JP5967852B1 - Synthetic fiber treatment agent aqueous liquid, synthetic fiber treatment agent emulsion, and synthetic fiber treatment method - Google Patents

Abstract

The aqueous solution of a synthetic fiber treating agent itself maintains long-term stability even in winter, and the amount of tar dirt generated on a godet roller is small in the spinning and drawing process of synthetic fibers using such an aqueous solution. An aqueous solution of a treating agent for synthetic fibers, which has good detergency for tar dirt, and can sufficiently suppress the problems of generation of spinning fluff, generation of dyeing spots, and generation of static electricity in post-processing steps, and such aqueous solution An emulsion of a treating agent for synthetic fibers prepared by further diluting with water, a method for treating synthetic fibers to which such an emulsion is attached, and a synthetic fiber obtained by such a treating method are provided. As an aqueous solution of a treating agent for synthetic fibers, a specific smoothing agent is 20 to 85% by mass, a specific nonionic surfactant is 5 to 70% by mass, and a specific antistatic agent is 1 to 20% by mass ( The synthetic fiber treatment agent and water are contained in a proportion of 100% by mass in total, containing water in a proportion of 3 to 20 parts by mass with respect to 100 parts by mass of the synthetic fiber treatment agent, and by ICP emission spectrometry. The total concentration of polyvalent metal ions required was 1 mg / kg or less. [Selection figure] None

Description

  The present invention provides a synthetic fiber in which the aqueous solution of the synthetic fiber treating agent itself maintains long-term stability even in winter, and the synthetic fiber using such an aqueous solution can exhibit excellent process passability in the spinning and drawing process. The present invention relates to an aqueous solution of a treating agent, an emulsion of an aqueous solution of a treating agent for synthetic fibers prepared by further diluting the aqueous solution with water, and a method for treating synthetic fibers to which the emulsion is attached.

  Conventionally, as an aqueous liquid of a treating agent for synthetic fibers to be subjected to a spinning and drawing process, a lubricant, an antistatic agent, and a specific hydroxy compound blocked at one end with an acyclic branched saturated hydrocarbon group having 9 carbon atoms. An aqueous liquid (for example, refer to Patent Document 1) containing a treating agent has been proposed. However, these conventional aqueous treatment solutions for synthetic fibers have a problem of insufficient winter stability. When the synthetic fiber using the conventional aqueous solution for synthetic fiber is subjected to the spinning drawing process, the amount of tar dirt generated on the godet roller is large, and the tar dirt is poorly washed. There is also a problem of generation of fuzz, generation of stained spots, and generation of static electricity in a post-processing process.

JP 2004-204388 A

  The problem to be solved by the present invention is that the aqueous solution of the synthetic fiber treating agent itself maintains stability for a long time even in winter, and the synthetic fiber is drawn on the godet roller in the spinning and drawing process using the aqueous solution. A treatment agent for synthetic fibers that has a small amount of tar dirt generation, good tar dirt detergency, and can sufficiently suppress problems of spinning fluff, dyeing spots, and generation of static electricity in post-processing steps. It is an object of the present invention to provide a synthetic fiber treating agent emulsion prepared by further diluting the aqueous liquid with water, and a synthetic fiber treating method for attaching the emulsion.

  As a result of investigations to solve the above-mentioned problems, the present inventors have found an aqueous solution of a synthetic fiber treatment agent containing a specific proportion of a synthetic fiber treatment agent containing three specific components and water in a specific proportion. Thus, it has been found that an aqueous liquid having a specific metal ion concentration of a specific value or less is suitable.

  That is, the present invention contains 20 to 85% by mass of the following smoothing agent, 5 to 70% by mass of the following nonionic surfactant, and 1 to 20% by mass (100% by mass in total) of the following antistatic agents. An aqueous solution of a synthetic fiber treatment agent comprising a synthetic fiber treatment agent and water, containing 3 to 20 parts by mass of water with respect to 100 parts by mass of the synthetic fiber treatment agent, and ICP emission analysis The total concentration of calcium ions and magnesium ions determined by the method is 0.5 mg / kg or less, and relates to an aqueous solution of a treating agent for synthetic fibers. The present invention also relates to an emulsion of a synthetic fiber treatment agent prepared by further diluting an aqueous solution of the synthetic fiber treatment agent with water, and a synthetic fiber treatment method to which the emulsion is attached.

  Smoothing agent: liquid paraffin oil and / or ester compound

  Nonionic surfactant: Ether type nonionic surfactant having a polyoxyalkylene group in the molecule

  Antistatic agent: at least one selected from organic fatty acid salt, organic phosphate ester salt, organic sulfonate salt, organic sulfate salt, organic quaternary ammonium salt, organic amine oxide, organic alanine compound and organic betaine compound

  First, an aqueous liquid of the synthetic fiber treating agent according to the present invention (hereinafter referred to as the aqueous liquid of the present invention) will be described. The aqueous liquid of the present invention has a ratio of 20 to 85% by mass of the smoothing agent, 5 to 70% by mass of the nonionic surfactant, and 1 to 20% by mass (100% by mass in total) of the antistatic agent. Calcium ions obtained by ICP emission analysis, containing 3 to 20 parts by mass of water with respect to 100 parts by mass of the synthetic fiber treatment agent. And an aqueous solution of a treating agent for synthetic fibers having a total concentration of magnesium ions of 0.5 mg / kg or less.

  As described above, the smoothing agent used for the synthetic fiber treating agent in the aqueous liquid of the present invention is liquid paraffin oil and / or an ester compound.

Examples of the liquid paraffin oil include various commercially available oils. Among them, Diana Fresia W32 (trade name, manufactured by Idemitsu Kosan Co., Ltd.) having a kinematic viscosity at 30 ° C. of 49.0 mm ² / s and a kinematic fluid at 30 ° C. Super oil N100 (trade name, Nippon oil Co., Ltd.) having a viscosity of 156.0mm ² / s and the like, preferably has a kinematic viscosity of 30 ℃ is 1~500mm ² / s, Diana Fresia W32 (trade name, Idemitsu Kosan And those having a kinematic viscosity at 30 ° C. of 1 to 200 mm ² / s, such as Super Oil N100 (trade name, manufactured by Nippon Oil Corporation).

