JP7153407B1 - Treatment agent for polyester synthetic fiber, composition containing treatment agent for polyester synthetic fiber, and polyester synthetic fiber - Google Patents

Abstract

Kind Code: A1 A polyester synthetic fiber treatment agent or the like is provided that can achieve both of the effects of improving the antistatic properties and improving the flexibility of fibers to which the synthetic fiber treatment agent is applied. The present invention provides a polyester synthetic fiber treatment agent containing a prescribed silicone (A), a prescribed silicone (B), an anion component, and optionally a prescribed silicone (C), wherein the polyester It is characterized in that the content of silicone (C) in the synthetic fiber treatment agent is less than 10% by mass. [Selection figure] None

Description

TECHNICAL FIELD The present invention relates to a treating agent for polyester synthetic fibers, a composition containing the treating agent for polyester synthetic fibers , and a polyester synthetic fiber.

For example, in the process of spinning and drawing synthetic fibers, the finishing process, etc., a treatment of attaching a synthetic fiber treatment agent to the surface of the fiber may be performed from the viewpoint of friction reduction, antistatic property, bundling property, etc. of the synthetic fiber. .

Conventionally, processing agents for synthetic fibers disclosed in Patent Documents 1 to 4 are known. Patent Document 1 discloses a silicone emulsion composition containing a silicone containing a modified silicone having a functional group such as an amino group as an essential component, a surfactant containing a polyalkylene oxide adduct as an essential component, and water. . Patent Document 2 discloses a water repellent composition containing an amino-modified silicone, a silicone resin, and an alkylpolysiloxane. Patent Document 3 discloses a silicone oil composition containing a silicone oil having a prescribed siloxane structure and a prescribed polyoxyalkylenealkyl or alkenyl ether. Patent Document 4 discloses a silicone emulsion composition comprising dimethylsilicone and/or amino-modified silicone, a surfactant that is a certain polyoxyalkylene alkyl ether, and water.

JP 2013-177495 A WO2019/131456 JP 2020-59799 A Japanese Patent No. 4749677

However, conventional processing agents for synthetic fibers have not been able to sufficiently achieve both of the effects of improving the antistatic properties and improving the flexibility of the fibers to which the processing agents for synthetic fibers have been applied.

As a result of research aimed at solving the above problems, the present inventors found that a composition containing a predetermined silicone and an anion component is suitable for a polyester synthetic fiber treatment agent.

In order to solve the above problems, the polyester synthetic fiber treatment agent of one embodiment of the present invention comprises the following silicone (A), the following silicone (B), an anion component, the following silicone (D), and optionally The gist is that the following silicone (C) is contained, and the content of the silicone (C) in the treatment agent is less than 10% by mass.

Silicone (A): modified silicone having an amino group in the molecule.
Silicone (B): A silane coupling agent having at least one functional group selected from a methoxy group, an ethoxy group, an amino group, and an isocyanate group in the molecule and containing no epoxy group.

Silicone (C): At least one selected from silicone resin, dimethyl silicone, and alkyl-modified silicone, excluding those corresponding to the silicone (A) and silanol-modified silicones having a number average molecular weight of 20000 or more and less than 200000 .

Silicone (D): A silanol-modified silicone having a number average molecular weight of 20,000 or more and less than 200,000.
In order to solve the above problems, the polyester synthetic fiber treatment agent of another aspect of the present invention comprises the following silicone (A), the following silicone (B), an anionic component, the following nonionic surfactant, and optionally contains the following silicone (C), and the content of the silicone (C) in the treatment agent is less than 10% by mass.

Silicone (A): modified silicone having an amino group in the molecule.
Silicone (B): A silane coupling agent having at least one functional group selected from a methoxy group, an ethoxy group, an amino group, and an isocyanate group in the molecule and containing no epoxy group.

Silicone (C): At least one selected from silicone resin, dimethyl silicone, and alkyl-modified silicone, excluding those corresponding to the silicone (A) and silanol-modified silicones having a number average molecular weight of 20000 or more and less than 200000 .

Nonionic surfactant: A compound obtained by adding a total of 3 to 50 mol or less of an alkylene oxide having 2 to 3 carbon atoms to 1 mol of a monovalent to tetravalent alcohol having 2 to 18 carbon atoms, and poly At least one selected from block copolymers of oxyethylene chains and polyoxypropylene chains.

In the polyester synthetic fiber treatment agent, the content of the silicone (B) may be 5 parts by mass or more and 200 parts by mass or less when the content of the silicone (A) is 100 parts by mass.

In the polyester synthetic fiber treatment agent, the anion component may include at least one selected from organic acids, alkylsulfonic acids, alkyl phosphates, polyoxyalkylene alkyl phosphates, and metal salts thereof.

The polyester synthetic fiber treatment agent may further contain the following nonionic surfactants.
Nonionic surfactant: A compound obtained by adding a total of 3 to 50 mol or less of an alkylene oxide having 2 to 3 carbon atoms to 1 mol of a monovalent to tetravalent alcohol having 2 to 18 carbon atoms, and poly At least one selected from block copolymers of oxyethylene chains and polyoxypropylene chains.

In the polyester synthetic fiber treatment agent, the silicone (A) is 5% by mass or more and 80% by mass or less, the silicone (B) is 1% by mass or more and 25% by mass or less, and the silicone (C) is 0% by mass or more. Less than 10% by mass, 5% to 90% by mass of the silicone (D), 1% to 25% by mass of the nonionic surfactant, and 0.1% to 25% by mass of the anionic component. may be contained at a ratio of

In order to solve the above-mentioned problems, another aspect of the present invention provides a composition containing a treating agent for polyester synthetic fibers, comprising the treating agent for polyester synthetic fibers and a solvent .
In order to solve the above problems, the gist of a polyester synthetic fiber according to another aspect of the present invention is that the polyester synthetic fiber treatment agent adheres to the polyester synthetic fiber.

The polyester synthetic fiber may be applied to wadding.

According to the present invention, it is possible to improve the antistatic property and flexibility of the fiber to which the synthetic fiber treatment agent is applied.

<First Embodiment>
A first embodiment of the polyester synthetic fiber treatment agent (hereinafter also referred to as treatment agent) of the present invention will be described below. The treatment agent of this embodiment contains silicone (A), silicone (B), and an anion component shown below. In addition, it may optionally contain a silicone (C) shown below. Furthermore, it contains a nonionic surfactant or silicone (D) shown below.

(Silicone (A))
The silicone (A) used for the treatment agent of this embodiment is a modified silicone having an amino group in the molecule. The amino group is a side chain type in which an amino group is introduced to a silicon atom other than the terminal of the main chain, even in a terminal amino-modified silicone in which an amino group is introduced to the terminal silicon atom of polydimethylsiloxane, which is the main chain. Amino-modified silicone may be used. In addition, silicone (A) may be a commercial product defined by viscosity and functional group equivalent.

The viscosity of the silicone (A) at 25° C. is preferably from 10 mPa·s to 30000 mPa·s, more preferably from 25 mPa·s to 10000 mPa·s. Ranges with any combination of the above upper and lower limits are also envisioned. By defining such a range, the handling of the formulation can be improved, and the effects of the present invention can be exhibited more effectively.

The functional group equivalent of silicone (A) is preferably 100 g/mol or more and 20000 g/mol or less, more preferably 500 g/mol or more and 15000 g/mol or less. Ranges with any combination of the above upper and lower limits are also envisioned. By setting the amount within such a range, the affinity with the polyester synthetic fiber can be improved, and the flexibility of the fiber to which the treatment agent is applied can be exhibited more effectively.

These silicones (A) may be used singly or in combination of two or more.
The lower limit of the content of silicone (A) in the treatment agent is preferably 3% by mass or more, more preferably 5% by mass or more. When the content is 3% by mass or more, the flexibility of the fibers to which the treatment agent is applied can be improved. The upper limit of the content of silicone (A) in the treatment agent is preferably 85% by mass or less, more preferably 80% by mass or less. When the content is 85% by mass or less, the bulkiness of the fiber to which the treatment agent is applied can be improved. Ranges with any combination of the above upper and lower limits are also envisioned.

(Silicone (B))
The silicone (B) used for the treatment agent of the present embodiment is a silane containing at least one functional group selected from methoxy, ethoxy, amino, and isocyanate groups in the molecule and not containing an epoxy group. It is a coupling agent. The silicone (B) can improve the flexibility of the treated fibers in particular. Specific examples of silicone (B) include N-2-(aminoethyl)-3-aminopropylmethyldimethoxysilane, 3-aminopropyltriethoxysilane, N-2-(aminoethyl)-3-aminopropyltri methoxysilane, methyltrimethoxysilane, methyltriethoxysilane, 3-isocyanatopropyltriethoxysilane and the like.

These silicones (B) may be used singly or in combination of two or more.
The lower limit of the content of silicone (B) in the treatment agent is preferably 0.5% by mass or more, more preferably 1% by mass or more. When the content ratio is 0.5% by mass or more, the flexibility of the fibers to which the treatment agent is applied can be improved. The upper limit of the content of silicone (B) in the treatment agent is preferably 30% by mass or less, more preferably 25% by mass or less. When the content is 30% by mass or less, the stability of the processing agent during use, particularly the emulsion stability when the processing agent is made into an emulsion state, can be improved. Ranges with any combination of the above upper and lower limits are also envisioned.

