TWI678445B - Treating agent for synthetic fiber and use thereof - Google Patents

Abstract

An object of the present invention is to provide a treatment agent for a synthetic fiber which can be used in the production of synthetic fibers, can reduce roll contamination, and is excellent in heat resistance. The present invention is a processing agent for synthetic fibers containing a smoothing component (A) and an organic sulfonic acid compound (B) represented by the following general formula (1). The organic sulfonic acid compound (B) is nonvolatile in the processing agent. The weight ratio of the components is 1.25 to 12% by weight. The weight ratio of the sulfate ion (SO ₄ ^2- ) detected from the non-volatile components of the treatment agent by ion chromatography is 200 ppm or less, and the chloride ion (Cl ^- ) The weight ratio is 200 ppm or less.

In Formula (1), a and b are integers of 0 or more and are integers satisfying a + b = 5 to 17, and M is a hydrogen atom, an alkali metal, an ammonium group, or an organic amine group.

Description

Treatment agent for synthetic fiber and use thereof

The present invention relates to a treating agent for synthetic fibers and its use. More specifically, the present invention relates to a synthetic fiber treatment agent used in the production of a synthetic fiber resin, a method for producing a synthetic fiber filament yarn using the same, and a fiber structure including the synthetic fiber filament yarn.

The fiber treated with the fiber oil has been temporarily crimped and used in the drawing step, but recently, a method of shortening this step and directly using an oiling yarn in the drawing step has been adopted.

In this method, once a problem such as yarn breakage occurs during the stretching step, a large amount of fiber loss is caused. Therefore, it is necessary to avoid the problem during the stretching step as much as possible. The main cause of the problem is fiber damage such as yarn breakage. To prevent this problem, a treatment agent for synthetic fibers having excellent lubricity and heat resistance is required.

In addition, attempts have been made to improve the physical properties of fibers with high strength and low shrinkage, to increase the productivity during production, and to increase the productivity at high speeds. Due to roller contamination that has not been a problem so far, fluff and yarn breakage have increased. The problem. It was pointed out that in order to keep the rollers in a clean state, the roller cleaning room The interval is shortened, the cleaning frequency is increased, and the productivity is reduced.

In response to this problem, Patent Document 1 proposes a treatment agent for synthetic fibers using a phosphate ester-based anionic surfactant and a sulfonate-based anionic surfactant in combination. However, this treatment agent has the following disadvantages when it is used in a spindle method: insufficient heat resistance and lubricity, oil components after thermal degradation, etc. accumulate on the stretching roller and cause friction to rise over time, which occurs during the stretching step. Yarn breakage and fiber quality deterioration.

Further, Patent Document 1 proposes a treatment agent using a specific ester and an antioxidant in combination with the anionic surfactant. However, even with such a treatment agent, heat resistance that satisfies stringent yarn-making conditions cannot be obtained.

In addition, in response to the above-mentioned problems, Patent Document 2 proposes a treatment using a combination of an ester of a polyol, an ester of a carboxylic acid and an alcohol having a thioether group, a secondary sulfonate, an alkyl phosphate, and a hindered phenol-based antioxidant Agent. However, fluff and yarn breakage caused by roll contamination, which has not been a problem so far, have been achieved by improving productivity by achieving high strength, low shrinkage, and high speed. Even if the treatment agent is used, it cannot be improved. In addition, when the antioxidant described in Patent Document 2 is used, there is a disadvantage that the fiber gradually discolors during storage of the fiber.

Therefore, it is desired to obtain a treatment agent capable of suppressing a decrease in productivity due to a shortened cleaning interval of the rollers and an increase in the number of cleanings, and is excellent in heat resistance.

[Prior technical literature] [Patent Literature]

[Patent Document 1] Japanese Patent Laid-Open No. 59-211680

[Patent Document 2] Japanese Unexamined Patent Publication No. 8-120563

An object of the present invention is to provide a synthetic fiber processing agent which can reduce roll contamination and is excellent in heat resistance, which is used when manufacturing synthetic resin, a method for manufacturing a synthetic fiber filament yarn using the same, and a method including the same. Fiber structure of the obtained synthetic fiber filament yarn.

As a result of intensive research conducted by the present inventors, it was first found that: 1) a raw material containing an organic sulfonic acid compound represented by the general formula (1) contains a large amount of sodium sulfate and sodium chloride; 2) sulfuric acid contained in a treatment agent Sodium or sodium chloride will fall off during the spinning and accumulate on the drawing roller, which will cause an increase in yarn breakage and thread breakage. On the roller that is subjected to hot drawing, tar accumulation will be accelerated, causing roller contamination. Thus, 3) sulfate ion (SO ₄ ^2-) by non-volatile components from the processing agent and chloride ions detected (Cl ^-) is set to a predetermined ratio or less, contamination of the roller can be drastically reduced, thus far The present invention has been completed.

That is, the processing agent for synthetic fibers of the present invention contains a smoothing component (A) and an organic sulfonic acid compound (B) represented by the following general formula (1), and the organic sulfonic acid compound (B) The weight ratio of the non-volatile components is 1.25 to 12% by weight. The weight ratio of the sulfate ion (SO ₄ ^2- ) detected from the non-volatile components of the treatment agent by ion chromatography is 200 ppm or less. The chloride ion (Cl ^-) a weight ratio of 200ppm or less.

(In the formula (1), a and b are integers of 0 or more and are integers satisfying a + b = 5 to 17. M is a hydrogen atom, an alkali metal, an ammonium group, or an organic amine group).

The weight ratio of the smoothing component (A) in the treatment agent is preferably 20 to 70% by weight.

The weight ratio of the organic sulfonic acid compound (B) in the non-volatile component of the treatment agent is preferably 1.25 to 7% by weight.

The treatment agent of the present invention further contains an organic phosphate compound (C), and the weight ratio of the phosphate ion (PO ₄ ^3- ) detected from the non-volatile component of the treatment agent by ion chromatography is preferably 500 ppm or less. .

The weight ratio of the organic phosphate compound (C) in the non-volatile component of the treatment agent is preferably 0.05 to 5% by weight.

The organic phosphate compound (C) is at least one selected from the group consisting of a compound represented by the following general formula (2) and a compound represented by the following general formula (3).

(In formula (2), R ¹ is a hydrocarbon group having 6 to 24 carbon atoms. A ¹ O is an oxyalkylene group having 2 to 4 carbon atoms, m is an integer of 0 to 15, and n is 1 to 1 An integer of 2. M ¹ is a hydrogen atom, an alkali metal, an ammonium group, or an organic amine group).

(In formula (3), R ¹ is a hydrocarbon group having 6 to 24 carbon atoms. A ¹ O is an oxyalkylene group having 2 to 4 carbon atoms, and m is an integer of 0 to 15. M ¹ is a hydrogen atom and a base Metal, ammonium or organic amine. Q ¹ is M ¹ or R ¹ O (A ¹ O) _m. Y is 1 or 2).

The treating agent of the present invention preferably contains a nonionic surfactant (D).

The weight ratio of the non-ionic surfactant (D) in the non-volatile component of the treatment agent is preferably 20 to 70% by weight.

The synthetic fiber filament yarn of the present invention is obtained by adding the above-mentioned treatment agent to a raw material synthetic fiber filament yarn.

Method for manufacturing synthetic fiber filament yarn of the present invention The method includes the step of applying the processing agent to the raw synthetic fiber filament yarn.

The fiber structure system of this invention contains the said synthetic fiber filament yarn and / or the synthetic fiber filament yarn obtained by the said manufacturing method.

When the processing agent for synthetic fibers of this invention is used, roll contamination at the time of manufacturing a synthetic fiber can be reduced, and heat resistance is excellent. As a result, the cleaning interval of the roller can be increased, the number of cleaning times can be reduced, and the productivity of synthetic fibers can be improved.

According to the manufacturing method of the present invention, the occurrence of scum or yarn breakage can be reduced, and a synthetic fiber filament yarn having excellent yarn quality can be obtained. The fiber structure of the present invention is excellent in quality.

The processing agent for synthetic fibers of the present invention contains a smoothing component (A) and an organic sulfonic acid compound (B) represented by the general formula (1), and sulfuric acid is detected from a nonvolatile component of the processing agent by ion chromatography. The root and chloride ions are below the specified concentration. The details are described below.

[Smoothing component (A)]

The smoothing component (A) is an essential component of the processing agent of the present invention. Examples of the smoothing component (A) include: 1) an ester compound (A1) having an ester bond structure formed by an aliphatic monohydric alcohol and a fatty acid, and 2) an ester compound having an ester bond structure formed by an aliphatic polyhydric alcohol and a fatty acid. (A2), 3) have aliphatic mono Ester compound (A3) with an ester bond structure formed by an alcohol and an aliphatic polycarboxylic acid, 4) Aromatic ester compound (A4) with an aromatic ring in the molecule, 5) Sulfur-containing ester compound (A5), 6) Mineral Oil (A6) and the like are generally used as well-known smoothing ingredients for synthetic fiber treating agents. The smoothing component (A) can be used alone or in combination of two or more.

1) Ester compound (A1)

The ester compound (A1) is a compound having an ester bond structure formed by an aliphatic monohydric alcohol and a fatty acid (aliphatic monocarboxylic acid), and is a compound having no polyoxyalkylene group in the molecule. The ester compound (A1) can be used singly or in combination.

The ester compound (A1) is preferably a compound represented by the following general formula (4).

R ² -COO-R ³    (4)

(In the formula, R ² represents an alkyl or alkenyl group having 4 to 24 carbon atoms, and R ³ represents an alkyl or alkenyl group having 6 to 24 carbon atoms.)

The number of carbon atoms in R ² is preferably 6 to 22, more preferably 8 to 20, and even more preferably 10 to 18. When the number of carbon atoms is less than 4, the oil film becomes weaker, which may cause an increase in fluff. On the other hand, if the number of carbon atoms exceeds 24, the friction between the fibers and the metal increases, and there is a possibility that the fluff may increase. R ² may be either an alkyl group or an alkenyl group, but is preferably an alkyl group from the viewpoint of excellent heat resistance.

