JP5881267B1 - Synthetic fiber treatment liquid and synthetic fiber treatment method - Google Patents

Abstract

An aqueous liquid of a treating agent for synthetic fiber itself maintains long-term stability even in winter, and the occurrence of jumping out, heater contamination, fluff and yarn breakage in the false twisting process of synthetic fiber to which the aqueous liquid is adhered. An aqueous liquid of a treating agent for synthetic fibers capable of sufficiently suppressing the above, a method for treating synthetic fiber using such an aqueous liquid, and a synthetic fiber obtained by such a treatment method are provided. An aqueous solution of a treating agent for synthetic fibers comprising a specific component in a specific ratio, wherein the total concentration of phosphate ion concentration, sulfate ion concentration and polyvalent metal cation is less than a specific value. An aqueous liquid of fiber treating agent was used. [Selection figure] None

Description

  The present invention relates to an aqueous solution of a treating agent for synthetic fibers and a method for treating synthetic fibers, and more specifically, the aqueous solution itself maintains long-term stability even in winter, and the synthetic fiber to which such an aqueous solution is attached is a false twisting step. The present invention relates to an aqueous solution of a treating agent for synthetic fibers that exhibits excellent process passability and a method for treating synthetic fibers using such an aqueous solution.

  Conventionally, as a processing agent for synthetic fibers to be subjected to a false twisting process, a compound containing a high molecular weight polyether compound and a quaternary ammonium salt (see, for example, Patent Document 1), a divalent fatty acid ester compound, an oxyethylene unit in the molecule A compound containing a divalent fatty acid ester compound, a polyether compound and an ethylene oxide adduct of a higher alcohol (for example, see Patent Document 2), a compound containing a quaternized alkylamine derivative and a smoothing agent (for example, see Patent Document 3) ), A nonionic surfactant, an ionic surfactant, an aliphatic ester compound and a polyether compound (see, for example, Patent Document 4), a specific three-component friction band between fibers A device in which the voltage is in a specific range (for example, see Patent Document 5) has been proposed. However, these conventional treatment agents for synthetic fibers have a problem that the stability in winter becomes insufficient when an aqueous solution is used, and the aqueous solution of the synthetic fiber treatment agent is adhered to the synthetic fibers. When the product is subjected to a false twisting process, jumping out is likely to occur, heater contamination is remarkable, and thus it is necessary to clean the heater in a short cycle, and there is a problem that there are many fuzz and yarn breakage.

JP-A-61-252370 JP 05-148766 A JP-A-10-183469 JP 2001-214372 A JP 2003-171879 A

  The problem to be solved by the present invention is that the aqueous solution of the treating agent for synthetic fibers itself maintains stability for a long time even in winter, jumping out in the false twisting process of synthetic fibers to which such an aqueous solution is adhered, heater contamination Another object of the present invention is to provide an aqueous solution of a synthetic fiber treating agent capable of sufficiently suppressing the occurrence of fluff and yarn breakage, and a synthetic fiber treatment method using such an aqueous solution.

  The present inventors have studied to solve the above problems, and as a result, an aqueous solution of a treatment agent for synthetic fibers in which water is mixed with a treatment agent for synthetic fibers containing a specific component, and having a phosphate ion concentration The inventors have found that a sulfate ion concentration and a total concentration of polyvalent metal cations of a specific value or less are correctly suitable.

  That is, the present invention includes 55 to 85% by mass of the following A component, 2 to 35% by mass of the following B component, 0.4 to 1.6% by mass of the following C component, and 6 to 15 of the following D component. It is an aqueous liquid of a treating agent for synthetic fibers in which water is blended in a proportion of 3 to 20 parts by mass with respect to 100 parts by mass of the treating agent for synthetic fibers formed in a proportion of mass% (total 100 mass%), The concentration of phosphate ions determined by ion chromatography is 200 mg / kg or less, and the concentration of sulfate ions determined by ion chromatography is 200 mg / kg or less. The present invention relates to an aqueous solution of a synthetic fiber treating agent having a total concentration of valent metal cations of 0.5 mg / kg or less. The present invention also relates to a method for treating synthetic fibers using an aqueous solution of the synthetic fiber treating agent.

  Component A: polyether compound represented by the following chemical formula 1 having a number average molecular weight of 1500 to 3000

In chemical formula 1,
A ¹ : monovalent hydrocarbon group, acyl group or hydrogen atom B ¹ : hydrogen of all hydroxyl groups from polyoxyalkylene glycol having a polyoxyalkylene group composed of oxyalkylene units having 2 to 4 carbon atoms in the molecule Residue excluding atoms T ¹ : monovalent hydrocarbon group, acyl group or hydrogen atom m: 1

Component B: at least one selected from the following polyether compounds represented by the following chemical formula 2 having a number average molecular weight of 5000 to 10,000 and the following polyether polyester compounds having a number average molecular weight of 3000 to 40000

In chemical formula 2,
A ² : monovalent hydrocarbon group, acyl group or hydrogen atom B ² : hydrogen of all hydroxyl groups from polyoxyalkylene glycol having a polyoxyalkylene group composed of oxyalkylene units having 2 to 4 carbon atoms in the molecule Residue excluding atom T ² : divalent or trivalent hydrocarbon group, or residue obtained by removing all hydroxyl groups from organic dicarboxylic acid n: 2 or 3 when T ² is a divalent or trivalent hydrocarbon group In the case where T ² is a residue obtained by removing all hydroxyl groups from an organic dicarboxylic acid, 2

  Polyether polyester compound: obtained by polycondensation reaction of the polyether polyester compound obtained by subjecting the following P component and the following Q component to a condensation polymerization reaction, and the following P component, the following Q component and the following R component. At least one selected from polyether polyesters

  P component: at least selected from aliphatic dicarboxylic acids having 4 to 22 carbon atoms, ester-forming derivatives obtained from aliphatic dicarboxylic acids having 4 to 22 carbon atoms, aromatic dicarboxylic acids and ester-forming derivatives of aromatic dicarboxylic acids One

  Q component: all having at least one selected from polyoxyalkylene monool, polyoxyalkylene diol and polyoxyalkylene triol having a polyoxyalkylene group composed of oxyalkylene units having 2 to 4 carbon atoms in the molecule

  R component: C2-C6 alkylene diol

  Component C: selected from quaternary ammonium salts, organic amine oxides, amphoteric compounds, fatty acid salts, organic sulfonates, organic sulfates and organic phosphate esters, and organic sulfonates and organic phosphates Contains salt

  Component D: (Poly) oxyalkylene adduct having a number average molecular weight of 118 to 650 obtained by adding an alkylene oxide having 2 to 4 carbon atoms to an aliphatic monohydric alcohol having 4 to 22 carbon atoms

  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 contains 55 to 85% by mass of the A component, 2 to 35% by mass of the B component, 0.4 to 1.6% by mass of the C component, and 6 to the D component. It is an aqueous liquid of a treating agent for synthetic fibers in which water is blended at a ratio of 3 to 20 parts by mass with respect to 100 parts by mass of the treating agent for synthetic fibers contained at a ratio of ˜15% by mass (total 100% by mass). The concentration of phosphate ions determined by ion chromatography is 200 mg / kg or less, and the concentration of sulfate ions determined by ion chromatography is 200 mg / kg or less, which is further determined by ICP emission spectrometry. The aqueous solution of the treating agent for synthetic fibers has a total concentration of polyvalent metal cations of 0.5 mg / kg or less.

The component A used for the synthetic fiber treating agent in the aqueous liquid of the present invention is a polyether compound having a number average molecular weight of 1500 to 3000 represented by Chemical Formula 1 as described above. In the polyether compound represented by Chemical Formula 1, A ^{1 in} Chemical Formula ¹ is a monovalent hydrocarbon group, an acyl group, or a hydrogen atom. The A ^1, 1) methyl, ethyl, propyl, butyl group, octyl group, a vinyl group, a butenyl group, a monovalent aliphatic hydrocarbon group having 1 to 18 carbon atoms such as hexadecenyl group, 2) phenoxy Group, monovalent hydrocarbon group having an aromatic ring such as propylphenoxy group, octylphenoxy group, benzyl group, 3) acetyl group, propanoyl group, butanoyl group, hexanoyl group, heptanoyl group, octanoyl group, nonanoyl group, decanoyl group An aliphatic acyl group having 2 to 22 carbon atoms such as a hexadecanoyl group, an octadecanoyl group, a hexadecenoyl group, an eicosenoyl group, and an octadecenoyl group, and 4) an acyl group having an aromatic ring such as a benzoyl group, a toluoyl group, and a naphthoyl group. 5) A hydrogen atom etc. are mentioned.