When the content of silicone (A) in the treatment agent is 100 parts by mass, the lower limit of the content of silicone (B) is preferably 5 parts by mass or more, more preferably 6 parts by mass or more. When the content is 5 parts by mass or more, the flexibility of the fibers to which the treatment agent is applied can be improved. When the content of silicone (A) is 100 parts by mass, the upper limit of the content of silicone (B) is preferably 200 parts by mass or less, more preferably 150 parts by mass or less. When the content is 200 parts by mass or less, the flexibility of the fiber to which the treatment agent is applied can be improved.

(Silicone (C))
The silicone (C) used in the treatment agent of the present embodiment is at least one selected from silicone resins, dimethyl silicones, and alkyl-modified silicones, and corresponds to the silicone (A) and has a number average molecular weight of Excludes silanol-modified silicones of 20,000 or more and less than 200,000. Silicone (C) may optionally be included in the treating agent.

Examples of the silicone resin include MQ silicone resin, MDQ silicone resin, T silicone resin, MTQ silicone resin, and the like.
Here, M, D, T and Q described with respect to the silicone resin will be explained. These notation methods are generally used as a notation method for components constituting silicone resins, where M is a monofunctional structural unit R ¹ R ² R ³ SiO _1/2 The functional building block R ⁴ R ⁵ SiO _2/2 , T is the trifunctional building block R ⁶ SiO _3/2 and Q is the tetrafunctional building block SiO _4/2 . R ¹ to R ⁶ are hydrocarbon groups having 1 to 24 carbon atoms, —R ^a NHR ^b NH ₂ (wherein R ^a and R ^b are hydrocarbon groups having 2 or 3 carbon atoms) or —R ^c NH ₂ ( In the formula, ^Rc is an organic amino group, a vinyl group, or a carbinol group represented by a hydrocarbon group having 2 or 3 carbon atoms.

The dimethyl silicone is not particularly limited, but preferably has a viscosity of 5 mPa·s or more and 5000 mPa·s or less at 25°C. Known dimethylsilicone defined by viscosity can be employed as appropriate.

Examples of the alkyl-modified silicone include those obtained by introducing an introduced organic group consisting of —C _a H _2a+1 into the side chain of a silicone oil, which is a linear polymer consisting of siloxane bonds.
The alkyl-modified silicone is not particularly limited, but preferably has a viscosity of 5 mPa·s or more and 5000 mPa·s or less at 25°C. Known alkyl-modified silicones defined by viscosity can be used as appropriate.

These silicones (C) may be used singly or in combination of two or more.
The content of silicone (C) in the treatment agent is less than 10% by mass. When the content of silicone (C) is less than 10% by mass, the antistatic properties of the fiber to which the treatment agent is applied are not impaired.

(anion component)
The anionic component used in the treatment agent of the present embodiment is an anionic compound, such as an acid or a salt thereof. The anionic component can improve the antistatic properties of the treated fibers in particular.

Examples of acids include inorganic acids, organic acids, fatty acids, alkylsulfonic acids, alkylsulfuric acids, polyoxyalkylenealkylsulfuric acids, alkylphosphates, polyoxyalkylenealkylphosphates, fatty acid sulfates, oil sulfates, and the like. and the like.

Specific examples of inorganic acids or salts thereof include hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, carbonic acid, sodium hydrogensulfate, sodium dihydrogenphosphate, disodium hydrogenphosphate, sodium hydrogencarbonate and the like.

Specific examples of organic acids include citric acid, tartaric acid, lactic acid, malic acid, succinic acid, fumaric acid, maleic acid, gluconic acid, glucuronic acid, and benzoic acid.
As the fatty acid, a known fatty acid can be appropriately used, and it may be a saturated fatty acid or an unsaturated fatty acid. Moreover, it may be linear or may have a branched chain structure. Moreover, it may be a monovalent fatty acid or a polyvalent carboxylic acid (polybasic acid).

Specific examples of saturated fatty acids include formic acid, acetic acid, propionic acid, butyric acid, valeric acid, hexanoic acid (caproic acid), octylic acid (2-ethylhexanoic acid), octanoic acid (caprylic acid), nonanoic acid, and decanoic acid. (capric acid), dodecanoic acid (lauric acid), tetradecanoic acid (myristic acid), hexadecanoic acid (palmitic acid), octadecanoic acid (stearic acid), eicosanoic acid (arachidic acid), docosanoic acid (behenic acid), tetracosanoic acid, etc. is mentioned.

Specific examples of unsaturated fatty acids include crotonic acid, myristoleic acid, palmitoleic acid, oleic acid, vaccenic acid, eicosenoic acid, linoleic acid, α-linolenic acid, γ-linolenic acid, and arachidonic acid.

Specific examples of polyvalent carboxylic acids (polybasic acids) include (1) dibasic acids such as succinic acid, fumaric acid, maleic acid, adipic acid and sebacic acid, (2) tribasic acids such as aconitic acid, (3) Aromatic dicarboxylic acids such as benzoic acid, terephthalic acid, isophthalic acid and 2,6-naphthalene dicarboxylic acid, (4) Aromatic tricarboxylic acids such as trimellitic acid, (5) Aromatic tetracarboxylic acids such as pyromellitic acid Carboxylic acid etc. are mentioned.

Among these fatty acids, fatty acids having 8 or more and 18 or less carbon atoms are preferable from the viewpoint of excellent antistatic properties of fibers to which a treatment agent is applied.
Specific examples of alkylsulfonic acids include laurylsulfonic acid (dodecylsulfonic acid), myristylsulfonic acid, cetylsulfonic acid, oleylsulfonic acid, stearylsulfonic acid, tetradecanesulfonic acid, dodecylbenzenesulfonic acid, secondary alkylsulfonic acid ( C13-15) and the like.

Specific examples of alkyl sulfuric acid include lauryl sulfate, oleyl sulfate, stearyl sulfate, and the like.
Specific examples of polyoxyalkylene alkyl sulfuric acid include polyoxyethylene lauryl ether sulfate, polyoxyalkylene (polyoxyethylene, polyoxypropylene) lauryl ether sulfate, polyoxyethylene dodecyl ether sulfate, and polyoxyethylene oleyl ether. Sulfuric acid ester and the like can be mentioned.

Specific examples of alkyl phosphates include lauryl phosphate, cetyl phosphate, octyl phosphate, oleyl phosphate, and stearyl phosphate.

Specific examples of the polyoxyalkylene alkyl phosphate include polyoxyethylene lauryl ether phosphate, polyoxyethylene oleyl ether phosphate, and polyoxyethylene stearyl ether phosphate.

Specific examples of fatty acid sulfates include castor oil fatty acid sulfate, sesame oil fatty acid sulfate, tall oil fatty acid sulfate, soybean oil fatty acid sulfate, rapeseed oil fatty acid sulfate, palm oil fatty acid sulfate, lard fatty acid sulfate, Examples include beef tallow fatty acid sulfate, whale oil fatty acid sulfate, and the like.

Specific examples of the fats and oils sulfate include castor oil sulfate, sesame oil sulfate, tall oil sulfate, soybean oil sulfate, rapeseed oil sulfate, palm oil sulfate, lard sulfate, Examples include beef tallow sulfate, whale oil sulfate, and the like.

Examples of salts include ammonium salts, amine salts, metal salts and the like. Examples of metal salts include alkali metal salts and alkaline earth metal salts. Specific examples of alkali metals constituting alkali metal salts include sodium, potassium, and lithium. Alkaline earth metals constituting the alkaline earth metal salt include metals corresponding to group 2 elements such as calcium, magnesium, beryllium, strontium, and barium.

Any of a primary amine, a secondary amine, and a tertiary amine may be sufficient as the amine which comprises an amine salt. Specific examples of amines constituting amine salts include (1) methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, N—N-diisopropylethylamine, butylamine, dibutylamine, 2-methylbutylamine, and tributylamine. , octylamine, dimethyllaurylamine, etc. (2) aromatic amines or heterocyclic amines such as aniline, N-methylbenzylamine, pyridine, morpholine, piperazine, and derivatives thereof, (3) monoethanolamine , N-methylethanolamine, diethanolamine, triethanolamine, isopropanolamine, diisopropanolamine, triisopropanolamine, dibutylethanolamine, butyldiethanolamine, octyldiethanolamine, lauryldiethanolamine and other alkanolamines; (5) polyoxyalkylene alkyl amino ethers such as polyoxyethylene lauryl amino ether and polyoxyethylene steryl amino ether; and (6) ammonia.

For example, among the anionic components described above, metal salts of fatty acids and the like constitute anionic surfactants. Therefore, an anionic surfactant may be applied as an anionic component.
These anion components may be used singly or in combination of two or more.