The number of carbon atoms of R ³ is preferably 6 to 22, more preferably 8 to 20, and even more preferably 10 to 18. When the number of carbon atoms is less than 6, the oil film becomes weaker, which may cause an increase in fluff. On the other hand, if the number of carbon atoms exceeds 24, the friction between the fibers and the metal increases, and there is a possibility that the fluff may increase. R ³ may be either an alkyl group or an alkenyl group, but is preferably an alkenyl group from the viewpoint of high oil film strength and less likely to generate fluff.

Although it does not specifically limit as an ester compound (A1), For example, 2-decyltetradecanoyl cis-sinamate, 2-decyltetradecanoyl oleate, 2-octyldodecyl hard Fatty acid esters, isooctyl palmitate, isooctyl stearate, butyl palmitate, butyl stearate, butyl oleate, isooctyl oleate, lauryl oleate , Isotridecyl stearate, cetyl stearate, isostearyl oleate, oleyl octanoate, oleyl laurate, oleyl palmitate, stearic acid Esters, oleyl oleates, and the like. Among these, 2-decyltetradecanoyl oleate, 2-octyldodecyl stearate, isooctyl palmitate, isooctyl stearate, and oleic acid are preferred. Lauryl ester, isotridecyl stearate, cetyl stearate, isostearyl oleate, oleyl oleate.

The ester compound (A1) can be synthesized by a known method using a commercially available fatty acid and an aliphatic monohydric alcohol.

2) Ester compound (A2)

The ester compound (A2) is a compound having an ester bond structure formed by an aliphatic polyol and a fatty acid (aliphatic monocarboxylic acid), and is a compound having no polyoxyalkylene group in the molecule. The ester compound (A2) can be used alone or in combination of two or more.

As long as the aliphatic polyol constituting the ester compound (A2) is There is no particular limitation on binary or more, and one kind or two or more kinds can be used. From the viewpoint of oil film strength, the polyhydric alcohol is preferably ternary or higher, more preferably ternary to quaternary, and even more preferably ternary.

Examples of the aliphatic polyhydric alcohol include ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, dipropylene glycol, tripropylene glycol, 1,2-butanediol, 1,3-butanediol, and 1 , 4-butanediol, 2-methyl-1,3-propanediol, 1,5-pentanediol, 1,6-hexanediol, neopentyl glycol, cyclohexanediol, cyclohexanedimethanol, Glycerin, trimethylolpropane, neopentaerythritol, erythritol, diglycerol, sorbitan, sorbitol, ditrimethylolpropane, diglycerol, triglycerol, tetraglycerol , Sucrose, etc. Among them, glycerol, trimethylolpropane, neopentyl alcohol, erythritol, diglycerol, sorbitan, sorbitol, ditrimethylolpropane, diglycerol, sucrose, and more preferably Preferably, it is glycerol, trimethylolpropane, neopentyl alcohol, erythritol, diglycerol, sorbitan, and still more preferably glycerol or trimethylolpropane.

The fatty acid constituting the ester compound (A2) may be saturated or unsaturated. The number of unsaturated bonds is not particularly limited, but when there are three or more, the degradation progresses due to oxidation and the treatment agent is thickened, thereby further impairing the lubricity. Therefore, it is preferably one or two. The number of carbon atoms of the fatty acid is preferably from 8 to 24, more preferably from 10 to 20, and even more preferably from 12 to 18 from the viewpoint of considering both film strength and lubricity. Fatty acids may be used singly or in combination of two or more kinds, and saturated fatty acids and unsaturated fatty acids may be used in combination.

Examples of fatty acids include butyric acid, crotonic acid, valeric acid, hexanoic acid, heptanoic acid, caprylic acid, nonanoic acid, capric acid, lauric acid, myristic acid, myristic acid, pentadecanoic acid, palmitic acid, Palmitoleic acid, isocetyl wax Acid, heptadecanoic acid, stearic acid, isostearic acid, oleic acid, trans oleic acid, isoleic acid, linoleic acid, linolenic acid, tuberculous stearic acid, arachidic acid, isacosanoic acid, cod Oleic acid (gadoleic acid), eicosenoic acid (eicosenoic acid), behenic acid, isosacosanoic acid, cis-erucic acid, behenic acid, isosacosanoic acid, neural acid, wax Acid, montanic acid, melic acid, etc.

Among these, octanoic acid, nonanoic acid, capric acid, lauric acid, myristic acid, myristic oleic acid, pentadecanoic acid, palmitic acid, palmitoleic acid, isocetyl acid, heptadecanoic acid, Stearic acid, isostearic acid, oleic acid, trans oleic acid, isoleic acid, linoleic acid, linolenic acid, tuberculous stearic acid, arachidic acid, isacosanoic acid, cocoic acid, eicosenoic acid , Behenic acid, iso-docosalic acid, cis-erucic acid, docosalic acid, iso-docosa carbonic acid, neural acid, more preferably capric acid, lauric acid, myristic acid, myristic acid , Pentadecanoic acid, palmitic acid, palmitoleic acid, isocetyl acid, heptadecanoic acid, stearic acid, isostearic acid, oleic acid, trans oleic acid, isoleic acid, linoleic acid, linolenic acid , Tuberculous stearic acid, arachidic acid, isacosanoic acid, cocoic acid, eicosenoic acid, and more preferably lauric acid, myristic acid, myristic acid, pentadecanoic acid, palmitic acid, palm oil Acid, isostearic acid, heptadecanoic acid, stearic acid, isostearic acid, oleic acid, trans oleic acid, isoleic acid, linoleic acid, linolenic acid.

The ester compound (A2) is a compound having two or more ester bonds in the molecule, but from the viewpoint of yarn-making property, a compound having three or more ester bonds in the molecule is preferred, and three compounds in the molecule are more preferred. Ester-bonded compounds.

The iodine value of the ester compound (A2) is not particularly limited.

The weight average molecular weight of the ester compound (A2) is preferably 300 It is 1200, more preferably 300 to 1,000, and even more preferably 500 to 1,000. When the weight-average molecular weight is less than 300, the oil film strength may be insufficient, and fluff may increase, or there may be an increase in smoke generation during heat treatment. On the other hand, when the weight-average molecular weight exceeds 1200, not only the smoothness is insufficient and the hairs are prone to produce high-quality fibers, but also the quality of the weaving or knitting step may be deteriorated. In addition, the weight-average molecular weight of the present invention is a gel permeation chromatography apparatus HLC-8220GPC manufactured by Tosoh Co., Ltd., which is injected into a separation column KF-402HQ manufactured by Showa Denko Co., Ltd. at a sample concentration of 3 mg / cc. KF-403HQ is calculated from the spectral peak measured by a differential refractive index detector.

Examples of the ester compound (A2) include trimethylolpropane tricaprylate, trimethylolpropane tridecanoate, trimethylolpropane trilaurate, and trimethylolpropane trioleate. Ester, trimethylolpropane (laurate, myristate, palmitate), trimethylolpropane (laurate, myristate, oleate), trimethylolpropane (tripalm Kernel fatty acid ester), trimethylolpropane (tri coconut oil fatty acid ester), trimethylolpropane dicaprylate, trimethylolpropane didecanoate, trimethylolpropane dilaurate, Trimethylolpropane dioleate, trimethylolpropane (laurate, myristate), trimethylolpropane (laurate, oleate), trimethylolpropane (myristic acid) Esters, oleates), trimethylolpropane (dipalmitine fatty acid esters), trimethylolpropane (di coconut oil fatty acid esters), coconut oil, rapeseed oil, palm oil, glyceryl trilaurate , Glycerol trioleate, glycerol tristearate, glycerol dioleate, glycerol monolaurate, diglycerol dioleate, sorbitan trioleate, dehydration Sorbitol (laurate, meat (Myristate, oleate), sorbitan dilaurate, sorbitan monooleate, neopentaerythritol tetracaprylate, neopentaerythritol tetradecanoate, neopentaerythritol tetra Lauryl ester, erythritol tetralaurate, neopentyl tetraol (tetrapalmitene fatty acid ester), neopentyl tetraol (tetra coconut oil fatty acid ester), erythritol trioleate, erythritol di Palmitate, 1,6-hexanediol dioleate, and the like.

As the ester compound (A2), a commercially available fatty acid and an aliphatic polyhydric alcohol can be used, which can be synthesized by a known method. In addition, naturally occurring natural esters such as natural fruits, seeds, or flowers can be directly used natural esters that satisfy the structure of the ester compound (A2), or if necessary, natural esters can be purified by known methods, or they can be used. The purified ester is an ester obtained by separating and refining the purified ester using a difference in melting point by a known method. Alternatively, an ester obtained by transesterification of two or more natural esters (oils and fats) may be used.

3) Ester compound (A3)

The ester compound (A3) is a compound having an ester bond structure formed by an aliphatic monohydric alcohol and an aliphatic polycarboxylic acid, and is a compound having no polyoxyalkylene group in the molecule. The ester compound (A3) can be used alone or in combination of two or more.

The aliphatic monohydric alcohol constituting the ester compound (A3) is not particularly limited, and one kind or two or more kinds can be used. The aliphatic monohydric alcohol may be saturated or unsaturated. The number of unsaturated bonds is not particularly limited, but when there are two or more, the oxidation progresses due to the deterioration and the treatment agent is thickened, and the lubricity is impaired, so it is preferably one. The number of carbon atoms of the aliphatic monohydric alcohol is preferably 8 to 24 from the viewpoint of smoothness and oil film strength, and more preferably 14 to 24, and still more preferably 18 to 22. The aliphatic monohydric alcohol may be used singly or in combination of two or more types, or a saturated fatty acid monohydric alcohol and an unsaturated aliphatic monohydric alcohol may be used in combination.

Examples of the aliphatic monohydric alcohol include octanol, isooctanol, lauryl alcohol, myristyl alcohol, myristyl alcohol, cetyl alcohol, isocetyl alcohol, palmityl alcohol, stearyl alcohol, and isostearyl alcohol. , Oleyl alcohol, trans oleyl alcohol, isooleyl alcohol, codyl alcohol, arachidyl alcohol, isoicosanol, eicosenoyl alcohol, behenyl alcohol, isodocosanol, cis mustard Alcohols, behenyl alcohols, isoscosanols, neuroalcohols, wax alcohols, montanol, benzyl alcohol, and the like. Among them, octanol, isooctanol, lauryl alcohol, myristyl alcohol, myristyl alcohol, cetyl alcohol, isocetyl alcohol, palmityl alcohol, stearyl alcohol, isostearyl alcohol, oleyl alcohol, trans alcohol Formula oleyl alcohol, isooleyl alcohol, codyl alcohol, arachidyl alcohol, isoicosanol, eicosanol, behenyl alcohol, isoaracosanol, cisanol, behenyl alcohol, isocosanol Tetracosanol, neuroalcohol, more preferably myristyl alcohol, palmityl alcohol, oleyl alcohol, oleyl alcohol, isooleyl alcohol, eicosyl alcohol, behenyl alcohol, cismarinol, neuroalcohol, further More preferred are oleyl alcohol, trans oleyl alcohol, isooleyl alcohol, codyl alcohol, eicosyl alcohol, and cisanol.

