KR101896536B1 - Finish for synthetic fibers and application thereof - Google Patents

Abstract

(상기 일반식(1) 중에서, a 및 b는, 0 이상의 정수이되, a＋b=5∼17을 만족시키는 정수이며, M은 수소 원자, 알칼리 금속, 암모늄기 또는 유기 아민기이다.)An object of the present invention is to provide a treatment agent for synthetic fibers which can be used in the production of synthetic fibers and which can reduce roll contamination and is excellent in heat resistance.
The present invention relates to a treatment agent for a synthetic fiber containing a smoothing component (A) and an organic sulfonic acid compound (B) represented by the following general formula (1), wherein the content of the organic sulfonic acid compound (B) in the non- this is 1.25~12% by weight ratio, ion chromatography, the weight ratio of sulfuric acid ion (SO ₄ ^2-) which is detected from the non-volatile content of the treating agent by this method is less than 200 ppm, a chlorine ion (Cl ^-) a weight ratio of 200 ppm or less.
[Chemical Formula 1]

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

Description

FINISH FOR SYNTHETIC FIBERS AND APPLICATION THEREOF FIELD OF THE INVENTION [0001]

The present invention relates to a treating agent for synthetic fibers and the use thereof. More particularly, the present invention relates to a treating agent for synthetic fibers used for producing synthetic fibers, a method for producing synthetic filament yarns using the treating agent, and a fiber structure including the synthetic fiber filament yarns.

Conventionally, a fiber treated with a fiber emulsion has been wound once and shifted to a stretching process. Recently, however, a method of shortening the process and shifting the oil refining yarn to a stretching process Has been adopted.

In this method, if a trouble such as breakage of the yarn once occurs in the stretching process, a large amount of fiber is lost, so that occurrence of troubles in the stretching process should be avoided as much as possible. The main cause of the trouble is fiber damage such as yarn breakage. To prevent this, a treating agent for synthetic fibers having excellent lubricity and heat resistance is required.

In addition, improvement in productivity, such as improvement in physical properties such as high strength and low shrinkage of fibers, and other end-time and high-speed production at the time of production are being promoted, and roll pollution, , There is a problem that the yarn breakage increases. As a result, in order to keep the roll in a clean state, the cleaning intervals of the rolls are short and the number of times of cleaning is increased, thereby pointing to a decrease in productivity.

With respect to this problem, Patent Document 1 proposes a treatment agent for synthetic fibers using a phosphate anionic surfactant and a sulfonate anionic surfactant in combination. However, in order to use this treating agent in the spindle method, heat resistance and lubricity are not sufficient, and the oil component, which is deteriorated by heat, accumulates in the stretching roll, friction rises over time, , Deteriorating the fiber quality.

In addition, Patent Document 1 proposes a treating agent in which a specific ester and an antioxidant are used in combination with the anionic surfactant. However, even with such a treating agent, satisfactory heat resistance can not be obtained under stringent yarn conditions.

With respect to the above-mentioned problem, Patent Document 2 discloses a treatment agent using a polyhydric alcohol ester, an ester of a carboxylic acid having a thioether group with an alcohol, a secondary sulphonate, an alkyl phosphate, and a hindered phenol antioxidant I am proposing. However, improvement in productivity such as high strength, low shrinkage ratio, and high speed production has not been improved even when this treatment agent is used for lint and thread breakage caused by roller contamination, which has not been a problem so far. Further, when the antioxidant described in Patent Document 2 is used, there is a problem that the fibers often discolor during fiber storage.

Therefore, a treatment agent having excellent heat resistance, which can suppress the decrease in productivity due to a short cleaning interval of rolls and a large number of times of cleaning, is desperately required.

Japanese Patent Application Laid-open No. 59-211680 Japanese Unexamined Patent Publication No. 8-120563

An object of the present invention is to provide a processing agent for synthetic fibers which can be used for producing synthetic fibers and which can reduce roll contamination and is excellent in heat resistance, a method for producing a synthetic fiber filament yarn using the treating agent, And to provide a fiber structure including a fiber filament yarn.

As a result of careful examination, the present inventors have 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 or sodium chloride, and 2) Sodium sulfate or sodium chloride is dropped on the stretching roll at the time of spinning and is accumulated so that the yarn breakage single yarn is increased and on the roll on which the thermal stretching is carried out, the accumulation of tar is accelerated, And the like. And 3) it is possible to dramatically reduce fluff, yarn breakage and roll contamination by reducing the sulfate ion (SO ₄ ^2- ) and chlorine ion (Cl ^- ) detected from the nonvolatile matter of the treatment agent to a predetermined ratio or less , The present invention has been reached.

That is, the treating agent for synthetic fibers according to the present invention comprises a smectic component (A) and an organic sulfonic acid compound (B) represented by the following general formula (1) the weight ratio of 1.25~12% by weight, ion chromatography, the weight ratio of sulfuric acid ion (SO ₄ ^2-) which is detected from the non-volatile content of the treating agent by this method is less than 200 ppm, a chlorine ion (Cl ^-) a weight ratio of Is not more than 200 ppm.

[Chemical Formula 1]

(In the general 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 treating agent is preferably 20 to 70% by weight.

The weight ratio of the organic sulfonic acid compound (B) to the nonvolatile matter of the treating agent is preferably 1.25 to 7% by weight.

It is preferable that the treating agent of the present invention further contains an organic phosphoric acid ester compound (C) and the weight ratio of phosphate ions (PO ₄ ^3- ) detected from the nonvolatile matter of the treating agent by ion chromatography is 500 ppm or less.

The weight ratio of the organophosphoric ester compound (C) to the nonvolatile matter of the treating agent is preferably 0.05 to 5 wt%.

The organic phosphoric ester compound (C) is preferably at least one selected from a compound represented by the following general formula (2) and a compound represented by the following general formula (3).

(2)

(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, and m is an integer of 0 to 15. 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.)

(3)

(In the above general formula (3), R ¹ is a hydrocarbon group of a carbon number of 6~24. A ¹ O is an oxyalkylene group of a carbon number of 2~4, m is an integer of 0~15. 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, and} Y is 1 or 2.

The treatment agent of the present invention preferably further comprises a nonionic surfactant (D).

The weight ratio of the nonionic surfactant (D) to the nonvolatile matter of the treating agent is preferably 20 to 70% by weight.

In the synthetic fiber filament yarn of the present invention, the above-mentioned treating agent is added to the raw synthetic fiber filament yarn.

The method for producing a synthetic fiber filament yarn according to the present invention includes a step of applying the above treating agent to a raw synthetic fiber filament yarn.

The fiber structure of the present invention includes the synthetic fiber filament yarns described above and / or the synthetic fiber filament yarns obtained by the above-described manufacturing method.

In the case of using the treating agent for synthetic fibers of the present invention, it is possible to reduce the contamination of the roll at the time of producing synthetic fibers, and is excellent in heat resistance. As a result, the cleaning intervals of the rolls can be lengthened, the number of cleaning times can be reduced, and the productivity of the synthetic fibers can be improved.

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

The treatment agent for synthetic fibers of the present invention is a treatment agent for synthetic fibers which contains a smoothing component (A) and an organic sulfonic acid compound (B) represented by the general formula (1) And chlorine ions to a predetermined concentration or less. Hereinafter, this will be described in detail.

[Smoothening component (A)]

The smoothing component (A) is an essential component of the treatment agent of the present invention. Examples of the smoothing component (A) include: 1) an ester compound (A1) having a structure in which an aliphatic monohydric alcohol and a fatty acid are ester-linked, 2) an ester compound (A2) having a structure in which an aliphatic polyhydric alcohol and a fatty acid are ester- (A5), (6) a mineral oil (A6), (6) an aromatic ester compound having an aromatic ring in the molecule, (6) an ester compound having a structure in which an alcohol and an aliphatic polycarboxylic acid are ester- And a known smoothing component which is generally employed as a synthetic fiber treatment agent. The smoothing component (A) may be used alone or in combination of two or more.

1) The ester compound (A1)

The ester compound (A1) is a compound having a structure in which an aliphatic monohydric alcohol and a fatty acid (aliphatic monocarboxylic acid) are ester-bonded, and is a compound having no polyoxyalkylene group in the molecule. The ester compound (A1) may be used alone or in combination of two or more.

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

[Chemical Formula 4]

(In the general formula (4), 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 carbon number of R ² is preferably from 6 to 22, more preferably from 8 to 20, and further preferably from 10 to 18. If the number of carbon atoms is less than 4, the oil film may be weak and the number of fuzz may increase. On the other hand, when the number of carbon atoms is more than 24, the friction between the fibrous metals increases, and the fluff may increase. R ² may be either an alkyl group or an alkenyl group, but an alkyl group is preferable from the viewpoint of excellent heat resistance.

