JP7595502B2 - Artificial hair fiber, head accessory product containing same, and method for manufacturing artificial hair fiber - Google Patents

Description

It relates to artificial hair fibers, head accessories containing the same, and a manufacturing method for artificial hair fibers.

In addition to human hair, artificial hair is used in head accessories such as wigs, hairpieces, false hair, hair bands, and doll hair. Fibers for artificial hair include various synthetic fibers such as polyvinyl chloride fibers, polyester fibers, acrylic fibers, and polyamide fibers, as well as collagen fibers such as regenerated collagen fibers. To improve the feel and combability of artificial hair, a fiber treatment agent is applied. For example, Patent Document 1 proposes that a flame-retardant treatment agent containing an oxazoline group-containing acrylic resin and an organically modified silicone is attached to the artificial fiber to improve combability and feel.

International Publication No. 2019/131117

However, head accessories such as wigs are often used for long periods of time, and there is an issue that the combability, i.e., combing durability, significantly decreases after long-term use, leaving room for improvement. In addition, the artificial hair fiber described in Prior Art 1 generates static electricity when combed, resulting in excessive volume and making it difficult to manage, and there remains an issue that it is difficult to apply to the hairstyle or hair product desired by the user.

The present invention relates to a fiber for artificial hair having a fiber treatment composition attached to its surface, the fiber treatment composition including at least a urethane bond structure and a silicone compound.

The present invention can provide artificial hair fibers that have a smooth feel and good combing durability, and head ornament products that contain the same. It can also provide artificial hair fibers that are not too voluminous and are less difficult to manage, and hair products that contain the same.

FIG. 1 is an explanatory diagram of a method for measuring comb durability.

The present inventors have conducted extensive research into artificial hair fibers having a fiber treatment composition attached to the surface of the artificial hair fiber and head ornament products containing the same, and have found that by attaching a specific amount of a fiber treatment composition containing a urethane bond structure and a silicone compound to an artificial hair fiber, an excellent hair product can be obtained that has a smoother feel than conventional artificial hair fibers, excellent combing durability, and is easy to manage because static electricity generation is suppressed, resulting in the present invention. The reason why an excellent hair product having a smooth feel, excellent combing durability, and easy to manage can be obtained is speculative, but is thought to be as follows. The urethane bond structure is a prepolymer and can be crosslinked at a relatively low temperature, so that the urethane bond structure can be crosslinked on the surface of the artificial hair fiber to easily form a coating on the fiber surface, and it is presumed that the coating improves the feel, etc. A fiber treatment composition with a high crosslinking temperature is not preferable because it dissolves polyvinyl chloride fibers in particular, but the urethane bond structure is preferable because it crosslinks at a relatively low temperature. Furthermore, the coexistence of a silicone compound further suppresses the generation of static electricity, so that hair products containing the fibers have excellent combability, a smooth feel, and can be easily styled to give the desired hairstyle.
<Urethane bond structure>
A fiber treatment composition is applied to the surface of the fiber for artificial hair of the present invention. The fiber treatment composition contains at least a urethane bond structure and a silicone oil compound.
The urethane bond structure has a structure represented by formula (1). Although not particularly limited, for example, a compound in which toluene diisocyanate is added to all hydroxyl groups of trimethylolpropane can be mentioned, and among them, a blocked urethane prepolymer in which all terminal isocyanate groups are blocked with methyl ethyl ketone oxime and a compound having a structure represented by formula (2) is preferred.