The aliphatic polycarboxylic acid constituting the ester (A3) is not particularly limited as long as it is binary or more, and one or two or more kinds may be used. The aliphatic polycarboxylic acid used in the present invention does not include sulfur-containing polycarboxylic acids such as thiodipropionic acid. The valence of the aliphatic polycarboxylic acid is preferably binary. Similarly, those having no hydroxyl group in the molecule are preferred.

Examples of the aliphatic polycarboxylic acid include citric acid, isocitric acid, malic acid, aconitic acid, acetic acid, oxalic acid, and succinic acid. Puric acid, fumaric acid, maleic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid and the like. Among them, aconitic acid, oxalic acid, oxalic acid, succinic acid, fumaric acid, maleic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, and more Preferred are fumaric acid, maleic acid, adipic acid, pimelic acid, suberic acid, azelaic acid, and sebacic acid.

Examples of the ester compound (A3) include dioctyl adipate, dilauryl adipate, dioleyl adipate, diisocetyl adipate, dioctyl sebacate, and sebacic acid. Dilauryl acid, dioleyl sebacate, diisocetyl sebacate and the like.

The ester compound (A3) is a compound having two or more ester bonds in the molecule. The iodine value of the ester compound (A3) is not particularly limited.

The weight average molecular weight of the ester compound (A3) is preferably 500 to 1,000, more preferably 500 to 800, and even more preferably 500 to 700. When the weight-average molecular weight is less than 500, the oil film strength may be insufficient, fluff may increase, or smoke generation during heat treatment may increase. On the other hand, when the weight-average molecular weight exceeds 1,000, the melting point becomes high, causing scum to be generated during the weaving or knitting step, and the quality may be deteriorated.

The ester compound (A3) can be synthesized using a commercially available aliphatic monohydric alcohol and an aliphatic polycarboxylic acid by a known method.

4) Aromatic ester compound (A4)

The aromatic ester compound (A4) is an ester compound having at least one aromatic ring in the molecule. Specifically, an ester compound (A4-1) having an ester bond structure formed by an aromatic carboxylic acid and an alcohol, and an aromatic alcohol and a carboxylic acid may be mentioned. An ester compound (A4-2) having an ester bond structure formed by an acid. The aromatic ester compound (A4) is a compound having no polyoxyalkylene group in the molecule. The aromatic ester compound (A4) can be used alone or in combination of two or more.

The aromatic carboxylic acid constituting the ester compound (A4-1) may be a monocarboxylic acid or a polycarboxylic acid. One type or two or more types may be used.

Examples of the aromatic carboxylic acid include benzoic acid, toluic acid, naphthoic acid, phthalic acid, isophthalic acid, terephthalic acid, salicylic acid, gallic acid, pyromellitic acid, cinnamic acid, Trimellitic acid, pyromellitic acid, etc. Among them, trimellitic acid, phthalic acid, isophthalic acid, and terephthalic acid are preferred, and trimellitic acid is more preferred.

The alcohol constituting the ester compound (A4-1) may be a monohydric alcohol or a polyhydric alcohol. Moreover, it may be any of an aliphatic alcohol, an alicyclic alcohol, and an aromatic alcohol. The monohydric alcohol may be used singly or in combination of two or more kinds. Among them, a monohydric alcohol is preferred, and an aliphatic monohydric alcohol is more preferred.

Examples of the monohydric alcohol include alkylphenol, dialkylphenol, octanol, isooctanol, lauryl alcohol, myristyl alcohol, myristyl alcohol, cetyl alcohol, isocetyl alcohol, palmitoleol, Stearyl alcohol, isostearyl alcohol, oleyl alcohol, oleyl alcohol, isooleyl alcohol, codyl alcohol, arachidyl alcohol, isoicosanol, eicosanol, behenyl alcohol, isodocosanol , Cis-sapanol, behenyl alcohol, iso-tecosanol, nerve alcohol, wax alcohol, montanol, benzyl alcohol, etc.

Examples of the polyol include aliphatic polyols described in the ester compound (A2), and aromatic polyols described in the ester compound (A4-2).

As the aromatic alcohol constituting the ester compound (A4-2), one kind or two or more kinds can be used. The aromatic alcohol is preferably an aromatic polyol, More preferred is an aromatic triol.

Examples of the aromatic alcohols include aromatic monohydric alcohols such as alkylbenzene alcohols; aromatic polyhydric alcohols such as dialkylbenzene alcohols, bisphenol A, bisphenol Z, and 1,3,5-trihydroxymethylbenzene. Among them, bisphenol A, bisphenol Z, 1,3,5-trihydroxymethylbenzene are preferred, and 1,3,5-trihydroxymethylbenzene is more preferred.

The carboxylic acid constituting the ester compound (A4-2) may be any of an aliphatic carboxylic acid and an aromatic carboxylic acid. Moreover, it may be either a monocarboxylic acid or a polycarboxylic acid. One type or two or more types can be used. Among these, a monocarboxylic acid is preferable, and a fatty acid is more preferable. From the viewpoint of residual properties, the fatty acid is preferably a saturated one. Fatty acids can be linear or branched.

Examples of the monocarboxylic acid include alkylbenzenecarboxylic acid, dialkylbenzenecarboxylic acid, butyric acid, crotonic acid, valeric acid, hexanoic acid, heptanoic acid, caprylic acid, nonanoic acid, capric acid, lauric acid, and nutmeg Acid, myristic acid, pentadecanoic acid, palmitic acid, palmitoleic acid, isocetyl, heptadecanoic acid, stearic acid, isostearic acid, oleic acid, trans oleic acid, isoleic acid, Linoleic acid, linolenic acid, tuberculous stearic acid, arachidic acid, isicosanoic acid, cocoic acid, eicosenoic acid, behenic acid, isodosanoic acid, maleic acid, docosadonic acid Alkanoic acid, isosacosanoic acid, neural acid, wax acid, montanic acid, melamine acid, etc.

Examples of the polycarboxylic acid include aliphatic polycarboxylic acids described in the ester compound (A3), and aromatic polycarboxylic acids described in the ester compound (A4-1).

5) Sulfur-containing ester compound (A5)

The sulfur-containing ester compound is selected from the group consisting of thiodipropionic acid and an aliphatic alcohol. At least one of an ester compound and a monoester compound of thiodipropionic acid and an aliphatic alcohol.

The sulfur-containing ester compound is a component having antioxidant ability. By using this sulfur-containing ester compound, the heat resistance of a processing agent can be improved. One kind or two or more kinds of sulfur-containing ester compounds can be used. The molecular weight of the thiodipropionic acid constituting the sulfur-containing ester compound is preferably 400 to 1,000, more preferably 500 to 900, and still more preferably 600 to 800. The aliphatic alcohol constituting the sulfur-containing ester compound may be saturated or unsaturated. In addition, the aliphatic alcohol may be a straight chain or a branched structure, but is preferably a branched structure. The number of carbon atoms of the aliphatic alcohol is preferably 8 to 24, more preferably 12 to 24, and still more preferably 16 to 24. Examples of the aliphatic alcohol include octanol, 2-ethylhexyl alcohol, decanol, lauryl alcohol, myristyl alcohol, isocetyl alcohol, oleyl alcohol, and isostearyl alcohol. Among them, oil is preferred Alcohol, isostearyl alcohol.

The sulfur-containing ester compound may be a diester compound of thiodipropionic acid and an aliphatic alcohol (this section is simply referred to as a diester), and a monoester compound of thiodipropionic acid and an aliphatic alcohol (in this section, Referred to as a monoester). At this time, the moles of the diester and monoester are preferably 100/0 to 70/30, more preferably 100/0 to 75/25, and still more preferably 100/0 to 80/20.

6) Mineral oil (A6)

Moreover, the processing agent for synthetic fibers of this invention may contain mineral oil as a smoothing component other than the above. The mineral oil referred to here is not a low-viscosity diluent used to dilute the treating agent, but is contained in a non-volatile component. The mineral oil is not particularly limited, and examples thereof include engine oil and spindles. Oil, liquid paraffin, etc. As the mineral oil, one kind or two or more kinds can be used. The viscosity of the mineral oil at 30 ° C is preferably 100 to 500 seconds.

As the smoothing component (A), from the viewpoint of improving heat resistance, it is preferable to use a purified catalyst by removing a catalyst or the like.

[Organic sulfonic acid compound (B)]

The organic sulfonic acid compound (B) represented by the said General formula (1) is an essential component of the processing agent of this invention. By containing the smoothing component (A) and the organic sulfonic acid compound (B), the weight ratio of the sulfate ion (SO ₄ ^2- ) detected from the non-volatile component of the treatment agent by ion chromatography is 200 ppm or less , chloride ion (Cl ^-) a weight ratio of 200ppm or less, it is possible to drastically reduce pile yarn breakage, contamination of the roller. It should be noted that the sulfate ion (SO ₄ ^2- ) is simply referred to as a sulfate ion, and the chloride ion (Cl ⁻ ) is simply referred to as a chloride ion.

In the general formula (1), a and b are integers of 0 or more and integers satisfying a + b = 5 to 17. When a + b is less than 5, the effect of reducing roller contamination becomes small. On the other hand, when a + b exceeds 17, the melting point is high and the compatibility in the treatment agent is deteriorated, making it unusable. a + b is preferably 7 to 17, more preferably 10 to 15.