  The number average molecular weight of each component constituting the treating agent for synthetic fibers in the aqueous liquid of the present invention can be determined by a conventional method as a polystyrene equivalent value by GPC.

In the polyether compound represented by Chemical Formula 1, B ^{1 in} Chemical Formula ¹ is a polyoxyalkylene group composed of oxyalkylene units having 2 to 4 carbon atoms such as oxyethylene units, oxypropylene units, and oxybutylene units in the molecule. It is the residue remove | excluding the hydrogen atom of all the hydroxyl groups from the polyoxyalkylene glycol which has this.

In the polyether compound represented by Chemical Formula 1, T ^{1 in} Chemical Formula ¹ is a monovalent hydrocarbon group, an acyl group, or a hydrogen atom. The T ^1, 1) methyl alcohol, butyl alcohol, octyl alcohol, lauryl alcohol, stearyl alcohol, ceryl alcohol, isobutyl alcohol, 2-ethylhexyl alcohol, iso-dodecyl alcohol, iso-hexadecyl alcohol, isostearyl alcohol, iso tetracosadione sulfonyl Alcohol, 2-propyl alcohol, 12-eicosyl alcohol, vinyl alcohol, butenyl alcohol, hexadecenyl alcohol, oleyl alcohol, eicosenyl alcohol, 2-methyl-2-propylene-1-ol, 6-ethyl- It is a residue obtained by removing a hydroxyl group from a monovalent aliphatic hydroxy compound having 1 to 40 carbon atoms such as 2-undecen-1-ol, 2-octen-5-ol, and 15-hexadecene-2-ol. Hydrocarbon group, 2) Hydrocarbon group that is a residue obtained by removing a hydroxyl group from a monovalent hydroxy compound having an aromatic ring such as phenol, propylphenol, octylphenol, tridecylphenol, etc. 3) Acetic acid, butyric acid, propionic acid, capron Carbon such as acid, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, 2-ethylhexanoic acid, isostearic acid, myristoleic acid, palmitoleic acid, oleic acid, linoleic acid, erucic acid Examples include acyl groups, which are residues obtained by removing all hydroxyl groups from fatty acids of formula 2 to 22, and 4) hydrogen atoms.

  In the polyether compound represented by Chemical Formula 1, m in Chemical Formula 1 is 1.

  The B component used for the synthetic fiber treating agent in the aqueous liquid of the present invention includes the polyether compound represented by Chemical Formula 2 having a number average molecular weight of 5000 to 10,000 and the polyether polyester compound having a number average molecular weight of 3000 to 40000. At least one selected.

In the polyether compound represented by Chemical formula 2, A ^{2 in} Chemical formula ² is a monovalent hydrocarbon group, acyl group or hydrogen atom. The A ^2, 1) methyl, ethyl, propyl, butyl group, octyl group, a vinyl group, a butenyl group, a monovalent aliphatic hydrocarbon group having 1 to 18 carbon atoms such as hexadecenyl group, 2) phenoxy Group, monovalent hydrocarbon group having an aromatic ring such as propylphenoxy group, octylphenoxy group, benzyl group, 3) acetyl group, propanoyl group, butanoyl group, hexanoyl group, heptanoyl group, octanoyl group, nonanoyl group, decanoyl group An aliphatic acyl group having 2 to 22 carbon atoms such as a hexadecanoyl group, an octadecanoyl group, a hexadecenoyl group, an eicosenoyl group, and an octadecenoyl group, and 4) an acyl group having an aromatic ring such as a benzoyl group, a toluoyl group, and a naphthoyl group. 5) A hydrogen atom etc. are mentioned.

In the polyether compound represented by Chemical Formula 2, B ^{2 in} Chemical Formula 2 is a polyoxyalkylene group composed of oxyalkylene units having 2 to 4 carbon atoms such as oxyethylene units, oxypropylene units, and oxybutylene units in the molecule. It is the residue remove | excluding the hydrogen atom of all the hydroxyl groups from the polyoxyalkylene glycol which has this.

In the polyether compound represented by Chemical Formula 2, T ^{2 in} Chemical Formula ² is ethylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, 1,6-hexanediol, neo Divalent or trivalent hydrocarbon groups obtained by removing all hydroxyl groups from divalent or trivalent aliphatic hydroxy compounds such as pentyl glycol, glycerin, trimethylolpropane, or oxalic acid, glutaric acid, adipic acid, pimelic acid, suberic acid Aliphatic dicarboxylic acids such as azelaic acid, phthalic acid, isophthalic acid, terephthalic acid, 5-sulfoisophthalic acid salt, 2,6-naphthalenedicarboxylic acid, 2,3-naphthalenedicarboxylic acid, 1,4-naphthalenedicarboxylic acid, etc. It is a residue obtained by removing all hydroxyl groups from the organic dicarboxylic acid.

In the polyether compound represented by the formula 2, n in the formula ² is an integer of 2 or 3 when T ² is a divalent or trivalent hydrocarbon group, and T ² is a residue obtained by removing all hydroxyl groups from the organic dicarboxylic acid. In the case of a group, it is 2.

  The polyether polyester compound is obtained by polycondensation reaction of the polyether polyester compound obtained by subjecting the P component and the Q component to a polycondensation reaction, and the P component, the Q component, and the R component. It is at least one selected from the polyether polyester obtained.

  In the polyether polyester compound, the P component is an aliphatic dicarboxylic acid having 4 to 22 carbon atoms, an ester-forming derivative obtained from an aliphatic dicarboxylic acid having 4 to 22 carbon atoms, an aromatic dicarboxylic acid, and an ester formation of an aromatic dicarboxylic acid. It is at least one selected from sex derivatives.

  As P component, 1) C4-C22 aliphatic such as succinic acid, adipic acid, azelaic acid, sebacic acid, α, ω-dodecanedicarboxylic acid, dodecenylsuccinic acid, octadecenyldicarboxylic acid, cyclohexanedicarboxylic acid, etc. 2) ester-forming derivatives obtained from aliphatic dicarboxylic acids having 4 to 22 carbon atoms of 1), such as dimethyl succinate, dimethyl adipate, dimethyl azelate, dimethyl sebacate, etc. 3) phthalic acid, isophthalic acid Acids, terephthalic acid, 5-sulfoisophthalate, 2,6-naphthalenedicarboxylic acid, 2,3-naphthalenedicarboxylic acid, aromatic dicarboxylic acids such as 1,4-naphthalenedicarboxylic acid, 4) dimethyl phthalate, isophthalic acid Dimethyl, dimethyl terephthalate, 5-sulfoisophthalic acid dimethyl salt, 2,6 -Ester-forming derivatives of aromatic dicarboxylic acids of the above 3) such as dimethyl naphthalenedicarboxylate, diethyl 2,6-naphthalenedicarboxylate, dimethyl 1,4-naphthalenedicarboxylate and the like.

  In the polyether polyester compound, the Q component has a polyoxyalkylene group composed of oxyalkylene units having 2 to 4 carbon atoms such as oxyethylene units, oxypropylene units, and oxybutylene units in the molecule. It is at least one selected from alkylene monool, polyoxyalkylene diol, and polyoxyalkylene triol.

  Examples of the polyoxyalkylene monool include those obtained by blocking one end of a polyoxyalkylene diol as described later with a monovalent hydrocarbon group. Examples of such monovalent hydrocarbon groups are 1) aliphatic carbon atoms having 1 to 22 carbon atoms such as methyl group, ethyl group, butyl group, n-octyl group, lauryl group, stearyl group, isopropyl group and 2-ethylhexyl group. Examples thereof include a hydrogen group, 2) a hydrocarbon group having an aromatic ring such as a phenyl group, a monobutylphenyl group, an octylphenyl group, and a nonylphenyl group.