R ³ preferably has ^{6 to 22} carbon atoms, more preferably 8 to 20 carbon atoms, and even more preferably 10 to 18 carbon atoms. If the number of carbon atoms is less than 6, the number of fluffs may increase because the oil film is weak. On the other hand, when the number of carbon atoms is more than 24, the friction between the fibrous metals increases, and the fluff may increase. R ³ may be either an alkyl group or an alkenyl group, but an alkenyl group is preferable from the viewpoint that the film strength is strong and fluffs are not readily formed.

Examples of the ester compound (A1) include, but are not limited to, esters of 2-decyltetradecanoyl, 2-decyltetradecanoyloleate, 2-octyldodecylstearate, isooctylpalmitate, isooctyl But are not limited to, stearate, butyl palmitate, butyl stearate, butyl oleate, isooctylolate, lauryl oleate, isotridecyl stearate, hexadecyl stearate, isostearyl oleate, oleyl octanoate, Oleyl palmitate, oleyl stearate, oleyl alcohol, and the like. Among them, 2-decyltodecanoyl oleate, 2-octyldodecyl stearate, isooctyl palmitate, isooctyl stearate, lauryl oleate, isotridecyl stearate, hexadecyl stearate, Lt; / RTI > is preferred.

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

2) ester compound (A2)

The ester compound (A2) is a compound having a structure in which an aliphatic polyhydric alcohol and a fatty acid (aliphatic monocarboxylic acid) are ester-bonded and has no polyoxyalkylene group in the molecule. The ester compound (A2) may be used alone or in combination of two or more.

The aliphatic polyhydric alcohol constituting the ester compound (A2) is not particularly limited as long as it is two or more valences, and one or more aliphatic polyhydric alcohols can be used. The polyhydric alcohol is preferably trivalent or more, more preferably 3 to 4, and more preferably 3, in consideration of the film strength.

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, Methyl-1,3-propanediol, 1,5-pentanediol, 1,6-hexanediol, neopentyl glycol, cyclohexanediol, cyclohexanedimethanol, glycerin, trimethylololane, pentaerythritol, Diglycerin, sorbitan, sorbitol, ditrimethylol propane, dipentaerythritol, triglycerin, tetraglycerin, sucrose and the like. Among these, glycerin, trimethylol propane, pentaerythritol, erythritol, diglycerin, sorbitan, sorbitol, ditrimethylol propane, dipentaerythritol and sucrose are preferable, and glycerin, trimethylolpropane, pentaerythritol, Glycerin, glycerin, glycerin, trimethylolpropane, glycerin, glycerin, glycerin and glycerin.

The fatty acid constituting the ester compound (A2) may be saturated or unsaturated. There are no particular restrictions on the number of unsaturated bonds, but if there are three or more, the number of unsaturated bonds is one or two because degradation due to oxidation causes the treatment agent to thicken and deteriorate lubricity. The number of carbon atoms in the fatty acid is preferably from 8 to 24, more preferably from 10 to 20, and even more preferably from 12 to 18, in consideration of compatibility between the film strength and lubricity. One or more fatty acids may be used, or a saturated fatty acid and an unsaturated fatty acid may be used in combination.

Examples of fatty acids include butyric acid, crotonic acid, valeric acid, caproic acid, enanthic acid, caprylic acid, pelargonic acid, capric acid, lauric acid, myristic acid, myristic oleic acid, pentadecanoic acid, palmitic acid, But are not limited to, tolylic acid, isocetic acid, margaric acid, stearic acid, isostearic acid, oleic acid, elaidic acid, parkic acid, linoleic acid, linolenic acid, tobacco stearic acid, arachidonic acid, isoeic acid, , Docosanoic acid, isodecanoic acid, erucic acid, tetracosonic acid, isotetracosonic acid, nerubonic acid, serotinic acid, montanic acid and melissic acid.

Among these, preferred are caprylic acid, pelargonic acid, capric acid, lauric acid, myristic acid, myristicoic acid, pentadecanoic acid, palmitic acid, palmitoleic acid, isocetic acid, margaric acid, stearic acid, But are not limited to, stearic acid, isostearic acid, oleic acid, elaidic acid, benzoic acid, linoleic acid, linolenic acid, tobacco stearic acid, arachidonic acid, isoeic acid, valoleic acid, eicosanoic acid, Isocetric acid, palmitoleic acid, isocetylic acid, margaric acid, stearic acid, isostearic acid, stearic acid, isostearic acid, isostearic acid and nerubonic acid are preferable, and capric acid, lauric acid, myristic acid, myristicoic acid, pentadecanoic acid, More preferred are acid, isostearic acid, oleic acid, elaidic acid, benzoic acid, linoleic acid, linolenic acid, tobacco colostearic acid, arachidonic acid, isoeic acid, valoleic acid and eicosanic acid, , Myristic oleic acid, pentadecanoic acid, Acid, palmitoleic resan, isopropyl three tilsan, Mar teaches acid, stearic acid, isostearic acid, oleic acid, El ride mountain night sensan, linoleic acid, linolenic acid is more preferable.

The ester compound (A2) is a compound having two or more ester bonds in the molecule, but it is preferably a compound having three or more ester bonds in the molecule from the viewpoint of preparation efficiency, and three esters Bond is more preferable.

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 to 1200, more preferably 300 to 1,000, and still more preferably 500 to 1,000. When the weight average molecular weight is less than 300, the film strength may be insufficient, fuzz may increase, or fumes may be increased during the heat treatment. On the other hand, when the weight average molecular weight is more than 1200, smoothness is insufficient and a lot of fluffs are generated, so that high-quality fibers can not be obtained, and the quality in the weaving or knitting process is inferior. The weight average molecular weight in the present invention was measured using a high-speed gel permeation chromatography apparatus HLC-8220GPC manufactured by Tosoh Corporation at a sample concentration of 3 mg / cc using a separation column (manufactured by Showa Denko K.K.) KF-402HQ, and KF-403HQ, and calculated from the peaks measured by the differential refractivity detector.

Examples of the ester compound (A2) include trimethylolpropane tricaprylate, trimethylolpropane tricaprate, trimethylolpropane triterate, trimethylolpropane trioleate, trimethylol propane (laurate, myristate , Palmitate), trimethylol propane (laurate, myristate, oleate), trimethylol propane (triphenyl nucleoside fatty acid ester), trimethylol propane (trichoconut fatty acid ester), trimethylolpropanedicarboxylate, trimethylolpropane (Laurate, oleate), trimethylolpropane (myristate, oleate), trimethylolpropane diolate, trimethylolpropane diolate, trimethylolpropane (laurate, myristate) ), Trimethylolpropane (diphenyl nucleobisate ester), trimethylolpropane (di-coconut fat Esters), coconut oil, rapeseed oil, palm oil, glycerin trioleate, glycerin trioleate, glycerin triisostearate, glycerin diolate, glycerin monolaurate, diglycerin diolate, sorbitan trioleate, sorbitan , Sorbitan monooleate, pentaerythritol tetracaprylate, pentaerythritol tetracaprate, pentaerythritol tetra laurate, erythritol tetra laurate, pentaerythritol tetraacrylate, Erythritol (tetraparm nucleosilicic acid ester), pentaerythritol (tetracoconut fatty acid ester), erythritol trioleate, erythritol dipalmitate, and 1,6 hexanediol diolate.

The ester compound (A2) may be a product obtained by synthesizing a commercially available fatty acid and an aliphatic polyhydric alcohol by a known method. Natural esters obtained from nature such as natural fruits, seeds or flowers can be obtained by using natural esters which satisfy the composition of the ester compound (A2) intact and, if necessary, by purifying natural esters by a known method, The ester may be separated and purified using a melting point difference by a known method. In addition, esters obtained by transesterifying two or more natural esters (oils) may be used.

3) The ester compound (A3)

The ester compound (A3) is a compound having a structure in which an aliphatic monohydric alcohol and an aliphatic polycarboxylic acid are ester-bonded and has no polyoxyalkylene group in the molecule. The ester compound (A3) may 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 or more aliphatic monohydric alcohols can be used. Aliphatic monohydric alcohols may be saturated or unsaturated. There is no particular limitation on the number of unsaturated bonds, but if there are two or more unsaturated bonds, it is preferable that the number of unsaturated bonds is one since deterioration is caused by oxidation and the treatment agent thickens and lubricity is impaired. The number of carbon atoms of the aliphatic monohydric alcohol is preferably from 8 to 24, more preferably from 14 to 24, and even more preferably from 18 to 22 from the viewpoints of smoothness and film strength. The aliphatic monohydric alcohol may be used singly or in combination of two or more kinds, and a saturated aliphatic monohydric alcohol and an unsaturated aliphatic monohydric alcohol may be used in combination.

