WO2006035868A1

WO2006035868A1 - Flame-retardant polyester artificial hair

Info

Publication number: WO2006035868A1
Application number: PCT/JP2005/017941
Authority: WO
Inventors: Toshiyuki Masuda
Original assignee: Kaneka Corporation
Priority date: 2004-09-29
Filing date: 2005-09-29
Publication date: 2006-04-06
Also published as: JPWO2006035868A1

Abstract

A polyester fiber for artificial hair which retains fiber physical properties (such as heat resistance, tenacity and elongation) inherent in current polyester fibers and is excellent in flame retardance, gloss, touch, easiness of combing, and settability; and artificial hair made by using the fiber. Such a fiber can be produced by subjecting polyester filaments obtained by melt-spinning a composition prepared by melt-kneading together 100 parts by weight of a polyester (A) consisting of one or more members selected from among polyalkylene terephthalates and copolyesters containing polyalkylene terephthalates as the main component, 0 to 10 parts by weight of an auxiliary flame retardant (B), and 0.1 to 5 parts by weight of organic fine particles (C) and/or inorganic fine particles (D) to exhaustion finish with a flame retardant (E) to incorporate the filaments with 2 to 20 wt% of the flame retardant (E).

Description

Specification

Flame retardant polyester artificial hair

Technical field

[oooi] The present invention relates to a flame retardant polyester obtained by exhausting a polyester filament formed from a composition containing a flame retardant assistant, organic fine particles and Z or inorganic fine particles in polyester. It relates to artificial hair. More specifically, it relates to artificial hair that maintains fiber properties such as flame retardancy, heat resistance, and high elongation, and is excellent in gloss, touch, comb, and setability.

Background art

[0002] Polyethylene terephthalate or a fiber made of polyester terephthalate mainly composed of polyethylene terephthalate has a high melting point, a high elastic modulus, and excellent heat resistance and chemical resistance. Therefore, curtains, rugs, clothing, Widely used in blankets, sheets, tablecloths, chair upholstery, wall coverings, human hair, automotive interior materials, outdoor reinforcements, safety nets, etc.

[0003] In hair products such as wigs, hair wigs, false hairs, hair bands, doll hairs, human hair and artificial hair (modacrylic fibers, polyvinyl chloride and vinyl fibers) have been used. Yes. However, the provision of human hair has become difficult, and the importance of artificial hair has increased.

[0004] As an artificial hair material, modacrylic fiber has been frequently used due to its flame-retardant characteristics, but it is insufficient in terms of heat resistance.

[0005] In recent years, artificial hair using fibers mainly composed of polyester typified by polyethylene terephthalate having excellent heat resistance has been proposed!

[0006] However, the fiber having a polyester strength represented by polyethylene terephthalate is insufficient in flame resistance since it is a flammable material.

[0007] Conventionally, various attempts have been made to improve the flame resistance of polyester fibers. For example, a method of kneading a flame retardant during melt-kneading or spinning, a flame retardant monomer containing a phosphorus atom, or the like. A method of copolymerizing at the time of polymerization and a method of impregnating a polyester fiber with a flame retardant by post-processing are known. [0008] As a method of kneading a flame retardant during melt-kneading or spinning, a flame-retardant polyester fiber is obtained by spinning a resin composition obtained by melt-kneading a phosphoric ester-based flame retardant into polyester. Although a method (Patent Document 1) has been proposed, there are problems that the fiber surface is sticky and that the flame retardant elutes during washing and shampooing.

[0009] Further, as a method of copolymerizing a flame retardant monomer, a polyester fiber copolymerized with a phosphorus compound (Patent Documents 2 and 3) has been proposed, but sufficient flame retardancy is obtained. In order to achieve this, the amount of copolymerization must be increased, and as a result, the heat resistance of the polyester is greatly reduced, making melt spinning difficult. Melting'drips would cause problems.

[0010] Further, as a method of incorporating a flame retardant into a polyester fiber by post-processing (flame retardant exhaustion), a method of incorporating a fine halogen-cycloalkane compound into a polyester fiber (Patent Document) 4) A method of containing a bromine atom-containing alkylcyclohexane (Patent Document 5) has been proposed. However, for these, in order to obtain sufficient flame resistance, it is necessary to make the content treatment time long, or a large amount of flame retardant must be used. If the flame retardant was eluted during shampooing, there were problems such as a problem, fiber properties decreased, productivity decreased, and manufacturing costs increased. In addition, Patent Document 4 discloses a technique for finely dispersing a halogenated cycloalkane compound in order to improve the exhaust efficiency of a flame retardant, but it is more than that of a halogenated cycloalkane compound. In the case of halogenated aromatic flame retardants having high hydrophobicity, there was a problem that it was difficult to stabilize the finely dispersed state.

[0011] Further, as a method for simultaneously performing dyeing and exhaustion of the flame retardant, by using polyethylene terephthalate having a glass transition temperature of 35 to 60 ° C copolymerized with an aliphatic dicarboxylic acid component as polyester, A method for improving dyeability and flame retardant exhaustion (Patent Document 6) has been proposed. However, this method has the problem that the heat resistance becomes insufficient due to the lowering of the melting point of the polyester itself, so that troubles in fusion are likely to occur, and the color change is likely to occur due to the decrease in light resistance. It was left behind.

[0012] Various proposals have been made in the past, but the high flame resistance required for artificial hair has been confirmed. In order to maintain this, it is necessary to use a large amount of flame retardant in any of the methods, and it has been difficult to maintain the physical properties of conventional polyester fibers such as heat resistance and high elongation. From these facts, it is the actual situation that the artificial hair that maintains the physical properties of fibers such as heat resistance and tensile strength of conventional polyester fibers and is excellent in flame retardancy, setability and combing properties has not been obtained yet. .

Patent Document 1: Japanese Patent Laid-Open No. 9-268423

Patent Document 2: Japanese Patent Laid-Open No. 3-27105

Patent Document 3: Japanese Patent Laid-Open No. 5-339805

Patent Literature 4: Japanese Patent Publication No. 3-57990

Patent Document 5: Japanese Patent Publication No. 1-24913

Patent Document 6: Japanese Patent Laid-Open No. 9-324315

Disclosure of the invention

Problems to be solved by the invention

[0013] The present invention solves the conventional problems as described above, maintains the fiber properties such as heat resistance and strength of ordinary polyester fiber, and has flame retardancy, gloss, touch, combing and setability. Another object of the present invention is to provide a flame-retardant polyester artificial hair which is excellent and has a controlled fiber wrinkle.