Among these, organic acids, alkylsulfonic acids, alkyl phosphates, polyoxyalkylene alkyl phosphates, and metal salts thereof are preferred. By using such a compound, it is possible to improve the stability of the processing agent, particularly the emulsion stability when the processing agent is made into an emulsion.

The lower limit of the content of the anion component in the treatment agent is preferably 0.1% by mass or more, more preferably 1% by mass or more. When the content is 0.1% by mass or more, the antistatic properties of the fibers to which the treatment agent is applied can be particularly improved. The upper limit of the content of the anion component in the treatment agent is preferably 80% by mass or less, more preferably 30% by mass or less, and particularly preferably 25% by mass or less. When the content is 80% by mass or less, the flexibility of the treated fiber can be improved. Ranges with any combination of the above upper and lower limits are also envisioned.

(Silicone (D))
The processing agent of this embodiment may further contain a silicone (D) shown below. By blending the silicone (D) with the treatment agent, the antistatic property of the fiber to which the treatment agent is applied can be improved.

The silicone (D) used in the treatment agent of this embodiment is a silanol-modified silicone having a number average molecular weight of 20,000 or more and less than 200,000. As the silanol-modified silicone, a dimethylsiloxane compound in which a hydroxyl group, also expressed as a silanol group, is directly bonded to the terminal silicon atom of the main chain can be applied.

The lower limit of the number average molecular weight of the silanol-modified silicone is 20,000 or more, preferably 100,000 or more. The upper limit of the number average molecular weight of the silanol-modified silicone is less than 200,000, preferably 150,000 or less. By specifying the number average molecular weight of the silanol-modified silicone within this range, the effect of the present invention can be improved. Ranges with any combination of the above upper and lower limits are also envisioned. The number average molecular weight of the silanol-modified silicone can be measured using gel permeation chromatography (GPC). These silicones (D) may be used singly or in combination of two or more.

The lower limit of the content of silicone (D) in the treatment agent is preferably 2% by mass or more, more preferably 5% by mass or more. When the content is 2% by mass or more, the bulkiness of the fiber to which the treatment agent is applied can be improved. The upper limit of the content of silicone (D) in the treatment agent is preferably 92% by mass or less, more preferably 90% by mass or less. When the content is 92% by mass or less, the stability of the processing agent, particularly the emulsion stability when the processing agent is in an emulsion state, can be improved. Ranges with any combination of the above upper and lower limits are also envisioned.

(Nonionic surfactant)
The treatment agent of the present embodiment may further contain a nonionic surfactant shown below. Containing a nonionic surfactant in the processing agent can improve the stability of the processing agent, particularly the emulsion stability when the processing agent is in an emulsion state.

As the nonionic surfactant provided for the treatment agent of the present embodiment, a total of 3 alkylene oxides having 2 to 3 carbon atoms are added to 1 mol of monovalent to tetravalent alcohol having 2 to 18 carbon atoms. At least one selected from a compound added with mol or more and 50 mol or less, and a block copolymer of a polyoxyethylene chain and a polyoxypropylene chain.

Specific examples of monovalent alcohols used as raw materials for nonionic surfactants include (1) ethanol, propanol, butanol, pentanol, hexanol, octanol, nonanol, decanol, undecanol, dodecanol, tridecanol, and tetradecanol. , pentadecanol, hexadecanol, heptadecanol, octadecanol and other linear alkyl alcohols, (2) isopropanol, isobutanol, isohexanol, 2-ethylhexanol, isononanol, isodecanol, isododecanol, isotridecanol (3) linear alkenyl alcohols such as (3) tetradecenol, hexadecenol, heptadecenol, octadecenol, etc.; 4) branched alkenyl alcohols such as isohexadecenol and isooctadecenol; (5) cyclic alkyl alcohols such as cyclopentanol and cyclohexanol; Aromatic alcohols and the like can be mentioned.

Specific examples of dihydric to tetrahydric polyhydric alcohols used as raw materials for nonionic surfactants include ethylene glycol, propylene glycol, 1,3-propanediol, 1,2-butanediol, 1,3- butanediol, 1,4-butanediol, 2-methyl-1,2-propanediol, 1,5-pentanediol, 1,6-hexanediol, 2,5-hexanediol, 2-methyl-2,4- pentanediol, 2,3-dimethyl-2,3-butanediol, glycerin, 2-methyl-2-hydroxymethyl-1,3-propanediol, trimethylolpropane, sorbitan, pentaerythritol and the like.

Examples of the alkylene oxide used as a raw material for forming the (poly)oxyalkylene structure of the nonionic surfactant include alkylene oxides having 2 or more and 3 or less carbon atoms. Specific examples of alkylene oxide include ethylene oxide and propylene oxide. The number of moles of alkylene oxide to be added is appropriately set, but is preferably 3 to 50 mol, more preferably 5 to 40 mol. Ranges with any combination of the above upper and lower limits are also envisioned. The number of moles of alkylene oxide added indicates the number of moles of alkylene oxide per 1 mole of alcohol in the starting material. One type of alkylene oxide may be used alone, or two types may be used in appropriate combination. When two types of alkylene oxides are applied, their addition form may be block addition, random addition, or a combination of block addition and random addition, and is not particularly limited.

A block copolymer of a polyoxyethylene chain and a polyoxypropylene chain is not particularly limited as long as it has a polyoxypropylene chain with low hydrophilicity and a polyoxyethylene chain with high hydrophilicity and has surface activity. . The number of polyoxyethylene chains and polyoxypropylene chains in the molecule is not particularly limited. and two polyoxyethylene chains sandwiching it.

The number of moles of ethylene oxide to be added to form a polyoxyethylene chain is not particularly limited, and may be, for example, 5 mol or more and 50 mol or less. The number of moles of propylene oxide to be added to form the polyoxypropylene chain is not particularly limited, and may be, for example, 5 mol or more and 50 mol or less.

Specific examples of nonionic surfactants include, for example, polyoxyethylene (6 mol: indicates the number of moles of alkylene oxide added (hereinafter the same)) polyoxypropylene (2) dodecyl ether, polyoxyethylene (10) C12-13 branched Examples include alkyl ethers, polyoxyethylene (25) polyoxypropylene (15) block ethers, and the like.

These nonionic surfactants may be used singly or in combination of two or more.
The lower limit of the nonionic surfactant content in the treatment agent is preferably 1% by mass or more, more preferably 3% by mass or more. When the content is 1% by mass or more, the stability of the processing agent during use, particularly the emulsification stability when the processing agent is made into an emulsion state, can be improved. The upper limit of the nonionic surfactant content in the treatment agent is preferably 30% by mass or less, more preferably 25% by mass or less. When the content is 30% by mass or less, the flexibility of the fibers to which the treatment agent is applied can be improved. Ranges with any combination of the above upper and lower limits are also envisioned.

In the treatment agent, silicone (A) is 5% by mass or more and 80% by mass or less, silicone (B) is 1% by mass or more and 25% by mass or less, silicone (C) is 0% by mass or more and less than 10% by mass, silicone (D ) in a proportion of 5 mass % to 90 mass %, a nonionic surfactant in a proportion of 1 mass % to 25 mass %, and an anionic component in a proportion of 0.1 mass % to 25 mass %. By defining such a range, the effect of the present invention can be improved.

(preservation form)
From the viewpoint of improving formulation stability, the treatment agent may be configured as a two-part treatment agent or a three-part treatment agent as shown below.

The two-component treatment agent is a two-component first treatment agent for polyester synthetic fibers containing silicone (A), an anion component, and optionally silicone (C) (hereinafter referred to as "two-component first treatment agent" ) and a two-component second treatment agent for polyester synthetic fibers containing silicone (B) (hereinafter referred to as a “two-component second treatment agent”). The two-component first treatment agent is contained so that the content of silicone (C) in the mixture in which the two-component first treatment agent and the two-component second treatment agent are mixed is less than 10% by mass. ing. In addition, the two-component first treatment agent may further contain a silicone (D) and a nonionic surfactant. The two-component processing agent consists of a two-component first processing agent and a two-component second processing agent that is separate from the two-component first processing agent during storage or distribution. It is The two-component treatment agent is prepared as a mixture in which the two-component first treatment agent and the two-component second treatment agent are mixed at the time of use.

The three-part treatment agent is a three-part first treatment agent for polyester synthetic fibers containing silicone (A), an anion component, and optionally silicone (C) (hereinafter, "three-part first treatment agent" ), a 3-component second treatment agent for polyester synthetic fibers containing silicone (D) (hereinafter referred to as “3-component second treatment agent”), and 3 for polyester synthetic fibers containing silicone (B) It is configured as a set including a formulation type third treatment agent (hereinafter referred to as "three formulation type third treatment agent").

The three-component first treatment agent has a silicone (C) content of 10 in the mixture in which the three-component first treatment agent, the three-component second treatment agent, and the three-component third treatment agent are mixed. It is contained so as to be less than mass %. The three-component treatment agent may contain the nonionic surfactant described above in either one or both of the three-component first treatment agent and the three-component second treatment agent. In addition, in the three-part type treatment agent, the anion component may be contained in the three-part type second treatment agent as well.