Examples of the aliphatic monohydric alcohol include octyl alcohol, isooctyl alcohol, lauryl alcohol, myristyl alcohol, myristole alcohol, cetyl alcohol, isocetyl alcohol, palmitoleyl alcohol, stearyl alcohol, isostearyl alcohol, oleyl alcohol , Allylidyl alcohol, benzyl alcohol, gadolyl alcohol, arachidyl alcohol, iso-xanthyl alcohol, eicosanoyl alcohol, behenyl alcohol, isododecanyl alcohol, erucanyl alcohol, lignocellenyl alcohol, isotetra Norbornyl alcohol, cellulatinyl alcohol, montanyl alcohol, melissicyl alcohol, and the like. Among them, mention may be made of octyl alcohol, isooctyl alcohol, lauryl alcohol, myristyl alcohol, myristyl alcohol, cetyl alcohol, isocetyl alcohol, palmity trail alcohol, stearyl alcohol, isostearyl alcohol, oleyl alcohol, , Benzyl alcohol, gadolyl alcohol, arachidyl alcohol, iso-co-decyl alcohol, eicosenoyl alcohol, behenyl alcohol, isododecanyl alcohol, erucanyl alcohol, lignocellenyl alcohol, isotetradosanoyl alcohol And norbornyl alcohol are preferable, and misterric alcohol, palmi trail alcohol, oleyl alcohol, elaidil alcohol, benzyl alcohol, gadolyl alcohol, eicosanoyl alcohol, erucanyl alcohol and norbornyl alcohol are more preferable, Oleyl alcohol, elaidil alcohol, benzyl alcohol, gadolyl alcohol, eicosenoyl alcohol, and erucanyl alcohol are more preferable All.

The aliphatic polycarboxylic acid constituting the ester (A3) is not particularly limited as long as it is a divalent or more, and one or more aliphatic polycarboxylic acids can be used. The aliphatic polycarboxylic acid used in the present invention does not contain a sulfur-containing polycarboxylic acid such as thiodipropionic acid. The valence of the aliphatic polyvalent carboxylic acid is preferably bivalent. Similarly, it is preferable not to include a hydroxyl group in the molecule.

Examples of the aliphatic polycarboxylic acid include citric acid, isocitric acid, malic acid, aconitic acid, oxaloacetic acid, oxalosuccinic acid, succinic acid, fumaric acid, maleic acid, glutaric acid, adipic acid, pimelic acid, Sekisui Mountain, and the like. Among them, aconitic acid, oxaloacetic acid, oxalo succinic acid, succinic acid, fumaric acid, maleic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid and sebacic acid are preferable, and fumaric acid, , Adipic acid, pimelic acid, suberic acid, azelaic acid, and sebacic acid are more preferable.

Examples of the ester compound (A3) include dioctyl adipate, adipic acid dilauryl, adipic acid diolrail, adipic acid diisocetyl, dioctyl sebacate, dilauryl 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 1000, more preferably 500 to 800, still more preferably 500 to 700. When the weight average molecular weight is less than 500, the film strength may be insufficient, the napping may increase, or the fuming may increase during the heat treatment. On the other hand, when the weight average molecular weight is more than 1000, the melting point becomes high, causing scum generation in the weaving or knitting process, and the quality may be poor.

The ester compound (A3) can be obtained by synthesizing 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 a structure in which an aromatic carboxylic acid and an alcohol are ester-bonded and an ester compound (A4-2) having a structure in which an aromatic alcohol and a carboxylic acid are ester-bonded are exemplified. The aromatic ester compound (A4) is a compound having no polyoxyalkylene group in the molecule. The aromatic ester compound (A4) may 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 or more of them 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, melissic acid, cinnamic acid, trimellitic acid and pyromellitic acid. Among these, trimellitic acid, phthalic acid, isophthalic acid and terephthalic acid are preferable, and trimellitic acid is more preferable.

The alcohol constituting the ester compound (A4-1) may be a monohydric alcohol or a polyhydric alcohol. In addition, any of aliphatic alcohol, alicyclic alcohol, and aromatic alcohol may be used. The monohydric alcohol may be used alone or in combination of two or more. Of these, monohydric alcohols are preferable, and aliphatic monohydric alcohols are more preferable.

Examples of the monohydric alcohol include alkylbenzene alcohols, dialkylbenzene alcohols, octyl alcohols, isooctyl alcohols, lauryl alcohols, myristyl alcohols, myristyl alcohols, cetyl alcohols, isocetyl alcohols, palmity trails alcohols, stearyl alcohols, But are not limited to, stearyl alcohol, oleyl alcohol, elaidyl alcohol, benzyl alcohol, gadolyl alcohol, arachidyl alcohol, iso-xanthyl alcohol, eicosanoyl alcohol, behenyl alcohol, isododecanyl alcohol, Nocerenyl alcohol, isotetracosanyl alcohol, norbornyl alcohol, cellulatinyl alcohol, montanyl alcohol, melissicyl alcohol, and the like.

Examples of the polyhydric alcohol include aromatic polyhydric alcohols described for the ester compound (A2) and aromatic polyhydric alcohols described for the ester compound (A4-2).

The aromatic alcohol constituting the ester compound (A4-2) may be used alone or in combination of two or more. As the aromatic alcohols, aromatic polyhydric alcohols are preferable, and aromatic trihydric alcohols are more preferable.

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 these, bisphenol A, bisphenol Z and 1,3,5-trihydroxymethylbenzene are preferable, and 1,3,5-trihydroxymethylbenzene is more preferable.

The carboxylic acid constituting the ester compound (A4-2) may be any of an aliphatic carboxylic acid and an aromatic carboxylic acid. Further, any one of a monovalent carboxylic acid and a polyvalent carboxylic acid may be used. One or more of them may be used. Among these, a monovalent carboxylic acid is preferable, and a fatty acid is more preferable. The fatty acid is preferably saturated in consideration of the residual property. Fatty acids may be linear or branched.

Examples of monovalent carboxylic acids include alkylbenzenecarboxylic acids, dialkylbenzenecarboxylic acids, butyric, crotonic, valeric, caproic, enantic, caprylic, pelaric, capric, lauric, , Stearic acid, isostearic acid, oleic acid, elaidic acid, benzoic acid, linoleic acid, linolenic acid, tobacco colostearic acid, maleic acid, fumaric acid, Examples include acids such as acetic acid, arachidic acid, isoic acid, valoleic acid, eicosanic acid, behenic acid, isodecanoic acid, erucic acid, lignoceric acid, isotetracarboxylic acid, nerubonic acid, .

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

5) The sulfur-containing ester compound (A5)

The sulfur-containing ester compound is at least one selected from diester compounds of thiodipropionic acid and aliphatic alcohol and monoester compounds of thiodipropionic acid and aliphatic alcohol.

The sulfur-containing ester compound is a component having antioxidant ability. By using the sulfur-containing ester compound, the heat resistance of the treating agent can be increased. The sulfur-containing ester compound may be used alone or in combination of two or more. The molecular weight of the thiodipropionic acid constituting the sulfur-containing ester compound is preferably 400 to 1000, 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. The aliphatic alcohol may be linear or branched, but preferably has a branched structure. The aliphatic alcohol preferably has 8 to 24 carbon atoms, more preferably 12 to 24 carbon atoms, and even more preferably 16 to 24 carbon atoms. Examples of the aliphatic alcohol include octyl alcohol, 2-ethylhexyl alcohol, decyl alcohol, lauryl alcohol, myristyl alcohol, isocetyl alcohol, oleyl alcohol and isostearyl alcohol. Monohydric alcohol, isostearyl alcohol is preferable.

The sulfur-containing ester compound is preferably a diester compound of thiodipropionic acid and aliphatic alcohol (referred to simply as diester in this paragraph), a monoester compound of thiodipropionic acid and aliphatic alcohol (in this paragraph, ). The molar ratio of the diester to the monoester is preferably 100/0 to 70/30, more preferably 100/0 to 75/25, and even more preferably 100/0 to 80/20.

6) Mineral oil (A6)

Further, the treating agent for synthetic fibers of the present invention may contain mineral oil as a smoothing component other than those described above. The mineral oil referred to here is not a low viscosity diluent used for diluting the treating agent but is included in the nonvolatile matter. The mineral oil is not particularly limited, and examples thereof include machine oil, spindle oil, liquid paraffin, and the like. The mineral oil may be used alone or in combination of two or more. The viscosity of the mineral oil at 30 캜 is preferably 100 to 500 seconds.

As the smoothing component (A), it is preferable to use a product obtained by removing the catalyst and the like from the viewpoint of improvement in heat resistance.

[Organic sulfonic acid compound (B)]

The organic sulfonic acid compound (B) represented by the above general formula (1) is an essential component of the treatment agent of the present invention. Smoothing the component (A) and contains an organic sulfonic acid compound (B), and further an ion chromatographic method sulfate ion to be detected from the non-volatile content of the treating agent by the (SO ₄ ^2-) weight ratio of not more than 200 ppm, a chlorine ion (Cl ^- ) is set to 200 ppm or less, lint, yarn breakage and roll contamination can be dramatically reduced. The sulfate ion (SO ₄ ^2- ) may be simply referred to as sulfate ion, and the chloride ion (Cl ^- ) may be referred to as chloride ion.