Means for solving the problem

[0014] As a result of intensive investigations to solve the above problems, the present inventors have found that a polyester filament formed of a composition containing a flame retardant aid, organic fine particles and Z or inorganic fine particles in polyester is used. Flame retardant polyester-based artificial fabric that maintains the physical properties of ordinary polyester fibers such as heat resistance and tensile strength, and has excellent flame retardancy, gloss, touch, combing and setability. The inventors have found that hair fibers can be obtained and have completed the present invention.

That is, the present invention relates to a flame retardant aid (B) 0 with respect to 100 parts by weight of a polyester (A) having at least one kind of polyalkylene terephthalate or a copolymer polyester mainly composed of polyalkylene terephthalate. Polyester filaments formed from a resin composition containing ˜10 parts by weight and organic fine particles (C) and Z or inorganic fine particles (D) 0.1 to 5 parts by weight A flame retardant polyester-based artificial hair fiber obtained by exhausting a flame retardant, wherein the flame retardant (E) has an exhaust amount of 2 to 20% by weight based on the polyester filament. This is related to synthetic polyester-based artificial hair. Sarakuko relates to a flame-retardant polyester artificial hair obtained by simultaneously dyeing the above-mentioned flame-retardant polyester artificial hair at the time of exhausting the flame retardant.

[0016] A preferable embodiment is the above-mentioned flame-retardant polyester artificial hair fiber, which is at least one polymer selected from the group consisting of polyethylene terephthalate, polypropylene terephthalate and polybutylene terephthalate. Preferably, the group power consisting of melamine cyanurate, antimony triacid, antimony triacid, antimony tetraacid, antimony pentaacid and sodium antimonate was also selected as the form of flame retardant aid (B). It is a flame-retardant polyester artificial hair fiber that is at least one type. Preferably, as an embodiment, the organic fine particles (C) are at least one selected from the group consisting of polyarylate, polyamide, fluorine resin, silicone resin, crosslinked acryl resin and crosslinked polystyrene. It is a fiber for polyester-based artificial hair. In a preferred embodiment, the inorganic fine particles (D) are at least one selected from the group force consisting of calcium carbonate, silicon oxide, titanium oxide, aluminum oxide, zinc oxide, talc, ferroline, montmorillonite, bentonite and my power. It is a fiber for flame retardant polyester-based artificial hair that is a seed. More preferably, as an aspect, the flame retardant (E) used for the flame retardant exhaust processing is a phosphorus flame retardant, a bromine-containing phosphorus flame retardant, a brominated aliphatic flame retardant, a brominated aromatic flame retardant. Flame retardants, brominated polystyrene flame retardants, brominated benzaryl acrylate flame retardants, brominated epoxy flame retardants, brominated polycarbonate flame retardants, tetrabromobisphenol A derivatives, bromine containing triazine compounds and bromine containing It is a flame-retardant polyester artificial hair which is at least one selected from the group consisting of isocyanuric acid compounds. A more preferred embodiment is a flame retardant polyester artificial hair in which the flame retardant (E) has a melting point of 160 ° C or higher. A more preferred embodiment is a flame-retardant polyester artificial hair in which the flame retardant (E) has a molecular weight of 200 to 4000. A more preferable embodiment is a flame retardant polyester artificial hair in which the exhaust amount of the flame retardant (E) is 3 to 20% by weight.

[0017] In a more preferred embodiment, dyeing and flame retardant absorption for polyester filaments are preferred. The present invention relates to a flame-retardant polyester artificial hair in which exhaustion is simultaneously performed at a temperature of 90 to 150 ° C., and the polyester artificial hair contains 0.1% by weight or more of a dye.

[0018] The flame-retardant polyester-based artificial hair fibers are preferably non-crimped raw silk and have a single fiber fineness of 10 to 1 OOdtex! / ヽ.

The invention's effect

According to the present invention, a polyester-based filament formed from a composition containing a flame retardant aid and organic fine particles and Z or inorganic fine particles in polyester is subjected to a flame retardant exhausting process, thereby obtaining a normal polyester. It is possible to obtain polyester-based artificial hair that maintains the fiber properties such as heat resistance and tensile strength of the fiber, and is excellent in flame retardancy, gloss, touch, combing and setability.

[0020] Furthermore, by using a filament coloring method as a dyeing method, it is possible to obtain polyester-based artificial hair having a hue superior to that of the original method.

BEST MODE FOR CARRYING OUT THE INVENTION

[0021] The flame retardant polyester artificial hair of the present invention comprises a polyester (A), a flame retardant aid (B), and a polyester (A), a copolymer polyester mainly composed of polyalkylene terephthalate or polyalkylene terephthalate. Further, it is an artificial hair obtained by subjecting a polyester filament (fiber), which also has a compositional force containing organic fine particles (C) and Z or inorganic fine particles (D), to a flame retardant exhaustion process.

[0022] Sarakuko is the flame retardant polyester artificial hair of the present invention, which is an artificial hair obtained by dyeing the polyester filament simultaneously with the flame retardant exhausting process.

[0023] The polyalkylene terephthalate or the copolyester mainly composed of polyalkylene terephthalate contained in the polyester (A) used in the present invention includes, for example, polyalkylene terephthalate such as polyethylene terephthalate, polypropylene terephthalate and polybutylene terephthalate. And z or a copolymerized polyester mainly composed of these polyalkylene terephthalates and containing a small amount of a copolymer component. Among the polyalkylene terephthalates, polyethylene terephthalate, polypropylene terephthalate, and polybutylene terephthalate are particularly preferred from the standpoint of availability and cost. Yes.

[0024] The main component refers to containing 80 mol% or more.

[0025] Examples of the copolymer component include isophthalic acid, orthophthalic acid, naphthalenedicarboxylic acid, para-phenolic dicarboxylic acid, trimellitic acid, pyromellitic acid, succinic acid, glutaric acid, adipic acid, speric acid, and azelain. Polycarboxylic acids such as acid, sebacic acid, dodecanedioic acid, rubonic acid, derivatives thereof, dicarboxylic acids including sulfonic acid salts such as 5-sodium sulfoisophthalic acid, dihydroxyethyl 5-sodium sulfoisophthalate, derivatives thereof, 1,2 propanediol, 1,3 propanediol, 1,4 butanediol, 1,6-hexanediol, neopentyl glycol, 1,4-cyclohexanedimethanol, diethylene glycolol, polyethylene glycol, trimethylolpropane , Pentaerythritol, 4-hydroxybenzoic acid Acid, epsilon prolatathon, etc.