M is a hydrogen atom, an alkali metal, an ammonium group, or an organic amine group. Examples of the alkali metal include lithium, sodium, and potassium. Examples of the ammonium group and the organic amine group include a group represented by NR ^a R ^b R ^c R ^d . R ^a , R ^b , R ^c , and R ^d are each independently a hydrogen atom, an alkyl group, an alkenyl group, or a polyoxyalkylene group. The number of carbon atoms of the alkyl group and the alkenyl group is preferably from 1 to 24, more preferably from 1 to 20, even more preferably from 1 to 18. The polyoxyalkylene group is represented by [-(A ¹ O) _m H], and (A ¹ O) _m is the same as that represented by the general formula (2).

Examples of the group represented by NR ^a R ^b R ^c R ^d include an ammonium group, a methyl ammonium group, an ethyl ammonium group, a propyl ammonium group, a butyl ammonium group, a hexyl ammonium group, and an octyl ammonium group. , Dimethyl ammonium, diethyl ammonium, dipropyl ammonium, dibutyl ammonium, dihexyl ammonium, dioctyl ammonium, trimethyl ammonium, triethyl ammonium, tripropyl Ammonium group, tributylammonium group, trihexylammonium group, trioctylammonium group, tetramethylammonium group, tetraethylammonium group, tetrapropylammonium group, tetrabutylammonium group, tetrahexylammonium group, Tetraoctylammonium, ethyltrimethylammonium, propyltrimethylammonium, butyltrimethylammonium, hexyltrimethylammonium, octyltrimethylammonium, methanol ammonium, ethanol Ammonium, propanol ammonium, butanol ammonium, hexanol ammonium, octanol ammonium, dimethanol ammonium, diethanol ammonium, dipropanol ammonium, dibutanol ammonium, dihexanol ammonium , Dioctanol ammonium group, trimethanol ammonium group, triethanol ammonium group, tripropanol ammonium group, tributanol ammonium group, trihexanol ammonium group, trioctanol ammonium group, (EO6) butylamino ether group (EO6) hexylamino ether group, (EO6) octylamino ether group, (EO6) decyl group Ether group, (EO6) lauryl amino ether group, (EO6) tetradecyl amino ether group, (EO6) cetyl amino ether group, (EO6) oleyl amino ether group, (EO6 ) Stearyl amino ether group, (EO6) codyl amino ether group, (EO6) behenyl alkyl ether group, (EO10) oleyl amino ether group, (EO10) oleyl amino group Ether group / cis erucic acid salt, (EO3) lauryl amino ether group, (EO3) lauryl amino ether group, (EO7) lauryl amino ether group, (EO15) oleyl amino ether group, (PO3 EO5) stearylamino ether group, (PO5, EO3) stearylamino ether group.

In a raw material (hereinafter, referred to as a raw material X) containing an organic sulfonic acid compound (B), a method for producing the raw material contains sodium sulfate and / or sodium chloride. The ratio of sodium sulfate and sodium chloride contained in this raw material X can be obtained by using The sub-chromatography is calculated based on the weight ratio of the sulfate ion and the chloride ion detected in the raw material X.

When the raw material X contains sodium sulfate, the weight ratio of the sulfate ion detected from the raw material X is 20,000 ppm or more with respect to the organic sulfonic acid compound (B). In addition, when the raw material X contains sodium chloride, the weight ratio of the chloride ion detected from the raw material X is 20,000 ppm or more with respect to the organic sulfonic acid compound (B).

When such a raw material X is used as a treatment agent, as described above, sodium sulfate and sodium chloride fall off during spinning and accumulate on a stretching roller, causing an increase in yarn breakage and thread breakage. In addition, on hot-rolled rolls, sodium sulphate and sodium chloride will accumulate tar and cause roll contamination. Examples of such a raw material X include HOSTAPUR SAS (manufactured by Hoechst), Mersolat H (manufactured by Bayer), and the like.

From the viewpoint of exerting the effects of the present invention, the processing agent of the present invention uses a raw material (hereinafter, referred to as raw material Y) containing an organic sulfonic acid compound (B) that reduces sodium sulfate and sodium chloride derived from raw material X. important. Specifically, it is preferable that the weight ratio of the sulfate ion detected from the raw material Y by ion chromatography to the organic sulfonic acid compound (B) is 5000 ppm or less, and the weight ratio of the chloride ion to the organic sulfonic acid compound is preferable. (B) is 5000 ppm or less.

From the viewpoint of further exerting the effects of the present application, the weight ratio of the sulfate ion detected from the raw material Y is more preferably 4000 ppm or less, further more preferably 3000 ppm or less, and particularly preferably, relative to the organic sulfonic acid compound (B). It is 2000 ppm or less. Similarly, with respect to the organic sulfonic acid compound (B), from The weight ratio of the chloride ion detected in the raw material Y is more preferably 4000 ppm or less, still more preferably 3000 ppm or less, and particularly preferably 2000 ppm or less.

The method for analyzing sulfate ions and chloride ions by ion chromatography in the present invention follows the method described in the examples.

The method for reducing sodium sulfate or sodium chloride from the raw material X containing the organic sulfonic acid compound (B) is not particularly limited, and a known method can be adopted. For example, when the raw material X contains sodium sulfate, a method of adding a solvent such as methanol and water to the raw material X, and precipitating and separating an inorganic substance such as sodium sulfate, and the like. In addition, when the raw material X contains sodium chloride, a method of removing sodium chloride included in the raw material X by an ion exchange membrane, and adsorption of sodium chloride contained in the raw material X by an ion exchange resin may be mentioned. Method, etc.

The organic sulfonic acid compound (B) is a monosulfonic acid compound having one sulfonic acid group. The treating agent of the present invention may contain a disulfonic acid compound represented by the following general formula (5) in addition to the monosulfonic acid compound.

In Formula (5), c, d, and e are integers of 0 or more, and are integers satisfying c + d + e = 4 to 16. When c + d + e is less than 4, the effect of reducing roller contamination may be small. On the other hand, when c + d + e exceeds 17, the compatibility in the treatment agent is deteriorated, and sometimes it cannot be used. c + d + e is preferably 6 to 16, more preferably 9 to 14.

M is a hydrogen atom, an alkali metal, an ammonium group, or an organic amine group. The description of M is the same as that of M described in the general formula (1).

When the disulfonic acid compound is contained, the weight ratio of the monosulfonic acid compound belonging to the organic sulfonic acid compound (B) to the disulfonic acid compound represented by the general formula (5) (monosulfonic acid compound / disulfonic acid compound ) Is preferably 50/50 to 99/1, more preferably 70/30 to 99/1, and even more preferably 80/20 to 98/2.

[Organic phosphate compound (C)]

The treatment agent of the present invention preferably contains an organic phosphate compound (C) in addition to the smoothing component (A) and the organic sulfonic acid compound (B) from the viewpoint of reducing fluff. The organic phosphate compound (C) is preferably at least one selected from the group consisting of a compound represented by the general formula (2) and a compound represented by the general formula (3).

In the general formulae (2) and (3), R ¹ is a hydrocarbon group having 6 to 24 carbon atoms. A ¹ O is an oxyalkylene group having 2 to 4 carbon atoms, and m is an integer of 0 to 15. n is an integer from 1 to 2. M ¹ is a hydrogen atom, an alkali metal, an ammonium group, or an organic amine group. Q ¹ is M ¹ or R ¹ O (A ¹ O) _m . Y is 1 or 2.

Examples of the hydrocarbon group of R ¹ include an alkyl group and an alkenyl group. The number of carbon atoms in R ¹ is preferably 8 to 24, and more preferably 12 to 24. The carbon atoms of R ¹ may have a distribution, and R ¹ may be linear or branched, or it may be saturated or unsaturated.

A ¹ O is an oxyalkylene group having 2 to 4 carbon atoms. The repeating number m of the oxyalkylene unit is an integer from 0 to 15, preferably from 0 to 10, more preferably from 0 to 3, and particularly preferably when m is 0, that is, when the polyoxyalkylene group is not included. (A ¹ O) _{m is} preferably a polyoxyalkylene group having 50 mol% or more of oxyethyl groups as oxyalkylene units.

n is an integer from 1 to 2. When n = 2, the two organic groups “R ¹ O (A ¹ O) _m ] constituting the compound represented by the general formula (2) may be the same or different.

When Q = R ¹ O (A ¹ O) _m , the two organic groups “R ¹ O (A ¹ O) _m ” constituting the compound represented by the general formula (3) may be the same or different. .

M ¹ is a hydrogen atom, an alkali metal, an ammonium group, or an organic amine group. Examples of the alkali metal include lithium, sodium, and potassium. Examples of the ammonium group and the organic amine group include a group represented by NR ^a R ^b R ^c R ^d . The group represented by NR ^a R ^b R ^c R ^d is the same as M described at the organic sulfonic acid compound (B).

The organic phosphate compound (C) preferably contains the organic phosphate compound (C1) represented by n = 1 in the general formula (2) and the organic phosphate compound (C2) represented by n = 2 in the general formula (2). The resulting mixture, or the organic phosphate compound (C3) represented by the organic phosphate compounds (C1), (C2), and Y = 1 and Q = R ¹ O (A ¹ O) _m in the general formula (3) Into a mixture. These mixtures may also contain an organic phosphate compound (C4) represented when Y = 1 and Q = hydrogen atom in the general formula (3).

The P-core integral ratio (%) of the organic phosphate compounds (C1), (C2), (C3), and (C4) and inorganic phosphoric acid can be calculated from the integral value of the spectral peak derived from each phosphorus atom in ³¹ P-NMR. In addition, the P-core integral ratio (%) is a value calculated as a total of 100% of the integral value of the organic phosphate compounds (C1), (C2), (C3), (C4) and inorganic phosphoric acid. The inorganic phosphoric acid system will be described later.

The P-core integral ratio (%) of the organic phosphate compound (C1) is preferably 25 to 82%, more preferably 35 to 80%, and still more preferably 40 to 70%. The P-core integral ratio (%) of the organic phosphate compound (C2) is preferably 15 to 65%, more preferably 20 to 60%, even more preferably 25 to 55%. The P-core integral ratio (%) of the organic phosphate compound (C3) is preferably 0 to 50%, more preferably 0 to 45%, and still more preferably 0 to 40%. The P-core integral ratio (%) of the organic phosphate compound (C4) is preferably 0 to 7%, more preferably 0 to 6%, and still more preferably 0 to 5%. The P-core integral ratio (%) of the inorganic phosphoric acid is preferably 0 to 10%, more preferably 0 to 9%, and still more preferably 0 to 8%.