In the general formula (1), a and b are integers of 0 or more and a + b = 5 to 17. When a + b is less than 5, the effect of reducing roll contamination is reduced. On the other hand, when a + b exceeds 17, the melting point is high and the compatibility in the treating 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, potassium and the like. Examples of the ammonium group and the organic amine group include groups 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 alkyl group and the alkenyl group preferably have 1 to 24 carbon atoms, more preferably 1 to 20 carbon atoms, and even more preferably 1 to 18 carbon atoms. 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 methylammonium group, an ethylammonium group, a propylammonium group, a butylammonium group, a hexylammonium group, an octylammonium group, a dimethylammonium group, a diethylammonium group, a dipropylammonium group, A tetraethylammonium group, a tetrabutylammonium group, a tetrabutylammonium group, a tetrabutylammonium group, a tetrabutylammonium group, a tetrabutylammonium group, a tetrabutylammonium group, a tetrabutylammonium group, a tetrabutylammonium group, a tetrabutylammonium group, a tetrabutylammonium group, a tetrabutylammonium group, a tetrabutylammonium group, a tetrabutylammonium group, A hexamethylammonium group, a hexamethylammonium group, a pentamethylammonium group, a pentamethylammonium group, a hexamethylammonium group, a hexamylammonium group, a tetraoctylammonium group, an ethyltrimethylammonium group, a propyltrimethylammonium group, a butyltrimethylammonium group, a hexyltrimethylammonium group, an octyltrimethylammonium group, (A), (b), and (d), the ammonium group, the diethanolammonium group, the diethanolammonium group, the dibutanolammonium group, the dihexanolammonium group, the dioctanolammonium group, the trimethanolammonium group, the triethanolammonium group, the tripropanolammonium group, the tributanolammonium group, the trihexanolammonium group, EO6) butylamino ether group, (EO6) hexylamino ether group, (EO6) octylaminoether group, (EO6) decylaminoether group, (EO6) laurylaminoether group, EO6) hexadecylaminoether group, (EO6) oleylaminoether group, (EO6) stearylaminoether group, (EO6) gadolylaminoether group, (EO6) tetracosylaminoether group, (EO10) oleylamino (EO) lauryl amino ether group, (EO7) lauryl amino ether group, (EO15) oleyl amino ether group (EO) lauryl amino ether group , (PO3, EO5) stearyl amide Is group an ether group, (PO5, EO3) stearyl amino ether.

The raw material containing the organic sulfonic acid compound (B) (hereinafter referred to as raw material X) contains sodium sulfate and / or sodium chloride due to the production method. The ratio of sodium sulfate or sodium chloride contained in the raw material X can be calculated from the weight ratio of sulfate ion or chloride ion detected from the raw material X by ion chromatography.

When the raw material X contains sodium sulfate, the weight ratio of the sulfate ion detected from the raw material X is 20000 ppm or more with respect to the organic sulfonic acid compound (B). When the raw material X contains sodium chloride, the weight ratio of the chloride ion detected from the raw material X is 20000 ppm or more with respect to the organic sulfonic acid compound (B).

When such a raw material X is used in the treating agent, sodium sulfate or sodium chloride falls off on the stretching roll at the time of spinning and accumulates to cause an increase in the yarn breakage single yarn, as described above. In addition, on the roll on which thermal stretching is performed, sodium sulfate or sodium chloride accelerates the accumulation of tar to cause roll contamination. Examples of such raw materials X include HOSTAPUR SAS (manufactured by Kostos), Mersolat H (manufactured by Bayer), and the like.

It is preferable to use a raw material (hereinafter referred to as raw material Y) containing an organic sulfonic acid compound (B) in which sodium sulfate or sodium chloride is reduced from raw material X in the treatment agent of the present invention It is important. Specifically, the weight ratio of the sulfate ion detected from the raw material Y by the ion chromatography method is preferably 5000 ppm or less with respect to the organic sulfonic acid compound (B), and the weight ratio of the chloride ion to the organic sulfonic acid compound (B) Is preferably not more than 5000 ppm.

The weight ratio of the sulfate ion detected from the raw material Y is more preferably 4000 ppm or less, more preferably 3,000 ppm or less, and still more preferably 2,000 ppm or less based on the organic sulfonic acid compound (B) Is particularly preferable. Similarly, the weight ratio of the chlorine ions detected from the raw material Y is preferably 4000 ppm or less, more preferably 3,000 ppm or less, and particularly preferably 2,000 ppm or less, based on the organic sulfonic acid compound (B).

The method for analyzing sulfate ions and chlorine ions by ion chromatography in the present invention is as described in the examples.

A 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 employed. For example, when the raw material X contains sodium sulfate, there is a method in which a solvent such as methanol or water is added to the raw material X, and an inorganic substance such as sodium sulfate is sedimented and separated. When the raw material X contains sodium chloride, the sodium chloride contained in the raw material X may be removed by an ion exchange membrane, or may be adsorbed by an ion exchange resin.

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

[Chemical Formula 5]

In the general formula (5), c, d and e are integers of 0 or more, and c + d + e = 4 to 16. When c + d + e is less than 4, the effect of reducing roll contamination may be reduced. On the other hand, when c + d + e exceeds 17, the compatibility in the treatment agent is deteriorated and it may become unusable. 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 details of M are the same as M described in the general formula (1).

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

[Organic phosphoric acid ester compound (C)]

The treatment agent of the present invention preferably further contains an organic phosphate ester compound (C) in addition to the above-mentioned smoothing component (A) and the organic sulfonic acid compound (B) in terms of reducing fluff. The organophosphorus ester compound (C) is preferably at least one selected from the compound represented by the general formula (2) and the compound represented by the general formula (3).

In the general formulas (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 of 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 represented by R ¹ include an alkyl group and an alkenyl group. The carbon number of R ¹ is preferably 8 to 24, more preferably 12 to 24. The number of carbon atoms of R ¹ may be distributed, R ¹ may be linear, branched, unsaturated or unsaturated.

A ¹ O is an oxyalkylene group having 2 to 4 carbon atoms. M, which is the number of repeating oxyalkylene units, is an integer of 0 to 15, preferably 0 to 10, more preferably 0 to 3, and most preferably, m does not contain a polyoxyalkylene group. (A ¹ O) _m is preferably a polyoxyalkylene group having an oxyalkylene unit of 50 mol% or more as an oxyethylene unit.

n is an integer of 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.

In the case of 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) , ≪ / RTI >

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, potassium and the like. Examples of the ammonium group and the organic amine group include groups 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 for the organic sulfonic acid compound (B).

The organic phosphate ester compound (C) includes an organic phosphate ester compound (C1) represented by n = 1 in the formula (2) and an organic phosphate ester compound (C2) represented by n = 2 in the formula (2) (C3) represented by Y = 1 and Q = R ¹ O (A ¹ O) _m in the organic phosphoric acid ester compounds (C1), (C2) and the general formula (3) Mixture. These mixtures may contain an organic phosphate ester compound (C4) represented by Y = 1 and Q = hydrogen atom in the general formula (3).

The P nuclear integral ratio (%) of the organic phosphate ester compounds (C1), (C2), (C3) and (C4) and inorganic phosphoric acid is calculated from the integral value of each phosphorus-derived peak in ³¹ P- . The P nuclear integral ratio (%) is calculated by taking the sum of the integral values of the organic phosphoric ester compounds (C1), (C2), (C3), (C4) and inorganic phosphoric acid as 100%. The inorganic phosphoric acid will be described later.

The percentage of P nuclei in the organic phosphate ester compound (C1) is preferably 25 to 85%, more preferably 35 to 80%, and even more preferably 40 to 70%. The percentage of P nuclei in the organophosphate ester compound (C2) is preferably 15 to 65%, more preferably 20 to 60%, and still more preferably 25 to 55%. The percentage of P nuclei integrated in the organic phosphate ester compound (C3) is preferably 0 to 50%, more preferably 0 to 45%, and even more preferably 0 to 40%. The P nuclear integral ratio (%) of the organic phosphoric ester compound (C4) is preferably 0 to 7%, more preferably 0 to 6%, and even more preferably 0 to 5%. The P nuclear integral ratio (%) of the inorganic phosphoric acid is preferably 0 to 10%, more preferably 0 to 9%, and even more preferably 0 to 8%.

The method for producing the organic phosphoric acid ester compound (C) is not particularly limited and a known method can be employed. For example, a method for producing an organic phosphoric acid ester compound (C) includes a step (I) of reacting an organic hydroxyl compound represented by R ¹ O (A ¹ O) _m H with an anhydrous phosphoric acid P ₂ O ₅ to obtain a reactant . In the step (I), inorganic phosphoric acid or water may be added to perform the reaction. The method for producing the organic phosphoric acid ester compound (C) may include a step (II) in which water is added to the reactant and hydrolyzed after the step (I). By including the step (II), the ratio of the organic phosphate ester compounds (C3) and (C4) contained in the organic phosphate ester compound (C) can be adjusted. The amount of water to be added to the reactant is preferably 0.01 to 5% by weight, more preferably 0.05 to 4% by weight, and even more preferably 0.1 to 3% by weight based on the organophosphorusester compound (C). When the addition amount of water is less than 0.01% by weight and exceeds 5% by weight, it may become difficult to control the amounts of the organic phosphoric ester compounds (C3) and (C4). The method for producing the organic phosphoric acid ester compound (C) may include a step (III) of neutralizing with an alkali compound having M ¹ after the step (I) or the step (II).