[0026] The copolyester is usually made to react by containing a small amount of a copolymer component in a polymer of terephthalic acid, which is the main component, and a derivative thereof (for example, methyl terephthalate) and alkylene glycol. Although it is preferable from the viewpoint of stability and ease of operation, a smaller amount of co-polymer is added to a mixture of the main terephthalic acid and cocoon or a derivative thereof (for example, methyl terephthalate) and alkylene glycol. Manufacture by polymerizing a monomer or oligomer component that is a polymerization component.

[0027] The copolymer polyester is not particularly limited in the way of copolymerization and the like as long as the copolymer component is polycondensed to the main chain and side or side chain of the main polyalkylene terephthalate. .

[0028] Specific examples of the copolymer polyester mainly composed of the polyalkylene terephthalate include, for example, a polyester mainly composed of polyethylene terephthalate and copolymerized with ethylene glycol ether of bisphenol, 1,4-cyclohexanedimethanol. Examples include polyesters copolymerized and polyesters copolymerized with 5-hydroxysulfoisophthalate dihydroxyethyl.

[0029] The polyalkylene terephthalate or copolyester may be used singly or in combination of two or more. Among these, polyethylene terephthalate Polypropylene terephthalate, polybutylene terephthalate, copolymerized polyester (polyester mainly composed of polyethylene terephthalate and copolymerized with ethylene glycol ether of bisphenol A, polyester copolymerized with 1,4-cyclohexanedimethanol, 5- Polyesters copolymerized with sodium sulfoisophthalate dihydroxyethyl) are preferred, and those in which two or more are mixed are also preferred.

[0030] The glass transition temperature of the polyester (A) used in the present invention is preferably 60 to 115 ° C, more preferably 65 to 105 ° C. When the glass transition temperature of the polyester (A) is lower than 60 ° C, the heat resistance tends to be inadequate and the ironing property tends to be reduced. When the glass transition temperature is higher than 115 ° C, the flame retardant There is a tendency for the dyeability to decrease.

[0031] The intrinsic viscosity of the polyester (A) used in the present invention is preferably 0.5 to 1.4, more preferably 0.6 to 1.2. If the intrinsic viscosity is less than 0.5, the mechanical strength of the resulting fiber tends to decrease, and if it exceeds 1.4, the melt viscosity increases with increasing molecular weight, making melt spinning difficult, There is a tendency for the fineness to become uneven.

[0032] The flame retardant aid (B) used in the present invention is difficult to interact with phosphorus-based flame retardants or bromine-containing flame retardants used in post-processing such as nitrogen-containing compounds or antimony compounds. As long as the effect of imparting flammability can be enhanced, it can be used without particular limitation.

[0033] Specific examples of the nitrogen-containing compound in the present invention include melamine cyanurate. Specific examples of the antimony compound in the present invention include, for example, antimony trimonate, antimony tetroxide, antimony pentoxide, and sodium antimonate. These may be surface-treated with an epoxy compound, a silane compound, an isocyanate compound, a titanate compound, or the like, if necessary.

[0034] The flame retardant aid (B) used in the present invention can be used if it has an average particle size of 15 m or less. When using a flame retardant aid (B) with an average particle size of 0.3 to 1 μm, the concealment ratio becomes the largest and the hue (color development) of artificial hair tends to decrease. The average particle size of the auxiliary agent (B) is preferably 0.2 m or less or 1.5 to 15 m, preferably 0.15 / zm or less or 1.7 to 12 111, more preferably 0 or less or 1.9. ~: LO / zm is more preferable.

[0035] The amount of the flame retardant aid (B) used in the present invention is 100 parts by weight of polyester. 0 to 10 parts by weight is preferred 0.5 to 10 parts by weight is more preferred 0.7 to 8 parts by weight is even more preferred. Flame retardancy is exhibited even when the amount of flame retardant aid (B) used is 0 parts by weight, but in order to obtain higher flame retardancy, it is preferable to use 0.5 parts by weight or more. When the amount of the flame retardant aid (B) used is more than 10 parts by weight, the processing stability, appearance and transparency tend to be impaired.

[0036] In the present invention, by blending organic fine particles (C) and Z or inorganic fine particles (D), irregularities are formed on the fiber surface and a stable gloss adjusting effect can be exhibited. it can.

[0037] As the organic fine particles (C) used in the present invention, any organic resin component having a structure that is incompatible with or partially incompatible with the main component polyester (A) is used. For example, polyarylate, polyamide, fluorine resin, silicone resin, bridged acrylic resin, crosslinked polystyrene, etc. are preferably used. These may be used alone or in combination of two or more. In order to stably exhibit a gloss adjusting effect, crosslinked polyester particles and crosslinked acrylic particles are preferred from the viewpoint of heat resistance and dispersibility.