The urethane bond structure is contained in the artificial hair fiber in an amount of 0.02% by weight or more and 0.2% by weight or less, preferably 0.025% by weight or more and 0.15% by weight or less. If it is less than 0.02% by weight, the film is formed, but the film is formed in small amounts, making it difficult to obtain excellent combing durability, which is not preferred. If it is more than 0.2% by weight, the film is formed in too large an amount, which makes the touch feel worse, which is not preferred.
<Silicone Compound>
The silicone compound is not particularly limited as long as it is dimethyl silicone and/or an organic modified silicone in which a portion of the methyl groups of dimethyl silicone are substituted with an organic functional group. For example, from the viewpoint of improving the feel and combing ease, amino modified silicone oil and/or epoxy modified silicone oil are preferred.
Amino-modified silicone oils are those in which some of the methyl groups of organochlorosilane are replaced with amino groups. The amino groups may be monoamines (-R ¹ -NH ₂ ) or diamines (-R ¹ -NH-R ² -NH ₂ ). ^{R 1} and R ² may be alkyl groups having 1 to 6 carbon atoms or alkylene groups having 1 to 6 carbon atoms.
The amino-modified silicone oil is not particularly limited, but from the viewpoint of easily imparting smoothness to the artificial hair fiber, it is desirable that the amine equivalent is in the range of 500 or more and less than 4000. Furthermore, from the viewpoint of improving the touch and combing durability of the artificial hair fiber, the weight average molecular weight is preferably 5000 to 200000, more preferably 5000 to 170000, and even more preferably 5000 to 150000.
The amino-modified silicone oil may be a commercially available product that is mixed with water, an emulsifier, etc. and is sold in the form of an aqueous emulsion or an aqueous solution.
The dimethyl silicone oil is not particularly limited, but from the viewpoint of further improving combability and tactile feel, the viscosity is preferably from 10,000 to 50,000,000 mm ² /s, and more preferably from 20,000 to 1,000,000 mm ² /s. The viscosity of the silicone compound is the kinetic viscosity (mm ² /s) measured at 25°C using an Ubbelohde viscometer according to ASTM D 445-46T.
As the dimethyl silicone oil, commercially available products that are marketed in the form of aqueous emulsion or aqueous solution containing water and emulsifier may be used. These silicone compounds may be used alone or in combination of two or more. Also, two or more silicone compounds may be used.
The silicone compound is preferably contained in an amount of 0.01% by weight or more and 0.3% by weight or less in terms of non-volatile matter relative to the fiber for artificial hair. When the content of the silicone compound in the fiber for artificial hair is within the above-mentioned range, the touch and combing durability are improved. The content of the silicone compound can be measured as described below.
<Polyalkylene oxide compound>
The fiber treatment composition may further contain a polyalkylene oxide compound. By containing a polyalkylene oxide compound, it is possible to impart antistatic properties to the artificial hair fiber.
The polyalkylene oxide compound is not particularly limited, but for example, a copolymer of ethylene oxide and propylene oxide can be suitably used. The polymerization of the alkylene oxide can be carried out according to a known method, and the alkylene oxide may be of a random type or a block type.
From the viewpoints of touch and antistatic properties, the polyalkylene oxide compound preferably has a weight average molecular weight of 2,000 to 25,000, and more preferably 5,000 to 20,000.
The polyalkylene oxide compound is contained in the artificial hair fiber in an amount of 0.005% by weight or more and 0.025% by weight or less, preferably 0.01% by weight or more and 0.02% by weight or less. If it is less than 0.005% by weight, the amount is too small and is not preferable from the viewpoint of antistatic properties. If it is more than 0.025% by weight, it is not preferable from the viewpoint of touch.
<Quaternary ammonium salt>
The fiber treatment composition may further contain a quaternary ammonium salt. By containing a quaternary ammonium salt, it is possible to impart antistatic properties to the artificial hair fiber. Examples of the quaternary ammonium salt include stearyl trimethyl ammonium chloride, octadecyl trimethyl ammonium chloride, and dodecyl trimethyl ammonium chloride.

The fiber treatment composition may further include an aqueous medium. The fiber treatment composition including the above-mentioned urethane bond structure, silicone compound, polyalkylene oxide compound, quaternary ammonium salt, etc. may be dispersed or dissolved in an aqueous medium. The aqueous medium is preferably water, and examples of the aqueous medium include distilled water, ion-exchanged water, and ultrapure water.
The content of the quaternary ammonium salt is preferably 0.005% by weight or more and 0.027% by weight or less based on the artificial hair fiber, from the viewpoint of antistatic properties.
<Artificial hair fibers>
As the fiber for artificial hair, one or more types selected from the group consisting of synthetic fibers and collagen fibers can be used. The synthetic fibers are not particularly limited, but examples thereof include polyvinyl chloride fibers, polyester fibers, acrylic fibers, polyamide fibers, etc. Among these, one or more types selected from the group consisting of polyvinyl chloride fibers, acrylic fibers, and polyester fibers are preferable.
Moreover, examples of collagen fibers include regenerated collagen fibers.
From the viewpoint of suitability for artificial hair, the fibers for artificial hair preferably have a single fiber fineness of 10 to 150 dtex, more preferably 30 to 120 dtex, and even more preferably 40 to 100 dtex.
If necessary, the artificial hair fiber may appropriately contain various known additives such as heat resistance agents, light stabilizers, fluorescent agents, stabilizing assistants, plasticizers, ultraviolet absorbers, antioxidants, antistatic agents, antistatic agents, fillers, flame retardants, pigments, lubricants, etc. In some cases, known additives such as foaming agents, crosslinking agents, tackifiers, conductivity imparting agents, fragrances, etc. may also be used.