The organophosphorus ester compound (C) is derived from an impurity in anhydrous phosphoric acid or inorganic phosphorus and contains a heavy metal compound such as arsenic. The treating agent of the present invention may contain a heavy metal compound such as arsenic. The weight ratio of the heavy metal compound to the nonvolatile matter in the treating agent is preferably 0.01% by weight or less, more preferably 0.005% by weight or less, still more preferably 0.001% by weight or less, from the viewpoint of the human body and safety against the environment Do.

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

[Nonionic surfactant (D)]

The treatment agent of the present invention is preferably added with a nonionic surfactant (D) in addition to the above-mentioned smoothing component (A) and the organic sulfonic acid compound (B) in order to impart film strength and agglomeration property to the yarn and improve formability. . The nonionic surfactant (D) means that the above-mentioned smoothing component (A) is excluded. The nonionic surfactant (D) may be used alone or in combination of two or more.

Examples of the nonionic surfactant (D) include polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol esters (hereinafter sometimes referred to as polyhydroxy esters), esters in which at least one of the polyhydroxy esters is blocked with a fatty acid, Polyoxyalkylene polyalcohol ethers, polyoxyalkylene polyalcohol fatty acid esters, polyoxyalkylene aliphatic alcohol ethers, fatty acid esters of polyalkylene glycols, polyhydric alcohol fatty acid esters and the like.

(Polyhydroxyester, ester in which at least one of the polyhydroxy esters is blocked with a fatty acid)

The polyhydroxy ester is an ester of a polyoxyalkylene group-containing hydroxy fatty acid and a polyhydric alcohol in structure, and it is preferable that at least two hydroxyl groups among the hydroxyl groups of the polyhydric alcohol are esterified. Therefore, the polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester is an ester having a plurality of hydroxyl groups.

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

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

Examples of the hydroxy fatty acid having 6 to 22 carbon atoms include hydroxycaprylic acid, hydroxycapric acid, hydroxylauric acid, hydroxystearic acid and ricinoleic acid, and hydroxyoctadecanoic acid, Acids are preferred. Examples of the polyhydric alcohol include ethylene glycol, glycerin, sorbitol, sorbitan, trimethylol propane, pentaerythritol and the like, and glycerin is preferable. Examples of the alkylene oxide include alkylene oxides having 2 to 4 carbon atoms such as ethylene oxide, propylene oxide and butylene oxide.

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

When two or more kinds of alkylene oxides are added, the addition order thereof is not particularly limited, and the additional form may be any of a block type and a random type. The addition of the alkylene oxide can be carried out by a known method, but is generally carried out in the presence of a basic catalyst.

The polyhydroxyester can be produced, for example, by esterifying a polyhydric alcohol and a hydroxy fatty acid (hydroxymonocarboxylic acid) under ordinary conditions to obtain an esterified product, and then subjecting the esterified product to an addition reaction with an alkylene oxide . ≪ / RTI > The polyhydroxy ester can be preferably produced also by using natural oils such as castor oil or the like, or using hardened castor oil in which hydrogen is added thereto and addition reaction of an alkylene oxide.

The nonionic surfactant (D) also includes esters in which at least one of the above-mentioned polyhydroxy esters is blocked with a fatty acid. The carbon number of the fatty acid to be blocked is preferably 6 to 24, more preferably 12 to 18. The number of carbon atoms of the hydrocarbon group in the fatty acid may be distributed, and the hydrocarbon group may be linear, 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 lignoceric acid. The method of esterification, reaction conditions and the like are not particularly limited, and known methods and ordinary conditions can be employed.

Examples of esters in which at least one of the polyhydroxy ester and the polyhydroxy ester is blocked with a fatty acid include a hardened castor oil free ethylene oxide adduct, a castor oil ethylene oxide adduct, a hardened castor oil free ethylene oxide adduct Water monooleate, hydrogenated castor oil free ethylene oxide adduct diolate, hydrogenated castor oil free ethylene oxide adduct triolate, castor oil ethylene oxide adduct triolate, hydrogenated castor oil ethylene oxide adduct tristearate , Castor oil ethylene adduct adduct tristearate, curing castor oil free ethylene oxide adduct, hardened castor oil free ethylene oxide adduct adduct triolate, hardening castor oil ethylene adduct adduct tristearate, A castor oil ethylene oxide adduct tristerate is preferred.

(Polyoxyalkylene polyhydric alcohol ether)

The polyoxyalkylene polyhydric alcohol ether is a compound having a structure in which an alkylene oxide such as ethylene oxide, propylene oxide or butylene oxide is added to a polyhydric alcohol.

Examples of the polyhydric alcohol include ethylene glycol, glycerin, trimethylol propane, pentaerythritol, diglycerin, sorbitan, sorbitol, ditrimethylol propane, dipentaerythritol, sucrose and the like. Of these, glycerin, trimethylolpropane and sucrose are preferred.

The number of moles of the alkylene oxide added is preferably 3 to 100, more preferably 4 to 70, and still more preferably 5 to 50. The proportion of ethylene oxide in the alkylene oxide is preferably at least 50 mol%, more preferably at least 80 mol%.

The weight average molecular weight of the polyoxyalkylene polyhydric alcohol ether is preferably 300 to 10000, more preferably 400 to 8000, and still more preferably 500 to 5,000. When the molecular weight is less than 300, the occurrence of fluff or monofilament may not be reduced. On the other hand, when the molecular weight exceeds 10000, the friction of the treatment agent becomes high, so that the occurrence of fluff and single yarn can not be reduced, and it may be rather deteriorated.

Examples of the polyoxyalkylene polyhydric alcohol ether include polyethylene glycol, glycerin ethylene oxide adduct, trimethylolpropane ethylene oxide adduct, pentaerythritol ethylene oxide adduct, diglycerin ethylene oxide adduct, sorbitan ethyleneoxide Adducts of sorbitan ethoxide, propylene oxide adducts, sorbitan ethylene oxide propylene oxide adducts, sorbitol ethylene oxide adducts, sorbitol ethylene oxide propylene oxide adducts, ditrimethylolpropane ethylene oxide adducts, dipentaerythritol ethylene oxide adducts , Sucrose ethylene oxide adduct, and the like, but are not limited thereto.

(Polyoxyalkylene polyhydric alcohol fatty acid ester)

The polyoxyalkylene polyhydric alcohol fatty acid ester is a compound having a structure in which a compound to which an alkylene oxide is added such as ethylene oxide, propylene oxide, butylene oxide and the like is ester-bonded to a polyhydric alcohol.

Examples of polyhydric alcohols include glycerin, trimethylol propane, pentaerythritol, erythritol, diglycerin, sorbitan, sorbitol, ditrimethylol propane, dipentaerythritol, sucrose and the like. Among these, glycerin, diglycerin, sorbitan and sorbitol are preferred.

Examples of fatty acids include fatty acids such as lauric acid, myristic acid, myristic oleic acid, palmitic acid, palmitoleic acid, isocetylic acid, stearic acid, isostearic acid, oleic acid, elaidic acid, linoleic acid, linolenic acid, arachidonic acid, Behenic acid, isodecanoic acid, erucic acid, lignoceric acid, isotetracosonic acid, and the like.

The number of moles of alkylene oxide added is preferably 3 to 100, more preferably 5 to 70, and still more preferably 10 to 50. The proportion of ethylene oxide in the alkylene oxide is preferably at least 50 mol%, more preferably at least 80 mol%.

The weight average molecular weight of the polyoxyalkylene polyhydric alcohol fatty acid ester is preferably 300 to 7000, more preferably 500 to 5,000, and still more preferably 700 to 3,000. When the molecular weight is less than 300, fuming may occur in the heat treatment process, which may deteriorate the environment. In addition, the occurrence of single yarns may not be reduced. On the other hand, when the molecular weight is more than 7000, the friction of the treatment agent becomes high, so that the occurrence of fluff and single yarn can not be reduced, which may be rather worse.

Examples of polyoxyalkylene polyhydric alcohol fatty acid esters include glycerin ethylene oxide adduct monolaurate, glycerin ethylene oxide adduct dilaurate, glycerin ethylene oxide adduct tribolate, trimethylolpropane ethylene oxide adduct tri Sorbitan ethylene oxide adduct adduct monooleate, sorbitan ethylene oxide adduct adduct diolate, sorbitan ethylene oxide adduct triolate, sorbitan ethylene oxide propylene oxide adduct monooleate, sorbitan Ethylene oxide propylene oxide adduct diolate, sorbitan ethylene oxide propylene oxide adduct triolate, sorbitan ethylene oxide propylene oxide adduct tallowate, sucrose ethylene oxide adduct tallowate, and the like. But are not limited thereto.