  Examples of ester compounds include 1) butyl stearate, octyl stearate, oleyl laurate, oleyl oleate, lauryl oleate, isopentacosanyl isostearate, octyl palmitate, isopropyl myristate, isotridecyl stearate, etc. An ester compound of an aliphatic monoalcohol and an aliphatic monocarboxylic acid, or an ester compound of an aliphatic monoalcohol with an adduct obtained by adding an alkylene oxide having 2 to 4 carbon atoms to an aliphatic monoalcohol, 2) 1, 6-hexanediol didecanoate trimethylolpropane monooleate monolaurate, trimethylolpropane trioleate, sorbitan trioleate, pentaerythritol tetraoleate, glycerin monolaurate, etc. And a complete ester compound of an aliphatic monocarboxylic acid and an addition product obtained by adding an alkylene oxide having 2 to 4 carbon atoms to an aliphatic polyhydric alcohol, and 3) dilauryl azimuth. Part ester, dioleyl adipate, dioleyl azelate, diisocetylthiodipropionate, bispolyoxyethylene lauryl adipate, etc. Complete ester compounds of adducts obtained by adding C2-C4 alkylene oxides to monoalcohols and aliphatic polycarboxylic acids, 4) Aromatic monoalcohols and aliphatic monocarboxylics such as benzyl oleate and benzyl laurate C2-C4 alkylene ester with ester compound with acid or aromatic monoalcohol Ester compound of side-added adduct and aliphatic monocarboxylic acid, 5) Partial ester compound of polyhydric alcohol and aliphatic monocarboxylic acid, such as sorbitan monooleate, glycerol monolaurate, etc. 6) Bisphenol A Complete ester compounds of aromatic polyhydric alcohols and aliphatic monocarboxylic acids, such as dioleate and bisphenol A dilaurate, and adducts of aliphatic polyhydric alcohols with addition of alkylene oxides having 2 to 4 carbon atoms and aliphatic monocarboxylic acids 7) Complete ester compounds with aliphatic monoalcohols and aromatic polycarboxylic acids, such as bis-2-ethylhexyl phthalate, diisostearyl isophthalate, trioctyl trimellitate, etc. C2-C4 alkylene oxide in monoalcohol Examples include complete ester compounds of added adducts and aromatic polycarboxylic acids, and 8) natural esters such as coconut oil, rapeseed oil, sunflower oil, soybean oil, castor oil, sesame oil, fish oil, and beef tallow.

  Among these, as the ester compound, an ester compound having 10 to 100 carbon atoms is preferable, and an ester compound having 20 to 70 carbon atoms is more preferable.

  The nonionic surfactant used for the synthetic fiber treating agent in the aqueous liquid of the present invention is an ether type nonionic surfactant having a polyoxyalkylene group in the molecule as described above. As ether type nonionic surfactants having a polyoxyalkylene group in the molecule, 1) polyoxyethylene dilaurate, polyoxyethylene oleate, polyoxyethylene laurate methyl ether, polyoxyethylene octyl ether, polyoxypropylene Lauryl ether methyl ether, polyoxybutylene oleyl ether, polyoxyethylene polyoxypropylene nonyl ether, polyoxypropylene nonyl ether, polyoxyethylene polyoxypropylene octyl ether, polyoxyethylene lauryl ether, polyoxyethylene tridecyl ether, polyoxy Organic acids, organic alcohols, organic amines and / or organic amines such as ethylene lauryl amino ether and polyoxyethylene lauroamide ether Nonionic surfactants obtained by adding alkylene oxides having 2 to 4 carbon atoms to the carbon dioxide, 2) Carbon number in partial ester compounds of polyhydric alcohols and fatty acids, such as polyoxyalkylene sorbitan trioleate and polyoxyalkylene glycerol monolaurate Nonionic surfactants with addition of 2 to 4 alkylene oxides, 3) Nonions with addition of C2-4 alkylene oxides to castor oil or hydrogenated castor oil, such as polyoxyethylene castor oil and polyoxyethylene hydrogenated castor oil Surfactants, 4) polyoxyethylene castor oil trioctanoate, polyoxyethylene hydrogenated castor oil trioleate, and the like, and adducts and fatty acids added with castor oil or hydrogenated castor oil with a C2-C4 alkylene oxide Nonionic surfactant obtained by esterification of 5) Such as polyoxyethylene diethanolamine mono oleyl amide, nonionic surfactant, and the like obtained by adding an alkylene oxide having 2 to 4 carbon atoms in the alkylene fatty acid amide compound.

  Examples of the polyoxyalkylene group in the molecule of the ether type nonionic surfactant include a polyoxyethylene group, a polyoxypropylene group, a polyoxybutylene group, and a (poly) oxyethylene (poly) oxypropylene group.

  As described above, the antistatic agent used in the treatment agent for synthetic fibers in the aqueous liquid of the present invention includes an organic fatty acid salt, an organic phosphate ester salt, an organic sulfonate salt, an organic sulfate salt, an organic quaternary ammonium salt, an organic It is at least one selected from an amine oxide, an organic alanine compound, and an organic betaine compound.

  Examples of the organic fatty acid salt include 1) an alkali metal salt of a fatty acid having 6 to 22 carbon atoms, 2) an amine salt of a fatty acid having 6 to 22 carbon atoms, and 3) a phosphonium salt of a fatty acid having 6 to 22 carbon atoms. . Examples of the fatty acid having 6 to 22 carbon atoms include caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, isostearic acid, behenic acid, oleic acid, erucic acid, linoleic acid, and dodecenyl succinic acid. .

  In the organic fatty acid salt, examples of the alkali metal constituting the alkali metal salt include sodium and potassium.

  As amines constituting the amine salt, 1) aliphatic amines such as methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, butylamine, dibutylamine, tributylamine, octylamine, 2) aniline, Aromatic amines or heterocyclic amines such as pyridine, morpholine, piperazine, and derivatives thereof 3) monoethanolamine, diethanolamine, triethanolamine, isopropanolamine, diisopropanolamine, triisopropanolamine, butyldiethanolamine, octyldiethanolamine, Alkanolamines such as lauryldiethanolamine, 4) polyoxyethylene lauryl amino ether, polyoxyethylene steryl amino ether Polyoxyalkylene alkyl amino ethers etc., 5) and ammonia.