[0038] The crosslinked polyester particles are obtained by water-dispersing the unsaturated polyester and the bull-type monomer, followed by crosslinking and curing. The unsaturated polyester used here is not particularly limited, for example, ex, j8-unsaturated acid or a mixture of it and a saturated acid and a dihydric alcohol or a trihydric alcohol polymerized. Can do. Examples of the unsaturated acid include fumaric acid, maleic acid, and itaconic acid. Examples of the saturated acid include phthalic acid, terephthalic acid, succinic acid, dartaric acid, tetrahydrophthalic acid, adipic acid, and sebacic acid. can give. Examples of dihydric alcohols and trihydric alcohols include ethylene glycol, diethylene glycol, propylene glycol, neopentyl glycol, 1,3-propanediol, 1,6-hexanediol, trimethylolpropane, and the like. can give. On the other hand, the vinyl monomer is not particularly limited, and examples thereof include styrene, chlorostyrene, butyltoluene, dibulene benzene, acrylic acid, methyl acrylate, acrylonitrile, ethyl acrylate and diallyl phthalate. It is done. [0039] The crosslinked acrylic particles are obtained by water-dispersing an acrylic monomer and a crosslinking agent and crosslinking and curing. Examples of acrylic monomers used herein include acrylic acid and acrylic acid derivatives such as methyl acrylate, butyl acrylate, hexyl acrylate, cyclohexyl acrylate, hydroxyethyl acrylate, and acrylonitrile. , Atylamide, N-methylolacrylamide, or derivatives of methacrylic acid and methacrylic acid, such as methyl methacrylate, butyl methacrylate, hexyl methacrylate, glycidyl methacrylate, benzyl methacrylate, cyclohexyl methacrylate, methacrylic acid Examples include N-but-2-pyrrolidone, metatali-tolyl, methacrylamide, N-methylolmethacrylamide, 2-methacrylic acid 2-hydroxyethyl having a single bull group in one molecule. . These can be used alone or in combination of two or more. Further, the crosslinking agent may be any monomer as long as it has two or more bur groups in one molecule, but one having two vinyl groups in one molecule is preferable. Examples of the preferable monomer include dibutenebenzene, a reaction product of glycol and methacrylic acid or acrylic acid (for example, ethylene glycol dimetatalylate, neopentyldaricol dimetatalylate, etc.). However, it is not limited to these. The addition amount of the crosslinking agent is preferably 0.02 to 5 parts by weight per 100 parts by weight of the monomer having one vinyl group. As the polymerization initiator, preferred are peroxide radical polymerization initiators such as benzoyl peroxide, 2-ethylhexyl perbenzoate, di-tert-butyl peroxide, cumene hydroperoxide, methyl. Ethyl ketone peroxide and the like. The radical polymerization initiator is preferably used in an amount of 0.05 to L0 parts by weight per 100 parts by weight of the monomer having one vinyl group.

[0040] The inorganic fine particles (D) used in the present invention preferably have a refractive index close to the refractive index of the polyester (A) because of the effect on the transparency and color developability of the fibers. Specific examples of inorganic fine particles include, for example, calcium carbonate, silicon oxide, titanium oxide, acid aluminum aluminum, acid sodium hydroxide, kaolin, montmorillonite, bentonite, my strength, and melamine resin. Also included are composite particles such as Z-silica composites, mainly composed of acid and oxide oxides. These may be used alone or in combination of two or more. Among these, particles close to a spherical shape have a higher gloss adjustment effect, so Preferred are composite particles mainly composed of phosphide and oxy-caine. The inorganic fine particles (D) used in the present invention may be surface-treated with an epoxy compound, a silane compound, an isocyanate compound, a titanate compound, or the like, if necessary.

[0041] The average particle size of the organic fine particles (C) and Z or inorganic fine particles (D) is preferably 0.1 to 15 m force S, more preferably 0.2 to 10 m force, and more preferably 0.5 to 8 111. preferable. When the particle size is smaller than 0.1 μm, the gloss adjustment effect tends to be small, and when the particle size is larger than 15 m, the gloss adjustment effect tends to be small or thread breakage tends to occur. There is.

[0042] The amount of organic fine particles (C) and Z or inorganic fine particles (D) used in the present invention is not particularly limited, but is preferably 0.1 to 5 parts by weight per 100 parts by weight of polyester. 2 to 3 parts by weight is more preferred 0.3 to 2 parts by weight is even more preferred. If the amount of organic fine particles (C) and Z or inorganic fine particles (D) used exceeds 5 parts by weight, appearance, hue and color development tend to be impaired. Since there are fewer fine protrusions formed on the surface, there is a tendency that gloss adjustment on the fiber surface is insufficient.

[0043] The polyester-based composition used in the present invention includes, for example, polyester (A), flame retardant aid (B), and organic fine particles (C) and Z or orientation fine particles (D) after dry blending. It can manufacture by melt-kneading using the general kneading machine.

[0044] Examples of the kneader include, for example, a single screw extruder, a twin screw extruder, a roll, a Banbury mixer, and a kneader. Of these, the twin screw extruder is also preferable because of adjustment of the kneading degree and ease of operation.

[0045] For example, using a twin screw extruder with a screw diameter of 45 mm, the barrel temperature is 260-300 ° C, the discharge rate is 50-150 kgZhr, the screw rotation speed is 150-200 rpm, and the strand is taken out from the die. After cooling with water, the composition of the present invention can be obtained by pelletizing with a strand cutter.

[0046] The flame-retardant polyester artificial hair of the present invention can be produced by melt spinning the flame-retardant polyester composition by a normal melt spinning method.

[0047] That is, for example, the temperature of the extruder, gear pump, die, etc. is set to 270 to 310 ° C, melt-spun, and the spun yarn is passed through a heating tube, and then cooled to the glass transition point or lower. ~ 500 A spun yarn is obtained by taking it up at a speed of OmZ. It is also possible to control the fineness by cooling the spun yarn in a water tank containing cooling water. The temperature and length of the heating cylinder, the temperature and amount of cooling air, the temperature of the cooling water tank, the cooling time, and the take-up speed can be adjusted as appropriate according to the discharge amount and the number of holes in the base.

[0048] The obtained unstretched yarn is heat-stretched, and stretching can be performed by either a two-step method in which the unstretched yarn is first wound and then stretched, or a direct spin-stretching method in which stretching is continuously performed without winding. It is also possible to use this method. The hot stretching is performed by a single-stage stretching method or a multi-stage stretching method having two or more stages. As a heating means in the heat stretching, a heating roller, a heat plate, a steam jet device, a hot water tank, or the like can be used, and these can be used in combination as appropriate.

[0049] The flame retardant polyester-based artificial hair of the present invention includes various kinds of heat-resistant agents, light stabilizers, fluorescent agents, antioxidants, antistatic agents, pigments, plasticizers, lubricants, and the like as necessary. Additives can be included. By incorporating a pigment, a primary fiber can be obtained.

[0050] The flame-retardant polyester artificial hair of the present invention can use a silicone fiber treatment agent, a non-silicone fiber treatment agent, and the like in order to improve the feel and combing.