  Examples of the polyoxyalkylene diol include alkylene having 2 to 6 carbon atoms such as ethylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, 1,6-hexanediol, neopentyl glycol, and the like. Examples of the diol include addition reaction of alkylene oxide having 2 to 4 carbon atoms.

  Examples of polyoxyalkylene triols include those obtained by addition reaction of alkylene oxides having 2 to 4 carbon atoms to alkylene triols having 2 to 6 carbon atoms such as glycerin and trimethylolpropane.

  In the polyether polyester compound, the R component is an alkylene diol having 2 to 6 carbon atoms. Examples of the R component include alkylene diols having 2 to 6 carbon atoms such as ethylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, 1,6-hexanediol, and neopentyl glycol. Is mentioned.

  The C component used for the synthetic fiber treating agent in the aqueous liquid of the present invention is selected from quaternary ammonium salts, organic amine oxides, amphoteric compounds, fatty acid salts, organic sulfonates, organic sulfates, and organic phosphate esters. However, two or more selected from these are preferable, and those containing an organic sulfonate salt and an organic phosphate ester salt are particularly preferable.

  Examples of the quaternary ammonium salt generally include those composed of a quaternary ammonium cation group and an anion group. As one quaternary ammonium cation group, 1) a quaternary ammonium cation group when the organic group 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 each of the organic groups bonded to the nitrogen atom is a hydroxyalkyl group having 1 to 6 carbon atoms. Quaternary ammonium cation group, 4) quaternary ammonium cation when 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 remaining part is a hydroxyalkyl group having 1 to 6 carbon atoms 6) a quaternary ammonium cation group in which a 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 and the remainder is a C1-C6 hydroxyalkyl group among the couple | bonded organic groups is 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.

  Any of the quaternary ammonium salts described above can be synthesized by a known method. For example, 1) a method of reacting a corresponding tertiary amine with a trialkyl phosphate ester, 2) a method of reacting a corresponding tertiary amine with a dialkyl sulfuric acid, and 3) water corresponding to the corresponding tertiary amine. Method of reacting ethylene oxide in the presence to form quaternary ammonium hydroxide and then reacting with sulfonate ester 4) After reacting corresponding tertiary amine and alkyl halide to form quaternary ammonium halide Examples thereof include a method of reacting a carboxylic acid metal salt.

  As the organic amine oxide of component C, 1) dimethylethylamine oxide, dimethylpropylamine oxide, dimethylhexylamine oxide, dimethyloctylamine oxide, dimethylnonylamine oxide, dimethyllaurylamine oxide, dimethylmyristylamine oxide, dimethylcetylamine oxide, Dimethylstearylamine oxide, dimethyleicosylamine 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 bonded 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, oleylamixone, linoleylamine oxide, eleostearylamine oxide, di-2-tetradecenylamine oxide, di-2-pentadecenylamine oxide, di-2-octa At least one of the aliphatic hydrocarbon groups bonded to the nitrogen atom such as decenylamine oxide, di15-hexadecenylamine oxide, dioleylamine oxide, dilinoleylamine oxide, dieleostearylamine oxide, etc. is carbon. Number 14-24 Organic amine oxide is an unsaturated aliphatic hydrocarbon group.

  As the amphoteric compound of component C, 1) a betaine-type amphoteric compound having at least one hydrocarbon group having 8 to 22 carbon atoms in the molecule, and 2) at least one hydrocarbon group having 8 to 22 carbon atoms in the molecule. And alanine-type amphoteric compounds.

  Specific examples of such betaine-type amphoteric compounds include octyldimethylammonioacetate, decyldimethylammonioacetate, dodecyldimethylammonioacetate, hexadecyldimethylammonioacetate, octadecyldimethylammonioacetate, nonadecyldimethyl. Ammonioacetate, octadecenyldimethylammonioacetate, dodecylaminopropyldimethylammonioacetate, octadecylaminopropyldimethylammonioacetate, octadecenylaminopropyldimethylammonioacetate, etc. Examples of alanine-type amphoteric compounds include N, N-bis (2-carboxyethyl) -octylamine, N, N-bis (2-carboxyethyl) -dodecylamine, N, N-bis (2-cal Xylethyl) -tetradecylamine, N, N-bis (2-carboxyethyl) -hexadecylamine, N, N-bis (2-carboxyethyl) -octadecylamine, N- (2-carboxyethyl) -dodecylamine, N- (2-carboxyethyl) -octadecylamine etc. are mentioned.

  Examples of the fatty acid salt of component C 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. It is done. 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. .

  Examples of the alkali metal that forms the alkali metal salt of fatty acid as described above include sodium and potassium. Examples of amines that form amine salts include 1) aliphatic amines such as methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, butylamine, dibutylamine, tributylamine, octylamine, and 2) aniline, Aromatic amines and heterocyclic amines such as pyridine, morpholine, piperazine and their derivatives, 3) monoethanolamine, diethanolamine, triethanolamine, isopropanolamine, diisopropanolamine, triisopropanolamine, butyldiethanolamine, octyldiethanolamine, And alkanolamines such as lauryldiethanolamine, and 4) ammonia.

  Further, as the phosphonium group forming the phosphonium salt of fatty acid as described above, 1) tetramethylphosphonium, tetraethylphosphonium, tetrabutylphosphonium, trimethylethylphosphonium trimethylpropylphosphonium, trimethyloctylphosphonium, trimethyldodecylphosphonium, trimethyloctadecylphosphonium, etc. Phosphonium group in which all organic groups bonded to phosphorus 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 below.

  As the organic sulfonate of component C, 1) an organic sulfonic acid alkali metal salt having 6 to 22 carbon atoms, 2) an organic sulfonic acid amine salt having 6 to 22 carbon atoms, and 3) an organic sulfonic acid having 6 to 22 carbon atoms. A phosphonium salt etc. are mentioned. As the organic sulfonic acid having 6 to 22 carbon atoms constituting the organic sulfonate, 1) alkyl sulfonic acid such as decyl sulfonic acid, dodecyl sulfonic acid, isotridodecyl sulfonic acid, tetradecyl sulfonic acid, hexadecyl sulfonic acid, etc. 2) Alkyl aryl sulfonic acids such as butyl benzene sulfonic acid, dodecyl benzene sulfonic acid, octadecyl benzene sulfonic acid, dibutyl naphthalene sulfonic acid, etc. 3) Dioctyl sulfosuccinic acid ester, dibutyl sulfosuccinic acid ester, dodecyl sulfoacetic acid ester, nonylphenoxypolyethylene glycol Examples thereof include ester sulfonic acids such as sulfoacetic acid esters.

  Further, 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 fatty acid salt.

  As organic sulfates of component C, 1) Alkyl sulfate alkali metal salts such as sodium decyl sulfate, sodium dodecyl sulfate, lithium tetradecyl sulfate, potassium hexadecyl sulfate, and 2) natural fats and oils such as beef tallow sulfated oil, castor oil sulfated oil, etc. Examples include alkali metal salts of sulfur oxides.

  As the organic phosphate ester salt of component C, 1) an alkyl phosphate ester alkali metal salt having an alkyl group having 4 to 22 carbon atoms, 2) an alkyl group having 4 to 22 carbon atoms and (poly) oxy (Poly) oxyalkylene alkyl ether phosphate alkali metal salt having 1 to 5 oxyalkylene units constituting the alkylene group, 3) alkyl phosphate amine salt having 4 to 22 carbon atoms in the alkyl group 4) a (poly) oxyalkylene alkyl ether phosphate amine 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; Can be mentioned.

  Examples of the alkyl phosphate alkali metal salts having 4 to 22 carbon atoms of 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 alkali metal salt, isooctyl phosphate alkali metal salt, 2-ethylhexyl phosphate alkali metal salt, decyl phosphate alkali metal salt, dodecyl phosphate alkali metal salt, tridecyl phosphate alkali metal salt, myristyl Phosphate ester alkali metal salt, cetyl phosphate ester alkali metal salt, stearyl phosphate ester alkali metal salt, eicosyl phosphate ester alkali metal salt, behenyl phosphate ester alkali gold Salts 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 There are isomers (symmetrical diesters) and diesters having different alkyl groups (asymmetrical diesters).