As the polyvinyl chloride fiber, a fiber composed of polyvinyl chloride can be used. Polyvinyl chloride may be a homopolymer of vinyl chloride, or a copolymer of vinyl chloride and other copolymerizable monomers. The other copolymerizable monomers are not particularly limited, but examples thereof include vinyl esters such as vinyl acetate and vinyl propionate, acrylic esters such as butyl acrylate and 2-ethylhexyl acrylate, and olefins such as ethylene and propylene. In terms of fiber properties and transparency, a homopolymer of vinyl chloride, a vinyl chloride-ethylene copolymer, a vinyl chloride-vinyl acetate copolymer, and the like are preferably used. In the copolymer, the content of the other copolymerizable monomer is not particularly limited and can be appropriately determined according to the purpose.

The polyvinyl chloride fiber may contain a heat stabilizer from the viewpoint of spinning stability. The heat stabilizer is not particularly limited, but for example, a tin-based heat stabilizer, a Ca-Zn-based heat stabilizer, a hydrotalcite-based heat stabilizer, an epoxy-based heat stabilizer, or a β-diketone-based heat stabilizer can be used. The heat stabilizer may be used alone or in combination of two or more types. The heat stabilizer is not particularly limited, but for example, 0.2 to 5 parts by weight can be blended with 100 parts by weight of polyvinyl chloride.

The polyvinyl chloride fiber may contain a lubricant from the viewpoint of spinning stability. The lubricant is not particularly limited, but for example, metal soap-based lubricants, polyethylene-based lubricants, higher fatty acid-based lubricants, ester-based lubricants, higher alcohol-based lubricants, etc. can be used. One type of lubricant may be used alone, or two or more types may be used in combination. The lubricant is not particularly limited, but for example, 0.2 to 5 parts by weight can be blended with 100 parts by weight of polyvinyl chloride.

The polyvinyl chloride fiber may contain a heat resistance improver from the viewpoint of heat resistance. The heat resistance improver is not particularly limited, but examples thereof include chlorinated polyvinyl chloride resin and AS resin (copolymer of acrylonitrile and styrene). The chlorinated polyvinyl chloride resin may be made by reacting polyvinyl chloride with chlorine to increase the chlorine content to 58 to 72 parts by weight. The heat resistance improver may be used alone or in combination of two or more types. The heat resistance improver is not particularly limited, but for example, 1 to 15 parts by weight may be blended with 100 parts by weight of polyvinyl chloride.

The polyester fiber is not particularly limited, but from the viewpoint of flame retardancy, it is preferable to use fibers obtained by melt-spinning a polyester resin composition containing a bromine-containing flame retardant and/or an antimony-based compound to one or more polyester resins selected from the group consisting of polyalkylene terephthalate and copolymer polyesters containing 80 mol % or more of polyalkylene terephthalate.

The polyalkylene terephthalate is not particularly limited, but it is preferable to use polyethylene terephthalate, polypropylene terephthalate, polybutylene terephthalate, etc., from the viewpoints of availability and cost.

The bromine-containing flame retardant is not particularly limited, but for example, from the viewpoint of imparting flame retardancy, bromine-containing phosphate ester flame retardants, brominated polystyrene flame retardants, brominated benzyl acrylate flame retardants, brominated epoxy flame retardants, brominated phenoxy resin flame retardants, brominated polycarbonate flame retardants, tetrabromobisphenol A derivatives, bromine-containing triazine compounds, bromine-containing isocyanuric acid compounds, etc. are preferred, and from the viewpoint of fiber properties, heat resistance, and processing stability, bromine-containing phosphate ester flame retardants, brominated epoxy flame retardants, brominated phenoxy resin flame retardants, etc. are more preferred, and brominated epoxy flame retardants are even more preferred. The bromine-containing flame retardants may be used alone or in combination of two or more. For example, 5 to 30 parts by weight, or 6 to 25 parts by weight, of the bromine-containing flame retardant may be blended per 100 parts by weight of polyester.

The antimony compound is not particularly limited, but examples thereof include antimony trioxide, antimony tetraoxide, antimony pentoxide, sodium antimonate, and the like. The antimony compounds may be used alone or in combination of two or more. The antimony compounds may be blended in an amount of, for example, 0.5 to 10 parts by weight, or 0.6 to 9 parts by weight, per 100 parts by weight of the polyester resin.