  Further, the phosphonium group constituting the phosphonium salt includes 1) phosphorus such as tetramethylphosphonium, tetraethylphosphonium, tetrabutylphosphonium, trimethylethylphosphonium, trimethylpropylphosphonium, trimethyloctylphosphonium, trimethyldodecylphosphonium, trimethyloctadecylphosphonium, etc. Phosphonium group in which all organic groups bonded to the atom are aliphatic hydrocarbon groups, 2) Phosphorus atom such as trimethylphenylphosphonium, triethylphenylphosphonium, tributylphenylphosphonium, dimethyldiphenylphosphonium, triphenylethylphosphonium, tetraphenylphosphonium A phosphonium group in which at least one of the bonded organic groups is an aromatic hydrocarbon group, etc. It is.

  Examples of the organic phosphate ester salt include 1) an alkyl phosphate ester alkali metal salt having an alkyl group having 4 to 22 carbon atoms, and 2) an alkyl group having 4 to 22 carbon atoms and (poly) oxyalkylene. A (poly) oxyalkylene alkyl ether phosphate alkali metal salt having 1 to 5 oxyalkylene units constituting the group, 3) an alkyl phosphate amine salt having 4 to 22 carbon atoms in the alkyl group, 4) (Poly) oxyalkylene alkyl ether phosphate amine salts, etc., wherein the alkyl group has 4 to 22 carbon atoms and the number of oxyalkylene units constituting the (poly) oxyalkylene group is 1 to 5. It is done.

  Alkyl phosphate alkali metal salts having 4 to 22 carbon atoms in the alkyl group include butyl phosphate alkali metal salts, pentyl phosphate alkali metal salts, hexyl phosphate alkali metal salts, heptyl phosphate alkali metal salts, octyl Phosphate ester alkali metal salt, isooctyl phosphate ester alkali metal salt, 2-ethylhexyl phosphate ester alkali metal salt, decyl phosphate ester alkali metal salt, dodecyl phosphate ester alkali metal salt, tridecyl phosphate ester alkali metal salt, myristyl phosphate Ester alkali metal salt, Cetyl phosphate alkali metal salt, Stearyl phosphate alkali metal salt, Eicosyl phosphate alkali metal salt, Behenyl phosphate alkali metal salt, etc. And the like.

  These alkyl phosphate ester alkali metal salts include monoesters alone, diesters alone, mixtures of monoesters and diesters, and diesters having the same alkyl group Bodies (symmetrical diesters) and diesters having different alkyl groups (asymmetrical diesters).

    Moreover, the alkali metal which comprises these alkyl phosphate ester alkali metal salts is the same as that mentioned above about the organic fatty acid salt.

  The (poly) oxyalkylene alkyl ether phosphate alkali metal salt in which the alkyl group has 4 to 22 carbon atoms and the number of oxyalkylene units constituting the (poly) oxyalkylene group is 1 to 5, Oxyalkylene butyl ether phosphate alkali metal salt, polyoxyalkylene pentyl ether phosphate alkali metal salt, polyoxyalkylene hexyl ether phosphate alkali metal salt, polyoxyalkylene heptyl ether phosphate alkali metal salt, polyoxyalkylene octyl Ether phosphate alkali metal salt, polyoxyalkylene isooctyl ether phosphate alkali metal salt, polyoxyalkylene-2-ethylhexyl ether phosphate alkali metal salt Polyoxyalkylene decyl ether phosphate alkali metal salt, polyoxyalkylene lauryl ether phosphate alkali metal salt, polyoxyalkylene tridecyl ether phosphate alkali metal salt, polyoxyalkylene myristyl ether phosphate alkali metal salt, poly Oxyalkylene cetyl ether phosphate alkali metal salt, polyoxyalkylene stearyl ether phosphate alkali metal salt, polyoxyalkylene eicosyl ether phosphate alkali metal salt, polyoxyalkylene behenyl ether phosphate alkali metal salt, etc. It is done.

  In such polyoxyalkylene alkyl ether phosphate alkali metal salts, examples of (poly) oxyalkylene groups include (poly) oxyethylene groups, (poly) oxypropylene groups, (poly) oxyethyleneoxypropylene groups, and the like.

  These polyoxyalkylene alkyl ether phosphate alkali metal salts include monoesters alone, diesters alone, and mixtures of monoesters and diesters. Diesters having a group (symmetrical diester) and diesters having a different alkyl group (asymmetrical diester) are included.

  The alkali metal constituting these polyoxyalkylene alkyl ether phosphate alkali metal salts is the same as described above for the organic fatty acid salts.

  An alkyl phosphate ester amine salt having an alkyl group with 4 to 22 carbon atoms, an alkyl group with 4 to 22 carbon atoms and a (poly) oxyalkylene group having 1 to 5 oxyalkylene units The amine used for a certain (poly) oxyalkylene alkyl ether phosphate amine salt is the same as described above for the organic fatty acid salt.

  The organic phosphate ester salt used in the present invention contains components such as monooctyl pyrophosphate alkali metal salt, dioctyl pyrophosphate alkali metal salt, pyrophosphate alkali metal salt, and tripolyphosphate in addition to the aforementioned organic phosphate. However, these components are preferably as small as possible.

  Examples of the organic sulfonate include 1) an alkali metal salt of an organic sulfonic acid having 6 to 22 carbon atoms, 2) an organic sulfonic acid amine salt having 6 to 22 carbon atoms, and 3) an phosphonium organic sulfonate having 6 to 22 carbon atoms. Examples include salts. Examples of the organic sulfonic acid having 6 to 22 carbon atoms constituting such an organic sulfonate include 1) decyl sulfonic acid, dodecyl sulfonic acid, isotridodecyl sulfonic acid, tetradecyl sulfonic acid, hexadecyl sulfonic acid, pentadecane sulfonic acid and the like 2) alkyl aryl sulfonic acids such as butyl benzene sulfonic acid, dodecyl benzene sulfonic acid, octadecyl benzene sulfonic acid, dibutyl naphthalene sulfonic acid 3) dioctyl sulfosuccinic acid ester, dibutyl sulfosuccinic acid ester, dodecyl sulfoacetic acid ester, Examples thereof include ester sulfonic acids such as nonylphenoxypolyethylene glycol sulfoacetate.