[0051] Examples of the silicone fiber treating agent include dimethylpolysiloxane, methylhydrogen polysiloxane, hydroxylated dimethylpolysiloxane at both terminals, vinyl group-containing organopolysiloxane, epoxy group-containing organopolysiloxane, and amino group-containing organopolysiloxane. Sun, ester group-containing organopolysiloxane, and polyoxyalkylene-containing organopolysiloxane. Examples of the non-silicone fiber treating agent include polyether compounds, fatty acid ester compounds, organic amine compounds, and organic amides. Examples thereof include organic compounds, organic fatty acid esters, organic ammonium salts, organic fatty acid salts, organic sulfonic acid salts, organic sulfuric acid ester salts, and organic phosphoric acid ester salts.

[0052] A necessary amount of the fiber treatment agent may be attached at the time of spinning, or may be attached at the time of exhausting the flame retardant, or may be attached after the exhausting of the flame retardant. .

[0053] The flame retardant (E) used in the present invention includes a phosphorus flame retardant, a bromine-containing phosphorus flame retardant, a brominated cycloalkane flame retardant, a brominated aromatic flame retardant, a brominated polystyrene flame retardant, Brominated benzaryl acrylate flame retardant, brominated epoxy flame retardant, brominated polycarbonate flame retardant, tetrabromobisphenol A derivative, bromine-containing triazine At least one selected from a compound and a bromine-containing isocyanuric acid compound

In particular, no limitation can be used.

[0054] Specific examples of the flame retardant (E) include, for example, 1,4-phenolenebis (dixylyl phosphate), biphenyl-rubis (dixylenyl phosphate), and the following formulas (1) to (4): );

[0055] [Chemical 1]

[0058] [Chemical 4] HOCH ₂ CH ₂ 0 -OCCHCH ₂ COOCH ₂ CH ₂

[0059] Phosphorus flame retardants such as a compound represented by the formula: Brominated aliphatic compounds such as dibromoneopentyldaricol, tribromoneopentyldaricol, hexasuboxycyclohexadecane, pentabromotoluene, hexabromobenzene, Decabromodiphenyl, Decabromodiphenyl ether, Bis (tribromophenoxy) ethane, Tetrabromophthalic anhydride, Ethylene bis (tetrabromophthalimide), Ethylene bis (pentabromophenyl), Otatab Mouth trimethylphenylindane Brominated aromatic flame retardants such as bromine-containing phosphorus flame retardants such as tris (tribromoneopentyl) phosphate, the following formula (5);

[0060] [Chemical 5]

[0061] Brominated polystyrenes represented by the following formula (6):

[0062] [Chemical 6]

[0063] Brominated polybenzyl acrylates represented by the following formula (7):

[0064] [Chemical 7]

[0065] Brominated epoxy oligomers represented by the following formula (8):

[0066] [Chemical 8]

[0067] Brominated polycarbonate oligomers represented by: Tetrabromobisphenol A, Tetrabromobisphenol A-bis (2,3-dibromopropinole ether), Tetrabromobisphenol A-bis (aryl ether) , Bromine-containing triazine compounds such as tetrabromobisphenol A-bis (hydroxychetyl ether), tetrabromobisphenol A derivatives, tris (tribromophenoxy) triazine, tris (2,3-dibromopropyl) iso cyanurate Bromine-containing isocyanuric acid compounds such as

[0068] Among these, from the viewpoint of heat resistance and exhaust processability, it is preferable that the flame retardant has a melting point of 160 ° C or higher, or the flame retardant has a molecular weight of 200 to 4000. [0069] Generally, when a fiber product is subjected to flame retardant processing by post-processing, the particle size of the flame retardant (E) used has an important effect on the flame retardant performance imparted to the fiber product. The smaller the is, the higher flame retardancy can be imparted to the textile.

[0070] In the present invention, the flame retardant is sufficiently diffused into the polyester fiber by post-processing, and the flame retardant performance of the flame retardant in the polyester fiber is durable. Therefore, the flame retardant (E) The average particle diameter is preferably from 0.1 to 15 111, more preferably from 0.2 to LO / zm.

[0071] In the present invention, the amount of the flame retardant to be contained is adjusted by exhausting the flame retardant to the polyester-based artificial hair, compared with the flame retardant kneading method or the copolymerization method. However, even in the same filament, the flame retardant content can be changed according to the required flame retardant level.

[0072] The exhaust amount of the flame retardant (E) in the present invention is preferably 2 to 20% by weight, more preferably 4 to 15% by weight, based on the polyester-based artificial hair. If the exhaust amount of the flame retardant (E) is less than 2% by weight, there is a tendency that sufficient flame retardancy cannot be imparted to the polyester-based artificial hair. May cause problems such as worsening.

[0073] The flame retardant (E) used in the flame retardant exhaust processing in the present invention is used as a dispersion liquid dispersed in water in the presence of a surfactant or a solution dissolved in an organic solvent.

[0074] When the flame retardant (E) is dispersed in water, the flame retardant (E) can be made fine particles by pulverization in a dry or wet manner. As the surfactant to be used as a dispersion, a non-ionic surfactant or a char-on surfactant is used, and a non-ionic surfactant and a char-on surfactant are used in combination. May be.

[0075] Examples of the above-mentioned nonionic activator include higher alcohol alkylene oxide adducts, alkylphenol alkylene oxide adducts, fatty acid alkylene oxide adducts, polyhydric alcohol aliphatic ester alkylene oxide adducts, and higher alkyls. Examples include polyoxyalkylene type nonionic surfactants such as minalkylene oxide adducts and fatty acid amide alkylene oxide adducts, and polyhydric alcohol type nonionic surfactants such as alkylglycoxides and sucrose fatty acid esters. . [0076] Examples of the above-mentioned surfactants include sulfates such as higher alcohol sulfates, higher alkyl ether sulfates, sulfated fatty acid ester salts, alkylbenzene sulfonates, alkyl naphthalene sulfones. Examples thereof include sulfonates such as acids, higher alcohol phosphate esters, and higher alcohol alkylene oxide adduct phosphate salts.

[0077] On the other hand, examples of the organic solvent include alcohols such as methanol, ethanol and isopronool, aromatic hydrocarbons such as benzene, toluene and xylene, ethers such as dioxane and ethylene glycol, acetone, Examples thereof include ketones such as methyl ethyl ketone, amides such as dimethylformamide, sulfoxides such as dimethyl sulfoxide, and halogenated hydrocarbons such as methylene chloride and chloroform.

[0078] The surfactant and the organic solvent may be used singly or in combination of two or more as required.