The polyamide-based fibers are not particularly limited, but for example, fibers obtained by melt-spinning a polyamide-based resin composition containing polyamide can be used. Examples of polyamides include homopolymers, copolymers, and mixtures of nylon 6, nylon 66, nylon 46, nylon 69, nylon 610, nylon 612, nylon 11, nylon 12, and polymetaxylylene adipamide (nylon MXD6). Among them, polyamides containing 80 mol% or more of nylon 6 and/or nylon 66 are preferred from the viewpoint of heat resistance. Also, from the viewpoint of flame retardancy, it is preferred to contain a bromine-based flame retardant and an antimony compound, as in the case of polyester-based fibers.

Polyamide fibers can contain various additives such as heat stabilizers, light stabilizers, fluorescent agents, antioxidants, antistatic agents, pigments, plasticizers, and lubricants, as needed.

Polyvinyl chloride fibers, polyester fibers, and polyamide fibers can be produced by conventional methods. For example, first, polyvinyl chloride, polyester, or polyamide is melt-kneaded with various compounding agents as necessary using a single-screw extruder, a twin-screw extruder, a roll, a Banbury mixer, a kneader, or the like, and pelletized by a conventional method to obtain a pellet-shaped polyvinyl chloride resin composition, a polyester resin composition, or a polyamide resin composition. The pellet-shaped resin composition obtained is melt-spun by a normal melt spinning method to obtain an undrawn yarn. Next, the obtained undrawn yarn can be drawn. The drawing may be performed by a two-step method in which the undrawn yarn is once wound and then drawn, or may be performed by a direct spinning drawing method in which the undrawn yarn is continuously drawn without being wound. Hot drawing may be performed by a one-stage drawing method or a multi-stage drawing method of two or more stages.

As the acrylic fiber, a fiber composed of an acrylic polymer can be used. The acrylic polymer is not particularly limited, but from the viewpoint of flame retardancy, for example, an acrylic polymer containing 35 to 75% by weight of acrylonitrile, 25 to 65% by weight of a halogen-containing vinyl monomer, and 0 to 10% by weight of other vinyl monomers copolymerizable therewith can be used. The halogen-containing vinyl monomer is not particularly limited, but examples thereof include vinyl chloride, vinylidene chloride, vinyl bromide, vinylidene bromide, etc. The halogen-containing vinyl monomer may be used alone or in combination of two or more types. As the other vinyl monomer, for example, a sulfonic acid-containing monomer may be used. The sulfonic acid-containing monomer is not particularly limited, but examples thereof include allyl sulfonic acid, methallyl sulfonic acid, styrene sulfonic acid, isoprene sulfonic acid, 2-acrylamido-2-methylpropane sulfonic acid, and metal salts such as sodium salts and amine salts thereof can be used. The other vinyl monomers may be used alone or in combination of two or more.

Acrylic fibers can be produced by a conventional method. For example, they can be obtained by wet spinning a spinning solution in which the acrylic polymer is dissolved in an organic solvent. Examples of organic solvents include dimethyl sulfoxide (DMSO), dimethylacetamide (DMAc), and N,N-dimethylformamide (DMF).

The collagen fibers are not particularly limited, and known regenerated collagen fibers can be used. The regenerated collagen fibers can be obtained, for example, by dissolving and solubilizing a collagen raw material, and spinning the solubilized collagen solution obtained.
<Fiber Treatment Composition>
In the fiber treatment composition, although there is no particular limitation, for example, from the viewpoint of easy attachment of the fiber treatment agent to the synthetic fiber, the weight ratio of the urethane bond structure:silicone compound is 1:10 to 3:1, preferably 1:5 to 2:1. A range other than 1:10 to 3:1 is not preferable in terms of deterioration of the touch and easy generation of static electricity. In the fiber treatment composition, although there is no particular limitation, for example, from the viewpoint of easy attachment of the fiber treatment agent composition to the artificial hair fiber, the fiber treatment composition may contain 25 to 130 parts by weight of the polyalkylene oxide compound per 100 parts by weight of the urethane bond structure. In addition, in the fiber treatment composition, although there is no particular limitation, for example, from the viewpoint of easy attachment of the fiber treatment agent to the artificial hair fiber, the fiber treatment composition may contain 10 to 55 parts by weight of the quaternary ammonium salt per 100 parts by weight of the urethane bond structure.
The fiber for artificial hair contains the fiber treatment composition in an amount of preferably 0.05% by weight or more, more preferably 0.08% by weight or more, calculated as solid content. The artificial hair contains the fiber treatment composition in an amount of preferably 0.5% by weight or less, more preferably 0.3% by weight or less, calculated as solid content. When the content of the fiber treatment composition in the fiber for artificial hair is within the above-mentioned range, the touch and combing durability are improved. The content of the fiber treatment composition (solid content) in the artificial hair can be measured as described below. The solid content includes a non-volatile silicone compound (and, in some cases, a non-volatile organic modified silicone oil, an epoxy modified silicone, and/or a dimethyl silicone oil).