  The alkali metal constituting the organic sulfonic acid alkali metal salt, the amine constituting the organic sulfonic acid amine salt, and the phosphonium group constituting the organic sulfonic acid phosphonium salt are the same as described above for the organic fatty acid salt.

  Organic sulfate salts include: 1) Alkyl sulfate alkali metal salts such as sodium decyl sulfate, sodium dodecyl sulfate, lithium tetradecyl sulfate, and potassium hexadecyl sulfate; 2) sulfates of natural fats and oils such as beef tallow sulfated oil, castor oil sulfated oil, etc. Examples include alkali metal salts. The alkali metal constituting the alkali metal salt is the same as described above for the organic fatty acid salt.

  The organic quaternary ammonium salt is generally composed of a quaternary ammonium cation group and an anion group. As one quaternary ammonium cation group, 1) a quaternary ammonium cation group in the case where each of the organic groups bonded to the nitrogen atom is an alkyl group having 1 to 25 carbon atoms, and 2) an organic bonded to the nitrogen atom. A quaternary ammonium cation group in which all the groups are alkenyl groups having 2 to 25 carbon atoms, and 3) a fourth case in which all of the organic groups bonded to the nitrogen atom are hydroxyalkyl groups having 1 to 6 carbon atoms. Quaternary ammonium cation group, 4) quaternary ammonium cation in the case where a part of the organic group bonded to the nitrogen atom is an alkyl group having 1 to 25 carbon atoms and the remainder is an alkenyl group having 2 to 25 carbon atoms Group, 5) quaternary ammonia in which a part of the organic group bonded to the nitrogen atom is an alkyl group having 1 to 25 carbon atoms and the remainder is a hydroxyalkyl group having 1 to 6 carbon atoms 6) a quaternary ammonium cation group in which part of the organic group bonded to the nitrogen atom is an alkenyl group having 2 to 25 carbon atoms and the remainder is a hydroxyalkyl group having 1 to 6 carbon atoms 7) Part of the organic group bonded to the nitrogen atom is an alkyl group having 1 to 25 carbon atoms, the other part is an alkenyl group having 2 to 25 carbon atoms, and the remainder is 1 to carbon atoms. And quaternary ammonium cation groups in the case of 6 hydroxyalkyl groups.

  Specific examples of quaternary ammonium cationic groups include 1) tetramethylammonium, trimethylethylammonium, tripropylmethylammonium, tributylmethylammonium, tetrabutylammonium, triethylisooctylammonium, trimethyloctylammonium, trimethyllaurylammonium, trimethylstearyl. A quaternary ammonium cation group in the case where any organic group bonded to a nitrogen atom, such as ammonium, is an alkyl group having 1 to 25 carbon atoms, 2) dibutenyl diethyl ammonium, dimethyl dioleyl ammonium, trimethyl oleyl ammonium, triethyl Among the organic groups bonded to the nitrogen atom, such as eicosenyl ammonium, a part is an alkyl group having 1 to 25 carbon atoms, and the remainder is 2 to 25 carbon atoms. A quaternary ammonium cation group in the case of an alkenyl group, 3) tributylhydroxyethylammonium, di (hydroxyethyl) dipropylammonium, tri (hydroxyethyl) octylammonium, tri (hydroxypropyl) methylammonium, etc. A quaternary ammonium cation group etc. in case one part is a C1-C25 alkyl group among the organic groups couple | bonded and the remainder is a C1-C6 hydroxyalkyl group etc. are mentioned.

  Examples of the other anionic group include anionic groups obtained by removing part or all of hydrogen ions from 1 to 3 valent organic acids such as organic phosphates, organic sulfates, organic sulfonates, and organic carboxylic acids.

  Specifically, as an anionic group, 1) C1-30 organic phosphoric acid such as methyl phosphate ester, diethyl phosphate ester, dioctyl phosphate ester, methyl oleyl phosphate ester, nonylphenyloxyethoxyethyl / methyl phosphate ester, etc. Anionic group obtained by removing a part or all of hydrogen ions from an ester, 2) Some or all of hydrogen ions from an organic sulfate having 1 to 30 carbon atoms such as methyl sulfate, ethyl sulfate, lauryl sulfate, octylphenyloxypolyethoxyethyl sulfate Anion group excluding all, 3) butyl sulfonate, lauryl sulfonate, stearyl sulfonate, oleyl sulfonate, p-toluene sulfonate, dodecyl phenyl sulfonate, oleyl phenyl sulfonate, naphthyl sulfo Anionic groups obtained by removing part or all of hydrogen ions from C1-C30 organic sulfonic acid esters such as diisopropyl naphthyl sulfonate, 4) acetic acid, caproic acid, lauric acid, 2-ethylhexanoic acid, isostearic acid, C1-C30 aliphatic carboxylic acids such as oleic acid, erucic acid, malonic acid, adipic acid, sebacic acid, pentadecenyl succinic acid, benzoic acid, phthalic acid, trimellitic acid, etc. 7-30 carbon atoms Aromatic carboxylic acids, lactic acid, ricinoleic acid, aliphatic hydroxycarboxylic acids having 3 to 30 carbon atoms such as 12-hydroxystearic acid, sulfur containing aliphatic carboxylic acids having 3 to 30 carbon atoms such as thiodipropionic acid, etc. An anionic group obtained by removing a part or all of hydrogen ions from an organic carboxylic acid having 1 to 30 carbon atoms is exemplified.