(Polyoxyalkylene aliphatic alcohol ether)

The polyoxyalkylene aliphatic alcohol ether is a compound having a structure in which an alkylene oxide such as ethylene oxide, propylene oxide, and butylene oxide is added to an aliphatic monohydric alcohol.

Examples of the polyoxyalkylene aliphatic alcohol ether include octyl alcohol, 2-ethylhexyl alcohol, decyl alcohol, lauryl alcohol, tridecyl alcohol, myristyl alcohol, stearyl alcohol, isostearyl alcohol, oleyl alcohol Of alkylene oxide adducts of aliphatic alcohols.

The molar number of addition of the alkylene oxide is preferably 1 to 100 moles, more preferably 2 to 70 moles, and still more preferably 3 to 50 moles. 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 esters of polyalkylene glycols)

The fatty acid ester of polyalkylene glycol is a compound having a structure in which polyoxyethylene glycol, polyoxyethylene polyoxypropylene glycol and fatty acid are ester-bonded. The weight average molecular weight of the polyalkylene glycol is preferably 100 to 1000, more preferably 150 to 800, and even 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, polyethylene glycol monostearate, polyethylene glycol distearate, polyethylene polypropylene glycol monolaurate , Polyethylene polypropylene glycol dilaurate, polyethylene polypropylene glycol monooleate, polyethylene polypropylene glycol diolate, and the like, but are not limited thereto.

(Polyhydric alcohol fatty acid ester)

The polyhydric alcohol fatty acid ester is a compound having a structure in which a polyhydric alcohol and a fatty acid are ester-bonded, excluding the above-mentioned smoothing component (A).

Examples of polyhydric alcohols include ethylene glycol, trimethylol propane, pentaerythritol, erythritol, diethylene glycol, diglycerin, sorbitan, sorbitol, ditrimethylol propane, sucrose and the like. Among these, ethylene glycol, glycerin, diglycerin, sorbitan and sorbitol are preferable.

Examples of the fatty acid include fatty acids such as lauric acid, myristic acid, myristic oleic acid, palmitic acid, palmitoleic acid, isocetylic acid, stearic acid, isostearic acid, oleic acid, elaidic acid, linoleic acid, linolenic acid, , Isoic acid, gadoleic acid, eicosanic acid, behenic acid, isodecanoic acid, erucic acid, lignoceric acid and the like.

The polyhydric alcohol fatty acid ester has at least one or two or more hydroxyl groups.

The weight average molecular weight of the polyhydric alcohol fatty acid ester is preferably 100 to 1000, more preferably 200 to 800, still more preferably 300 to 600.

Examples of the fatty acid ester include glycerin monolaurate, glycerin dilaurate, glycerin monooleate, glycerin diolate, sorbitan monooleate, sorbitan diolate, sucrose monolaurate and sucrose dilaurate. But are not limited thereto.

As the nonionic surfactant (D), it is preferable to use a product obtained by removing the catalyst and the like from the viewpoint of improvement in heat resistance.

[Treatment agent for synthetic fibers]

The treatment agent of the present invention contains a smoothing component (A) and an organic sulfonic acid compound (B) represented by the above general formula (1). Further, the weight ratio of sulfate ions (SO ₄ ^2- ) detected from the nonvolatile matter of the treatment agent by the ion chromatography method is 200 ppm or less, and the weight ratio of the chloride ion (Cl ^- ) is 200 ppm or less. As described above, by setting the sulfuric acid ion and the chlorine ion detected from the nonvolatile matter of the treatment agent to a predetermined weight ratio or less, napping, thread breakage, and roll contamination can be dramatically reduced.

When the weight ratio of the sulfate ion exceeds 200 ppm or when the weight ratio of the chloride ion exceeds 200 ppm, sodium sulfate or sodium chloride is dropped on the stretching roll at the time of spinning and accumulated, On a roll that causes an increase in single yarn or thermal stretching, tar accumulation is accelerated to cause roll contamination.

The method for analyzing sulfate ions and chlorine ions by ion chromatography in the present invention is as described in the examples. The non-volatile component in the present invention refers to an absolutely dry component when the treating agent is heat-treated at 105 ° C to remove a solvent or the like and reaches a constant amount.

From the viewpoint of further enhancing the effect of the present invention, the weight ratio of the sulfate ion is preferably 200 ppm or less, more preferably 150 ppm or less, and further preferably 100 ppm or less. Similarly, the weight ratio of the chlorine ions is preferably 200 ppm or less, more preferably 150 ppm or less, and further preferably 100 ppm or less.

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

The proportion by weight of the smoothing component (A) in the nonvolatile matter of the treating agent is preferably 20 to 70% by weight, more preferably 30 to 65% by weight, still more preferably 40 to 65% Is particularly preferable. If the weight ratio is less than 20% by weight, the napping may increase due to insufficient smoothness. On the other hand, when the weight ratio is more than 70% by weight, when the aggregate is insufficient or when it is emulsified and used, the emulsion stability may be poor and it may become unusable.

The weight ratio of the organic sulfonic acid compound (B) in the nonvolatile matter of the treating agent is 1.25 to 12 wt%, preferably 1.25 to 10 wt%, more preferably 1.25 to 8 wt%, and further preferably 1.25 to 7 wt% Particularly preferably 1.5 to 6% by weight. If the weight ratio is less than 1.25% by weight, roll contamination may not be reduced. On the other hand, when the weight ratio is more than 12% by weight, the friction may increase and the nap may increase.

When the treating agent of the present invention contains the organic phosphoric acid ester compound (C), the weight ratio of the phosphate ion (PO ₄ ^3- ) detected from the nonvolatile matter of the treating agent by the ion chromatography method is preferably 500 ppm or less. If the weight ratio of the phosphate ions is more than 500 ppm, it may fall off on the stretching roll and increase the yarn breakage single yarn. The weight ratio of the phosphate ions is more preferably 400 ppm or less, still more preferably 300 ppm or less, and particularly preferably 200 ppm or less. In some cases, the phosphate ion (PO ₄ ^3- ) is simply referred to as a phosphate ion.

The method of adjusting the weight ratio of the phosphate ions can be carried out by reducing the inorganic phosphoric acid and / or salt thereof contained in the raw material Z containing the organic phosphoric acid ester compound (C), adjusting the amount of the raw material Z, A method of filtering the treatment agent using a filter aid such as diatomaceous earth can be used.

When the treating agent of the present invention includes the organic phosphoric acid ester compound (C), the weight ratio of the organic phosphoric ester compound (C) in the nonvolatile matter of the treating agent is preferably 0.05 to 10 wt%, more preferably 0.08 to 8 wt% , More preferably from 0.1 to 7% by weight.

When the treating agent of the present invention contains a nonionic surfactant (D), the weight ratio of the nonionic surfactant (D) in the nonvolatile matter of the treating agent is preferably 20 to 70% by weight, more preferably 25 to 65% , More preferably from 30 to 65 wt%, and particularly preferably from 30 to 60 wt%.

(Other components)

The treating agent for synthetic fibers according to the present invention is preferably used in order to impart emulsification of the treating agent, adhesion assisting property to the fibers, washing of the treating agent from the fibers, antistatic property to the fibers, A surfactant other than the organic sulfonic acid compound (B), the organic phosphoric acid ester compound (C) and the nonionic surfactant (D) may be contained. Examples of such surfactants include anionic surfactants such as fatty acid soap; Cationic surfactants such as alkylamine salts, alkylimidazolinium salts and quaternary ammonium salts; Amphoteric surfactants such as lauryldimethylbetaine and stearyldimethylbetaine; Dimethyl lauryl amine oxide, and the like. These surfactants may be used alone or in combination of two or more. The weight ratio of the surfactant to the nonvolatile matter of the treating agent in the case of containing these surfactants is not particularly limited, but is preferably 0.01 to 15% by weight, more preferably 0.1 to 10% by weight. The surfactant herein means a substance having a weight average molecular weight of less than 1,000.

In addition, the treating agent for synthetic fibers of the present invention may further contain an antioxidant to impart heat resistance. Examples of the antioxidant include known ones such as phenol-based, thio-based, and phosphite-based ones. The antioxidant may be used alone or in combination of two or more. The weight ratio of the antioxidant to the non-volatile content of the treating agent when the antioxidant is contained is not particularly limited, but is preferably 0.1 to 5 wt%, more preferably 0.1 to 3 wt%.

The treating agent for synthetic fibers of the present invention may further contain a stock stabilizer (e.g., water, ethylene glycol, propylene glycol). The weight ratio of the stock stabilizer to the treating agent is preferably from 0.1 to 30% by weight, and more preferably from 1 to 20% by weight.

The treating agent for synthetic fibers of the present invention may be composed of the above-mentioned components consisting solely of non-volatile components, may consist of non-volatile components and an undiluted stabilizer, may be diluted with low-viscosity mineral oil, Emulsified water-based emulsion. When the treating agent for synthetic fibers of the present invention is an aqueous emulsion in which nonvolatile matter is emulsified in water, the concentration of nonvolatile matter is preferably 5 to 35% by weight, more preferably 6 to 30% by weight. The viscosity (30 캜) of the treatment agent diluted with the low-viscosity mineral oil is preferably 3 to 120 mm ² / s and more preferably 5 to 100 mm ² / s in view of uniformly imparting the nonvolatile matter to the fiber material .