  The alkali metals constituting these alkyl phosphate alkali metal salts are the same as those described above for the fatty acid salts.

  As 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 , Polyoxyalkylene 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, polyoxy Alkylene 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, polyoxyalkylene 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. 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. There are diesters having groups (symmetrical diesters) and diesters having different alkyl groups (asymmetrical diesters).

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

  The alkyl phosphate amine salt wherein the alkyl group has 4 to 22 carbon atoms, and the alkyl group has 4 to 22 carbon atoms and the number of oxyalkylene units constituting the (poly) oxyalkylene group is 1 to Regarding the amine in the five (poly) oxyalkylene alkyl ether phosphate amine salts, it is the same as described above for the fatty acid salts.

  In addition to the organic phosphates described above, the organic phosphate ester salt of component C contains components such as alkali metal monooctyl pyrophosphate, alkali metal dioctyl pyrophosphate, tetraalkali metal pyrophosphate, tripolyphosphoric acid, etc. However, these components are preferably as small as possible.

  The D component used for the synthetic fiber treating agent in the aqueous liquid of the present invention has a number average molecular weight of 118 to 650, which is obtained by adding an alkylene oxide having 2 to 4 carbon atoms to an aliphatic monohydric alcohol having 4 to 22 carbon atoms. Poly) oxyalkylene adduct. Examples of aliphatic monohydric alcohols having 4 to 22 carbon atoms that form D component include butyl alcohol, hexyl alcohol, octyl alcohol, nonyl alcohol, decyl alcohol, undecyl alcohol, dodecyl alcohol, tridecyl alcohol, tetradecyl Alcohol, pentadecyl alcohol, hexadecyl alcohol, hexadecenyl alcohol, heptadecyl alcohol, octadecyl alcohol, octadecenyl alcohol, nonadecyl alcohol, eicosyl alcohol, eicosenyl alcohol, docosyl alcohol, 2-ethylhexyl alcohol 3,5,5-trimethylhexyl alcohol and the like, and examples of the alkylene oxide having 2 to 4 carbon atoms include ethylene oxide, propylene oxide, 1 2-butylene oxide, 1,4-butylene oxide, and the like. Two or more kinds of these alkylene oxides can be used. In this case, examples of the addition form of the alkylene oxide to the aliphatic monohydric alcohol having 4 to 22 carbon atoms include random addition, block addition, and random block addition. .

  The aqueous liquid of the present invention has a phosphate ion concentration determined by ion chromatography of 200 mg / kg or less, and a sulfate ion concentration determined by ion chromatography of 200 mg / kg or less. . There is no restriction | limiting in the measurement conditions of an ion chromatograph method, It can obtain | require by a well-known method. For example, a sample obtained by uniformly adding distilled water or ultrapure water and, if necessary, a water-soluble organic solvent to a synthetic fiber treating agent aqueous solution, is included in the synthetic fiber treating agent aqueous solution. And a method for measuring the amount of phosphate ions and sulfate ions.

  To reduce the phosphate ion concentration and sulfate ion concentration in the aqueous liquid to 200 mg / kg or less, control the phosphate ion and sulfate ion concentrations in the lubricant and antistatic agent used in the fiber treatment agent. However, the method is not particularly limited, and a known method can be adopted.

  In the treatment agent for synthetic fibers, a polyether compound is often used as a lubricant in order to impart lubricity. Conventionally, an alkaline catalyst such as potassium hydroxide or triethylamine has been used as a catalyst for synthesizing a polyether compound. However, if these catalysts remain used as a treating agent for synthetic fibers, these catalysts are used. Not only do yarn breakage and fluffing occur in the spinning process due to hydrolysis, coloring, etc. derived from the yarn, but also adversely affects the yarn quality after spinning.

  For this reason, these alkaline catalysts are often neutralized with phosphoric acid or sulfuric acid. However, when neutralized, a large amount of phosphate ions and sulfate ions remain in the polyether compound. It is necessary to perform a catalyst removal step such as adsorption treatment of the neutralized salt or filtration treatment. Phosphoric acid or sulfuric acid is not used for neutralization of the catalyst, or when used, phosphoric acid remaining in the aqueous solution of the treating agent for synthetic fibers by performing the catalyst removal step or reducing the amount used as much as possible The amount of ions and sulfate ions can be reduced.

  In addition, an anionic compound is often used as the antistatic agent in the synthetic fiber treatment agent in order to impart antistatic properties. In general, the antistatic agent is rarely used alone, and in consideration of the characteristics, the antistatic agent is often used in combination of two or more antistatic agents. For example, when an organic sulfonate is used as the ionic compound, a sulfate may be mixed as a by-product in the organic sulfonate. If this is used as an antistatic agent as it is, sulfate ions may be mixed in the synthetic fiber treating agent at 200 mg / kg or more. For this reason, it is necessary to remove by-product sulfate by filtration or the like, or to reduce the amount used as much as possible.

  Further, when an organic phosphate salt is used as the anionic compound, an inorganic phosphate may be mixed as a by-product in the organic phosphate salt. If this is used as an antistatic agent as it is, phosphate ions may be mixed in the synthetic fiber treating agent at 200 mg / kg or more. For this reason, it is necessary to reduce the usage amount as much as possible or to remove the by-product phosphate by a method such as ion exchange treatment, recrystallization treatment, or adsorption treatment.

  Although the above method is mentioned as a method of setting the phosphate ion and sulfate ion concentration in the aqueous solution of the synthetic fiber treatment agent to 200 mg / kg or less, the amount of organic phosphate ester salt and organic sulfonate can be used. The method of reducing as much as possible is preferable.

  The aqueous liquid of the present invention has a total concentration of polyvalent metal cations determined by ICP emission analysis of 0.5 mg / kg or less. There is no restriction | limiting in the measurement conditions of ICP emission spectrometry, and it can obtain | require by a well-known method. For example, use a sample that is uniformly dissolved by adding distilled water or ultrapure water and, if necessary, a water-soluble organic solvent to an aqueous solution of a synthetic fiber treatment agent, and compare it with a standard sample of a polyvalent metal cation. By this, the method etc. which measure the total amount of the polyvalent metal cation contained in the aqueous | water-based liquid of the processing agent for synthetic fibers are mentioned.

  In order to reduce the total concentration of polyvalent metal cations in the aqueous liquid to 0.5 mg / kg or less, it is necessary to control the concentration of the polyvalent metal cations contained in the lubricant and antistatic agent used in the processing agent for synthetic fibers. However, the method is not particularly limited, and a known method can be adopted.

  For example, for polyether compounds used as lubricants for synthetic fiber treating agents, when calcium hydroxide or magnesium hydroxide is used as a catalyst for synthesizing the polyether compounds, these are adsorbed after the reaction. The method of removing by is mentioned.

  In the case where the polyether ester compound has a high viscosity and is difficult to remove by an adsorbent alone, it may be mixed with another polyether compound having a low viscosity and then removed by an adsorbent or the like.

  In addition, as for the anionic compound used as the antistatic agent for the treating agent for synthetic fiber, if the polyvalent metal cation is not selected, or if the polyvalent metal cation is used in the synthesis process, the polyvalent metal cation The method of removing a metal cation with an adsorbent etc. is mentioned.

  On the other hand, water is used when preparing an aqueous solution of a treating agent for synthetic fibers, and generally used water contains a large amount of polyvalent metal cations as a natural mineral component. For example, general tap water in Japan contains a total of 10 mg / kg or more of polyvalent metal cations such as calcium and magnesium. In some cases, the total concentration of metal cations cannot be reduced to 0.5 mg / kg or less.

  For this reason, it is necessary to reduce the amount of water used 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, a treatment with an ion exchange resin, etc., but there is no particular limitation on the removal method, and a known method can be adopted. Among them, a method of adsorbing the water used when preparing the aqueous solution of the synthetic fiber treating agent with an ion exchange resin is preferable.