  Examples of the organic amine oxide include 1) dimethylethylamine oxide, dimethylpropylamine oxide, dimethylhexylamine oxide, dimethyloctylamine oxide, dimethylnonylamine oxide, dimethyllaurylamine oxide, dimethylmyristylamine oxide, dimethylcetylamine oxide, dimethyl Stearylamine oxide, dimethyl eicosylamine oxide, dihexylmethylamine oxide, dioctylmethylamine oxide, dinonylmethylamine oxide, dilaurylmethylamine oxide, dimyristylmethylamine oxide, dicetylmethylamine oxide, distearylmethylamine oxide, Nitrogen atoms such as dieicosylmethylamine oxide Organic amine oxide in which all aliphatic hydrocarbon groups are saturated aliphatic hydrocarbon groups having 1 to 24 carbon atoms, 2) 2-tetradecenylamine oxide, 2-pentadecenylamine oxide, 2-octa Decenylamine oxide, 15-hexadecenylamine oxide, oleylamine oxide, linoleylamine oxide, eleostearylamine oxide, di-2-tetradecenylamine oxide, di-2-pentadecenylamine oxide, di-2-octadeceni At least one of the aliphatic hydrocarbon groups bonded to the nitrogen atom, such as ruamine oxide, di15-hexadecenylamine oxide, dioleylamine oxide, dilinoleylamine oxide, dieleostearylamine oxide, etc. 14-24 Organic amine oxide is an unsaturated aliphatic hydrocarbon group.

  Examples of the organic alanine compound include sodium N, N-bis (2-carboxyethyl) -octylamine, sodium N, N-bis (2-carboxyethyl) -dodecylamine, and N, N-bis (2-carboxyethyl). ) -Tetradecylamine potassium, N, N-bis (2-carboxyethyl) -hexadecylamine sodium, N, N-bis (2-carboxyethyl) -octadecylamine sodium, N- (2-carboxyethyl) -dodecyl Examples include amine, sodium N- (2-carboxyethyl) -octadecylamine, sodium N-oleoyl-N′-carboxyethyl-N′-hydroxyethylethylenediamine, and the like.

  Examples of the organic betaine compound include octyldimethylammonioacetate, decyldimethylammonioacetate, dodecyldimethylammonioacetate, hexadecyldimethylammonioacetate, octadecyldimethylammonioacetate, nonadecyldimethylammonioacetate. , Octadecenyldimethylammonioacetate, dodecylaminopropyldimethylammonioacetate, octadecylaminopropyldimethylammonioacetate, octadecenylaminopropyldimethylammonioacetate and the like.

  The aqueous liquid of the present invention has a total concentration of calcium ions and magnesium ions determined by ICP emission spectrometry of 0.5 mg / kg or less. There are no limitations on the measurement conditions of the ICP emission analysis method, and the total concentration of calcium ions and magnesium ions can be determined by a known method. For example, using a sample in which distilled water or ultrapure water is added to an aqueous solution of a synthetic fiber treatment agent, and then a water-soluble organic solvent is added and dissolved uniformly as necessary. Examples thereof include a method for obtaining the total concentration of calcium ions and magnesium ions contained in the aqueous liquid.

  In order to reduce the total concentration of calcium ions and magnesium ions in the aqueous liquid of the present invention to 0.5 mg / kg or less, calcium ions and magnesium contained in the nonionic surfactant and antistatic agent used in the treating agent for synthetic fibers It is necessary to control the ion concentration, but the method is not particularly limited.

  For example, regarding nonionic surfactants for synthetic fiber treatment agents, when calcium hydroxide or magnesium hydroxide is used as a catalyst for synthesizing ether type nonionic surfactants, these are adsorbed after the reaction. The method of removing is mentioned. In addition, as for anionic compounds used as antistatic agents for synthetic fiber treatment agents, it was decided not to select those containing calcium ions or magnesium ions, or compounds containing calcium ions or magnesium ions were used during the synthesis of anionic compounds. In some cases, a method of removing these ions with an adsorbent or the like can be mentioned.

  Water is used in preparing the aqueous liquid of the present invention, and generally used water contains a large amount of calcium ions and magnesium ions as natural minerals. For example, in general tap water in Japan, calcium ions and magnesium ions are contained in a total of 10 mg / kg or more. When such tap water is used, calcium ions and magnesium in the aqueous solution of the synthetic fiber treatment agent are used. The total concentration of ions may exceed 1 mg / kg.

  For this reason, it is necessary to reduce the amount of tap water used as described above as much as possible, or to remove polyvalent metal cations in the water used. For example, there are a treatment with an ultrafiltration membrane, a treatment with an adsorbent, an adsorption treatment with an ion exchange resin, and the removal method is not particularly limited, and a known method can be adopted. A method of adsorbing the water used in preparing the aqueous liquid of the agent with an ion exchange resin is preferable.

  The aqueous liquid of the present invention has a ratio of 20 to 85% by mass of the smoothing agent, 5 to 70% by mass of the nonionic surfactant, and 1 to 20% by mass (100% by mass in total) of the antistatic agent. The synthetic fiber treatment agent is an aqueous liquid containing 30 to 75% by mass of the smoothing agent, 10 to 60% by mass of the nonionic surfactant, and the antistatic agent. Are preferably contained in a proportion of 2 to 15% by weight (100% by mass in total).

  The aqueous liquid of the present invention is formed by blending water at a ratio of 3 to 20 parts by mass with respect to 100 parts by mass of the synthetic fiber treatment agent described above, and above all, 100 parts by mass of the synthetic fiber treatment agent. On the other hand, what mix | blends water in the ratio of 5-15 mass parts is preferable.

  Next, an emulsion of the treating agent for synthetic fibers according to the present invention (hereinafter referred to as the emulsion of the present invention) will be described. The emulsion of the present invention was prepared by further diluting the aqueous liquid of the present invention with water, containing 200 to 5000 parts by mass of water with respect to 100 parts by mass of the synthetic fiber treating agent, and by ICP emission spectrometry. A synthetic fiber treatment agent emulsion characterized in that the total concentration of calcium ions and magnesium ions required is 0.5 mg / kg or less and the dissolved oxygen in the emulsion is 10 mg / L or less.

  The IPC emission analysis method, the total concentration of calcium ions and magnesium ions, and the like are as described above for the aqueous liquid of the present invention. The water used for dilution needs to remove calcium ions and magnesium ions in the water. The total concentration of calcium ions and magnesium ions in the emulsion of the present invention is 0.5 mg / kg or less.