The three-component type processing agent includes a three-component type first processing agent and a three-component type second processing agent that are separate from the three-component type first processing agent during storage or distribution. The first treatment agent and the second three-part treatment agent are separately composed of the third treatment agent of three-part type. The three-component treatment agent is prepared by mixing the three-component first treatment agent, the three-component second treatment agent, and the three-component third treatment agent at the time of use.

(solvent)
The treatment agent of the present embodiment is mixed with a solvent as necessary to prepare a composition containing a treatment agent for polyester synthetic fibers (hereinafter referred to as a "treatment agent-containing composition"), and in the form of a treatment agent-containing composition, It may be stored or distributed.

The solvent is a solvent having a boiling point of 105° C. or lower at atmospheric pressure. Examples of solvents include water and organic solvents. Specific examples of organic solvents include lower alcohols such as ethanol and propanol, and low-polar solvents such as hexane. These solvents may be used singly or in combination of two or more. Among these, polar solvents such as water and lower alcohols are preferred from the viewpoint of excellent dispersibility or solubility of each component, and water is more preferred from the viewpoint of excellent handling properties.

Assuming that the total content of the treating agent and the solvent is 100 parts by mass in the treating agent-containing composition, the treating agent is preferably contained in an amount of 10 parts by mass or more and 80 parts by mass or less.
The effects of the treatment agent of the first embodiment will be described.

(1-1) The treatment agent of the first embodiment contains the above-described predetermined silicone and anionic components. Therefore, it is possible to improve the antistatic property and flexibility of the fiber to which the treatment agent is applied. In addition, the stability of the processing agent, particularly the emulsification stability when the processing agent is in an emulsion state, can be improved. Also, the bulkiness of the fiber to which the treatment agent is applied can be improved.

(1-2) The treatment agent of the first embodiment contains a two-component first treatment agent containing silicone (A), an anion component, and optionally silicone (C), and silicone (B). It may be configured as a set including a two-agent type second treatment agent. Such a configuration can improve the formulation stability, particularly storage stability, of the treatment agent.

(1-3) When the treatment agent of the first embodiment contains silicone (D) and the nonionic surfactant described above, silicone (A), an anionic component, and optionally silicone (C). A set comprising a first treatment agent, a second treatment agent containing silicone (D), and a second treatment agent containing silicone (B). Either one or both of the 1-part type second treatment agent and the 3-part type second treatment agent may contain the nonionic surfactant described above. Such a configuration can improve the formulation stability, particularly storage stability, of the treatment agent.

< Reference Embodiment 1 >
Next, Reference Embodiment 1 , which embodies a two -pack type first treatment agent, will be described. The following description focuses on differences from the above embodiment.

The two-component first treatment agent of the present embodiment contains silicone (A), an anion component, and optionally silicone (C). The two-part type first treating agent is used in combination with a two-part type second treating agent containing silicone (B) at the time of use. The two-component first treatment agent has a silicone (C) content of less than 10% by mass in the mixture at the time of use, that is, in the mixture in which the two-component first treatment agent and the two-component second treatment agent are mixed. It is contained so that Moreover, when the processing agent further contains the silicone (D) and the nonionic surfactant described above, the two-component first processing agent may contain the silicone (D) and the nonionic surfactant.

Silicone (A), silicone (B), anionic component, silicone (C), silicone (D), and nonionic surfactant are the same as the components described in the first embodiment.

(solvent)
The two-component first treating agent of the present embodiment is mixed with a solvent as necessary to form a two-component first treating agent-containing composition for polyester synthetic fibers (hereinafter, "two-component first treating agent-containing composition"). ) may be prepared and stored or distributed in the form of a two-part first treatment agent-containing composition.

As the solvent, those exemplified in the first embodiment can be adopted. Assuming that the total content of the two-part first treating agent and the solvent in the two-part first treating agent-containing composition is 100 parts by mass, the two-part first treating agent is 10 parts by mass or more and 80 parts by mass or less. It is preferable to contain at

The effects of the two-pack type first treatment agent of Reference Embodiment 1 will be described. Reference Embodiment 1 has the following effects in addition to the effects of the above embodiment.
(2-1) The two-component first treatment agent of Reference Embodiment 1 contains silicone (A), an anion component, and optionally silicone (C), and two components containing silicone (B) when used. Used in combination with a mold secondary treatment agent. Therefore, it is possible to improve formulation stability, particularly storage stability, of the two-agent type first treatment agent. Further, by adjusting the mixing ratio with the two-pack type second treatment agent, the components of the obtained treatment agent can be adjusted. Also, only the two-pack type first treatment agent can be distributed separately from the two-pack type second treatment agent.

< Reference Embodiment 2 >
Next, Reference Embodiment 2 , which embodies the two-agent type second treatment agent of the present invention, will be described. The following description focuses on differences from the above embodiment.

The two-pack type second treatment agent of the present embodiment contains silicone (B). The two-part second treatment agent is used in combination with a two-part first treatment agent containing silicone (A), an anionic component, and optionally silicone (C). The two-component first treatment agent has a silicone (C) content of less than 10% by mass in the mixture at the time of use, that is, in the mixture in which the two-component first treatment agent and the two-component second treatment agent are mixed. It is contained so that Moreover, when the processing agent further contains the silicone (D) and the nonionic surfactant described above, the two-component first processing agent may contain the silicone (D) and the nonionic surfactant.

Silicone (A), silicone (B), anionic component, silicone (C), silicone (D), and nonionic surfactant are the same as the components described in the first embodiment.

The effects of the two-agent type second treatment agent of Reference Embodiment 2 will be described. Reference Embodiment 2 has the following effects in addition to the effects of the above embodiments.
(3-1) The two-agent type second treatment agent of Reference Embodiment 2 contains silicone (B). Then, when used, it is used in combination with a two-component first treatment agent containing silicone (A), an anionic component, and optionally silicone (C). Therefore, it is possible to improve the formulation stability, particularly the storage stability, of the two-agent type second treatment agent. Further, by adjusting the mixing ratio with the two-pack type first treatment agent, the components of the obtained treatment agent can be adjusted. Also, only the two-pack type second treatment agent can be distributed separately from the two-pack type first treatment agent.

< Reference Embodiment 3 >
Next, Reference Embodiment 3 , which embodies the three-pack type first treatment agent of the present invention, will be described. The following description focuses on differences from the above embodiment.

The three-component first treatment agent of the present embodiment contains silicone (A), an anion component, and optionally silicone (C). The three-component first treatment agent is used in combination with a three-component second treatment agent containing silicone (D) and a three-component third treatment agent containing silicone (B). The nonionic surfactant described above is contained in either one or both of the three-part type first treatment agent and the three-part type second treatment agent.

The three-component first treatment agent contains silicone (C ) is contained so as to be less than 10% by mass. Silicone (A), silicone (B), anionic component, silicone (C), silicone (D), and nonionic surfactant are the same as the components described in the first embodiment.

(solvent)
The three-part first treating agent of the present embodiment is mixed with a solvent as necessary to form a three-part first treating agent-containing composition for polyester synthetic fibers (hereinafter, "three-part first treating agent-containing composition"). ) may be prepared and stored or distributed in the form of a three-part first treatment agent-containing composition.

As the solvent, those exemplified in the first embodiment can be adopted. Assuming that the total content of the 3-part type first treating agent and the solvent is 100 parts by mass in the composition containing the 3-part type first treating agent, the amount of the 3-part type first treating agent is 10 parts by mass or more and 80 parts by mass or less. It is preferable to contain at

The effects of the three-pack type first treatment agent of Reference Embodiment 3 will be described. Reference Embodiment 3 has the following effects in addition to the effects of the above embodiments.
(4-1) The three-part first treatment agent of Reference Embodiment 3 contains silicone (A), an anion component, and optionally silicone (C), and contains silicone (D) at the time of use. It is used in combination with a three-component third treatment agent containing a type second treatment agent and a silicone (B). The nonionic surfactant is contained in either one or both of the three-part type first treatment agent and the three-part type second treatment agent. Therefore, it is possible to improve formulation stability, particularly storage stability, of the 3-dose type first treatment agent. Further, by adjusting the mixing ratio with the 3-part type second and third treatment agents, the components of the resulting treatment agent can be adjusted. In addition, only the three-part type first treatment agent can be distributed separately from the three-part type second and third treatment agents.

< Reference Embodiment 4 >
Next, Reference Embodiment 4 , which embodies the three-agent type second treatment agent of the present invention, will be described. The following description focuses on differences from the above embodiment.

The three-pack type second treatment agent of the present embodiment contains silicone (D). The three-part type second treatment agent includes a three-part type first treatment agent containing silicone (A), an anion component, and optionally silicone (C) and a three-part type third treatment agent containing silicone (B) at the time of use. Used in combination with a treatment agent. The nonionic surfactant described above is contained in either one or both of the three-part type first treatment agent and the three-part type second treatment agent. In addition, in the three-part type treatment agent, the anion component may be contained in the three-part type second treatment agent as well.

The three-component first treatment agent contains silicone (C ) is contained so as to be less than 10% by mass. Silicone (A), silicone (B), anionic component, silicone (C), silicone (D), and nonionic surfactant are the same as the components described in the first embodiment.