  As polyvalent metal cations, 1) magnesium ion, calcium ion, strontium ion, barium ion, cadmium ion, nickel (II) ion, zinc ion, copper (II) ion, mercury (II) ion, iron (II) ion , Cobalt (II) ion, tin (II) ion, lead (II) ion, manganese (II) ion, tetraammine zinc (II) ion, tetraammine copper (II) ion, tetraaqua copper (II) ion, thiocyanide iron ( III) ions, divalent metal cations such as hexaamminenickel (II) ions, 2) aluminum ions, iron (III) ions, chromium (III) ions, hexaamminecobalt (III) ions, hexaaquacobalt (III) Ion, hexaammine chromium (III) Examples include trivalent metal cations such as ON, and 3) tetravalent metal cations such as tin (IV) ions and manganese (IV) ions, among which calcium ions and / or magnesium ions are most easily mixed. It is a polyvalent metal cation, and it is particularly preferable to conduct analysis while paying attention to these.

  The treating agent for synthetic fibers in the aqueous liquid of the present invention is 55 to 85% by mass of component A described above, 2 to 35% by mass of component B, 0.4 to 1.6% by mass of component C and D component. Is contained in a proportion of 6 to 15% by mass (total of 100% by mass), but preferably further contains an E component.

  E component used for the processing agent for synthetic fibers in the aqueous liquid of the present invention is an ester compound having 17 to 60 carbon atoms obtained by esterification reaction of a monovalent aliphatic alcohol and a monovalent or divalent fatty acid, 1 to An ester compound having a number average molecular weight of 300 to 650 and a monovalent compound obtained by esterification of a (poly) oxyalkylene adduct obtained by adding an alkylene oxide having 2 to 4 carbon atoms to a hexavalent aliphatic alcohol and a monovalent fatty acid At least one selected from ester compounds having a number average molecular weight of 300 to 650 obtained by an esterification reaction of a (poly) oxyalkylene adduct obtained by adding an alkylene oxide having 2 to 4 carbon atoms to an aliphatic alcohol and a divalent fatty acid. Among them, the number of carbon atoms obtained by esterification reaction of a monovalent aliphatic alcohol and a monovalent or divalent fatty acid is 2 A number average molecular weight of 300 to 630 obtained by an esterification reaction of a (poly) oxyalkylene adduct obtained by adding an alkylene oxide having 2 to 4 carbon atoms to an ester compound of .about.36 and a monovalent aliphatic alcohol and a monovalent fatty acid. It is preferable that it is at least one selected from these ester compounds.

  Monovalent aliphatic alcohols that form ester compounds having 17 to 60 carbon atoms as the E component include methanol, ethanol, butanol, 2-ethylhexanol, lauryl alcohol, palmityl alcohol, palmitoleyl alcohol, stearyl. Alcohol, isostearyl alcohol, oleyl alcohol, behenyl alcohol, etc. are mentioned, and mono- or divalent fatty acids include acetic acid, butyric acid, caproic acid, caprylic acid, capric acid, undecanoic acid, lauric acid, tridecanoic acid, myristic acid, Pentadecanoic acid, palmitic acid, stearic acid, nonadecanoic acid, arachidic acid, behenic acid, serotic acid, montanic acid, melicic acid, Linderic acid, palmitoleic acid, oleic acid, elaidic acid, vaccenic acid, linoleic acid, linoleic acid Acid, arachidonic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, pentadecenyl succinic acid.

  Specifically, examples of the ester compound having 17 to 60 carbon atoms as the E component include lauryl oleate, stearyl oleate, oleyl oleate, octyl oleate, tridecyl oleate, methyl oleate, butyl oleate, 2- Ethylhexyl oleate, oleyl stearate, oleyl palmitate, oleyl laurate, oleyl isostearate, oleyl octanoate, octyl stearate, dilauryl malonate, dilauryl succinate, dilauryl glutarate, dilauryl adipate, dilauryl pimelate, Dilauryl suberate, dilauryl azelate, dilauryl sebacate, distearyl glutarate, distearyl adipate, distearyl pimelate, distearyl suberate, distearyl azelate Examples include distearyl sebacate, lauryl oleate, stearyl oleate, oleyl oleate, octyl oleate, tridecyl oleate, butyl oleate, 2-ethylhexyl oleate, oleyl stearate, oleyl palmitate , Oleyl laurate, oleyl isostearate, oleyl octanoate, octyl stearate, dilauryl malonate, dilauryl succinate, dilauryl glutarate, dilauryl adipate, dilauryl pimelate, dilauryl suberate, dilauryl azelate, dilauryl sebacate Ester compounds having 22 to 36 carbon atoms, such as, are preferred.

  Number average molecular weight of 300 to 650 obtained by esterification reaction of (poly) oxyalkylene adduct obtained by adding alkylene oxide of 2 to 4 carbon atoms to 1 to 6 valent aliphatic alcohol as E component and monovalent fatty acid As 1 to 6 valent aliphatic alcohols that will form the ester compounds of: 1) methanol, ethanol, butanol, 2-ethylhexanol, lauryl alcohol, palmityl alcohol, palmitoleyl alcohol, stearyl alcohol, isostearyl alcohol , Monovalent aliphatic alcohols such as oleyl alcohol and behenyl alcohol, 2) 2 to 6 valences such as ethylene glycol, propylene glycol, butanediol, hexanediol, glycerin, trimethylolpropane, sorbitol, pentaerythritol Examples include aliphatic alcohols, among which monovalent fats such as methanol, ethanol, butanol, 2-ethylhexanol, lauryl alcohol, palmityl alcohol, palmitoleyl alcohol, stearyl alcohol, isostearyl alcohol, oleyl alcohol, and behenyl alcohol. Group alcohols are preferred. Examples of the alkylene oxide having 2 to 4 carbon atoms include ethylene oxide, propylene oxide, 1,2-butylene oxide, 1,4-butylene oxide and the like. Furthermore, monovalent fatty acids include acetic acid, butyric acid, caproic acid, caprylic acid, capric acid, undecanoic acid, lauric acid, tridecanoic acid, myristic acid, pentadecanoic acid, palmitic acid, stearic acid, nonadecanoic acid, arachidic acid, behenic acid , Serotic acid, montanic acid, melissic acid, Linderic acid, palmitoleic acid, oleic acid, elaidic acid, vaccenic acid, linoleic acid, linolenic acid, arachidonic acid and the like.

  Specifically, as the ester compound as the E component, an ester compound of 1 mol of a compound obtained by adding 5 mol of ethylene oxide to octyl alcohol and 1 mol of lauric acid, an ester compound of 1 mol of diethylene glycol and 2 mol of lauric acid, An ester compound of 1 mol of dipropylene glycol and 1 mol of stearic acid, an ester compound of 1 mol of 1,4-butanediol added with 2 mol of ethylene oxide and 1 mol of palmitic acid, and ethylene in 1,6-hexanediol Examples include an ester compound of 1 mole of a compound obtained by adding 2 moles of oxide and 1 mole of propylene oxide and 2 moles of lauric acid, an ester compound of 1 mole of a compound obtained by adding 3 moles of ethylene oxide to glycerol and 1 mole of lauric acid, and the like. It is ok among them (Poly) oxyalkylene addition in which a C2-C4 alkylene oxide is added to a monovalent aliphatic alcohol, such as an ester compound of 1 mol of a compound obtained by adding 5 mol of ethylene oxide to 1 alcohol and 1 mol of lauric acid An ester compound having a number average molecular weight of 300 to 630 obtained by esterification reaction of a product with a monovalent fatty acid is preferred.

  Ester having a number average molecular weight of 300 to 650 obtained by esterification reaction of a (poly) oxyalkylene adduct obtained by adding an alkylene oxide having 2 to 4 carbon atoms to a monovalent aliphatic alcohol as component E and a divalent fatty acid The monovalent aliphatic alcohol and the alkylene oxide having 2 to 4 carbon atoms that form the compound are the same as described above, and the divalent fatty acids include malonic acid, succinic acid, glutaric acid, adipine Examples include acids, pimelic acid, suberic acid, azelaic acid, sebacic acid, pentadecenyl succinic acid and the like.