[0079] The dispersion used in the present invention can be obtained using an emulsifier or a disperser such as a homogenizer, a colloid mill, a ball mill, or a sand grinder.

[0080] In the present invention, when polyester artificial hair is subjected to flame retardant processing, the solid content concentration of the aqueous dispersion of the flame retardant (E) or the organic solvent solution depends on the dispersion stability and the efficiency of exhaust processing. In this respect, 1 to 50% by weight is preferable, and 5 to 40% by weight is more preferable.

[0081] The exhaust amount of the flame retardant (E) in the present invention can be adjusted by adjusting the concentration of the flame retardant dispersion, the exhaust processing temperature, or the time.

[0082] The method for exhausting the flame retardant of the present invention is not particularly limited. For example, the flame retardant dispersion or solution is attached to the polyester artificial hair by spraying and dried. Then, there is a method in which heat treatment is performed at a temperature of 100 to 220 ° C, more preferably 140 to 190 ° C for 30 seconds to 10 minutes. If the heat treatment temperature is less than 100 ° C, the amorphous regions in the polyester fiber molecules cannot relax or expand to a level that can accept the flame retardant molecules or particles, and tend to be sufficiently exhausted. If the heat treatment temperature is higher, the flame retardant can be more firmly fixed. If the heat treatment temperature exceeds 220 ° C, the fiber strength of the artificial hair may be lowered, or there may be a problem in the separation of the fibers. .

[0083] As another method of exhausting the flame retardant, for example, using a high-pressure dyeing machine, There is a method in which a polyester artificial hair is immersed in a fuel dispersion or solution, and heat treatment is performed at a temperature of 90 to 150 ° C, more preferably 110 to 140 ° C for 3 to 60 minutes. . If the immersion heat treatment temperature is less than 90 ° C, the non-crystalline region force flame retardant molecules or particles in the polyester fiber molecules cannot relax or expand to an acceptable level and tend to be sufficiently exhausted. If the immersion heat treatment temperature exceeds 150 ° C, the fiber strength of the artificial hair may be lowered, or a fiber separation failure may occur.

[0084] By performing the heat treatment process as described above, flame retardant (E) force polyester filament

(Fiber) It is stably and more firmly fixed to the amorphous region in the molecule, and sufficient flame retardancy and durability can be obtained for the polyester filament (fiber).

[0085] In the present invention, as described above, in the conventional flame retardant fine dispersion technology, since the hydrophobicity is strong, the dispersion stability is difficult! Even in the case of aromatic flame retardants, it is difficult to select a non-ionic surfactant or a type of surfactant on the dispersion of flame retardant (E) and mix it. The dispersion stability of the flame retardant (E) can be improved.

[0086] Therefore, in the present invention, even when a polyester (A) having a high glass transition temperature and sufficient heat resistance is used, the flame retardant is exhausted in the above processing temperature range. When using flame retardant polyester fiber obtained by using polyester resin with a low glass transition temperature as artificial hair, use a hair iron for fusion because of its reduced heat resistance. The problem that curling is difficult can be improved.

[0087] The thus obtained flame retardant polyester-based artificial hair fiber of the present invention is a non-crimped raw fiber-like fiber, and its fineness is usually 10 to: LOOdtex, further 20 to 90 dtex. Some are suitable for artificial hair. The artificial hair fiber has heat resistance that can be used for beauty heat appliances (hair irons) at 160-200 ° C, and has self-extinguishing properties that are difficult to ignite.

[0088] When the flame-retardant polyester fiber of the present invention is attached, it can be used as it is, but when it is not attached, it is dyed under the same conditions as ordinary flame-retardant polyester fiber. can do.

[0089] Pigments, dyes, auxiliaries and the like used for dyeing have good weather resistance and flame retardancy Is preferred.

[0090] In general, by using a dyeing method as a method for coloring polyester filaments (fibers), it is possible to obtain polyester artificial hair having a hue superior to that of the original method.

[0091] The fiber for flame retardant polyester-based artificial hair of the present invention is characterized in that, when performing exhaustion processing of a flame retardant for imparting flame retardancy, dyeing is performed simultaneously and the fiber can be colored.

[0092] In the present invention, by simultaneously performing the flame retardant exhaust processing and dyeing, the cost can be reduced by omitting the process, and the physical properties by heating and the like can be reduced compared to the case where exhaust processing and dyeing are performed separately. It is possible to obtain a flame-retardant polyester artificial hair that does not cause deterioration in quality.

[0093] The dye used in the present invention is not particularly limited as long as it is generally used, and can be arbitrarily used, such as black, yellow, red, brown, etc. It may be used. Specific dyes include, for example, benzeneazo (monoazo, disazo, etc.), heterocyclic azo (thiazonolezo, benzothiazonolezo, quinolineazo, pyridine azo, imidazolazo, thiophenazo, etc.), anthraquinone, Condensed dyes (quinophthalene, styryl, coumarin, etc.) disperse dyes.

In the present invention, dyeing is preferably performed in an alkaline dyeing bath having a pH of 8.0 to LO: 0, preferably pH 8.5 to 9.0. In other words, if the pH is 8.0 or more, preferably 8.5 or more, it is superior in dyeing property and color development as compared to acidic dyeing, and more effective in removing oligomers and preventing reattachment. It can be carried out. However, if the pH of the dye bath exceeds 10.0, the tendency to cause hydrolysis of the dye becomes strong, and it becomes necessary to select a dye that has a high possibility of hue change. The pH in the alkaline range where most dyes can be used without problems is most preferably in the range of pH 8.5 to 9.0. Here, the pH 8.0-: LO. 0 dyeing bath is the pH in a dyeing bath containing dyes, dyeing assistants, pH adjusting agents, and the like. As the dye, a disperse dye is mainly used, and as a dyeing assistant, a dispersant, a leveling agent, an oligomer remover, and the like are used, but the dye is not particularly limited thereto. As the pigment, dye, auxiliary agent, and the like used for dyeing, those having good weather resistance and flame retardancy are preferable.

[0095] As the dyeing assistant, a dispersant, a leveling agent, and a leveling agent, which are agents that promote dispersibility and leveling properties, can be blended. Examples of dyeing assistants include naphthalenesulfonic acid formaldehyde condensate, polyoxyalkylene alkyl aryl ether, Oxyalkylene alkyl ester, polyoxyalkylene alkyl aryl ether sulfate, polyoxyalkylene alkyl ether sulfate, and the like can be used. Strong dyeing assistants are preferably used in the range of 0.5 to 2 gZL.