In the emulsion of the present invention, the dissolved oxygen concentration in the emulsion is not particularly limited in its measuring method, and can be determined by a known method. Examples thereof include a titration method that is a chemical analysis method, a diaphragm electrode method that is an electrochemical analysis method, and a fluorescence method that is a photochemical analysis method. The method for preparing the dissolved oxygen concentration of the emulsion in the emulsion to be 10 mg / L or less is not particularly limited, and this includes a method for heating treatment, a method for standing treatment, a method for reducing pressure, and a combination thereof. Although there are methods, for example, a method through the following steps 1 to 3 can be mentioned.
Process 1: The process of heating the water used for preparation of an emulsion.
Process 2: The process of preparing the processing agent for synthetic fibers using the water obtained at the process 1.
Step 3: A step of allowing the emulsion obtained in Step 2 to stand.

  Finally, the synthetic fiber processing method according to the present invention (hereinafter referred to as the processing method of the present invention) will be described. The treatment method of the present invention is a method of adhering the emulsion of the present invention to a synthetic fiber so as to be 0.1 to 3% by mass as a synthetic fiber treatment agent.

  Examples of the process for attaching the emulsion of the present invention to the synthetic fiber include a spinning process, a stretching process, and a process in which spinning and stretching are performed simultaneously. Moreover, as a method of attaching the emulsion of the present invention to the synthetic fiber, a known oiling method such as a roller oiling method, a guide oiling method using a metering pump, an immersion oiling method, or a spray oiling method can be applied.

  In the present invention, the synthetic fibers to be treated are: 1) polyester mainly composed of ethylene terephthalate, 2) polyamide such as nylon 6 and nylon 66, 3) polyacryl such as polyacrylonitrile and modacrylic, 4) Polyolefins such as polyethylene and polypropylene are listed, but the effect is high when applied to polyester partially drawn yarn, polyamide partially drawn yarn, and polyester direct-spun drawn yarn, and effective when applied to cationic dyeable polyester. Higher expression.

  According to the present invention described above, the aqueous solution of the synthetic fiber treating agent itself retains long-term stability even in winter, and the tar dirt on the godet roller in the spinning and drawing process of the synthetic fiber using such an aqueous solution. There is an effect that the amount of generation of tar is small, the detergency of tar dirt is good, and generation of spinning fluff, generation of stained spots, and generation of static electricity in the post-processing step can be sufficiently suppressed.

  Hereinafter, examples and the like will be given in order to make the configuration and effects of the present invention more specific, but the present invention is not limited to these examples. In the following examples and comparative examples, “part” means “part by mass”, and “%” means “% by mass” unless otherwise specified.

Test Category 1 (Preparation of aqueous solution of synthetic fiber treatment agent and evaluation of aqueous solution)
Example 1 {Preparation of aqueous solution (P-1) of synthetic fiber treatment agent}
As a smoothing agent, 44 parts of A-1 shown in Table 1 and 30 parts of A-2, 10 parts of B-1 shown in Table 2 and 2 parts of B-2 as nonionic surfactants, and Table 3 as antistatic agents 14 parts of C-1 described above, 10 parts of water purified by the following method, 10 parts of the above were uniformly mixed, and the total concentration of calcium ions and magnesium ions determined by the following ICP emission analysis method was 0.3 mg / A synthetic liquid treating agent aqueous solution (P-1) of kg was prepared.

  Water purification method: tap water is made from H-type strongly acidic cation exchange resin (trade name Amberlite IR-120B manufactured by Organo) and OH-type strongly basic anion exchange resin (trade name Amberlite IRA-400J manufactured by Organo). ), And the concentration of calcium ions, the concentration of magnesium ions, or the total concentration of calcium ions and magnesium ions was treated to 0.1 mg / L or less.

  ICP emission analysis method: 5 g of a sample was accurately weighed and diluted with distilled water to make a total amount of 100 g. The prepared diluted solution was subjected to an ICP emission spectrometer (trade name SPS-3100 manufactured by Hitachi High-Tech Science Co., Ltd.). Quantification is performed by comparing the strength value with a commercially available standard sample of known concentration to determine the concentration of calcium ions, the concentration of magnesium ions, or the total concentration of calcium ions and magnesium ions in the aqueous solution of the treatment agent for synthetic fibers. Asked.

Examples or Reference Examples 2 to 12, Comparative Examples 2 and 3 {Preparation of aqueous solutions (P-2) to (P-12), (R-2) and (R-3) of synthetic fiber treatment agents}
In the same manner as the synthetic fiber treating agent aqueous liquid (P-1), synthetic fiber treating agent aqueous liquids (P-2) to (P-12), (R-2) and (R-3) were prepared. .

Comparative Example 1 {Preparation of aqueous solution (R-1) of synthetic fiber treatment agent}
Calcium ions obtained by the above ICP emission analysis method in the same manner as the aqueous solution (P-1) of the synthetic fiber treatment agent, except that water containing 185 mg / kg of calcium ions and 40 mg / kg of magnesium ions was used. An aqueous liquid (R-1) of a synthetic fiber treating agent having a total magnesium ion concentration of 22.3 mg / kg was prepared.

Comparative Examples 6 to 8 {Preparation of aqueous solution (R-6) to (R-8) of synthetic fiber treatment agent}
In the same manner as the synthetic fiber treating agent aqueous liquid (R-1), synthetic fiber treating agent aqueous liquids (R-6) to (R-8) were prepared.

Comparative Example 4 {Preparation of Synthetic Fiber Treatment Agent Aqueous Liquid (R-4)}
ICP emission analysis as described above in the same manner as the aqueous solution (P-1) of synthetic fiber treatment agent, except that water containing 36 mg / kg of calcium ions, 3 mg / kg of magnesium ions, and 1 mg / kg of iron ions was used. An aqueous solution (R-4) of a synthetic fiber treating agent having a total concentration of calcium ions and magnesium ions determined by the method of 8.5 mg / kg was prepared.

Comparative Example 5 {Preparation of aqueous solution of synthetic fiber treatment agent (R-5)}
ICP emission analysis as described above in the same manner as the aqueous solution (P-1) of synthetic fiber treatment agent, except that water containing 210 mg / kg calcium ion, 44 mg / kg magnesium ion, and 4 mg / kg iron ion was used. An aqueous solution (R-5) of a synthetic fiber treating agent having a total concentration of calcium ions and magnesium ions determined by the method of 42.0 mg / kg was prepared.