The manufacturing method of an organic phosphate compound (C) is not specifically limited, A well-known method can be employ | adopted. For example, the method for producing an organic phosphate compound (C) includes a step (I) of reacting an organic hydroxy compound represented by R ¹ O (A ¹ O) _m H with phosphoric anhydride P ₂ O ₅ to obtain a reactant. In addition, in step (I), inorganic phosphoric acid and water may be added to carry out the reaction. The method for producing an organic phosphate compound (C) may include step (II) of adding water to the reactant after step (I) to perform hydrolysis. By including step (II), the ratio of the organic phosphate compounds (C3) and (C4) contained in the organic phosphate compound (C) can be adjusted. The amount of water added to the reactant is preferably 0.01 to 5% by weight, more preferably 0.05 to 4% by weight, and still more preferably 0.1 to 3% by weight based on the organic phosphate compound (C). When the amount of water added is less than 0.01% by weight or more than 5% by weight, it may be difficult to adjust the amounts of the organic phosphate compounds (C3) and (C4). As a method for producing the organic phosphate compound (C), a step (III) of neutralizing with a basic compound having M ¹ may be included after step (I) or step (II).

The organic phosphate compound (C) contains a heavy metal compound such as arsenic, which is a source of impurities in phosphoric anhydride or inorganic phosphorus. The treatment agent of the present invention may contain a heavy metal compound such as arsenic. From the standpoint of impact on the human body or environmental safety, the weight ratio of the heavy metal compound to the non-volatile components of the treatment agent is preferably 0.01% by weight or less, more preferably 0.005% by weight or less, even more preferably 0.001% by weight or less.

When the organic phosphate compound (C) is produced, inorganic phosphoric acid and / or a salt thereof is produced. Therefore, the raw material containing the organic phosphate compound (C) (hereinafter referred to as the raw material Z) contains inorganic phosphoric acid and / or a salt thereof. The ratio of the inorganic phosphoric acid and / or its salt can be adjusted by the ratio of the organic hydroxy compound to the phosphoric anhydride P ₂ O ₅ , reaction conditions, and the like.

[Nonionic Surfactant (D)]

The treatment agent of the present invention preferably contains a nonionic interface in addition to the smoothing component (A) and the organic sulfonic acid compound (B) from the viewpoint of imparting strength, bunching properties, and yarn-making properties to the oil film of the silk. Active agent (D). The non-ionic surfactant (D) refers to a substance other than the above-mentioned smoothing component (A). The nonionic surfactant (D) may be used alone or in combination of two or more.

Examples of the nonionic surfactant (D) include polyoxyalkylene-containing hydroxy fatty acid polyol esters (hereinafter, sometimes referred to as polyhydroxy esters), and at least one hydroxyl group in the polyhydroxy esters is sealed with a fatty acid. Esters, polyoxyalkylene polyol ethers, polyalkylene oxide polyols Fatty acid esters, polyalkylene oxide aliphatic alcohol ethers, fatty acid esters of polyalkylene glycols, polyhydric alcohol fatty acid esters, and the like.

(Polyhydroxyester, an ester in which at least one hydroxyl group in the polyhydroxyester is blocked with a fatty acid)

The polyhydroxy ester is preferably an ester of a hydroxy fatty acid containing a polyoxyalkylene group and a polyol in terms of structure, and more preferably two or more of the hydroxyl groups of the polyol are esterified. Therefore, a hydroxy fatty acid polyol ester containing a polyoxyalkylene group is an ester having a plurality of hydroxyl groups.

The polyoxyalkylene-containing hydroxy fatty acid has a structure in which a polyoxyalkylene group is bonded to an alkyl group of a fatty acid through an oxygen atom, and one end of the polyoxyalkylene group which is not bonded to the fatty acid hydrocarbon group becomes a hydroxyl group .

Examples of the polyhydroxy ester include an alkylene oxide adduct of an esterified product of a hydroxy fatty acid having 6 to 22 carbon atoms (preferably 16 to 20) and a polyhydric alcohol.

Examples of the hydroxy fatty acid having 6 to 22 carbon atoms include hydroxyoctanoic acid, hydroxydecanoic acid, hydroxylauric acid, hydroxystearic acid, and ricinoleic acid, and hydroxyoctadecanoic acid and ricinoleic acid are preferred. . Examples of the polyhydric alcohol include ethylene glycol, glycerin, sorbitol, sorbitan, trimethylolpropane, neopentyl alcohol, and glycerin is preferred. Examples of the alkylene oxide include alkylene oxides having 2 to 4 carbon atoms, such as ethylene oxide, propylene oxide, and butylene oxide.

The addition mole number of the alkylene oxide is preferably from 3 to 60, more preferably It is 8 to 50. The proportion of ethylene oxide in the alkylene oxide is preferably 50 mol%, and more preferably 80 mol%.

In the case of adding two or more kinds of alkylene oxides, the order of these additions is not particularly limited, and the addition form may be either a block shape or a random shape. The addition of the alkylene oxide can be performed by a known method, but it is usually performed in the presence of a basic catalyst.

The polyhydroxyester system can be produced, for example, by esterifying a polyhydric alcohol with a hydroxy fatty acid (hydroxymonocarboxylic acid) to obtain an esterified product under normal conditions, followed by an addition reaction of an alkylene oxide with the esterified product. . Polyhydroxyesters can also be appropriately produced by, for example, using naturally-occurring oils and fats such as castor oil or hydrogenated castor oil obtained by adding hydrogen thereto, followed by an addition reaction with alkylene oxide.

The nonionic surfactant (D) also contains an ester obtained by blocking at least one hydroxyl group of the polyhydroxyester with a fatty acid as described above. The number of carbon atoms of the blocked fatty acid is preferably 6 to 24, and more preferably 12 to 18. The number of carbon atoms of the hydrocarbon group in the fatty acid may have a distribution, and the hydrocarbon group may be linear or branched, saturated or unsaturated, or may have a polycyclic structure. Examples of such fatty acids include lauric acid, myristic acid, palmitic acid, palmitoleic acid, stearic acid, oleic acid, eicosanoic acid, behenic acid, and tetracosanoic acid. The method of esterification, reaction conditions, etc. are not specifically limited, A well-known method and normal conditions can be used.

Examples of the polyhydroxy ester and an ester obtained by blocking at least one hydroxyl group in the polyhydroxy ester with a fatty acid include hydrogenated castor oil ethylene oxide adduct, castor oil ethylene oxide adduct, and hydrogenated castor oil ring. Oxyethane Adduct monooleate, hydrogenated castor oil ethylene oxide adduct dioleate, hydrogenated castor oil ethylene oxide adduct trioleate, castor oil ethylene oxide adduct trioleic acid Ester, hydrogenated castor oil ethylene oxide adduct tristearate, and castor oil ethylene oxide adduct tristearate, among them, from the viewpoint of compatibility of the treatment agent, oil film strength, and reduction of fluff Preferably, it is hydrogenated castor oil ethylene oxide adduct, hydrogenated castor oil ethylene oxide adduct trioleate, and hydrogenated castor oil ethylene oxide adduct tristearate.

(Polyalkylene oxide polyol ether)

The polyalkylene oxide polyol ether refers to a compound having a structure in which an alkylene oxide such as ethylene oxide, propylene oxide, and butylene oxide is added to a polyol.

Examples of the polyhydric alcohol include ethylene glycol, glycerol, trimethylolpropane, neopentaerythritol, diglycerol, sorbitan, sorbitol, ditrimethylolpropane, dinepentaerythritol, Sucrose, etc. Among them, glycerin, trimethylolpropane, and sucrose are preferred.

The addition mole number of the alkylene oxide is preferably 3 to 100, more preferably 4 to 70, and still more preferably 5 to 50. The ratio of ethylene oxide in the alkylene oxide is preferably 50 mol% or more, and more preferably 80 mol% or more.

The weight average molecular weight of the polyalkylene oxide polyol ether is preferably 300 to 10,000, more preferably 400 to 8000, and still more preferably 500 to 5000. When the molecular weight is less than 300, generation of fluff and yarn breakage cannot be reduced. On the other hand, when the molecular weight exceeds 10,000, the friction of the treatment agent becomes high, and not only the occurrence of fluff or yarn breakage cannot be reduced, but it also deteriorates.

Examples of the polyalkylene oxide polyol ether include polyethylene glycol, glycerol ethylene oxide adduct, trimethylolpropane ethylene oxide adduct, and neopentyl tetraol ethylene oxide adduct. Products, diglycerol ethylene oxide adducts, sorbitan anhydride ethylene oxide adducts, sorbitan anhydride ethylene oxide propylene oxide adducts, sorbitol ethylene oxide adducts, Sorbitol ethylene oxide propylene oxide adduct, ditrimethylolpropane ethylene oxide adduct, dineopentaerythritol ethylene oxide adduct, sucrose ethylene oxide adduct, etc. , But not limited to this.

(Polyalkylene oxide polyol fatty acid ester)

The polyalkylene oxide polyol fatty acid ester is a compound having an ester bond structure formed by adding a compound obtained by adding an alkylene oxide such as ethylene oxide, propylene oxide, and butylene oxide to a polyol, and a fatty acid.

Examples of the polyhydric alcohol include glycerol, trimethylolpropane, neopentaerythritol, erythritol, diglycerol, sorbitan, sorbitol, ditrimethylolpropane, dinepentaerythritol, Sucrose, etc. Among them, glycerin, diglycerin, sorbitan, and sorbitol are preferred.

Examples of fatty acids include lauric acid, myristic acid, myristic acid, palmitic acid, palmitoleic acid, isocetyl acid, stearic acid, isostearic acid, oleic acid, trans oleic acid, and linoleic acid Acids, linolenic acid, arachidic acid, eicosenoic acid, behenic acid, isoaracosic acid, cis erucic acid, behenic acid, isosacosanoic acid, and the like.

The addition mole number of the alkylene oxide is preferably from 3 to 100, more preferably from 5 to 70, even more preferably from 10 to 50. In addition, epoxy The proportion of ethane in the alkylene oxide is preferably 50 mol% or more, and more preferably 80 mol% or more.