[0096] The pH adjuster has a function of controlling and maintaining the pH of the dyeing bath in the range of 8.0 to: LO. 0, preferably 8.5 to 9.0. For example, a combination of sodium acetate Z pyrophosphate, sodium dihydrogen phosphate, or an organic phosphorus compound and polycarboxylic acid can be used. Powerful pH adjuster, preferably 0.5-2g

Used in the ZL range.

[0097] In the present invention, it is preferable that the dye is exhausted by 0.1% by weight or more with respect to the polyester-based filament. However, in artificial hair, a dark color such as black hair, brown or red hair is used. There are many color variations, such as neutral colors such as, and light colors such as blonde hair and gray hair! Therefore, it is necessary to adjust appropriately for each color.

[0098] The dye exhaust amount in the present invention can be adjusted by the concentration of the dyeing bath, the dyeing temperature, and the time.

[0099] The flame retardant polyester artificial hair fiber of the present invention is excellent in curl setting using a beauty heat instrument (hair iron) and also excellent in curl retention. In addition, the flame retardant polyester-based artificial hair fibers are moderately erased by the irregularities on the fiber surface, and can be used as artificial hair.

[0100] The flame-retardant polyester artificial hair fiber of the present invention comprises a modacrylic fiber, a polyvinyl chloride,

-It may be used in combination with other artificial hair materials such as fiber or nylon fiber, or in combination with human hair.

[0101] Human hair used in hair products such as wigs, hair wigs, and false hairs is generally treated, decolorized and dyed with a cuticle. The fiber surface treatment agent and softener used in the present invention are flammable unlike untreated human hair, but the fiber for flame-retardant polyester artificial hair of the present invention and human hair are mixed with human hair. When mixed at a rate of 60% or less, good flame retardancy is exhibited.

Example [0102] Next, the present invention will be described more specifically based on examples, but the present invention is not limited thereto.

[0103] The method for measuring the characteristic value is as follows.

[0104] (Flame retardant exhausted amount)

The amount of flame retardant exhausted is converted to a flame-retardant processed filament, and the resulting powder lOOmg is compression-molded, and then fluorescent using an X-ray fluorescence analyzer (manufactured by Shimadzu Corporation, EDX-700HS). X-ray analysis was performed to determine and calculate the phosphorus atom content or bromine atom content.

[0105] (Dye concentration)

The dye concentration was determined by dissolving the obtained dyed drawn yarn in orthochlorophenol and measuring the absorbance at a wavelength of 720 nm using a colorimeter (manufactured by Tokyo Koden Co., Ltd., ANA-18A +). The exhausted dye concentration was determined.

[0106] (Strength and elongation)

Using a tensile and compression tester (INTESCO Model 201, manufactured by Intescone Earth), measure the tensile strength and elongation of the filament. Take a 40 mm long filament, sandwich 10 mm of both ends of the filament with a backing sheet (thin paper) to which a double-sided adhesive tape has been applied, and let it air dry overnight to produce a 20 mm long sample. Place the sample on the tester, perform the test at a temperature of 24 ° C, humidity of 80% or less, load lZ30gF X fineness (denier), tensile speed 20mmZ, and measure the tensile strength and elongation at break. Repeat the test 10 times under the same conditions, and use the average value as the filament elongation.

[0107] (Flame retardancy)

Cut a filament with a fineness of about 50dtex into a length of 150mm, bundle 0.7g, hold one end with a clamp, fix it on a stand and hang it vertically. An evaluation was made by injecting a 20 mm flame into a fixed filament with an effective length of 120 mm for 3 seconds and burning it.

Combustion quality

◎: Afterflame time 0 seconds (Do not ignite!)

○: Less than 3 seconds

△: 3 ~ 10 X: 10 seconds or more

—Drip resistance—

◎: Number of drip is 0

○: 5 or less

△: 6〜: LO

X: l l or more.

[0108] (Glossy)

A tow filament with a length of 30 cm and a total fineness of 100,000 dtex is visually evaluated under sunlight.

[0109] A: U for human hair, etc., gloss adjusted for level

◯: Gloss is adjusted moderately

Δ: Slightly too glossy or slightly glossy

X: Too much gloss or too little gloss.

[0110] (Hue)

[0111] ○: Color development close to the original color of pigment or dye

Δ: Slightly lower color developability (slightly white tsupo)

X: Deterioration in color developability is seen (whiter).

[0112] (feel)

Touch a tow filament with a length of 30 cm and a total fineness of 100,000 dtex by hand to evaluate the stickiness of the filament surface.

[0113] ○: No stickiness

Δ: Slightly sticky

X: There is a sticky feeling.

[0114] (Combination street)

POZEO random copolymer (manufactured by Maruhishi Oil Chemical Co., Ltd., KWC-Q) and cationic antistatic agent (Maruhishi) as a fiber surface treatment agent on tow filament with a length of 30 cm and a total fineness of 100,000 dtex Immerse in a 3% aqueous solution containing 50% of 50Z50, manufactured by Yuka Kogyo Co., Ltd., so that 0.1% of each will adhere, and dry at 80 ° C for 5 minutes. A comb (made by Delrin Sabah) is passed through the treated tofufilament, and the ease of passing the comb is evaluated.

[0115] ○: Almost no resistance (light)

△: Some resistance (heavy)

X: There is considerable resistance, or it is caught on the way.

[0116] (Iron set property)

It is an indicator of curling set by hair iron and curling shape retention. Hold the filament in a hair iron heated to 180 ° C and handle it three times to preheat it. At this time, the fusion between filaments, combing, filament shrinkage, and thread breakage are visually evaluated. Next, wind the preheated filament on the hair iron, hold it for 10 seconds, and pull out the iron. Evaluate the ease of removal at this time (rod-out property) and the retention of curl when removed.

Fusion between filaments

○: No fusion

Δ: Slight fusion

X: Fusion

Crimp Z thread breakage

○: No shrinkage or thread breakage

Slightly curled and has thread breakage

X: There is a shrinkage or thread breakage

Rod out

○: Iron rod comes out smoothly

Δ: Slightly difficult to remove iron rod ヽ

X: Iron rod is hard to come off

—Set characteristics—

○: The shape of the curl is maintained

Δ: Slightly collapsed curl shape X: The shape of the curl is broken.