The method for producing the treating agent for synthetic fibers of the present invention is not particularly limited and a known method can be employed. The treating agent for synthetic fibers is prepared by adding and mixing the respective constituent components described above in an arbitrary order or in a specific order. From the viewpoint of improving the heat resistance, each component may be purified by removing the catalyst and the like. Particularly, the smoothing component (A) or the nonionic surfactant (D) used in the present invention may contain an inorganic substance. When the effect of the present invention is remarkably lowered, it is preferable to remove the inorganic substance and purify Do. As a method for removing inorganic substances, a known method can be used. For example, if the smoothing component (A) is used, it can be removed by filtration using diatomaceous earth, and a nonionic surfactant (D) And purification can be carried out by adsorption / desorption.

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

The method for producing a synthetic fiber filament yarn according to the present invention includes a step of applying the treating agent for a synthetic fiber of the present invention to a raw synthetic fiber filament yarn. According to the manufacturing method of the invention, it is possible to reduce the occurrence of scum and yarn breakage, and to obtain a synthetic fiber filament yarn excellent in real quality. The raw synthetic fiber filament yarn in the present invention means a synthetic fiber filament yarn which is not treated with a treating agent.

The step of applying the treatment agent for synthetic fibers is not particularly limited and a known method can be adopted. Normally, a treating agent for synthetic fibers is applied in the spinning process of raw synthetic fiber filament yarn. After the treatment agent is applied, it is stretched by a heat roller, heat set is performed, and wound. In this way, when the treatment agent is applied and then the film is heat-elongated without winding once, the treating agent for a synthetic fiber of the present invention can be preferably used. For example, in the case of polyester or nylon, 210 to 260 deg. C for industrial materials and 110 to 220 deg. C for medical use are assumed.

As described above, the synthetic fiber treating agent to be imparted to the raw synthetic fiber filament yarn may be a treating agent consisting solely of non-volatile matter, a treating agent diluted with non-volatile matter to a low viscosity mineral oil, or an aqueous emulsion treating agent emulsifying non- For example. Examples of the applying method include, but are not limited to, guide lubrication, roller lubrication, dipping lubrication, spray lubrication, and the like. Of these, guide lubrication and roller lubrication are preferred in view of ease of management of the applied amount.

The non-volatile matter content of the treating agent for synthetic fibers is preferably 0.05 to 5% by weight, more preferably 0.1 to 3% by weight, and even more preferably 0.1 to 2% by weight based on the raw material synthetic fiber filament yarn. If it is less than 0.05% by weight, the effect of the present invention may not be exhibited. On the other hand, if it exceeds 5% by weight, the nonvolatile matter of the treatment agent tends to fall off into a yarn path, and the tar on the heat roller remarkably increases, leading to fluff and single yarn.

(Raw Materials) Examples of the synthetic fiber filament yarns include filament yarns of synthetic fibers such as polyester fibers, polyamide fibers and polyolefin fibers. The treating agent for synthetic fibers of the present invention is suitable for synthetic fibers such as polyester fibers, polyamide fibers and polyolefin fibers. As the polyester fiber, a polyester (PET) having ethylene terephthalate as a main constituent unit, a polyester (PTT) having trimethylene ethylene terephthalate as a main constituent unit, a polyester having a main constituent unit of butylene ethylene terephthalate (PBT), and a polyester (PLA) having lactic acid as a main constituent unit. Examples of the polyamide fiber include nylon 6 and nylon 66. Examples of the polyolefin fiber include polypropylene, polyethylene, and the like For example. A method for producing the synthetic fiber filament yarn is not particularly limited and a known method can be employed.

(Fiber structure)

The fiber structure of the present invention includes the synthetic fiber filament yarn obtained by the above-mentioned production method of the present invention. Specifically, a fabric woven with a water-jet loom, an air-jet loom, or a rapier loom using a synthetic fiber filament yarn of the present invention for a synthetic fiber, and a fabric woven with a loom, a warp, It is knitted. Examples of the use of the fiber structure include industrial materials such as a tire cord, a seat belt, an air bag, a fishing net, a rope, and a medical use. A method for producing a fabric or a knitted fabric is not particularly limited and a known method can be employed.

[Example]

Hereinafter, the present invention, which describes the present invention by way of examples, is not limited to the examples described herein. In the sentence and in the table, "%" means "% by weight".

[Raw material X containing the 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 Corp., organic sulfonic acid compound (B) 93 wt%) was used. The raw material X-1 contains a large amount of glauber's salt. The content (weight ratio) of the sulfate ion (SO ₄ ^2- ) and the chloride ion (Cl ^- ) contained in the raw material X-1 was measured by ion chromatography to find that the sulfate ion was added to the organic sulfonic acid compound (B) 25950 ppm, and the chlorine ion was 62 ppm.

(Raw material X-2)

As the raw material X-2 containing the organic sulfonic acid compound (B), Mercolat 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. The content (weight ratio) of the sulfate ion (SO ₄ ^2- ) and the chloride ion (Cl ^- ) contained in the raw material X-2 was measured by ion chromatography to find that the sulfate ion was added to the organic sulfonic acid compound (B) 820 ppm, and the chlorine ion was 30170 ppm.

[Preparation of raw material Y containing the 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 raw materials X-1 and X-2 containing the organic sulfonic acid compound (B) and removing the inorganic substances. The inorganic substance removal method may be a publicly known method and is not limited to the purification method described in the examples.

(Preparation of raw material Y-1)

550 parts of methanol and 400 parts of ion-exchanged water were mixed and warmed at 45 ± 5 ° C. 700 parts of the above raw material X-1 was slowly added with stirring to dissolve completely. Next, this solution was allowed to stand at room temperature for 20 hours, and the drip was settled. The supernatant containing no gum was taken out and subjected to vacuum distillation at 60 to 80 캜 to remove a part of methanol and water to obtain a raw material Y-1 containing 70% by weight of the organic sulfonic acid compound (B).

The content (weight ratio) of the sulfate ion (SO ₄ ^2- ) and the chloride ion (Cl ^- ) contained in the raw material Y-1 was measured by ion chromatography to find that the sulfate ion was added to the organic sulfonic acid compound (B) 1085 ppm, and the chlorine ion was 60 ppm.

(Preparation of raw material Y-2)

600 parts of ion-exchanged water was heated to 80 ± 5 ° C, and 400 parts of the raw material X-2 was slowly added thereto with stirring to completely dissolve it. Next, this solution was cooled to 40 占 폚, and sodium chloride was then removed using an ion exchange resin to obtain a raw material Y-2 containing 40 wt% of the organic sulfonic acid compound (B).

The content (weight ratio) of the sulfate ion (SO ₄ ^2- ) and the chloride ion (Cl ^- ) contained in the raw material Y-2 was measured by ion chromatography to find that the sulfate ion was added to the organic sulfonic acid compound (B) 105 ppm, and the chlorine ion was 2115 ppm.

[Preparation of raw materials Z-1 to Z-6 containing an organic phosphoric acid ester compound (C)] [

(Preparation of raw material Z-1)

820 parts of isocetyl alcohol was added to the reaction vessel, and 180 parts of pentanoic acid at a temperature of 60 占 폚 and 5 占 폚 were added in small amounts while paying attention to the reaction temperature. Thereafter, the raw material Z-1 was aged at 75 占 폚 for 3 hours to prepare a raw material Z-1 containing 100% by weight of the organic phosphoric acid ester compound (C).

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

(Preparation of raw material Z-2)

800 parts of an alcohol having a carbon number of C11 to 15 was added to the reaction vessel and 200 parts of pentanoic acid at a temperature of 60 占 폚 and 5 占 폚 were added in small amounts while paying attention to the reaction temperature. Thereafter, the mixture was aged at 75 ± 5 ° C for 3 hours to prepare a raw material Z-2 containing the organic phosphate ester compound (C).

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

(Preparation of raw material Z-3)

To 997 parts of the raw material Z-2 prepared above, 3 parts of ion-exchanged water was added and subjected to hydrolysis treatment at 90 占 폚 for 3 hours. Thereafter, dehydration treatment was carried out at 115 캜 for 3 hours to prepare a raw material Z-3 containing the organic phosphate ester compound (C).

The P nuclear integrating ratios of the organic phosphate ester compounds (C1), (C2), (C3), (C4) and inorganic phosphoric acid were 56.72%, 40.49%, 0.00%, 0.00% and 2.78%, respectively.

(Preparation of raw material Z-4)

600 parts of oleyl alcohol was added to the reaction vessel, and 110 parts of pentanoic acid at a temperature of 70 占 폚 and 5 占 폚 were added in small amounts while paying attention to the reaction temperature. Thereafter, the mixture was aged at 75 占 폚 for 3 hours to prepare a raw material Z-4 containing the organic phosphate ester compound (C).