The weight average molecular weight of the polyalkylene oxide polyol fatty acid ester is preferably 300 to 7000, more preferably 500 to 5000, and still more preferably 700 to 3000. When the molecular weight is less than 300, smoke may be generated in the heat treatment step and the environment may be deteriorated. In addition, the occurrence of yarn breakage cannot be reduced. On the other hand, when the molecular weight exceeds 7,000, the friction of the treatment agent increases, which not only cannot reduce the occurrence of fluff or yarn breakage, but also worsens it.

Examples of the polyalkylene oxide polyol fatty acid ester include glycerol ethylene oxide adduct monolaurate, glycerol ethylene oxide adduct dilaurate, and glycerol ethylene oxide adduct. Laurate, trimethylolpropane ethylene oxide adduct trilaurate, sorbitan ethylene oxide adduct monooleate, sorbitan ethylene oxide adduct second oil Acid ester, sorbitan ethylene oxide adduct trioleate, sorbitan ethylene oxide propylene oxide adduct monooleate, sorbitan ethylene oxide propylene oxide addition Dioleate, sorbitan ethylene oxide propylene oxide adduct trioleate, sorbitan ethylene oxide propylene oxide adduct trilaurate, sucrose ethylene oxide Adducts, such as trilaurate, are not limited thereto.

(Polyalkylene oxide aliphatic alcohol ether)

The polyalkylene oxide aliphatic alcohol ether is a compound having a structure obtained by adding an alkylene oxide such as ethylene oxide, propylene oxide, and butylene oxide to an aliphatic monohydric alcohol.

Examples of the polyalkylene oxide aliphatic alcohol ether include octanol, 2-ethylhexanol, decanol, lauryl alcohol, tridecyl alcohol, myristyl alcohol, stearyl alcohol, isostearyl alcohol, An alkylene oxide adduct of an aliphatic alcohol such as oleyl alcohol.

The addition mole number of the alkylene oxide is preferably 1 to 100 moles, more preferably 2 to 70 moles, and still more preferably 3 to 50 moles. In addition, the ratio of ethylene oxide to the entire alkylene oxide is preferably 20 mol% or more, more preferably 30 mol% or more, and still more preferably 40 mol% or more.

(Fatty acid ester of polyalkylene glycol)

The fatty acid ester of polyalkanediol refers to a compound having an ester bond structure formed by polyoxyethylene glycol, polyoxyethylene polyoxypropylene glycol, and fatty acids. The weight average molecular weight of the polyalkylene glycol is preferably 100 to 1,000, more preferably 150 to 800, and still more preferably 200 to 700.

Examples of the polyalkylene glycol fatty acid ester include polyethylene glycol monolaurate, polyethylene glycol dilaurate, polyethylene glycol monooleate, polyethylene glycol dioleate, and polyethylene glycol monolaurate. Ethylene glycol monostearate, polyethylene glycol distearate, polyethylene polypropylene glycol monolaurate, polyethylene polypropylene glycol dilaurate, polyethylene polypropylene glycol monooleate, Polyethylene polypropylene glycol dioleate and the like are not limited thereto.

(Polyol fatty acid ester)

Polyol fatty acid esters are esters of polyols and fatty acids The compound having a bond structure is a compound other than the above-mentioned smoothing component (A).

Examples of the polyhydric alcohol include ethylene glycol, trimethylolpropane, neopentaerythritol, erythritol, diethylene glycol, diglycerol, sorbitan, sorbitol, and ditrimethylolpropane. , Sucrose, etc. Among them, ethylene glycol, glycerin, diglycerin, sorbitan, and sorbitol are preferred.

Examples of fatty acids include lauric acid, myristic acid, myristic acid, palmitic acid, palmitoleic acid, isocetyl acid, stearic acid, isostearic acid, oleic acid, trans oleic acid, and linoleic acid Acids, linolenic acid, tuberculous stearic acid, isosaic carbonic acid, cocoic acid, eicosenoic acid, behenic acid, isodosanoic acid, maleic acid, behenic acid, and the like

The polyol fatty acid ester system has at least one or two or more hydroxyl groups.

The weight average molecular weight of the polyol fatty acid ester is preferably 100 to 1,000, more preferably 200 to 800, and still more preferably 300 to 600.

Examples of fatty acid esters include glycerol monolaurate, glyceryl dilaurate, glycerol monooleate, glycerol dioleate, sorbitan monooleate, and sorbitan dioleate , Sucrose monolaurate, sucrose dilaurate, and the like, but are not limited thereto.

As the non-ionic surfactant (D), it is preferred to use a purified catalyst by removing a catalyst or the like from the viewpoint of improving heat resistance.

[Treatment agent for synthetic fibers]

The processing agent of this invention is a thing containing a smoothing component (A) and the organic sulfonic acid compound (B) represented by the said General formula (1). In addition, the weight ratio of the sulfate ion (SO ₄ ^2- ) detected from the non-volatile component of the treatment agent by ion chromatography was 200 ppm or less, and the weight ratio of the chloride ion (Cl ⁻ ) was 200 ppm or less. As described above, by setting the sulfate ion and the chloride ion detected from the non-volatile components of the treatment agent to a predetermined weight ratio or less, fluff, yarn breakage, and roll contamination can be reduced drastically.

When the weight ratio of the sulfate ion exceeds 200 ppm or the weight ratio of the chloride ion exceeds 200 ppm, sodium sulfate and sodium chloride fall off during spinning and accumulate on the stretching roller, causing an increase in thread and yarn breakage. For rolls subjected to hot drawing, the accumulation of tar is accelerated, causing roll contamination.

The method for analyzing sulfate ion and chloride ion by ion chromatography in the present invention is as described in the examples. In addition, the non-volatile component in the present invention refers to an absolute dry component when the treatment agent is heat-treated at 105 ° C. to remove a solvent and the like, and then reaches a constant weight.

From the viewpoint of further exerting the effects of the present invention, the weight ratio of the sulfate ion is preferably 200 ppm or less, more preferably 150 ppm or less, and still more preferably 100 ppm or less. Similarly, the weight ratio of this chloride ion is preferably 200 ppm or less, more preferably 150 ppm or less, and still more preferably 100 ppm or less.

As described above, the method for adjusting the weight ratio of sulfate ion and chloride ion can be achieved by reducing the sodium sulfate and sodium chloride contained in the raw material X containing the organic sulfonic acid compound (B).

The weight ratio of the smoothing component (A) in the non-volatile component of the treatment agent is preferably 20 to 70% by weight, more preferably 30 to 65% by weight, still more preferably 40 to 65% by weight, and particularly preferably 40 To 60% by weight. in When the weight ratio is less than 20% by weight, fluff may increase due to insufficient smoothness. On the other hand, when the weight ratio exceeds 70% by weight, the bundling property is insufficient, or in the case of emulsified use, the emulsification stability may be deteriorated and the use may not be possible.

The weight ratio of the organic sulfonic acid compound (B) in the non-volatile component of the treatment agent is 1.25 to 12% by weight, preferably 1.25 to 10% by weight, more preferably 1.25 to 8% by weight, and even more preferably 1.25 To 7% by weight, particularly preferably 1.5 to 6% by weight. When the weight ratio is less than 1.25% by weight, roll contamination may not be reduced. On the other hand, when the weight ratio exceeds 12% by weight, friction is increased and fluff is increased.

When the processing agent of the present invention contains an organic phosphate compound (C), the weight ratio of the phosphate ion (PO ₄ ^3- ) detected from the non-volatile components of the processing agent by ion chromatography is preferably 500 ppm the following. When the weight ratio of the phosphate ion exceeds 500 ppm, there is a possibility that thread breakage and yarn breakage may increase due to falling off on the stretching roll. The weight ratio of this phosphate ion is more preferably 400 ppm or less, still more preferably 300 ppm or less, and particularly preferably 200 ppm or less. In addition, the phosphate ion (PO ₄ ^3- ) is sometimes simply referred to as a phosphate ion.

As described above, as a method for adjusting the weight ratio of the phosphate ion, the inorganic phosphoric acid and / or its salt contained in the raw material Z containing the organic phosphate compound (C) can be reduced or the blending of the raw material Z can be adjusted. The amount is realized by using a filter aid such as diatomaceous earth to filter the treatment agent.

When the processing agent of the present invention contains the organic phosphate compound (C), the organic phosphate compound (C) is The weight ratio in the fraction is preferably from 0.05 to 10% by weight, more preferably from 0.08 to 8% by weight, even more preferably from 0.1 to 7% by weight.

In the case where the treating agent of the present invention contains a nonionic surfactant (D), the weight ratio of the nonionic surfactant (D) in the nonvolatile component of the treating agent is preferably 20 to 70% by weight, more It is preferably 25 to 65% by weight, more preferably 30 to 65% by weight, and particularly preferably 30 to 60% by weight.

(Other ingredients)

The processing agent for synthetic fibers of the present invention may also contain the organic sulfonic acid for the purpose of emulsifying the processing agent, assisting the adhesion to the fibers, washing the processing agent from the fibers, imparting electrical properties to the fibers, lubricity, and bunching properties. An acid compound (B), an organic phosphate compound (C), and a surfactant other than the nonionic surfactant (D). Examples of such surfactants include anionic surfactants such as fatty acid soaps; cationic surfactants such as alkylamine salts, alkylimidazolium salts, and quaternary ammonium salts; lauryldimethylbetaine, and stearyl groups. Amphoteric surfactants such as dimethyl betaine; dimethyl laurylamine oxides, etc. These surfactants can be used alone or in combination of two or more. When such a surfactant is contained, the weight ratio of the surfactant in the non-volatile component of the treatment agent is not particularly limited, but is preferably 0.01 to 15% by weight, and more preferably 0.1 to 10% by weight. The term "surfactant" as used herein refers to those having a weight average molecular weight of less than 1,000.

Moreover, in order to provide heat resistance, the processing agent for synthetic fibers of this invention may contain an antioxidant. As an antioxidant, you can give Out: well-known antioxidants such as phenol-based, sulfur-based, and phosphite-based. As the antioxidant, one kind or two or more kinds can be used. In the case where the antioxidant is contained, the weight ratio of the antioxidant to the non-volatile components of the treatment agent is not particularly limited, but is preferably 0.1 to 5% by weight, and more preferably 0.1 to 3% by weight.

In addition, the processing agent for synthetic fibers of the present invention may further contain a stock solution stabilizer (for example, water, ethylene glycol, and propylene glycol). The weight ratio of the stock solution stabilizer in the treatment agent is preferably 0.1 to 30% by weight, and more preferably 1 to 20% by weight.