(solvent)
The three-component second treatment agent of the present embodiment can be mixed with a solvent if necessary to obtain a composition containing a three-component second treatment agent for polyester synthetic fibers (hereinafter referred to as a "composition containing a three-component second treatment agent"). ) may be prepared and stored or distributed in the form of a three-part second treatment agent-containing composition.

As the solvent, those exemplified in the first embodiment can be adopted. Assuming that the total content of the 3-part type second treating agent and the solvent in the composition containing the 3-part type second treating agent is 100 parts by mass, the amount of the 3-part type second treating agent is 10 parts by mass or more and 80 parts by mass or less. It is preferable to contain at

The effects of the three-pack type second treatment agent of Reference Embodiment 4 will be described. Reference Embodiment 4 has the following effects in addition to the effects of the above embodiments.
(5-1) In the three-agent type second treatment agent of Reference Embodiment 4 , the silicone (D) is contained, and when used, the silicone (A), the anion component, and optionally the silicone (C). It is used in combination with a type 1st treatment agent and a 3-component type 3rd treatment agent containing silicone (B). The nonionic surfactant described above is contained in either one or both of the three-part type first treatment agent and the three-part type second treatment agent. Therefore, it is possible to improve formulation stability, particularly storage stability, of the 3-dose type second treatment agent. Also, by adjusting the mixing ratio with the 3-part type first and third treatment agents, the components of the resulting treatment agent can be adjusted. Also, only the three-pack type second treatment agent can be distributed separately from the three-pack type first and third treatment agents.

< Reference Embodiment 5 >
Next, Reference Embodiment 5 , which embodies the three-pack type third treatment agent of the present invention, will be described. The following description focuses on differences from the above embodiment.

The three-part type third treatment agent of the present embodiment contains silicone (B). The three-part type third treatment agent includes a three-part type first treatment agent containing silicone (A), an anion component, and optionally silicone (C) when used, and a three-part type second treatment agent containing silicone (D). Used in combination with a treatment agent. The nonionic surfactant described above is contained in either one or both of the three-part type first treatment agent and the three-part type second treatment agent.

The three-component first treatment agent contains silicone (C ) is contained so as to be less than 10% by mass. Silicone (A), silicone (B), anionic component, silicone (C), silicone (D), and nonionic surfactant are the same as the components described in the first embodiment.

The effects of the three-pack type third treatment agent of Reference Embodiment 5 will be described. Reference Embodiment 5 has the following effects in addition to the effects of the above embodiments.
(6-1) The three-component third treatment agent of Reference Embodiment 5 contains a silicone (B), and when used, a silicone (A), an anion component, and optionally a silicone (C). It is used in combination with a type 1st treatment agent and a 3-component type 2nd treatment agent containing silicone (D). The nonionic surfactant described above is contained in either one or both of the three-part type first treatment agent and the three-part type second treatment agent. Therefore, it is possible to improve formulation stability, particularly storage stability, of the three-dose type third treatment agent. In addition, by adjusting the mixing ratio with the three-pack type first and second treatment agents, the components of the resulting treatment agent can be adjusted. Also, only the three-pack type third treatment agent can be distributed separately from the three-pack type first and second treatment agents.

<Seventh Embodiment>
Next, a seventh embodiment of the polyester synthetic fiber treatment method of the present invention (hereinafter referred to as "fiber treatment method") will be described.

In the fiber treatment method of the present embodiment, in the case of a two-part treatment agent, a solvent, a two-part first treatment agent of Reference Embodiment 1 , and a two-part second treatment agent of Reference Embodiment 2 are used. It is characterized by applying a diluted solution of the processing agent contained to the polyester synthetic fiber. A method for preparing the diluent includes, for example, a method of adding a two-part type first treatment agent or a composition containing a two-part type first treatment agent and a two-part type second treatment agent to a solvent. The diluent is preferably prepared by adding the two-component first treatment agent-containing composition of Reference Embodiment 1 and the two-component second treatment agent of Reference Embodiment 2 to a solvent. The ratio of the contents of the two-component first processing agent and the two-component second processing agent is such that the mass ratio of the non-volatile matter is the two-component first processing agent and the two-component second processing agent = 99.5/0. .5 to 70/30 is preferred. Operability can be improved by being defined within this range. The non-volatile content is obtained from the mass of the absolute dry matter obtained by heat-treating the object at 105° C. for 2 hours to sufficiently remove volatile substances (the same applies hereinafter).

In the fiber treatment method of the present embodiment, in the case of a three-part treatment agent, a solvent, a three-part first treatment agent of Reference Embodiment 3 , a three-part second treatment agent of Reference Embodiment 4 , It is characterized by applying a diluted solution of the treatment agent containing the 3-pack type third treatment agent of Reference Embodiment 5 to the polyester synthetic fiber. A method of preparing a diluent includes, for example, a solvent, a three-part first treatment agent or a composition containing a three-part first treatment agent, a three-part second treatment agent or a composition containing a three-part second treatment agent, and A method of adding a three-pack type third treatment agent may be mentioned. The diluents consisted of the solvent containing the three-part type first treating agent-containing composition of Reference Embodiment 3 , the three-part type second treating agent-containing composition of Reference Embodiment 4 , and the three-part type third treating agent-containing composition of Reference Embodiment 5 . It is preferably prepared by adding a processing agent.

Examples of the solvent used for preparing the diluent include those exemplified in the first embodiment. The diluent preferably has a non-volatile content of 0.01% by mass or more and 10% by mass or less from the viewpoint of operability.

A form in which a two-part type first treatment agent and a two-part type second treatment agent are used in combination, or a form in which a three-part type first treatment agent, a three-part type second treatment agent and a three-part type third treatment agent are used in combination can arbitrarily change the mixing ratio of each agent. Therefore, even under different manufacturing conditions such as differences in manufacturing facilities or climates such as temperature and humidity, processing agents or dilutions are required to fine-tune the blending ratio and always provide optimal fiber characteristics or fiber manufacturing characteristics. It becomes easier to prepare the liquid.

In order to emulsify the processing agent, each processing agent or composition and solvent may be mixed and stirred using a known stirrer such as a homomixer, homogenizer, colloid mill, line mixer and the like.

The method of treating the fiber is a method of applying the diluted solution obtained as described above to the fiber in, for example, a spun yarn manufacturing process including a spinning or drawing process, a finishing process, or the like.
Fibers to which the diluent is applied include polyester synthetic fibers. Specific examples of polyester synthetic fibers include polyethylene terephthalate (PET), polytrimethylene terephthalate, polybutylene terephthalate, polyethylene naphthalate, polylactic acid, composite fibers containing these polyester resins, and the like. .

Applications of the fibers are not particularly limited, and examples thereof include batting, short fibers, long fibers, spun yarns, and non-woven fabrics. Short fibers generally correspond to staples and do not include long fibers generally called filaments. The length of the short fibers is not particularly limited as long as it corresponds to short fibers in this technical field, and is, for example, 100 mm or less. Among these, the diluent of the present invention is preferably applied to polyester synthetic fibers for wadding. By applying it to polyester synthetic fibers for batting, it is possible to impart texture such as smoothness to stuffing such as stuffed animals, futons, and clothing.

Although there is no particular limitation on the ratio of the diluent attached to the fiber, the final solid content of the diluent is preferably 0.01% by mass or more and 10% by mass or less, more preferably 0.1% by mass or more. It is made to adhere so that the ratio is 3% by mass or less. With such a configuration, the effect of each component can be effectively exhibited. In addition, the method of attaching the diluent is not particularly limited, and known methods depending on the type, form, application, etc. of the fiber, such as roller lubrication, guide lubrication using a metering pump, immersion lubrication, spray lubrication, and the like. can be adopted. When the immersion oiling method is used, the immersion time is preferably 1 minute or more and 5 minutes or less.

The fibers to which the diluent has been applied may be dried or heat treated using known methods. A solvent such as water is volatilized by drying or heat treatment, and fibers to which the components contained in the first treatment agent, the second treatment agent, and the third treatment agent are attached are obtained.

Heat treatment is performed to form a silicone coating on the fiber surface. The heat treatment is preferably performed under conditions of 100° C. or higher and 200° C. or lower. The heating time is appropriately set depending on the treatment temperature and the like, and is preferably 1 minute or more and 20 minutes or less, more preferably 1 minute or more and 15 minutes or less. Such heat treatment accelerates the reaction between the silicone (A) and the silicone (B), forming a silicone coating made of the crosslinked polymer compound on the fiber.

The effects of the fiber treatment method of the seventh embodiment will be described. The seventh embodiment has the following effects in addition to the effects of the above embodiments.
(7-1) The fiber treatment method of the seventh embodiment is a method in which a diluent is applied to the fibers in a spun yarn manufacturing process such as a spinning or drawing process, a finishing process, or the like. In particular, a diluent prepared by adding the two-part first treatment agent of Reference Embodiment 1 or the composition containing the two-part first treatment agent of Reference Embodiment 1 and the two-part second treatment agent of Reference Embodiment 2 to a solvent. In the case of , a diluent having excellent emulsification stability can be obtained. Alternatively, the solvent contains the three-part first treatment agent of Reference Embodiment 3 or the composition containing the three-part first treatment agent and the three-part second treatment agent or three-part second treatment agent of Reference Embodiment 4 . In the case of a diluent prepared by adding the composition and the three-part type third treatment agent of Reference Embodiment 5 , a diluent having excellent emulsification stability can be obtained. Therefore, the effect of each component on batting, short fibers, long fibers, spun yarns, non-woven fabrics, etc. can be effectively exhibited.