  Specifically, as the ester compound as the E component, bis [alkoxypoly (oxyethylene)] = malonate, bis [alkoxypoly (oxyethylene)] = succinate, bis [alkoxypoly (oxyethylene)] = glutarate, Bis [alkoxypoly (oxyethylene)] = adipate, bis [alkoxypoly (oxyethylene)] = suberoate, bis [alkoxypoly (oxyethylene)] = azelaate, bis [alkoxypoly (oxyethylene)] = sevacoart, bis [ Alkoxypoly (oxypropylene)] = malonate, bis [alkoxypoly (oxypropylene)] = succinate, bis [alkoxypoly (oxypropylene)] = glutarate, bis [alkoxypoly (oxypropylene)] = adipo Bis [alkoxypoly (oxypropylene)] = suberoate, bis [alkoxypoly (oxypropylene)] = azelaate, bis [alkoxypoly (oxypropylene)] = sebacoate, bis [alkoxypoly (oxyethylene / oxypropylene) ] = Malonate, bis [alkoxy poly (oxyethylene oxypropylene)] = succinate, bis [alkoxy poly (oxyethylene oxypropylene)] = adipate, bis [alkoxy poly (oxyethylene oxypropylene)] = suberoate, bis [Alkoxypoly (oxyethylene / oxypropylene)] = azelaate, bis [alkoxypoly (oxyethylene / oxypropylene)] = sebacoate, etc. (Oxyethylene)] = Ajipoato, bis [alkoxy poly (oxyethylene)] = Suberoato, bis [alkoxy poly (oxyethylene)] = Azeraato, bis [alkoxy poly (oxyethylene)] = Sebakoato like.

  When the treatment agent for synthetic fibers in the aqueous liquid of the present invention further contains an E component in addition to the A component, the B component, the C component and the D component, the ratio of the E component is not particularly limited, but the A component is 55 ~ 85 mass%, B component is 2 to 35 mass%, C component is 0.4 to 1.6 mass%, D component is 6 to 15 mass%, and E component is 2 to 15 mass% (total 100 mass%) It is preferable to contain it in a proportion of

  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.

  When the amount of water is small, the hydrophilic component in the synthetic fiber treatment agent is likely to precipitate in winter, and the appearance is likely to change. On the other hand, when the amount of water is large, the moisture in the treatment agent for synthetic fibers tends to freeze in winter, and the appearance changes such as separation of the water phase and the oil phase.

  Next, 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 in which the aqueous liquid of the present invention is diluted as it is or further with water, and is made to adhere to 0.1 to 2% by mass as a synthetic fiber treatment agent to the synthetic fiber subjected to the false twisting step. is there.

  As with the water used for the preparation of the aqueous liquid of the present invention, the water used for dilution needs to remove polyvalent metal cations in water, and the total amount of polyvalent metal cations is preferably 1 mg / kg or less, What was made into 0.1 mg / kg or less is more preferable.

  Examples of the adhesion method include known methods such as a roller oiling method, a guide oiling method using a metering pump, an immersion oiling method, and a spray oiling method, but a roller oiling method or a guide oiling method using a metering pump is preferable.

  As the false twisting machine used in the false twisting process, 1) a contact heater type in which a heater having a heater temperature of 150 to 230 ° C. and a heater length of 150 to 250 cm is mounted and the synthetic fiber filament yarn runs while contacting the heater plate. False twisting machine, 2) Short heater type false twisting machine, etc., equipped with a heater having a heater temperature of 300 to 600 ° C. and a heater length of 20 to 150 cm, and a synthetic fiber filament running on the heater plate in a non-contact manner. .

  Synthetic fibers obtained by the treatment method of the present invention include 1) polyester having ethylene terephthalate as a main structural unit, 2) polyamide such as nylon 6 and nylon 66, 3) polyacryl such as polyacrylonitrile and modacrylic, and 4) polyethylene. Polyolefins such as polypropylene can be mentioned, but the effect is high when applied to polyester partially drawn yarn, polyamide partially drawn yarn, polyester direct spun drawn yarn, and the effect is exhibited when applied to cationic dyeable polyester. Is higher.

  According to the present invention described above, the aqueous solution of the synthetic fiber treating agent itself maintains long-term stability even in winter, and jumping out in the false twisting process of the synthetic fiber to which the aqueous solution is adhered, heater contamination, fluff In addition, there is an effect that the occurrence of yarn breakage can be sufficiently suppressed.

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

Test Category 1 (Synthesis of each component constituting the synthetic fiber treatment agent)
Synthesis of polyether compound (A-1) as component A A pressure vessel equipped with a stirrer and a thermometer was charged with 296 parts of butyl alcohol and 16 parts of potassium hydroxide, and the inside of the vessel was replaced with nitrogen. The temperature was raised to ° C. to dissolve potassium hydroxide. Under a nitrogen atmosphere, 3872 parts of ethylene oxide and 3886 parts of propylene oxide were simultaneously injected and reacted at a reaction temperature of 100 to 150 ° C. Further, after aging at 100 to 150 ° C. for 3 hours, adding 80 parts of an inorganic synthetic adsorbent (trade name Kyoward 600S manufactured by Kyowa Chemical Industry Co., Ltd.) and stirring and treating at 120 ° C. under a nitrogen stream for 2 hours, The catalyst and the synthetic adsorbent were removed by filtration to obtain a polyether compound (A-1) having a number average molecular weight of 2000.

-Synthesis | combination of the polyether compound (A-2 to A-6) as A component The polyether compound (A-2 to A-6) was synthesize | combined like the polyether compound (A-1).

-Synthesis | combination of the polyether compound (B-1 to B-7) as B component The polyether compound (B-1 to B-7) was synthesize | combined like the polyether compound (A-1).

・ Synthesis of polyetherester compound (B-8) as component B: adipic acid 29.2 parts, terephthalic acid 132.9 parts, oxyethylene unit / oxypropylene unit = 25/75 (ratio by mole) 1,200 parts of a polyoxyalkylene glycol having a number average molecular weight of 1200 having a polyoxyalkylene group bonded to 1, 0.54 parts of zinc acetate dihydrate and 0.13 parts of antimony trioxide are charged into a reaction vessel, and the inside of the reaction vessel is purged with nitrogen After that, the reaction vessel was sealed and heated to 200 ° C. over 2 hours. Further, the temperature was raised to 240 ° C. over 2 hours while removing by-product water in the reaction vessel out of the system. Thereafter, the pressure in the reaction vessel was gradually returned to normal pressure, the temperature was raised to 250 ° C., and esterification was performed for 1 hour to obtain an esterified product. Thereafter, a polyether polymerization compound having a number average molecular weight of 20000 is obtained by performing a condensation polymerization reaction at 220 to 250 ° C. for 60 minutes under a reduced pressure of 20 mmHg and further for 60 minutes at 250 to 280 ° C. under a reduced pressure of 0.8 to 0.6 mmHg. (B-8) was obtained.

-Synthesis | combination of the polyetherester compound (B-9 and B-10) as B component Polyetherester compound (B-9 and B-10) was synthesize | combined similarly to the polyetherester compound (B-8). .

Synthesis of (poly) oxyalkylene adduct (D-1 to D-5) as component D In the same manner as the polyether compound (A-1), (poly) oxyalkylene adduct (D-1 to D-5) ) Was synthesized.

・ Synthesis of (poly) oxyalkylene adduct (RD-1) corresponding to component D Into a pressure vessel equipped with a stirrer and a thermometer, 1345 parts of octadecenyl alcohol and 6 parts of potassium hydroxide were charged. Was replaced with nitrogen and heated to 100 ° C. to dissolve potassium hydroxide. Under a nitrogen atmosphere, 1760 parts of ethylene oxide was injected and reacted at a reaction temperature of 100 to 150 ° C. Further, after aging at 100 to 150 ° C. for 3 hours, the mixture was neutralized with 12.3 parts of 85% phosphoric acid to synthesize a (poly) oxyalkylene adduct (RD-1) having a number average molecular weight of 620. When the (poly) oxyalkylene adduct (RD-1) was measured by ion chromatography, the phosphate ion contained was 3200 mg / kg.

Synthesis of ester compound (E-4) as E component In a reaction vessel equipped with a thermometer, stirrer, dropping funnel and condenser, 1751 parts of α-octyl-ω-hydroxy (polyoxyethylene (5 mol)) and 1002 parts of dodecanoic acid and 14 parts of sulfuric acid as a catalyst were added, stirring was continued at 120 ° C. to 140 ° C. for 8 hours under reduced pressure, and the produced water was distilled off to complete the esterification reaction. After neutralizing the catalyst sulfuric acid with soda ash, 80 parts of an inorganic synthetic adsorbent (trade name Kyoword 600S manufactured by Kyowa Chemical Industry Co., Ltd.) was added, and the mixture was stirred at 120 ° C. under a nitrogen stream for 2 hours. The catalyst and the synthetic adsorbent were removed by filtration to obtain an ester compound (E-4) having a number average molecular weight of 530.