The processing agent for synthetic fibers of the present invention may be composed of the above-mentioned components including only non-volatile components, or may be composed of non-volatile components and a stock solution stabilizer, or may be one which has been diluted with a low-viscosity mineral oil, It may be an aqueous emulsion obtained by emulsifying non-volatile components in water. In the case where the treating agent for a synthetic fiber of the present invention is an aqueous emulsion obtained by emulsifying a non-volatile component in water, the concentration of the non-volatile component is preferably 5 to 35% by weight, and more preferably 6 to 30% by weight. From the viewpoint of uniformly imparting to the fiber material, the viscosity (30 ° C.) of the treatment agent after diluting the nonvolatile component with a low viscosity mineral oil is preferably 3 to 120 mm ² / s, and more preferably 5 to 100 mm ² / s.

The manufacturing method of the processing agent for synthetic fibers of this invention is not specifically limited, A well-known method can be employ | adopted. The processing agent for synthetic fibers is manufactured by adding and mixing the said each component comprised in arbitrary or specific order. From the viewpoint of improving heat resistance, each component can be purified by removing a catalyst or the like. In particular, the smoothing component (A) and the non-ionic surfactant (D) used in the present invention may contain an inorganic substance. When the effect of the present invention is significantly reduced, the inorganic substance is removed and advanced. Line refiners are expected. As a method for removing and purifying inorganic substances, a known method can be used. For example, if it is a smoothing component (A), it can be removed by filtration using diatomaceous earth. If it is a nonionic surfactant (D), It can be purified by adsorption removal using an inorganic synthetic adsorbent.

[Manufacturing method of synthetic fiber filament yarn and fiber structure]

The method for producing a synthetic fiber filament yarn of the present invention includes applying a synthetic fiber treatment agent of the present invention to a raw synthetic fiber filament yarn. According to the manufacturing method of the present invention, the occurrence of scum or yarn breakage can be reduced, and further, a synthetic fiber filament yarn having excellent yarn quality can be obtained. The raw material synthetic fiber filament yarn in the present invention refers to a synthetic fiber filament yarn to which a treatment agent is not added.

The step of applying the treatment agent for synthetic fibers is not particularly limited, and a known method can be adopted. Usually, a processing agent for synthetic fibers is provided in the spinning step of the raw synthetic fiber filament yarn. After the treatment agent is applied, it is stretched by a heat roller, thermosetting, and wound up. In this way, when there is a step of thermally stretching without temporarily winding up after applying the treatment agent, the treatment agent for a synthetic fiber of the present invention can be suitably used. Examples of the temperature during thermal stretching include 210 to 260 ° C for industrial materials in the case of polyester and nylon, and 110 to 220 ° C in the case of clothing.

As mentioned above, the synthetic fiber treatment agent to be applied to the raw synthetic fiber filament yarn includes a treatment containing only non-volatile components. Agent, a treatment agent in which a non-volatile component is diluted with a low viscosity mineral oil, or an aqueous emulsion treatment agent in which the non-volatile component is emulsified in water. The application method is not particularly limited, and examples thereof include guide oil supply, roller oil supply, immersion oil supply, and spray oil supply. Among them, it is preferable to guide the oil supply and the roller oil supply from the point that the management of the applied amount is easy.

The amount of the non-volatile component added to the synthetic fiber processing agent is preferably 0.05 to 5% by weight, more preferably 0.1 to 3% by weight, and still more preferably 0.1 to 2% by weight relative to the raw synthetic fiber filament yarn. When it is less than 0.05% by weight, the effects of the present invention may not be exhibited. On the other hand, when it exceeds 5% by weight, the non-volatile components of the treatment agent easily fall off in the yarn path, and the tar on the heat roller significantly increases, which may cause tangling with fluff or broken yarn.

Examples of the (raw material) synthetic fiber filament yarn include filament yarns of synthetic fibers such as polyester fibers, polyamide fibers, and polyolefin fibers. The processing agent for synthetic fibers of the present invention is suitable for synthetic fibers such as polyester fibers, polyamide fibers, and polyolefin fibers. Examples of the polyester fiber include polyester (PET) containing ethylene terephthalate as a main constituent unit, and polymer containing trimethylene butylene ethyleneterephtalate as a main constituent unit. Ester (PTT), polyester (PBT) with butylene ethyleneterephtalate as the main structural unit, polyester (PLA) with lactic acid as the main structural unit, etc. Examples include nylon 6, nylon 66, and the like. Examples of polyolefin fibers include polypropylene and polyethylene. The method for producing synthetic fiber filament yarn is not particularly limited, and a known method can be adopted. Methods.

(Fiber structure)

The fiber structure system of this invention contains the synthetic fiber filament yarn obtained by the manufacturing method of this invention mentioned above. Specifically, the synthetic fiber filament yarn to which the treatment agent for a synthetic fiber of the present invention has been applied is woven with a water jet loom, an air jet loom, or a rapier loom, and a circular knitting machine and a longitudinal weaving are used. Knitting machine or flat knitting machine. Examples of applications of the fiber structure include industrial materials such as tire cords, seat belts, cushioning airbags, fishing nets, and ropes, and clothing. There is no particular limitation on the method for producing the fabric or knitted fabric, and a known method can be adopted.

(Example)

Hereinafter, the present invention will be described by way of examples, but the present invention is not limited to the examples described herein. In addition, "%" in the text and the table means "weight%".

[Raw material X containing organic sulfonic acid compound (B)] (Raw material X-1)

As the raw material X-1 containing the organic sulfonic acid compound (B), HOSTAPUR SAS93 (manufactured by Hoechst, 93% by weight of the organic sulfonic acid compound (B)) was used. A large amount of thenardite is contained in the raw material X-1. By ion chromatography of sulfate ion (SO ₄ ^2-) and chloride ions (Cl ^-) material X-1 was measured contained in an amount (weight ratio), with respect to the results of an organic sulfonic acid compound (B), The sulfate ion was 25950 ppm and the chloride ion was 62 ppm.

(Raw material X-2)

As a raw material X-2 containing an organic sulfonic acid compound (B), Mersolat H95 (manufactured by Bayer, organic sulfonic acid compound (B)) 95% by weight) was used. The raw material X-2 contains a large amount of sodium chloride. By ion chromatography of sulfate ion (SO ₄ ^2-) and chloride ions (Cl ^-) X-2 feedstock contained content was measured (weight ratio), with respect to the results of an organic sulfonic acid compound (B), The sulfate ion was 820 ppm and the chloride ion was 30,170 ppm.

[Preparation of raw material Y containing organic sulfonic acid compound (B)]

The raw materials Y-1 and Y-2 containing the organic sulfonic acid compound (B) can be obtained by purifying the raw materials X-1 and X-2 containing the organic sulfonic acid compound (B) and removing inorganic substances. A known method can be used for the inorganic substance removal method, and it is not limited to the purification method shown in an Example.

(Modulation of raw material Y-1)

550 parts of methanol and 400 parts of ion-exchanged water were mixed, and the temperature was adjusted at 45 ± 5 ° C. While stirring, 700 parts of the above-mentioned raw material X-1 was slowly added to completely dissolve. Next, this solution was left at room temperature for 20 hours to precipitate thenardite. The supernatant containing no thenardite was taken out, and distilled under reduced pressure at 60 to 80 ° C. to remove a part of methanol and water to obtain a raw material Y-1 containing 70% by weight of an organic sulfonic acid compound (B).

By ion chromatography of sulfate ion (SO ₄ ^2-) and chloride ions (Cl ^-) contained in the raw material Y-1 content was measured (weight ratio), with respect to the results of an organic sulfonic acid compound (B), The sulfate ion was 1085 ppm and the chloride ion was 60 ppm.

(Material Y-2)

600 parts of ion-exchanged water were heated to 80 ± 5 ° C., and 400 parts of the above-mentioned raw material X-2 was slowly added while stirring to completely dissolve. Next, after this solution was cooled to 40 ° C, sodium chloride was removed using an ion exchange resin to obtain a raw material Y-2 containing 40% by weight of an organic sulfonic acid compound (B).

By ion chromatography of sulfate ion (SO ₄ ^2-) and chloride ions (Cl ^-) contained in the raw material Y-2 content was measured (weight ratio), with respect to the results of an organic sulfonic acid compound (B), sulfuric acid The root ion was 105 ppm and the chloride ion was 2115 ppm.

[Preparation of raw materials Z-1 to Z-6 containing organic phosphate compound (C)] (Modulation of raw material Z-1)

820 parts of isocetyl alcohol was added to the reaction vessel, and 180 parts of phosphorus pentoxide was added in small amounts at a time while paying attention to the reaction temperature at 60 ± 5 ° C while stirring. Then, it was aged at 75 ± 5 ° C for 3 hours to prepare a raw material Z-1 containing an organic phosphate compound (C) having a non-volatile content of 100% by weight.

The P-core integral ratios of the organic phosphate compounds (C1), (C2), (C3), (C4) and inorganic phosphoric acid were 33.05%, 29.81%, 33.82%, 2.76%, and 0.56%, respectively.

(Modulation of raw material Z-2)

In the reactor, 800 parts of C11 to 15 alcohols were added, and 200 parts of phosphorus pentoxide was added in small amounts at a time while paying attention to the reaction temperature at 60 ± 5 ° C while stirring. Then, it was aged at 75 ± 5 ° C for 3 hours to prepare a raw material Z-2 containing an organic phosphate compound (C).

The P-core integral ratios of the organic phosphate compounds (C1), (C2), (C3), (C4) and inorganic phosphoric acid were 44.23%, 40.31%, 13.79%, 1.09%, and 0.58%, respectively.

(Modulation of raw material Z-3)

3 parts of ion-exchanged water was added to the above-prepared raw material Z-2997, and water treatment was performed at 90 ° C for 3 hours. Then, dehydration treatment was performed at 115 ° C for 3 hours to prepare a raw material Z-3 containing an organic phosphate compound (C).

The P-core integral ratios of the organic phosphate compounds (C1), (C2), (C3), (C4) and inorganic phosphoric acid were 56.72%, 40.49%, 0.00%, 0.00%, 2.78%.