The P nuclear integral ratios of the organic phosphate ester compounds (C1), (C2), (C3), (C4) and inorganic phosphoric acid were 57.65%, 35.26%, 4.57%, 0.44% and 2.07%, respectively.

(Preparation of raw material Z-5)

600 parts of oleyl alcohol was added to the reaction vessel, and 110 parts of pentanoic acid at a temperature of 70 占 폚 and 5 占 폚 were added in small amounts while paying attention to the reaction temperature. Thereafter, the mixture was aged at 70 ± 5 ° C for 3 hours. Subsequently, 15 parts of ion-exchanged water was added, hydrolysis was carried out at 90 占 폚 for 3 hours, and then 200 parts of dibutylethanolamine was slowly added thereto to neutralize the raw material Z- 5 was prepared.

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

(Preparation of raw material Z-6)

To 970 parts of the raw material Z-1 prepared above, 30 parts of ion-exchanged water was added and subjected to hydrolysis treatment at 90 占 폚 for 3 hours. Thereafter, dehydration treatment was carried out at 115 캜 for 3 hours to prepare a raw material Z-3 containing the organic phosphate ester compound (C).

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

The P nuclear integral ratio of the organic phosphate ester compounds (C1), (C2), (C3), (C4) and inorganic phosphoric acid was calculated by the following method using ³¹ P-NMR.

Weighed (稱量) a nonvolatile content of about 30 mg of a measurement sample in a sample tube for NMR of 5 ㎜ diameter, were subjected to addition of heavy water (D2O) of about 0.5 ml by dissolving a deuterated solvent, ³¹ P-NMR measurements ( AVANCE 400, 162 MHz, manufactured by BRUKER).

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

The components described in Tables 2 and 3 were mixed and stirred until homogeneous to prepare a treating agent. Using each of the prepared treating agents, the fouling accumulation of the fins, the wiping of the fins, and the fluctuation of the tensile force were evaluated by the following method. The results are shown in Tables 2 and 3.

The numerical values of the non-volatile components in the treating agents shown in Tables 2 and 3 indicate the weight ratios of the respective components (raw materials X, Y and Z, these non-volatile components) in the non-volatile component of the treating agent. Details of the treating agent components in Tables 2 and 3 are shown in Table 1.

(Method of measuring sulfuric acid ion (SO ₄ ^2- ), chlorine ion (Cl ^- ), phosphate ion (PO ₄ ^3- )

5 g of the sample (nonvolatile matter of the treatment agent or the nonvolatile matter of the raw materials X, Y and Z) was precisely weighed and 95 g of ultrapure water was added little by little with stirring to prepare an aqueous solution. . 2 ml of the prepared aqueous solution is passed through a pre-treatment cartridge (ODS (chemically bonded to an octadecyl group) with silica gel, and the lipophilic substance is removed, and the resulting solution is subjected to ion chromatography analysis. The detection was carried out under the following ion chromatographic conditions. The amount of sulfate ion (SO ₄ ^2- ), phosphoric acid ion (PO ₄ ^3- ) and chlorine ion (Cl ^- ) were calculated by measuring the amount of detection by the peak area ratio to the standard solution of the concentration. The quantitative limit was 0.6 ppm or less for sulfate ion (SO ₄ ^2- ), 1.0 ppm or less for chlorine ion (Cl ^- ), and 0.3 ppm or less for phosphate ion (PO ₄ ^3- ). * In Tables 2 and 3 indicates the quantitative limit or less.

<Conditions for Ion Chromatography>

Device: manufactured by Dionex, using ICS-1500 suppressor

Analytical column: manufactured by Dionex, IonPac AS14 inner diameter 4.0 mm length 50 mm

Guard column: manufactured by Dionex, IonPac AG14 inner diameter 4.0 mm x length 250 mm

Eluent: 3.5 mmol Na ₂ CO ₃ , 1.0 mmol NaHCO ₃

Flow rate: 1.5 ml / min

(Contamination accumulation of pins, contamination wiping of pins, evaluation of tension fluctuation)

The treating agent prepared above was quantitatively added in an amount of 20% by weight to 1000 deniers and 96 filaments of non-poured polyester filaments, passed through rollers heated to 150 캜 by a running yarn friction meter, volatile components were removed , Contacted with a transparent chromium pin which had been heated to 250 DEG C and was transparently painted, was run for 4 hours at an initial tension of 500 g and a scanning speed of 2 m / min, and the degree of fouling accumulation of fins, The tension fluctuation was evaluated. In order to make a more stringent evaluation, 20 wt% of a treating agent was added.

The degree of fouling accumulation of the pins was evaluated according to the following criteria.

◎: little contamination is recognized

○: Some contamination is recognized

×: Contamination is surely accumulated

The tension variation value was calculated by the following equation.

(G) = initial tension (g) = tension (g) after running yarn for 4 hours

The tension fluctuation was evaluated from the tension fluctuation value by the following criteria.

◎: 0 g to less than 30 g

○: 30 g or more and less than 50 g

×: 50 g or more

The contamination wiping property of the pin was evaluated by the following method.

The contamination on the chrome pin which formed the spot and was transparent was dipped in a solution of sodium hydroxide dissolved in water and glycerin and wiped off. The wipeability was evaluated by the number of times required until wiping.

◎: Less than 5 wipes can wipe off contamination

○: can be wiped with less than 5 times and less than 20 wipes

×: Can not be wiped with more than 20 wipes

[Table 1]

[Table 2]

[Table 3]

As can be seen from Tables 2 and 3, in the examples, the treating agent which makes the sulfate ions and chlorine ions detected from the nonvolatile matter of the treating agent to be a predetermined ratio or less is used, so that there is almost no fouling accumulation of the fins, This is extremely good. That is, the roll contamination at the time of producing the synthetic fibers can be reduced, and the cleaning intervals of the rolls can be lengthened to reduce the cleaning frequency. It is also understood that the tension fluctuation value is extremely small and the fluff and yarn breakage can be dramatically reduced.

On the other hand, in the comparative example, the proportion of sulfate ion or chloride ion detected from the nonvolatile matter of the treatment agent is high, and accordingly, the contamination accumulation of fins is large, and the wiping property is poor. In addition, it can be seen that the tension fluctuation value is extremely large, and a lot of fluff and yarn breakage occur.

[Industrial applicability]

The synthetic fiber treating agent of the present invention is preferable for synthetic fiber filament yarns used for industrial materials such as tarpaulins, tire cords, seat belts, air bags, fishing nets, ropes, sling and the like, and medical applications such as fabrics and knits.

Claims (11)

A smoothing component (A); And
The organic sulfonic acid compound (B) represented by the following general formula (1)
Wherein the treating agent for synthetic fibers comprises,
The weight ratio of the organic sulfonic acid compound (B) to the nonvolatile matter of the treating agent is 1.25 to 12 wt%
Treating agent for synthetic fibers having a weight ratio of sulfate ions (SO ₄ ^2- ) detected from nonvolatile matter of the treating agent by ion chromatography to 200 ppm or less and a weight ratio of chlorine ion (Cl ^- ) of 200 ppm or less,
[Chemical Formula 1]

(Wherein a and b are integers of 0 or more and a + b = 5 to 17, and M is a hydrogen atom, an alkali metal, an ammonium group or an organic amine group). The method according to claim 1,
Wherein the weight ratio of the smoothing component (A) in the treating agent is 20 to 70 wt%. 3. The method according to claim 1 or 2,
Wherein the weight ratio of the organic sulfonic acid compound (B) to the nonvolatile matter of the treating agent is 1.25 to 7 wt%. 3. The method according to claim 1 or 2,
Further contains an organic phosphate ester compound (C)
Wherein the weight ratio of the phosphate ion (PO ₄ ^3- ) detected from the nonvolatile matter of the treating agent by the ion chromatography method is 500 ppm or less. 5. The method of claim 4,
Wherein the weight ratio of the organic phosphoric ester compound (C) to the nonvolatile matter of the treating agent is 0.05 to 5 wt%. 5. The method of claim 4,
Wherein the organic phosphoric acid ester compound (C) is at least one selected from a compound represented by the following general formula (2) and a compound represented by the following general formula (3)
(2)

(In the general 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 And M ¹ is a hydrogen atom, an alkali metal, an ammonium group or an organic amine group)
(3)

(In the general 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, 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 , and Y is 1 or 2. 3. The method according to claim 1 or 2,
A treatment agent further comprising a nonionic surfactant (D). 8. The method of claim 7,
Wherein the weight ratio of the nonionic surfactant (D) to the nonvolatile matter of the treating agent is 20 to 70% by weight. A synthetic fiber filament yarn to which a treating agent according to claim 1 is added to a raw filament yarn. A process for producing a synthetic fiber filament yarn comprising the step of applying the treating agent according to claim 1 to a raw synthetic fiber filament yarn. A fibrous structure comprising the synthetic fiber filament yarn of claim 9 and / or the synthetic fiber filament yarn obtained by the manufacturing method of claim 10.