Comparative Example 9 {Preparation of aqueous solution of synthetic fiber treating agent (R-9)}
Calcium ions obtained by the above ICP emission analysis method in the same manner as in the aqueous solution (P-1) of the synthetic fiber treatment agent, except that water containing 40 mg / kg calcium ions and 4 mg / kg magnesium ions was used. An aqueous solution (R-9) of a synthetic fiber treating agent having a total concentration of magnesium ions of 6.2 mg / kg was prepared.

・ Low-temperature stability of aqueous solution of synthetic fiber treatment agent The aqueous solution of synthetic fiber treatment agent of each example prepared above is stored in an incubator at −5 ° C. for 1 month, and appearance before and after storage The change of was visually evaluated according to the following criteria. Table 4 summarizes the contents of the treatment agents prepared above and the results of product low-temperature stability.

○: No change and no problem in practical use.
X: Since the appearance becomes non-uniform or separates, there is a practical problem.

  In each of the above examples, Table 1 shows the smoothing agent used in the preparation of the aqueous treatment solution for synthetic fibers, Table 2 shows the nonionic surfactant, and Table 3 shows the antistatic agent. Table 4 summarizes the contents of the aqueous liquid, the total concentration of polyvalent metal ions, and the low-temperature stability of the synthetic fiber treating agent prepared in each of the above examples.

In Table 4,
Water (parts): parts by mass of water per 100 parts by mass of the treating agent for synthetic fibers Comparative Example 9: 1% of a chelating agent, ethylenediaminetetraacetic acid Na, was used as an additive.

Test category 2 (preparation of emulsion for synthetic fiber treatment agent, adhesion to synthetic fiber, evaluation)
Example 13
The synthetic fiber treating agent aqueous liquid (P-1) prepared in Test Category 1 was diluted by adding 700 parts of water to 100 parts of this aqueous liquid (P-1) and subjected to the following ICP emission spectrometry. An emulsion was prepared in which the total concentration of calcium ions and magnesium ions required was 0.2 mg / kg, and the dissolved oxygen concentration determined by the following dissolved oxygen measurement method was 5.0 mg / L. The water used for the preparation was prepared by adjusting the temperature of purified water similar to that used in the synthetic liquid treating agent aqueous liquid (P-1) to 30 ° C.

  ICP emission analysis method: The same as the ICP emission analysis method described above except that the prepared emulsion was directly used in an ICP emission analysis apparatus.

  Dissolved oxygen measurement method: Weigh about 100 ml of emulsion in a beaker, put a detection probe of a diaphragm electrode type dissolved oxygen meter (trade name dissolved oxygen meter DO meter B-506 manufactured by Iijima Electronics Co., Ltd.) into the emulsion, and dissolve oxygen. Concentration was measured.

-Examples or Reference Examples 14-24
In the same manner as in Example 13, emulsions of the synthetic fiber treating agents of Examples or Reference Examples 14 to 24 were prepared.

Comparative Example 10
Except for using water containing 12 mg / kg of calcium ions and 3 mg / kg of magnesium ions, the total concentration of calcium ions and magnesium ions determined by the ICP emission analysis method was 15.8 mg, as in Example 13. A synthetic fiber treating agent emulsion having a dissolved oxygen concentration of 7.3 mg / L determined by the above-described dissolved oxygen concentration measurement method was prepared.

Comparative examples 11 and 12
Synthetic fiber treatment agents of Comparative Examples 11 and 12 were prepared in the same manner as in Example 13 except that purified water used for the preparation was adjusted to 5 ° C.

Comparative Example 13
Except for using water containing 26 mg / kg of calcium ions and 4 mg / kg of magnesium ions, the total concentration of calcium ions and magnesium ions determined by the ICP emission analysis method was 27.5 mg in the same manner as in Example 13. A synthetic fiber treating agent emulsion having a dissolved oxygen concentration of 7.4 mg / L determined by the above-described dissolved oxygen concentration measurement method was prepared.

Comparative Examples 14-16 and 18
In the same manner as in Comparative Example 10, emulsions of synthetic fiber treating agents of Comparative Examples 14 to 16 and 18 were prepared.

Comparative Example 17
An emulsion of the treating agent for synthetic fiber of Comparative Example 17 was prepared in the same manner as in Example 13 except that water containing 12 mg / kg of calcium ions and 3 mg / kg of magnesium ions and temperature-controlled at 5 ° C. was used.

-Adhesion and evaluation of synthetic fiber processing agent emulsion to synthetic fiber After drying polyethylene terephthalate with intrinsic viscosity of 0.64 and titanium oxide content of 0.2% by a conventional method, using an extruder at 295 ° C The running yarn after spinning, discharging from the die, and cooling and solidifying the emulsion of each example described above by the guide oiling method using a metering pump has an adhesion amount as a processing agent for synthetic fibers of 1.0%. After being attached so as to be converged with a guide, after stretching with a first codet roller having a surface speed of 5000 m / min and a surface temperature of 90 ° C. and a second codet roller having a surface speed of 5500 m / min and a surface temperature of 150 ° C., Winding was performed at a speed of 5500 m / min to obtain a drawn yarn of 83 dtex 36 filaments.

・ Evaluation of spinning fluff Immediately before winding of a drawn yarn of 550000 m, the number of fluffs per hour was measured with a fluff counting device (trade name DT-105, manufactured by Toray Engineering Co., Ltd.) and evaluated according to the following criteria. did.

A: The number of fluffs measured is 0. ○: The number of fluffs measured is 1-5. X: The number of fluffs measured is 6 or more.

・ Evaluation of tar dirt on godet roller (tar dirt in Table 5)
After continuously operating for 30 days under the spinning conditions described above, the dirt state due to tar on the surfaces of the first godet roller and the second godet roller was visually observed and evaluated according to the following criteria.

◎: Almost tar dirt on the godet roller is hardly recognized. ○: Tar dirt on the godet roller is slightly recognized. X: Tar dirt on the godet roller is clearly recognized.