Synthesis of ester compounds (E-1 to E-3 and E-5 to E-7) as E component In the same manner as the ester compound (E-4), ester compounds (E-1 to E-3 and E -5 to E-7) were synthesized.

Synthesis of ester compound (RE-1) corresponding to component E: 1751 parts of α-octyl-ω-hydroxy (polyoxyethylene (5 mol)) in a reaction vessel equipped with a thermometer, stirrer, dropping funnel and condenser And 1002 parts of dodecanoic acid and 10 parts of sulfuric acid as a catalyst were added, stirring was continued at 120 ° C. to 140 ° C. for 8 hours under reduced pressure, and the produced water was distilled off to complete the esterification reaction. The catalyst sulfuric acid was neutralized with soda ash to obtain an ester compound (RE-1) having a number average molecular weight of 530. When the ester compound (RE-1) was measured by ion chromatography, the sulfate ion contained was 3500 mg / kg.

The contents of the A component, B component, D component, E component and the like synthesized above and the contents of the prepared C component are summarized in Tables 1 to 5.

In Table 1,
A ¹ , B ¹ , m, T ¹ : correspond to symbols in chemical formula ¹

A ² , B ² , n, T ² : Corresponds to symbols in chemical formula ²

Test Category 2 (Preparation of aqueous solution of synthetic fiber treatment agent)
Example 1
80 parts of A-1 listed in Table 1 as the A component, 9 parts of B-1 listed in Table 2 as the B component, 1 part of C-1 listed in Table 3 as the C component, and Table 4 as the D component 7 parts of D-1 described in the above, 3 parts of E-1 described in Table 5 as the E component, and 10 parts of water purified by the following method were uniformly mixed in the following ion chromatographic method. The amount of phosphate ions determined by the above is 100 mg / kg, the amount of sulfate ions determined by the following ion chromatography method is 50 mg / kg, and the total concentration of polyvalent metal cations determined by the following ICP emission analysis method is An aqueous solution (Example 1) of a synthetic fiber treating agent at 0.1 mg / 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). ) Was passed through a mixed bed column packed at an equal volume ratio to treat the total concentration of polyvalent metal cations to 0.1 mg / kg or less.

Ion chromatograph method: A sample of 10 g was accurately weighed and diluted with distilled water / isopropyl alcohol = 90/10 (volume ratio) to make a total amount of 100 g. 1 mL of the prepared diluted solution was passed through a pretreatment cartridge for the purpose of removing cations (heavy metal, etc.) and organic substances in the sample that interfered with the measurement, and subjected to ion chromatography analysis. The amount of phosphate ions and sulfate ions contained in the sample was determined by comparing the area with a commercially available standard sample with a known concentration. The conditions are shown below.
Apparatus: Product name IC-2001 manufactured by Tosoh Technosystem Corporation
Analytical column: Trade name TSKgel SuperIC-AZ column manufactured by Tosoh Technosystem Co., Ltd., inner diameter 4.6 mm × length 75 mm
Guard column: Trade name TSKgel guardcolumn SuperIC-AZ, manufactured by Tosoh Technosystem Co., Ltd., inner diameter 4.6 mm × length 10 mm
Pretreatment cartridge: Trade name TOYOPA IC-SP M manufactured by Tosoh Technosystem
Eluent: 4.8 mmol Na ₂ CO ₃ , 2.85 mmol NaHCO ₃
Flow rate: 0.6mL / min

ICP emission analysis: 5 g of sample was accurately weighed and diluted with distilled water to make a total amount of 100 g. The prepared diluted solution was subjected to ICP emission analysis. For the quantification, the total concentration of the polyvalent metal cation contained in the sample was determined by comparing the intensity value with a commercially available standard sample of known concentration. The conditions are shown below.
Apparatus: Product name SPS-3100 manufactured by Hitachi High-Tech Science

Examples 2-12, Reference Examples 13-19, 21-28, 30 and Comparative Examples 2-8
In the same manner as the aqueous solution of the synthetic fiber treatment agent (Example 1), the aqueous solution of the synthetic fiber treatment agent (Examples 2 to 12, Reference Examples 13 to 19, 21 to 28, 30 and Comparative Examples 2 to 8). Prepared.

Reference Example 20 {Preparation of synthetic fiber treating agent aqueous solution (P-32)}
70 parts of A-4 listed in Table 1 as the A component, 10 parts of B-8 listed in Table 2 as the B component, 9 parts of D-2 listed in Table 4 as the D component, and Table 5 as the E component 1 part of E-3 described in 1 above was uniformly mixed, and then 1 part of an inorganic synthetic adsorbent (trade name Kyoword 600S, manufactured by Kyowa Chemical Industry Co., Ltd.) was added. After stirring and treating, the catalyst and synthetic adsorbent contained in the B-8 were removed by filtration. Thereafter, 1 part of C-7 described in Table 3 as C component and 10 parts of water purified by the above method are uniformly mixed, and the phosphate ion obtained by the above-mentioned ion chromatography method is used. The amount is 100 mg / kg, the amount of sulfate ion determined by the ion chromatography method is 50 mg / kg, and the total concentration of polyvalent metal cations determined by the ICP emission analysis method is 0.3 mg / kg. An aqueous solution of the synthetic fiber treating agent (Reference Example 20) was prepared.

Reference examples 29, 31 and 32
Synthetic fiber treating agent aqueous liquids (Reference Examples 29, 31 and 32) were prepared in the same manner as the synthetic fiber treating agent aqueous liquid (Reference Example 20).

Comparative example 1
Phosphate ions determined by the above-mentioned ion chromatography method in the same manner as in the aqueous solution of the synthetic fiber treating agent (Example 1) except that water containing 40 mg / kg calcium and 4 mg / kg magnesium is used. The amount of sulfate ion determined by the ion chromatographic method is 10 mg / kg, and the total concentration of polyvalent metal cations determined by the ICP emission analysis method is 5 mg / kg. An aqueous liquid of fiber treating agent (Comparative Example 1) was prepared.

The contents of the aqueous solution of the synthetic fiber treating agent prepared in each example are summarized in Tables 6 and 7.

Test Category 3 (Evaluation of aqueous liquid, adhesion of aqueous liquid to synthetic fiber and evaluation in false twisting process)
・ Evaluation of low-temperature stability of aqueous solution of synthetic fiber treatment agent The aqueous solution of synthetic fiber treatment agent of each example prepared in Test Category 2 was stored in an incubator at −5 ° C. for 1 month and before storage. The following changes were visually evaluated for changes in appearance. The results are summarized in Table 8.

A: No change B: Slight swell occurs, but no problem in practical use because it becomes uniform by heating or dilution with water.
X: Obvious swelling or separation occurs, and there is a problem in practical use because it does not become uniform due to heating or dilution with water.

-Adhesion of aqueous solution of synthetic fiber treating agent to partially stretched polyester filament yarn After drying 5-isophthalic acid-modified polyethylene terephthalate chip with intrinsic viscosity of 0.64 and titanium oxide content of 0.2% by an ordinary method, an extruder The aqueous liquid of each example prepared in Test Category 2 is attached to the running yarn after being spun at 295 ° C. and cooled and solidified by discharging from the die by the roller oiling method, accompanied by mechanical stretching. Without scraping, a 10 kg combed cake of 128 dtex 36 filament partially stretched yarn having a synthetic fiber treating agent adhering to the yarn as shown in Table 8 was wound at a speed of 3300 m / min.

・ Measurement of adhesion amount of treating agent for synthetic fiber In accordance with JIS-L1073 (synthetic fiber filament yarn test method), the above partial stretching using a normal hexane / ethanol (50/50 volume ratio) mixed solvent as an extraction solvent The amount of synthetic fiber treating agent attached to the yarn was measured. The results are summarized in Table 8.