From the viewpoint of being easily smooth to the touch, it is more preferable that the average coefficient of friction (MIU value) of the artificial hair fiber measured using a KES-SE friction tester (manufactured by Kato Tech Co., Ltd.) is 0.20 or less, even more preferably 0.18 or less, and particularly preferably 0.15 or less. The average coefficient of friction is measured as described below.

From the viewpoint of excellent combing durability, the artificial hair fiber is preferably shaken 50 times or more, more preferably 55 times or more, even more preferably 60 times or more, even more preferably 65 times or more, and particularly preferably 70 times or more. The number of shakes is measured as described below.

From the viewpoint of suppressing static electricity, the static electricity of the artificial hair fiber after combing the fiber is preferably 3.0 kV or less, more preferably 2.0 kV or less, and even more preferably 1.5 kV or less. If the static electricity is less than this value, the volume of the fiber due to static electricity is suppressed, and the desired hairstyle can be achieved. The method for measuring static electricity is not particularly limited, but for example, after combing an artificial hair fiber having a fiber length of 20 cm and a weight of 15 g 10 times with a plastic comb, the amount of electricity generated can be measured using a static electricity measuring device STATIRON-DZ4 manufactured by Shishido Electrostatic Corporation, and the static electricity can be evaluated.
<Head decoration products>
The artificial hair fibers can be used to form head accessories, such as hair wigs, hairpieces, weavings, hair extensions, braided hair, hair accessories, and doll hair.

The head ornament product may be formed only from the artificial hair fiber. The head ornament product may be formed by combining the artificial hair fiber with other synthetic fibers such as polyvinyl chloride fibers, polyester fibers, polyamide fibers, and acrylic fibers, collagen fibers such as regenerated collagen fibers, and natural fibers such as human hair and animal hair.
<Production Method>
The application of the fiber treatment composition to the artificial hair fiber is not particularly limited, and may be carried out, for example, by immersing the fiber in the fiber treatment composition, by spraying the fiber treatment composition onto the surface of the artificial hair fiber, or by winding the synthetic fiber around a roll onto which the fiber treatment composition has been applied. Thereafter, if necessary, the fiber may be dried at 30 to 50°C for 1 to 3 hours, or after drying, may be heat-treated under tension at 80 to 150°C for 2 to 10 minutes. The application of the fiber treatment composition may be carried out after the artificial hair fiber is processed into a head ornament product.

The present invention will be described in more detail below with reference to examples. However, the present invention is not limited to these examples. In the following, unless otherwise specified, "%" and "parts" mean "% by weight" and "parts by weight", respectively.
(Textile treatment agent)
The following fiber treatment set was used:

Fiber treatment agent 1: urethane bond structure (weight average molecular weight 1800, solvent: water, 40% by weight). The urethane bond structure is a crosslinking agent made of trimethylolpropane, TDI (2,4 toluene diisocyanate), and MEK oxime.
Fiber treatment agent 2: Amino-modified silicone oil (weight average molecular weight 13,000, emulsion, solvent: water, 40% by weight)
Fiber treatment agent 3: dimethyl silicone oil (emulsion, solvent: water, viscosity 100,000 mm ² /s, 55% by weight)
Fiber treatment agent 4: Polyalkylene oxide compound (copolymer of ethylene oxide and propylene oxide, weight average molecular weight 20,000, emulsion, solvent: water, 20% by weight)
Fiber treatment agent 5: Quaternary ammonium salt (emulsion, solvent: water, 29% by weight)
(Analysis of the composition of fiber treatment agents)
The composition of the fiber treatment agent 1 was confirmed by GC-MS analysis, the molecular weight distribution was measured by GPC measurement, and then the composition ratio of the components contained in the solid content was confirmed by NMR analysis under the following measurement conditions. In the GC-MS analysis, the fiber treatment agent 1 was diluted with acetone and used. In the GPC measurement, about 30 mg of the solid content of the fiber treatment agent 1 was weighed out and dissolved in 10 mL of THF for HPLC, and the sample solution was filtered with a disposable filter, and a part of it was used for the TFH-based GPC measurement. In the NMR analysis, deuterated chloroform was added to the solid content of the fiber treatment agent 1 and used for the analysis.
<GC-MS analysis>
(a) Equipment: Shimadzu GC-17A GCMS-QP5050A
(b) Column: DB-5MS, 0.25 mm φ × 30 m
(c) Column temperature: 45° C. (2 min) → 10° C./min → 320° C. (10 min)
(d) Carrier gas: Helium, 100 kPa
(e) Injection method: splitless (f) Injection port temperature: 300° C.
(g) Interface temperature: 300° C.
(h) Measurement mass range: m/z 29-900
<GPC Measurement>
(a) Apparatus: Tosoh HLC-8220GPC
(b) Guard column: TSK guard column HXL-H
(c) Column: Tosoh TSKgel GM H _XL 2, TSKgel G3000 H _XL 1, TSKgel G2000 H _XL 1 (d) Column temperature: 40° C.
(e) Eluent: THF for high performance liquid chromatography
(f) Eluent flow rate: 1.0 mL/min (g) Sample solution filtration: PTFE 0.45 μm pore size disposable filter unit (h) Injection volume: 200 μL
(i) Analysis time: 50 minutes (j) Analysis software: Tosoh GPC8020 model II
(k) Detector: RI
(l) Standard sample: Shodex STANDARD polystyrene SM-105, molecular weight 3.73E+06, 2.48E+06, 6.66E+05, 1.33E+05, 5.51E+04, 3.14E+04, 1.3E+04, 2.94E+03, 1.28E+03
Shodex Polystyrene A-300, molecular weight 3.70E+02
<NMR Analysis>
(a) A sample was dissolved in deuterated chloroform, and measurement was carried out using a VNMRS600 manufactured by VARIAN.

Example 1
<Spinning process>
To 100 parts by weight of vinyl chloride homopolymer (manufactured by Kaneka Corporation, product name "S-1001"), 1.4 parts by weight of vinyl chloride-vinyl acetate copolymer (manufactured by Kaneka Corporation, product name "K1F"), 0.9 parts by weight of plasticizer, 1.1 parts by weight of heat stabilizer, 2.93 parts by weight of processing aid, and 0.88 parts by weight of lubricant were added, and the mixture was stirred and mixed with a Henschel mixer to obtain a polyvinyl chloride resin compound. The compound was charged into the hopper of a single-screw extruder having a diameter of 40 mm, and the compound was extruded and melt-spun at a cylinder temperature of 170°C and a nozzle temperature of 180±15°C. A nozzle with a cocoon-shaped nozzle hole was used. The extruded filament was heat-treated for about 0.5 to 1.5 seconds in a heating cylinder (atmosphere of 330°C) provided directly below the nozzle, and the undrawn yarn after heat treatment was wound around a bobbin by a take-up roll. Next, the undrawn yarn was drawn about 2 to 4 times in a hot air circulating box adjusted to a temperature of 110° C. Next, a 38% relaxation treatment was continuously performed in the hot air circulating box adjusted to a temperature of 110° C., and the multifilament was wound up to obtain a polyvinyl chloride fiber (single fiber fineness about 72 dtex).

<Step of applying fiber treatment composition>
(1) Fiber treatment compositions 1, 2, 3, 4 and 5 were mixed with pure water in the proportions shown in Table 1 below to prepare fiber treatment composition a.
(2) 300 g of fiber treatment composition a was placed in a disposable cup, and 25 g of the polyvinyl chloride fiber obtained above was immersed in it for 5 minutes (bath ratio 1:12).
(3) The polyvinyl chloride fiber was squeezed to a squeezing rate of 24%, and the fiber treatment composition a was dropped onto the fiber.
(4) Then, it was dried at 40°C for 2 hours.
(5) The sample was fixed in a taut state and heat-treated at 130°C for 5 minutes.
(6) After cooling in the air, the tension was released and the hair was combed.
Example 2
The fiber treatment compositions were applied to polyvinyl chloride fibers in the same manner as in Example 1, except that fiber treatment composition b was prepared by mixing fiber treatment agents 1, 2, 3, 4 and 5 with pure water in the proportions shown in Table 1 below.
Example 3
The fiber treatment compositions were applied to polyvinyl chloride fibers in the same manner as in Example 1, except that fiber treatment composition c was used, which was prepared by mixing fiber treatment agents 1, 2, 3, 4 and 5 with pure water in the proportions shown in Table 1 below.
Example 4
The fiber treatment compositions were applied to polyvinyl chloride fibers in the same manner as in Example 1, except that fiber treatment composition d was prepared by mixing fiber treatment agents 1 and 2 with pure water in the proportions shown in Table 1 below.
(Comparative Example 1)
The fiber treatment compositions were applied to polyvinyl chloride fibers in the same manner as in Example 1, except that fiber treatment composition e was used, which was prepared by mixing fiber treatment agents 2, 3, 4 and 5 with pure water in the proportions shown in Table 1 below.
(Comparative Example 2)
The fiber treatment compositions were applied to polyvinyl chloride fibers in the same manner as in Example 1, except that fiber treatment composition f was used, which was prepared by mixing fiber treatment agents 1, 3, 4 and 5 with pure water in the proportions shown in Table 1 below.
(Comparative Example 3)
The fiber treatment compositions were applied to polyvinyl chloride fibers in the same manner as in Example 1, except that fiber treatment compositions g prepared by mixing fiber treatment agents 3, 4 and 5 with pure water in the proportions shown in Table 1 below were used.
(Comparative Example 4)
The fiber treatment compositions were applied to polyvinyl chloride fibers in the same manner as in Example 1, except that fiber treatment composition h, which was prepared by mixing fiber treatment agents 4 and 5 with pure water in the proportions shown in Table 1 below, was used.