・ Evaluation of cleanability of tar dirt on godet roller (determination of tar dirt in Table 5)
After evaluating the tar stain on the godet roller, the surface of the godet roller was covered with a cloth soaked with a godet roller detergent, and left for 30 minutes. The cloth was removed after standing, and the adhered tar on the godet roller was wiped off with another cloth, and finally washed with water. At this time, the detergency of tar dirt was evaluated according to the following criteria.

◎: Tar dirt on the godet roller can be easily cleaned ○: Tar dirt on the godet roller can be cleaned, but a little work is required ×: Extremely clean of tar dirt on the godet roller It takes time and is problematic in practice

-Evaluation of dyeing spots Using the drawn yarn evaluated for the above-mentioned spinning fluff, a knitted fabric having a diameter of 70 mm and a length of 1.2 m was prepared with a cylindrical knitting machine. The produced knitted fabric was dyed by a high-pressure dyeing method using a disperse dye (trade name Kayalon Polyester Blue EBL-E manufactured by Nippon Kayaku Co., Ltd.). The dyed knitted fabric is washed with water, reduced, washed and dried according to a conventional method, then attached to an iron tube having a diameter of 70 mm and a length of 1 m, and the number of darkly dyed portions on the surface of the knitted fabric is counted with the naked eye. The stained spots were evaluated.

A: There is no deeply dyed portion. ○: There are 1 to 7 darkly dyed portions.

・ Evaluation of generated electricity in post-processing process (static electricity in Table 5)
The yarn was rewound using the drawn yarn evaluated for the spinning fluff to obtain a cheese having a yarn amount of 200 g. The cheese was conditioned for 3 days in an atmosphere of 20 ° C. and a relative humidity of 40%, and the generated electricity was measured and evaluated under the following conditions. In an atmosphere of 20 ° C and relative humidity of 40%, 20 cheeses were placed on a creel stand, the yarn was unwound, and after passing through a washer tensor, the entrance angle and exit angle were adjusted to 10 degrees. And 3 alumina pins having a length of 5 cm were brought into contact with each other and wound up at a speed of 200 m / min. At this time, the static electricity (generated electricity) of the traveling sheet of 20 filaments was measured by a collecting potential measuring device at a position 20 cm from the third alumina pin. The measured value was evaluated according to the following criteria. The results are summarized in Table 5.

A: The generated electricity is less than 0.5 kV and the antistatic property is excellent. O: The generated electricity is 0.5 kV or more and less than 2 kV, and the antistatic property is good. X: The generated electricity is 2 kV or more. And anti-static property is bad

  Table 5 summarizes the contents and evaluation results of the aqueous emulsion of the synthetic fiber treating agent prepared in each of the above examples.

  As is clear from the results of Table 5 corresponding to Table 4, according to the present invention, the aqueous solution of the synthetic fiber treating agent itself retains long-term stability even in winter, and the synthetic fiber using such an aqueous solution is used. In the spinning and drawing process, the amount of tar dirt generated on the godet roller is small, the tar dirt is easy to clean, the problem of spinning fluff, the occurrence of dyeing spots, and the generation of static electricity in the post-processing process is sufficient. There is an effect that can be deterred.

Claims (9)

A synthetic fiber treatment containing 20 to 85% by mass of the following smoothing agent, 5 to 70% by mass of the following nonionic surfactant, and 1 to 20% by mass (100% by mass in total) of the following antistatic agent. an aqueous solution of agent consisting of water synthetic fiber-processing agent, relative to 100 parts by weight of treating agent for synthetic fibers in a proportion of 3 to 20 parts by weight of water, that obtained by and ICP emission spectrometry aqueous solution of synthetic fiber-processing agent total concentration of Ca Rushiumuion and magnesium ions equal to or less than 0.5 mg / kg.
Smoothing agent: Liquid paraffin oil and / or ester compound Nonionic surfactant: Ether type nonionic surfactant having a polyoxyalkylene group in the molecule Antistatic agent: Organic fatty acid salt, organic phosphate ester salt, organic sulfonate salt, At least one selected from organic sulfate salts, organic quaternary ammonium salts, organic amine oxides, organic alanine compounds, and organic betaine compounds The aqueous liquid of the treating agent for synthetic fibers according to claim 1, wherein the smoothing agent contains liquid paraffin oil having a kinematic viscosity at 30 ° C of 1 to 500 mm ² / s. The aqueous liquid of the treating agent for synthetic fibers according to claim 1, wherein the smoothing agent contains liquid paraffin oil having a kinematic viscosity at 30 ° C of 1 to 200 mm ² / s.   The aqueous solution of the treating agent for synthetic fibers according to any one of claims 1 to 3, wherein the smoothing agent contains an ester compound having 10 to 100 carbon atoms.   The aqueous solution of the treating agent for synthetic fibers according to any one of claims 1 to 3, wherein the smoothing agent contains an ester compound having 20 to 70 carbon atoms.   A synthetic fiber treating agent containing 30 to 75% by weight of a smoothing agent, 10 to 60% by weight of a nonionic surfactant and 2 to 15% by weight (100% by weight in total) of an antistatic agent. The aqueous liquid of the processing agent for synthetic fibers according to any one of claims 1 to 5.   The aqueous liquid of the processing agent for synthetic fibers according to any one of claims 1 to 6, comprising water at a ratio of 5 to 15 parts by mass with respect to 100 parts by mass of the processing agent for synthetic fibers. A synthetic fiber treatment agent aqueous solution prepared by further diluting the synthetic fiber treatment agent aqueous solution according to any one of claims 1 to 7 with water, the synthetic fiber treatment agent 100 relative parts by weight of water in a proportion of 200 to 5,000 parts by weight, the total concentration of sought Luca Rushiumuion and magnesium ions by ICP emission spectrometry is not more than 0.5 mg / kg, and the dissolved oxygen in the emulsion The emulsion of the processing agent for synthetic fibers characterized by a density | concentration being 10 mg / L or less.   9. A synthetic fiber treatment method, wherein the synthetic fiber treatment agent emulsion according to claim 8 is attached to a synthetic fiber so as to be 0.1 to 3% by mass as a synthetic fiber treatment agent.