(7-2) In the fiber treatment method of the seventh embodiment, the fiber applied with the diluted treatment agent may be heat-treated at 100° C. or higher and 200° C. or lower. Such heat treatment accelerates the reaction between the silicone (A) and the silicone (B) to form a silicone coating made of the crosslinked polymer compound on the fiber. Thereby, a more durable coating is formed and the softness of the fiber can be improved.

Note that the above embodiment may be modified as follows. The above embodiments and the following modifications can be combined with each other within a technically consistent range.
The method for preparing the diluent of the treatment agent in the above embodiment is not particularly limited, and a method other than the preparation method described in the section on the method for treating fibers in the seventh embodiment may be employed. For example, after mixing each silicone, nonionic surfactant, and anionic component which were mentioned above, you may mix with a solvent.

- In each treatment agent, each composition, or diluent of the above-described embodiments, other ingredients are added to maintain the quality of each treatment agent, each composition, or diluent within a range that does not impair the effects of the present invention. As, other solvents, stabilizers, antistatic agents, binders, antioxidants, UV absorbers, organic acids, surfactants other than the above, etc. good. From the viewpoint of efficiently exhibiting the effects of the present invention, the amount of other components other than the solvent that are usually used in processing agents is preferably 10% by mass or less in each processing agent.

Examples will be given below in order to make the configuration and effect of the present invention more specific, but the present invention is not limited to these examples. In the following examples and comparative examples, parts means parts by weight, and % means % by weight, unless otherwise specified.

Test category 1 (preparation of treatment agent)
(Example 1)
As shown in Table 1, modified silicone having an amino group as silicone (A) (side chain type, viscosity: 6000 mPa s, functional group equivalent: 11000 g / mol) (A-1) 6 parts (%), silicone N-2-(aminoethyl)-3-aminopropylmethyldimethoxysilane (functional group: amino group, methoxy group) as (B) (B-1) 5 parts (%), both ends silanol-modified as silicone (D) Silicone (number average molecular weight: 100000) (D-1) 80 parts (%), dodecylsulfonic acid sodium salt (E-1) 4 parts (%) as an anion component, polyoxyethylene (6) polyoxyethylene (6) as a nonionic surfactant A processing agent of Example 1 containing 5 parts (%) of oxypropylene (2) dodecyl ether (F-1) was prepared.

(Examples 2-27, Reference Examples 28-31, Comparative Examples 1-10)
The treating agents of Examples 2 to 27, Reference Examples 28 to 31, and Comparative Examples 1 to 10 consisted of silicone (A) to silicone (D), an anionic component, and a nonionic surfactant in the same manner as the treating agent of Example 1. was prepared so as to contain the ratio shown in Table 1.

Type and content of silicone (A), type and content of silicone (B), type and content of silicone (C), type and content of silicone (D), type and content of anion component, and nonion The type and content of the surfactant are shown in Table 1, "Silicone (A)" column, "Silicone (B)" column, "Silicone (C)" column, "Silicone (D)" column, and "Anion component" column. , respectively shown in the column "Nonionic surfactant". In addition, the content of silicone (B) when the content of silicone (A) in the treatment agent is 100 parts by mass is calculated as "parts by mass of silicone (B) with respect to 100 parts by mass of silicone (A)" in Table 1. column.

表１に記載するシリコーン（Ａ）、シリコーン（Ｂ）、シリコーン（Ｃ）、シリコーン（Ｄ）、アニオン成分、及びノニオン界面活性剤の詳細は以下のとおりである。

Details of silicone (A), silicone (B), silicone (C), silicone (D), anionic components, and nonionic surfactants listed in Table 1 are as follows.

(Silicone (A))
A-1: Modified silicone having an amino group (side chain type, viscosity: 6000 mPa s, functional group equivalent: 11000 g/mol)
A-2: Modified silicone having an amino group (dual-end type, viscosity: 25 mPa s, functional group equivalent: 800 g/mol)
A-3: Modified silicone having an amino group (side chain type, viscosity: 600 mPa s, functional group equivalent: 3700 g/mol)
A-4: Modified silicone having an amino group (side chain type, viscosity: 5000 mPa s, functional group equivalent: 7000 g/mol)
A-5: Modified silicone having an amino group (side chain type, viscosity: 3500 mPa s, functional group equivalent: 1700 g/mol)
A-6: Modified silicone having an amino group (dual-end type, viscosity: 520 mPa s, functional group equivalent: 7000 g/mol)
(Silicone (B))
B-1: N-2-(aminoethyl)-3-aminopropylmethyldimethoxysilane (functional groups: amino group, methoxy group)
B-2: 3-aminopropyltriethoxysilane (functional groups: amino group, methoxy group)
B-3: N-2-(aminoethyl)-3-aminopropyltrimethoxysilane (functional groups: amino group, methoxy group)
B-4: methyltrimethoxysilane (functional group: methoxy group)
B-5: methyltriethoxysilane (functional group: ethoxy group)
B-6: 3-isocyanatopropyltriethoxysilane (functional groups: isocyanate group, ethoxy group)
b-1: 3-glycidoxypropylmethyldimethoxysilane (functional groups: epoxy group, methoxy group)
(Silicone (C))
C-1: polydimethylsiloxane (viscosity: 1000 mPa s)
C-2: Alkyl-modified silicone (viscosity: 500 mPa s)
C-3: Silicone resin (MQ type) (normal temperature solid)
(Silicone (D))
D-1: both terminal silanol-modified silicone (number average molecular weight: 100,000)
D-2: both terminal silanol-modified silicone (number average molecular weight: 150000)
D-3: both terminal silanol-modified silicone (number average molecular weight: 20000)
D-4: both terminal silanol-modified silicone (number average molecular weight: 50000)
D-5: both terminal silanol-modified silicone (number average molecular weight: 200000)
(anion component)
E-1: Dodecylsulfonic acid sodium salt E-2: Octyl phosphate potassium salt E-3: Oleic acid E-4: Acetic acid E-5: Polyoxyethylene (3) dodecyl sulfate sodium salt (nonionic surfactant)
F-1: polyoxyethylene (6) polyoxypropylene (2) dodecyl ether F-2: polyoxyethylene (10) C12-13 branched alkyl ether F-3: polyoxyethylene (25) polyoxypropylene (15) Block ether f-4: polyoxyethylene (40) hydrogenated castor oil test category 2 (emulsifying)
Each treatment agent prepared in Test Section 1 was diluted with deionized water to prepare a diluted solution (emulsion) having a concentration of non-volatile matter of 1.0%. Emulsibility as stability was evaluated using such a diluted solution.

The light transmittance (%) at a wavelength of 750 nm was measured under conditions of 20° C. and 60% RH for the diluted solution of each treatment agent. A spectrophotometer UV-1800 SPECTROPHOTOMETER manufactured by Shimadzu Corporation was used as a measuring device. Emulsifiability of the diluted solution was evaluated according to the following criteria. The results are shown in the "emulsibility" column of Table 1.

Evaluation criteria for emulsifiability ◎ (good): no separation and light transmittance of 50% or more ○ (acceptable): no separation and light transmittance of 30% or more and less than 50% × (poor): If there is separation Test category 3 (flexibility)
Polyester synthetic fiber cotton of 7 denier and cut length of 32 mm, which is generally used for padding of cushions, futons, etc., was used for evaluation. In order to remove the influence of lubricants and the like used in manufacturing polyester synthetic fibers, the fibers were first washed with warm water at 40°C, dried at 80°C for 2 hours, and then evaluated.

The treatment agent of each example prepared in test section 1 was diluted to an active ingredient concentration of 12.5% to prepare a diluted solution in the form of an emulsion. 2.4 g of the emulsion was evenly sprayed onto 100 g of polyester synthetic cotton. After that, it was heat-treated (dried) at 180° C. for 10 minutes, and used as a cotton sample for evaluation. 0.3 g of the treatment agent adheres to 100 g of cotton.

Evaluation of softness The softness of the sample cotton after drying was scored according to the following criteria by five experts in fiber texture evaluation, and the average score of the five people was rounded off to two significant figures. Based on the calculated average points, flexibility was evaluated according to the following criteria. The results are shown in the "Flexibility" column of Table 1.