(Comparative Example 5)
The fiber treatment compositions were applied to polyvinyl chloride fibers in the same manner as in Example 1, except that fiber treatment composition i, which was prepared by mixing fiber treatment agents 1, 4 and 5 with pure water in the ratios shown in Table 1 below, was used.

For the fibers of the Examples and Comparative Examples, the amount of the fiber treatment composition (solid content) adhered, the average coefficient of friction, the combing durability, and the spinnability were measured and evaluated as described below, and the results are shown in Table 2 below.
(Deposition amount in terms of solid content of fiber treatment composition)
2 g of the core fiber of each of the examples and comparative examples was immersed in 30 g of a mixed solvent of ethanol:cyclohexane (manufactured by Wako Pure Chemical Industries, Ltd.) = 1:1 (weight ratio) to dissolve the fiber treatment composition. Only the solvent was extracted from the resulting solution of the fiber treatment composition and evaporated, and the weight of the remaining fiber treatment composition (solid content) was measured. Next, the fiber treatment composition was dissolved in THF (tetrahydrofuran), and the solution was analyzed using a gas chromatograph (manufactured by Agilent Technologies, "GC6890N"), and the MS spectrum of the detected peak was searched in a library to identify the various fiber treatment components in the fiber treatment composition (solid content) and to determine the content of the various fiber treatment components (solid content). Then, the adhesion amount of the solid content of the fiber treatment composition and the adhesion amount of the solid content of each fiber treatment component were calculated using the following formula. In addition, when the various fiber treatment agent components and their contents in the solid content of the fiber treatment agent composition are known in advance, the adhesion amount of the various fiber treatment agent components (solid content) can be calculated based on the following formula by simply measuring the weight of the fiber treatment agent composition (solid content) on the fiber. The solid content of the silicone compound means the non-volatile content of the silicone oil. In Examples 1 to 3, the solid content of the fiber treatment agent composition contains the non-volatile amino-modified silicone oil, dimethyl silicone oil, and urethane bond structure, the solid content of Example 4 contains the non-volatile amino-modified silicone oil and urethane-based prepolymer, the solid content of Comparative Example 1 contains the non-volatile amino-modified silicone oil and dimethyl silicone oil, and the solid content of Comparative Examples 2 and 3 contains the non-volatile dimethyl silicone oil. Comparative Example 4 does not contain the urethane bond structure and the silicone compound, and Comparative Example 5 contains the urethane bond structure and does not contain the silicone compound.
Adhesion amount (wt %) of fiber treatment composition (solid content)=[(weight of solid content of fiber treatment composition/weight of fiber]×100
Adhesion amount (wt %) of each fiber treatment component (solid content)=[(weight of solid content of fiber treatment composition×content of each fiber treatment component in solid content of fiber treatment composition)/weight of fiber]×100
(Average static friction coefficient/average dynamic friction coefficient)
Sample 1 (fiber length 20 cm, weight 15 g) of artificial hair fiber was fixed on the stage of a static and dynamic friction tester (manufactured by Trinity Labs), and sample 2, a friction element made of urethane resin imitating a fingerprint pattern, was used as the contact, and sample 1 and sample 2 were rubbed together under conditions of a sliding speed of 5 mm/s and a static weight of 500 g to measure the static and dynamic friction coefficients. The measurements were made five times, and the average value was calculated. The lower the average value, the smoother the artificial hair fiber is in combability.
(Combing durability: number of vibrations)
The number of vibrations was evaluated as the combing durability. Preparation of a sample: 15 g of fibers with a fiber length of 24 inches were bundled, and a 4-inch gap was intentionally created between the fibers by hackling to make the length of the fiber bundle 28 inches. Then, the center of the fiber bundle was tied with a string and folded in half to prepare a sample for measuring combing durability with a length of 14 inches. Next, the sample was sprayed evenly with artificial finger grease (manufactured by Hayashi Pure Chemical Industries, Ltd., product name "artificial finger grease") to 6.7% omf (% on mass of fiber), and dried at 40°C for 2 hours to obtain a sample after the artificial finger grease treatment as shown in (a) of Figure 1. Next, as shown in (b) of Figure 1, the end of the sample after the artificial finger grease treatment tied with a string was fixed to a mannequin and hand-kneaded twice to give the sample damage equivalent to that of a head ornament product such as a wig worn for a long period of about 2 weeks. Next, as shown in FIG. 1(c), the damaged sample was swung around by hand to measure the number of times it became impossible to comb through (the number of times of shaking). The more the number of times of shaking, the less likely it was to become tangled, and the higher the durability of combing. For both evaluations, a number of times of shaking of 70 or more was deemed to pass.
(Volume and volume caused by static electricity)
Regarding static electricity, a sample of artificial hair fiber (fiber length 20 cm, weight 15 g) was combed 10 times with a plastic comb, and the amount of electricity generated was measured using a static electricity measuring device STATIRON-DZ4 manufactured by Shishido Electrostatic Co., Ltd., and the volume and manageability of the artificial hair fiber were evaluated. The sample was rated as x if it generated static electricity, causing it to become voluminous and spread out, affecting manageability, △ if it was voluminous but still manageable, and ◯ if it was completely problem-free in terms of volume and manageability.