-False twisting by contact heater type false twisting machine The cake obtained above was subjected to false twisting as follows. Using a contact heater type false twisting machine (trade name SDS1200, manufactured by Teijin Seiki Co., Ltd.), processing speed = 1200 m, draw ratio = 1.652, twisting method = triaxial disk circumscribing friction method (entrance side guide disk) 1 sheet, 1 exit guide disk, 4 rigid polyurethane disks), twisting side heater = 2.5 m in length, surface temperature 210 ° C, untwisting side heater = none, target number of twists = 3300 T / m Then, false twisting was performed by continuous operation for 25 days.

-Evaluation of heater contamination property After continuously operating for 25 days under the above conditions, the heater tar generation on the yarn path of the twisted heater surface was visually observed and evaluated according to the following criteria. The results are summarized in Table 8.

◎: Heater contamination is hardly recognized ○: Heater contamination is slightly recognized, but it can be easily cleaned and has no problem in practical use ×: Heater contamination is clearly recognized, and it takes time and effort for cleaning. Is a problem

-Evaluation of anti-jumping property When operating continuously for 25 days under the above conditions, the number of jumping generated during that time was converted to the number per hour and evaluated according to the following criteria. The results are summarized in Table 8.

◎: Occurrence frequency is 0 to 1 O: Occurrence frequency is 2 to 3 times ×: Occurrence frequency is 4 times or more

-Evaluation of fluff After operating continuously for 25 days on the said conditions and winding up false twisted yarn, the number of fluff per hour was measured with the fluff counter (trade name DT-105 by Toray Engineering Co., Ltd.). The same operation and measurement of the number of fluff were performed three times in total, and evaluated according to the following criteria. The results are summarized in Table 8.

◎: Not generated ○: Generated 5 or less ×: Generated 6 or more

-Evaluation of yarn breakage Continuous operation was performed for 25 days under the above conditions, and the number of yarn breaks generated during that time was converted to the number per day. The same operation and conversion of the number of yarn breaks were performed three times in total, and evaluated according to the following criteria. The results are summarized in Table 8.

◎: Not generated ○: Less than once / day generated ×: Generated once / day or more

In Table 8,
* 1: Could not spin

  As is clear from the results in Table 8 corresponding to Tables 1 to 7, according to the present invention, the aqueous solution of the synthetic fiber treating agent itself maintains long-term stability even in winter, and the aqueous solution is allowed to adhere. Further, there is an effect that the occurrence of jumping out, heater contamination, fluff and yarn breakage in the false twisting process of the synthetic fiber can be sufficiently suppressed.

Claims (7)

55 to 85% by mass of the following A component , 2 to 35% by mass of the following B component, 0.4 to 1.6 % by mass of the following C component, and 6 to 15% by mass of the following D component ( 100 in total) The synthetic fiber treatment agent is an aqueous liquid containing 3 to 20 parts by mass of water with respect to 100 parts by mass of the synthetic fiber treatment agent contained at a ratio of (mass%) by ion chromatography. The total concentration of polyvalent metal cations determined by the ICP emission analysis method, wherein the required concentration of phosphate ions is 200 mg / kg or less, and the concentration of sulfate ions determined by ion chromatography is 200 mg / kg or less. An aqueous solution of a treating agent for synthetic fibers, wherein the concentration is 0.5 mg / kg or less.
Component A: polyether compound represented by the following chemical formula 1 having a number average molecular weight of 1500 to 3000

(In chemical formula 1,
A ¹ : monovalent hydrocarbon group, acyl group or hydrogen atom B ¹ : hydrogen of all hydroxyl groups from polyoxyalkylene glycol having a polyoxyalkylene group composed of oxyalkylene units having 2 to 4 carbon atoms in the molecule Residue excluding atoms T ¹ : monovalent hydrocarbon group, acyl group or hydrogen atom m : 1 )
Component B: at least one selected from the following polyether compounds represented by the following chemical formula 2 having a number average molecular weight of 5000 to 10,000 and the following polyether polyester compounds having a number average molecular weight of 3000 to 40000

(In chemical formula 2,
A ² : monovalent hydrocarbon group, acyl group or hydrogen atom B ² : hydrogen of all hydroxyl groups from polyoxyalkylene glycol having a polyoxyalkylene group composed of oxyalkylene units having 2 to 4 carbon atoms in the molecule Residue excluding atom T ² : divalent or trivalent hydrocarbon group, or residue obtained by removing all hydroxyl groups from organic dicarboxylic acid n: 2 or 3 when T ² is a divalent or trivalent hydrocarbon group 2) when T ² is a residue obtained by removing all hydroxyl groups from an organic dicarboxylic acid
Polyether polyester compound: obtained by polycondensation reaction of the polyether polyester compound obtained by subjecting the following P component and the following Q component to a condensation polymerization reaction, and the following P component, the following Q component and the following R component. At least one selected from polyether polyesters to be obtained: P component: aliphatic dicarboxylic acid having 4 to 22 carbon atoms, ester-forming derivative obtained from aliphatic dicarboxylic acid having 4 to 22 carbon atoms, aromatic dicarboxylic acid and aromatic dicarboxylic acid At least one selected from ester-forming derivatives obtained from acids Q component: all having a polyoxyalkylene group composed of oxyalkylene units having 2 to 4 carbon atoms in the molecule, polyoxyalkylene monool, polyoxy At least selected from alkylene diols and polyoxyalkylene triols One R component: alkylenediol C component having 2 to 6 carbon atoms: quaternary ammonium salts, organic amine oxide, amphoteric compounds, fatty acid salts, organic acid salts, those selected from the organic sulfates and organic phosphoric acid ester salt Containing an organic sulfonate and an organic phosphate ester salt
Component D: (Poly) oxyalkylene adduct having a number average molecular weight of 118 to 650 obtained by adding an alkylene oxide having 2 to 4 carbon atoms to an aliphatic monohydric alcohol having 4 to 22 carbon atoms   The aqueous solution of the treating agent for synthetic fibers according to claim 1, wherein the polyvalent metal cation is calcium ion and / or magnesium ion. The aqueous solution of the treating agent for synthetic fibers according to claim 1 or 2 , wherein the treating agent for synthetic fibers further contains the following E component.
E component: an ester compound having 17 to 60 carbon atoms obtained by esterification reaction of a monovalent aliphatic alcohol and a monovalent or divalent fatty acid, an alkylene oxide having 2 to 4 carbon atoms in a 1 to 6 valent aliphatic alcohol An alkylene oxide having 2 to 4 carbon atoms is added to an ester compound having a number average molecular weight of 300 to 650 and a monovalent aliphatic alcohol obtained by an esterification reaction of a (poly) oxyalkylene adduct added with a monovalent fatty acid At least one selected from ester compounds having a number average molecular weight of 300 to 650 obtained by esterification reaction of a (poly) oxyalkylene adduct and a divalent fatty acid E component is an ester compound having 22 to 36 carbon atoms obtained by esterification reaction of a monovalent aliphatic alcohol and a monovalent or divalent fatty acid, and an alkylene oxide having 2 to 4 carbon atoms to the monovalent aliphatic alcohol. The treatment agent for synthetic fibers according to claim 3, which is at least one selected from ester compounds having a number average molecular weight of 300 to 630 obtained by an esterification reaction of an added (poly) oxyalkylene adduct and a monovalent fatty acid. Aqueous liquid. The treating agent for synthetic fibers is 55 to 85% by mass of component A, 2 to 35% by mass of component B, 0.4 to 1.6% by mass of component C, 6 to 15% by mass of component D and 6 to 15% by mass of component E. The aqueous solution of the treating agent for synthetic fibers according to claim 3 or 4, which is contained at a ratio of 2 to 15 mass% (total of 100 mass%). The aqueous liquid of the synthetic fiber treatment agent according to any one of claims 1 to 5 , wherein water is blended at a ratio of 5 to 15 parts by mass with respect to 100 parts by mass of the synthetic fiber treatment agent. The aqueous liquid of the synthetic fiber treatment agent according to any one of claims 1 to 6 is used as it is or further diluted with water, and 0.1 to 2 mass as a synthetic fiber treatment agent for the synthetic fiber subjected to the false twisting process. %. A method for treating synthetic fibers, characterized by adhering to a percentage.