1 point: When it has the same degree of flexibility as cotton of polyester synthetic fiber to which no treatment agent is attached 2 points: When it feels more flexible than cotton of polyester synthetic fiber to which no treatment agent is attached 3 Score: When feeling greater flexibility than polyester synthetic fiber cotton without treatment ◎ (Good): The average score of 5 people is 2.5 points or more ○ (Good): The average score of 5 people is 2.0 points or more and less than 2.5 points × (bad): the average score of 5 people is less than 2.0 points Test category 4 (antistatic property)
5 g of sample cotton to which each treatment agent prepared in test section 3 was attached was conditioned in a constant temperature room at 20° C. and a relative humidity of 45% for 24 hours. Thereafter, using a known resistance measuring device, the electrical resistance of the polyester synthetic fiber was measured and evaluated according to the following evaluation criteria. The results are shown in the "antistatic property" column of Table 1.

· Evaluation criteria for antistatic property ◎ (good): surface resistance is less than 1.0 × 10 ¹¹ Ω ○ (acceptable): surface resistance is 1.0 × 10 ¹¹ Ω or more and less than 1.0 × 10 ¹² Ω × (poor ): Surface resistance is 1.0 × 10 ¹² Ω or more Test category 5 (bulky)
The bulkiness was evaluated by measuring the compression elastic recovery rate. The compression elastic recovery rate is JIS
Measured by a test method similar to L 2001.

40 g of sample cotton to which each treatment agent was attached prepared in test section 3 was applied to a roller card machine to prepare a 30 cm×100 cm web to which the treatment agent was attached. Four fabrics were prepared by cutting this web into 15 cm×15 cm pieces. A rectangular parallelepiped was prepared by stacking four fabrics so that the fiber directions were perpendicular to each other.

After standing at 20° C. and 40% RH for 30 minutes, a 15 cm×15 cm metal plate (135 g) was placed on the rectangular parallelepiped, and the height (h1) of the rectangular parallelepiped after 1 minute was recorded in units of 0.1 cm. Furthermore, a weight of 1125 g was placed on the metal plate, and after standing still for 24 hours, the height (h2) was recorded and removed. The height of the cuboid (h3) was recorded 1 minute after the weight was removed.

The recovery rate was calculated by the following formula.
Recovery rate (%) = 100 x (h3-h2)/(h1-h2)
It was judged that the higher the recovery rate, the better the bulkiness of the test cotton.

◎ (good): recovery rate (%) is 80% or more ○ (acceptable): recovery rate (%) is 50% or more and less than 80% × (poor): recovery rate (%) is less than 50% Test category 6 (2 Preparation of dosage form first treatment agent)
(Two-component first treatment agent (P-1))
Modified silicone having an amino group as silicone (A) (side chain type, viscosity: 6000 mPa s, functional group equivalent: 11000 g / mol) (A-1) 6.3 parts (%), both ends as silicone (D) Silanol-modified silicone (number average molecular weight: 100000) 84.2 parts (%), dodecylsulfonic acid sodium salt (E-1) 4.2 parts (%) as an anion component, polyoxyethylene (6) as a nonionic surfactant A two-component first treatment agent (P-1) containing 5.3 parts (%) of polyoxypropylene (2) dodecyl ether (F-1) was prepared.

(Two agent type first treatment agents P-2 to P-31)
The two-component first treating agents P-2 to P-31 are similar to the two-component first treating agent (P-1), and contain silicone (A), silicone (C), silicone (D), an anion component, and a nonionic surfactant in the proportions shown in Table 2.

Type and content of silicone (A), type and content of silicone (C), type and content of silicone (D), type and content of anionic component, type and content of nonionic surfactant are shown in the table. 2 "Silicone (A)" column, "Silicone (C)" column, "Silicone (D)" column, "Anionic component" column, and "Nonionic surfactant" column, respectively.

試験区分７（２剤型第２処理剤の調製）
（２剤型第２処理剤（Ｓ－１））
２剤型第２処理剤（Ｓ－１）は、シリコーン（Ｂ）としてＮ－２－（アミノエチル）－３－アミノプロピルメチルジメトキシシラン（官能基：アミノ基、メトキシ基）（Ｂ－１）１００部（％）を含むようにした。

Test section 7 (preparation of two-component second treatment agent)
(Two-agent type second treatment agent (S-1))
The two-component second treatment agent (S-1) contains N-2-(aminoethyl)-3-aminopropylmethyldimethoxysilane (functional groups: amino group, methoxy group) as the silicone (B) (B-1). It was made to contain 100 parts (%).

(Two-part type second treatment agents S-2 to S-6)
The two-part type second treatment agents S-2 to S-6 were prepared so as to contain silicone (B) in the ratio shown in Table 3. The type and content of silicone (B) are shown in the "Silicone (B)" column of Table 3.

試験区分８（製剤安定性の評価）
・２剤型第１処理剤の製剤安定性評価
各２剤型第１処理剤へイオン交換水を加えて濃度を４０％に調整し、ホモジナイザーにより乳化させ、乳化液（２剤型第１処理剤含有組成物）を調製した。得られた乳化液を２０℃、６０％ＲＨの恒温室内にて２４時間温調した。外観を目視で判断し、以下の基準により評価した。結果を表２の「製剤安定性」欄に示す。

Test Category 8 (Evaluation of Formulation Stability)
・Evaluation of formulation stability of two-component first treatment agents agent-containing composition) was prepared. The obtained emulsion was temperature-controlled in a constant temperature room at 20° C. and 60% RH for 24 hours. The appearance was judged visually and evaluated according to the following criteria. The results are shown in the "formulation stability" column of Table 2.

- Formulation stability evaluation of 2-component second treatment agents Each of the 2-component second treatment agents was temperature-controlled in a thermostatic chamber at 20°C and 60% RH for 24 hours. The appearance was judged visually and evaluated according to the following criteria. The results are shown in the "formulation stability" column of Table 3.

・ Evaluation criteria for formulation stability (two-component first treatment agent and two-component second treatment agent)
◎ (Good): No separation × (Not good): Separation Test Category 9 (Preparation of treatment agent from 2-part type 1st treatment agent and 2-part type 2nd treatment agent)
(Example 32)
Treatment of Example 32 by mixing 95% (parts) of the two-component first treatment agent (P-1) shown in Table 4 and 5% (parts) of the two-component second treatment agent (S-1) formulations were prepared.

(Examples 33-58 , Reference Examples 59-62 )
In the same manner as in Example 32, the two-pack type first treatment agent and the two-pack type second treatment agent shown in Table 4 were mixed to prepare the treatment agents of each example. The type and mass ratio of the two-component first processing agent and the type and mass ratio of the two-component second processing agent are shown in Table 4 in the "Two-component first processing agent" column and the "Two-component second processing agent" column. shown in each column.

Emulsifiability, antistatic properties, flexibility, and bulkiness were evaluated in the same manner as in Example 1 using the obtained processing agent of each example. The results are shown in Table 4, "Emulsifiability" column, "Antistatic property" column, "Flexibility" column, and "Bulkiness" column, respectively.

試験区分１０（３剤型第１処理剤の調製）
（３剤型第１処理剤（ＴＰ－１））
シリコーン（Ａ）としてアミノ基を有する変性シリコーン（側鎖型、粘度：６０００ｍＰａ・ｓ、官能基当量：１１０００ｇ／ｍｏｌ）（Ａ－１）９０．５部（％）、アニオン成分としてドデシルスルホン酸ナトリウム塩（Ｅ－１）４．２部（％）、ノニオン界面活性剤としてポリオキシエチレン（６）ポリオキシプロピレン（２）ドデシルエーテル（Ｆ－１）５．３部（％）を含む３剤型第１処理剤（ＴＰ－１）を調製した。

Test section 10 (preparation of 3-dosage first treatment agent)
(3-component first treatment agent (TP-1))
Modified silicone having an amino group as silicone (A) (side chain type, viscosity: 6000 mPa s, functional group equivalent: 11000 g/mol) (A-1) 90.5 parts (%), sodium dodecyl sulfonate as an anion component 3 dosage forms containing 4.2 parts (%) of salt (E-1) and 5.3 parts (%) of polyoxyethylene (6) polyoxypropylene (2) dodecyl ether (F-1) as a nonionic surfactant A first treatment agent (TP-1) was prepared.

(Three agent type first treatment agents TP-2 to TP-26)
The 3-agent type first treatment agents TP-2 to TP-26 contain silicone (A), silicone (C), an anionic component, and a nonionic surfactant in the same manner as the 3-agent type first treatment agent (TP-1). was prepared to contain the ratio shown in Table 5.

The type and content of the silicone (A), the type and content of the silicone (C), the type and content of the anionic component, and the type and content of the nonionic surfactant are shown in the "Silicone (A)" column of Table 5. These are shown in the "Silicone (C)" column, the "Anionic component" column, and the "Nonionic surfactant" column, respectively.

試験区分１１（３剤型第２処理剤の調製）
（３剤型第２処理剤（ＴＳ－１））
シリコーン（Ｄ）として両末端シラノール変性シリコーン（数平均分子量：１０００００）（Ｄ－１）９０．５部（％）、アニオン成分としてドデシルスルホン酸ナトリウム塩（Ｅ－１）４．２部（％）、ノニオン界面活性剤としてポリオキシエチレン（６）ポリオキシプロピレン（２）ドデシルエーテル（Ｆ－１）５．３部（％）を含む３剤型第２処理剤（ＴＳ－１）を調製した。

Test section 11 (preparation of 3-dosage second treatment agent)
(3-component second treatment agent (TS-1))
Both terminal silanol-modified silicone (number average molecular weight: 100000) (D-1) 90.5 parts (%) as silicone (D), dodecylsulfonic acid sodium salt (E-1) 4.2 parts (%) as an anion component A three-part type second treatment agent (TS-1) containing 5.3 parts (%) of polyoxyethylene (6), polyoxypropylene (2), and dodecyl ether (F-1) as nonionic surfactants was prepared.