As can be seen from the results in Table 2, the artificial hair fibers of Examples 1 to 4, which have a urethane bond structure and a silicone compound attached, have a small average static friction coefficient and average dynamic friction coefficient, a smooth feel, an average number of vibrations of 70 or more, good combing durability, and reduced volume and manageability, satisfying all of the required characteristics. On the other hand, the comparative examples showed poor results in any of the average static friction coefficient, average dynamic friction coefficient, number of vibrations, volume, and manageability.

Claims (12)

An artificial hair fiber having a fiber treatment composition attached to a surface thereof,
The fiber treatment composition contains at least a urethane bond structure and a silicone compound,
The urethane bond structure is a crosslinking agent, and crosslinks to form a coating on the surface of the artificial hair fiber,
The silicone compound includes an amino-modified silicone oil and/or an epoxy-modified silicone oil,
The fiber treatment composition is for artificial hair fibers, and does not contain an oxazoline group-containing acrylic resin. The artificial hair fiber according to claim 1, wherein the weight ratio of the urethane bond structure and the silicone compound contained in the fiber treatment composition is 1:10 to 3:1. The artificial hair fiber according to claim 1 or 2, which contains the fiber treatment composition in an amount of 0.05% by weight or more and 0.5% by weight or less in terms of solid content. The fiber for artificial hair according to any one of claims 1 to 3 contains 0.02% by weight or more and 0.2% by weight or less of the urethane bond structure. The fiber for artificial hair according to any one of claims 1 to 4 contains the silicone compound in an amount of 0.01% by weight or more and 0.3% by weight or less in terms of non-volatile content. The fiber for artificial hair according to any one of claims 1 to 5, which contains at least one selected from the group consisting of polyvinyl chloride fibers, acrylic fibers, and polyester fibers. The artificial hair fiber according to any one of claims 1 to 6, wherein the silicone compound includes an amino-modified silicone oil. The fiber for artificial hair according to any one of claims 1 to 7, wherein the fiber treatment composition further contains a polyalkylene oxide compound. The fiber for artificial hair according to any one of claims 1 to 8, wherein the fiber treatment composition further contains a quaternary ammonium salt. The artificial hair fiber according to any one of claims 1 to 9, wherein the urethane bond structure is a compound in which toluene diisocyanate is added to all hydroxyl groups of trimethylolpropane. A head accessory product comprising the artificial hair fiber according to any one of claims 1 to 10. A method for producing an artificial hair fiber according to any one of claims 1 to 10, comprising the steps of:
A method for producing an artificial hair fiber, comprising a step of adhering a fiber treatment composition to the surface of an artificial hair fiber.