000001

     (化1において、
     R:炭素数7~23の飽和炭化水素基、又は炭素数7~23の不飽和炭化水素基。
     R:炭素数8~24の飽和炭化水素基、又は炭素数8~24の不飽和炭化水素基。
     但し、R、及びRの少なくとも1つが分岐鎖構造を有する。)
    Figure JPOXMLDOC01-appb-C000002

     (化2において、
     R:炭素数7~23の飽和炭化水素基、又は炭素数7~23の不飽和炭化水素基。
     R:炭素数8~24の飽和炭化水素基、又は炭素数8~24の不飽和炭化水素基。
     但し、R、及びRが直鎖構造を有する。)
    An aqueous solution of a treatment agent for synthetic fibers containing a smoothing agent, a non-ionic surfactant, and an ionic surfactant, wherein the smoothing agent is the ester A1 shown in the following Chemical formula 1 and optionally the following chemical formula. Assuming that the ester A2 represented by 2 is contained, the ester A1 is contained in the smoothing agent at a ratio of 40 to 100% by mass, and the total content of the ester A1 and the ester A2 is 100% by mass. The ester A1 is contained in a ratio of 50 to 100% by mass, and the kinematic viscosity of the synthetic fiber treatment agent at 30 ° C. is 40 to 150 mm 2 / s, and the content ratio of the synthetic fiber treatment agent is 100% by mass. An aqueous solution of a treatment agent for synthetic fibers, characterized in that the content ratio of water is 30 parts by mass or less.
    Figure JPOXMLDOC01-appb-C000001

    (In Chemical formula 1
    R 1 : Saturated hydrocarbon group having 7 to 23 carbon atoms or unsaturated hydrocarbon group having 7 to 23 carbon atoms.
    R 2 : Saturated hydrocarbon group having 8 to 24 carbon atoms or unsaturated hydrocarbon group having 8 to 24 carbon atoms.
    However, at least one of R 1 and R 2 has a branched chain structure. )
    Figure JPOXMLDOC01-appb-C000002

    (In Chemical formula 2
    R 3 : Saturated hydrocarbon group having 7 to 23 carbon atoms or unsaturated hydrocarbon group having 7 to 23 carbon atoms.
    R 4 : Saturated hydrocarbon group having 8 to 24 carbon atoms or unsaturated hydrocarbon group having 8 to 24 carbon atoms.
    However, R 3 and R 4 have a linear structure. )
  2.  前記合成繊維用処理剤の水性液の冷却曇点が、10℃以下のものである請求項1に記載の合成繊維用処理剤の水性液。 The aqueous solution of the synthetic fiber treatment agent according to claim 1, wherein the cooling cloud point of the aqueous solution of the synthetic fiber treatment agent is 10 ° C. or lower.
  3.  さらに酸化防止剤を含有する合成繊維用処理剤の水性液であって、前記平滑剤、前記非イオン界面活性剤、前記イオン界面活性剤、及び前記酸化防止剤の含有割合の合計を100質量%とすると、前記酸化防止剤を0.01~0.5質量%で含有する請求項1又は2に記載の合成繊維用処理剤の水性液。 Further, it is an aqueous solution of a treatment agent for synthetic fibers containing an antioxidant, and the total content of the smoothing agent, the nonionic surfactant, the ionic surfactant, and the antioxidant is 100% by mass. Then, the aqueous solution of the treatment agent for synthetic fibers according to claim 1 or 2, which contains the antioxidant in an amount of 0.01 to 0.5% by mass.
  4.  前記化1のRの炭素数が7~17及びRの炭素数が8~18であり、かつ前記化2のRの炭素数が7~17及びRの炭素数が8~18である請求項1~3のいずれか一項に記載の合成繊維用処理剤の水性液。 The carbon number of R 1 of the chemical 1 is 7 to 17 and the carbon number of R 2 is 8 to 18, and the carbon number of R 3 of the chemical 2 is 7 to 17 and the carbon number of R 4 is 8 to 18. The aqueous solution of the treatment agent for synthetic fibers according to any one of claims 1 to 3.
  5.  請求項1~4のいずれか一項に記載の合成繊維用処理剤の水性液を合成繊維に付着させる工程を含むことを特徴とする合成繊維の製造方法。 A method for producing a synthetic fiber, which comprises a step of adhering an aqueous solution of the treatment agent for synthetic fiber according to any one of claims 1 to 4 to the synthetic fiber.
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