(Three formulation type second treatment agents TS-2 to TS-26)
The three-part type second treatment agents TS-2 to TS-26 are similar to the three-part type second treatment agent (TS-1), and the silicone (D), the anionic component, and the nonionic surfactant are shown in Table 6. It was prepared to contain at the same ratio.

The type and content of the silicone (D), the type and content of the anionic component, and the type and content of the nonionic surfactant are shown in Table 6 in the "Silicone (D)" column, the "Anionic component" column, and the "Nonionic surfactant Agent” column.

試験区分１２（３剤型第３処理剤の調製）
（３剤型第３処理剤（ＴＴ－１））
３剤型第３処理剤（ＴＴ－１）は、シリコーン（Ｂ）としてＮ－２－（アミノエチル）－３－アミノプロピルメチルジメトキシシラン（官能基：アミノ基、メトキシ基）（Ｂ－１）１００部（％）を含むようにした。

Test section 12 (preparation of 3-dosage third treatment agent)
(3-agent type third treatment agent (TT-1))
The three-component third treatment agent (TT-1) contains N-2-(aminoethyl)-3-aminopropylmethyldimethoxysilane (functional groups: amino group, methoxy group) as silicone (B) (B-1). It was made to contain 100 parts (%).

(Three formulation third treatment agents TT-2 to TT-6)
Three-part type third treatment agents TT-2 to TT-6 were prepared so as to contain silicone (B) in the ratio shown in Table 7. The type and content of silicone (B) are shown in the "Silicone (B)" column of Table 7.

試験区分１３（製剤安定性の評価）
・３剤型第１処理剤の製剤安定性評価
各３剤型第１処理剤へイオン交換水を加えて濃度を４０％に調整し、ホモジナイザーにより乳化させ、乳化液（３剤型第１処理剤含有組成物）を調製した。得られた乳化液を２０℃、６０％ＲＨの恒温室内にて２４時間温調した。外観を目視で判断し、以下の基準により評価した。結果を表５の「製剤安定性」欄に示す。

Test category 13 (evaluation of formulation stability)
・Evaluation of formulation stability of 3-dosage-type first treatment agent agent-containing composition) was prepared. The obtained emulsion was temperature-controlled in a constant temperature room at 20° C. and 60% RH for 24 hours. The appearance was judged visually and evaluated according to the following criteria. The results are shown in the "formulation stability" column of Table 5.

・Evaluation of formulation stability of 3 dosage form 2nd treatment agent Add ion exchange water to each 3 dosage form 2nd treatment agent to adjust concentration to 40%, emulsify with a homogenizer agent-containing composition) was prepared. The obtained emulsion was temperature-controlled in a constant temperature room at 20° C. and 60% RH for 24 hours. The appearance was judged visually and evaluated according to the following criteria. The results are shown in the "formulation stability" column of Table 6.

- Formulation stability evaluation of 3-dose type 3rd treatment agents Each 3-dose type 3rd treatment agent was temperature-controlled in a constant temperature room at 20°C and 60% RH for 24 hours. The appearance was judged visually and evaluated according to the following criteria. The results are shown in the "formulation stability" column of Table 7.

・Evaluation criteria for formulation stability (3-dosage type 1st treatment agent, 3-dosage type 2nd treatment agent, and 3-dosage type 3rd treatment agent)
◎ (good): No separation × (improper): Separation preparation)
(Example 63)
3 dosage type first treatment agent (TP-1) shown in Table 8 6.6% (part), 3 dosage type second treatment agent (TS-1) 88.4% (part), and 3 dosage type No. A processing agent of Example 63 was prepared by mixing 5% (parts) of 3 processing agent (TT-1).

(Examples 64-88)
In the same manner as in Example 63, the 3-pack type first treatment agent, the 3-pack type second treatment agent, and the 3-pack type third treatment agent shown in Table 8 were mixed to prepare the treatment agents of each example. The type and mass ratio of the three-component first treatment agent, the type and mass ratio of the three-component second treatment agent, and the type and mass ratio of the three-component third treatment agent are shown in Table 8, "Three-component first treatment "Third treatment agent" column, "Third agent type second treatment agent" column, and "Three agent type third treatment agent" column.

Emulsifiability, antistatic properties, flexibility, and bulkiness were evaluated in the same manner as in Example 1 using the obtained processing agent of each example. The results are shown in the "emulsibility" column, the "antistatic property" column, the "flexibility" column, and the "bulky property" column in Table 8, respectively.

各表の比較例に対する各実施例の評価結果からも明らかなように、本発明の処理剤は、乳化性を向上できる。また処理剤が付与された繊維は、帯電防止性、柔軟性、及び嵩高性を向上できる。また、本発明の各第１処理剤、第２処理剤、及び第３処理剤は、製剤安定性を向上できる。

As is clear from the evaluation results of each example relative to the comparative examples in each table, the treatment agent of the present invention can improve emulsifiability. In addition, fibers to which a treatment agent is applied can be improved in antistatic properties, flexibility, and bulkiness. Moreover, each of the first treatment agent, the second treatment agent, and the third treatment agent of the present invention can improve formulation stability.

Claims (9)

The following silicone (A), the following silicone (B), an anion component, the following silicone (D), and optionally the following silicone (C), and the content ratio of the silicone (C) in the treatment agent is less than 10% by mass, a treating agent for synthetic polyester fibers.
Silicone (A): modified silicone having an amino group in the molecule.
Silicone (B): A silane coupling agent having at least one functional group selected from a methoxy group, an ethoxy group, an amino group, and an isocyanate group in the molecule and containing no epoxy group.
Silicone (C): At least one selected from silicone resin, dimethyl silicone, and alkyl-modified silicone, excluding those corresponding to the silicone (A) and silanol-modified silicones having a number average molecular weight of 20000 or more and less than 200000 .
Silicone (D): A silanol-modified silicone having a number average molecular weight of 20,000 or more and less than 200,000. The following silicone (A), the following silicone (B), an anionic component, the following nonionic surfactant, and optionally the following silicone (C), and the content ratio of the silicone (C) in the treatment agent is less than 10% by mass, a treating agent for synthetic polyester fibers.
Silicone (A): modified silicone having an amino group in the molecule.
Silicone (B): A silane coupling agent having at least one functional group selected from a methoxy group, an ethoxy group, an amino group, and an isocyanate group in the molecule and containing no epoxy group.
Silicone (C): At least one selected from silicone resin, dimethyl silicone, and alkyl-modified silicone, excluding those corresponding to the silicone (A) and silanol-modified silicones having a number average molecular weight of 20000 or more and less than 200000 .
Nonionic surfactant: A compound obtained by adding a total of 3 to 50 mol or less of an alkylene oxide having 2 to 3 carbon atoms to 1 mol of a monovalent to tetravalent alcohol having 2 to 18 carbon atoms, and poly At least one selected from block copolymers of oxyethylene chains and polyoxypropylene chains. The treatment agent for polyester synthetic fibers according to claim 1 or 2 , wherein the content of the silicone (B) is 5 parts by mass or more and 200 parts by mass or less when the content of the silicone (A) is 100 parts by mass. 4. The anion component according to any one of claims 1 to 3 , wherein the anion component contains at least one selected from organic acids, alkylsulfonic acids, alkyl phosphates, polyoxyalkylene alkyl phosphates, and metal salts thereof. A treatment agent for polyester synthetic fibers. The treating agent for polyester synthetic fibers according to Claim 1, further comprising the following nonionic surfactant.
Nonionic surfactant: A compound obtained by adding a total of 3 to 50 mol or less of an alkylene oxide having 2 to 3 carbon atoms to 1 mol of a monovalent to tetravalent alcohol having 2 to 18 carbon atoms, and poly At least one selected from block copolymers of oxyethylene chains and polyoxypropylene chains. In the polyester synthetic fiber treatment agent, the silicone (A) is 5% by mass or more and 80% by mass or less, the silicone (B) is 1% by mass or more and 25% by mass or less, and the silicone (C) is 0% by mass or more. Less than 10% by mass, 5% to 90% by mass of the silicone (D), 1% to 25% by mass of the nonionic surfactant, and 0.1% to 25% by mass of the anionic component. The polyester synthetic fiber treatment agent according to claim 5 , which is contained in a ratio of A polyester synthetic fiber treatment agent-containing composition comprising the polyester synthetic fiber treatment agent according to any one of claims 1 to 6 and a solvent. A polyester synthetic fiber to which the polyester synthetic fiber treatment agent according to any one of claims 1 to 6 is adhered. 9. Polyester synthetic fiber according to claim 8 applied to wadding.