(Modulation of raw material Z-4)

600 parts of oleyl alcohol was added to the reaction container, and 110 parts of phosphorus pentoxide was added in small amounts at a time while paying attention to the reaction temperature at 70 ± 5 ° C while stirring. Then, it was aged at 75 ± 5 ° C for 3 hours to prepare a raw material Z-4 containing an organic phosphate compound (C).

Organic phosphate compounds (C1), (C2), (C3), (C4) and inorganic phosphoric acid The P-core points ratios were 57.65%, 35.26%, 4.57%, 0.44%, and 2.07%.

(Modulation of raw material Z-5)

600 parts of oleyl alcohol was added to the reaction container, and 110 parts of phosphorus pentoxide was added in small amounts at a time while paying attention to the reaction temperature at 70 ± 5 ° C while stirring. Then, it was aged at 70 ± 5 ° C for 3 hours. Next, 15 parts of ion-exchanged water was added, and water treatment was performed at 90 ° C. for 3 hours, and then 200 parts of dibutylethanolamine was slowly added to neutralize the raw material Z-5 containing an organic phosphate compound (C).

The P-core integral ratios of the organic phosphate compounds (C1), (C2), (C3), (C4) and inorganic phosphoric acid were 55.18%, 35.38%, 2.43%, 0.00%, 7.01%, respectively.

(Modulation of raw material Z-6)

30 parts of ion-exchanged water was added to 970 parts of the raw material Z-1 prepared above, and water treatment was performed at 90 ° C for 3 hours. Then, dehydration treatment was performed at 115 ° C for 3 hours to prepare a raw material Z-3 containing an organic phosphate compound (C).

The P-core integral ratios of the organic phosphate compounds (C1), (C2), (C3), (C4) and inorganic phosphoric acid were 65.43%, 31.74%, 0.00%, 0.00%, 2.83%, respectively.

In addition, the organic phosphate compound (C1), (C2), (C3), (C4) and inorganic phosphate P core integral ratio were calculated by the following method using ³¹ P-NMR.

Approximately 30 mg of the non-volatile content of the measurement sample was weighed into a 5 mm diameter NMR test tube, and approximately 0.5 ml of deuterated water (D ₂ O) was added to dissolve the sample. A ³¹ P-NMR measurement device ( AVANCE 400 (162 MHz, manufactured by BRUKER) was used for measurement.

[Examples 1 to 11, Comparative Examples 1 to 9]

The components described in Tables 2 and 3 were mixed and stirred until they were uniform to prepare a treatment agent. Using each prepared treatment agent, the following methods were used to evaluate the accumulation of pin contamination, the contamination erasability of the pin, and the change in tension. The results are shown in Tables 2 and 3.

In addition, the numbers of the non-volatile composition of the processing agents of Tables 2 and 3 indicate the weight ratio of each component (the non-volatile components of the raw materials X, Y, and Z, etc.) to the non-volatile components of the processing agent. In addition, the details of the treatment agent components in Tables 2 and 3 are shown in Table 1.

(Sulfate ion (SO ₄ ^2-), chloride ion (Cl ^-), phosphate ion (PO ₄ ^3-) measuring method)

Accurately weigh 5 g of the sample (the non-volatile components of the treatment agent or the non-volatile components of the raw materials X, Y, and Z), and add 95 g of ultrapure water in a small amount each time while stirring to make an aqueous solution. Set the volume. 2 ml of the prepared aqueous solution was passed through a pretreatment column of ODS (after octadecyl group was chemically bonded to silica gel), and the liquid after removing the lipophilic substance was used for ion chromatography analysis. The detection was performed under the following ion chromatography analysis conditions. Using a standard solution of known concentration for the peak area ratio of measured to detect the amount and converted sulfate ion (SO ₄ ^2-),, chloride ion (Cl ^-) phosphate ion (PO ₄ ^3-) amount. Further, the limit of quantification sulfuric ion (SO ₄ ^2-) is 0.6ppm or less, chloride ion (Cl ^-) is 1.0ppm or less, phosphate ion (PO ₄ ^3-) is 0.3ppm or less. * In Tables 2 and 3 indicates the limit of quantification.

<Ion chromatography conditions>

Device: Dionex manufactures ICS-1500 use suppressor

Analytical column: Dionex IonPac AS14 inner diameter 4.0mm × length 50mm

Guard column: Dionex IonPac AG14 inner diameter 4.0mm × length 250mm

Eluent: 3.5mmolNa ₂ CO ₃ , 1.0mmolNaHCO ₃

Flow: 1.5ml / min

(Evaluation of needle contamination accumulation, needle contamination erasability, and tension change)

The prepared treatment agent was added to 1000 deniers and 96 oil-free polyester filaments at a basis weight of 20% by weight, and the filaments were passed through a roller heated to 150 ° C. using a sweeping method friction measuring machine to remove volatilization. After the composition, it was brought into contact with a satin chrome needle heated to 250 ° C., and moved for 4 hours at an initial tension of 500 g and a sweeping speed of 2 m / min. The degree of contamination accumulation of the needle, contamination erasability of the needle, and tension change were evaluated. Moreover, in order to perform a more stringent evaluation, 20 weight% of processing agents are provided.

The degree of needle contamination was evaluated by the following criteria.

◎: Pollution is hardly confirmed

○: Slightly confirmed contamination

×: Obvious accumulation of pollution

The tension fluctuation value is calculated by the following formula.

Tension fluctuation value (g) = tension (g) after yarn movement for 4 hours-initial tension (g)

In addition, the tension fluctuation was evaluated based on the tension fluctuation value using the following criteria.

◎: 0g to less than 30g

○: 30g to less than 50g

×: 50g or more

The contamination erasability of the needle was evaluated by the following method.

The solution made by dissolving sodium hydroxide in water and glycerin was immersed in the gauze to remove the pollution caused by the satin chrome needles. The erasability was evaluated by the number of times required until erasing.

◎: Contamination can be erased with less than 5 erases

○: Contamination can be erased by erasing more than 5 times and less than 20 times

×: Not erased with more than 20 erases

As can be seen from Tables 2 and 3, in the examples, the treatment agent in which the sulfate ion and the chloride ion detected from the non-volatile components of the treatment agent were set to a predetermined ratio or less, there was almost no accumulation of needle contamination and erasability. Excellent. That is, it is possible to reduce roll contamination when manufacturing synthetic fibers, and to increase the cleaning interval of the rolls, thereby reducing the number of cleanings. In addition, the tension fluctuation value is extremely small, which can drastically reduce fluff and yarn breakage.

On the other hand, in the comparative example, since the ratio of the sulfate ion or the chloride ion detected from the non-volatile component of the processing agent was high, the needle contamination accumulated a lot and the erasability was not good. In addition, it can be seen that the tension variation value is extremely large, and fluff and yarn breakage are repeatedly generated.

(Industrial applicability)

The synthetic fiber treating agent of the present invention is suitable for synthetic fiber filament yarns used in industrial materials such as waterproof canvas, tire curtains, safety belts, airbags, fishing nets, ropes, slings, etc., and fabrics or knitted fabrics.

Claims (11)

A processing agent for synthetic fibers, comprising a smoothing component (A) and an organic sulfonic acid compound (B) represented by the following general formula (1), wherein the organic sulfonic acid compound (B) is a non-volatile component of the processing agent weight ratio occupied in 1.25 to 12 wt% by ion chromatography from the non-volatile components of the treatment agent sulfate ion (SO ₄ ^2-) in the weight ratio of 200ppm or less, chloride ion (Cl ^- ) 'S weight ratio is 200 ppm or less, In Formula (1), a and b are integers of 0 or more and are integers satisfying a + b = 5 to 17, and M is a hydrogen atom, an alkali metal, an ammonium group, or an organic amine group. The processing agent for synthetic fibers according to item 1 of the scope of patent application, wherein the weight ratio of the smoothing component (A) in the processing agent is 20 to 70% by weight. The processing agent for synthetic fibers according to item 1 or 2 of the scope of the patent application, wherein the weight ratio of the organic sulfonic acid compound (B) in the non-volatile component of the processing agent is 1.25 to 7% by weight. The treatment agent for synthetic fibers as described in the scope of claims 1 or 2 of the patent application, further contains an organic phosphate compound (C), and phosphate ions (PO ₄ ) detected from the non-volatile components of the treatment agent by ion chromatography. ^3- ) The weight ratio is 500 ppm or less. The processing agent for synthetic fibers according to item 4 of the scope of the patent application, wherein the weight ratio of the organic phosphate compound (C) to the non-volatile components of the processing agent is 0.05 to 5% by weight. The treating agent for synthetic fibers according to item 4 of the scope of patent application, wherein the organic phosphate compound (C) is selected from a compound represented by the following general formula (2) and a compound represented by the following general formula (3) At least one of the compounds, In formula (2), R ¹ is a hydrocarbon group having 6 to 24 carbon atoms, A ¹ O is an oxyalkylene group having 2 to 4 carbon atoms, m is an integer of 0 to 15, and n is an integer of 1 to 2, M ¹ is a hydrogen atom, an alkali metal, an ammonium group, or an organic amine group, In formula (3), R ¹ is a hydrocarbon group having 6 to 24 carbon atoms, A ¹ O is an oxyalkylene group having 2 to 4 carbon atoms, m is an integer of 0 to 15, and M ¹ is a hydrogen atom and an alkali metal , Ammonium or organic amine, Q ¹ is M ¹ or R ¹ O (A ¹ O) _m , and Y is 1 or 2. The treating agent for synthetic fibers as described in the first or second item of the patent application scope further contains a nonionic surfactant (D). The processing agent for synthetic fibers according to item 7 of the scope of the patent application, wherein the weight ratio of the non-ionic surfactant (D) in the non-volatile component of the processing agent is 20 to 70% by weight. A synthetic fiber filament yarn is a raw material synthetic fiber filament yarn that is provided with a treatment agent for a synthetic fiber according to any one of claims 1 to 8 of the scope of patent application. A method for manufacturing a synthetic fiber filament yarn includes the steps of imparting a processing agent for a synthetic fiber according to any one of claims 1 to 8 in a raw material synthetic fiber filament yarn. A fiber structure is composed of the synthetic fiber filament yarn described in item 9 of the patent application scope and / or the synthetic fiber filament yarn obtained by the manufacturing method described in item 10 of the patent application scope.