The raw materials used in the examples and comparative examples are as follows.

Polyester):

'Polyethylene terephthalate, Kanebo Gosei Co., Ltd., EFG-85A, glass transition temperature 67 ° C

'Polyethylene terephthalate, manufactured by Mitsubishi Chemical Corporation, BK-2180, glass transition temperature 67 ° C' Polybutylene terephthalate, manufactured by KOLON, KP-210, glass transition temperature 37 ° C Flame retardant aid (B):

'Melamine cyanurate, manufactured by Nissan Chemical Co., Ltd., MC—610

• Antimony trioxide, average particle size 3 m, manufactured by Nippon Seiko Co., Ltd., PATOX—P

'Sodium antimonate, average particle size (primary particles) 2.4 μι, Nippon Seiko Co., Ltd., SA A

Organic fine particles (C):

'Cross-linked acrylic particles, average particle size 1. 8 / ζ πι, manufactured by Soken Chemical Co., Ltd., MX—180TA inorganic fine particles (D):

• Phosphate-treated calcium carbonate, average particle size 9 m, manufactured by Maruo Calcium Co., Ltd., HAP-90 P

'Melamine resin Z silica composite, average particle size 1.9 ^ πι, manufactured by Nissan Chemical Industries, Ltd.

Flame retardant (Ε):

'Organic cyclic phosphorus compound, Sanko Co., Ltd., SANKO-BCA

[Chemical 9]

'Tris (tribromoneopentyl) phosphate, manufactured by Daihachi Chemical Industry Co., Ltd., CR-900 'Pentabromotoluene, Manac Co., PBT

'Tetrabromobisphenol A diglycidyl ether, manufactured by Sakamoto Pharmaceutical Co., Ltd., SR-T

BA400

Surfactant:

• Carotenol with 12 moles of norphenol ethylene oxide

Todecyl phenol ether sulfonate sodium

• Sodium dioctyl sulfosuccinate

Silicone defoamer:

• Nippon Zukar Co., Ltd., FZ-5221

Textile treatment agent:

• Matsumoto Yushi Seiyaku Co., Ltd., KRE—05, KRE—08, KRE—101

Dye:

• Disperse dye, manufactured by Dystar Co., Ltd., Dianix Black SPN Liquid

• Dispersant, manufactured by Meisei Chemical Co., Ltd., DISPER TL

'Neon-based surfactant, manufactured by Daiichi Kogyo Co., Ltd., Amyrazine D

(Production Examples 1 to 4)

100 parts of a composition containing polyethylene terephthalate, antimony flame retardant aid, melamine cyanurate, organic fine particles or organic fine particles dried to a water content of lOOppm or less with the types and mixing ratios shown in Table 1 are colored. Polyester pellets for use PESM6100 B LACK (manufactured by Dainichi Seika Kogyo Co., Ltd., carbon black content 30%, polyester content is included in the polyester (A) component) 2 parts are added and dry blended (Japan) It was supplied to Steelworks Co., Ltd. (TEX44), melt-kneaded at a barrel set temperature of 280 ° C, pelletized, and dried to a water content of lOOppm or less.

Next, using a melt spinning machine (SV30, manufactured by Shinko Machinery Co., Ltd.), from a spinneret (set temperature 280 ° C) having a round cross-section nozzle hole with a nozzle diameter of 0.5 mm at a barrel set temperature of 280 ° C. The molten polymer was discharged, cooled in a water bath at a water temperature of 50 ° C. set at a position 30 mm below the base, and wound at a speed of lOOmZ to obtain an undrawn yarn. The obtained undrawn yarn is drawn in a hot water bath at 80 ° C to make a 4-fold drawn yarn, and a heat roll heated to 200 ° C is used. Then, it was wound up at a speed of lOOmZ and heat treated to obtain a polyester fiber (multifilament) having a single fiber fineness of around 50 dtex.

[table 1]

* 1 Polyethylene terephthalate, Kanebo Gosei Co., Ltd.

* 2 Polyethylene terephthalate, manufactured by Mitsubishi Igaku Co., Ltd.

* 3 Polybutylene terephthalate, manufactured by KOLON

* 4 Melamine cyanurate, manufactured by Nissan Chemical Co., Ltd.

* 5 Antimony trioxide, average particle size 3 / z m, manufactured by Nippon Seiko Co., Ltd.

* 6 Sodium antimonate, average particle size (primary particle) 2.4 m, manufactured by Nippon Seiko Co., Ltd.

* 7 Cross-linked acrylic particles, average particle size 1.8 m, manufactured by Soken Chemical Co., Ltd.

* 8 Phosphate-treated calcium carbonate, average particle size 9 μm, manufactured by Maruo Calcium Co., Ltd. * 9 Melamine resin Z silica composite, average particle size 1.9 ^ πι, manufactured by Nissan Chemical Industries, Ltd.

(Production Examples 5-8)

After dry blending a composition containing polyethylene terephthalate, antimony flame retardant aid, melamine cyanurate, organic fine particles or organic fine particles dried to a water content of lOOppm or less in the types and mixing ratios shown in Table 2. The mixture was supplied to a twin screw extruder (manufactured by Nippon Steel Works Co., Ltd., TEX44), melt kneaded at a barrel setting temperature of 280 ° C, pelletized, and dried to a water content of lOOppm or less. Next, using a melt spinning machine (SV30, manufactured by Shinko Machinery Co., Ltd.), from a spinneret (set temperature 280 ° C) having a round cross-section nozzle hole with a nozzle diameter of 0.5 mm at a barrel set temperature of 280 ° C. The molten polymer was discharged, cooled in a water bath at a water temperature of 50 ° C set at a position 30 mm below the base, and wound at a speed of lOOmZ to obtain an undrawn yarn. The obtained undrawn yarn is drawn in a hot water bath at 80 ° C to make a 4-fold drawn yarn, wound using a heat roll heated to 200 ° C at a speed of lOOmZ, heat treated, and A polyester fiber (multifilament) with a fiber fineness of around 50 dtex was obtained.

[Table 2]

* 1 Polyethylene terephthalate, Kanebo Gosei Co., Ltd.

* 2 Polyethylene terephthalate, manufactured by Mitsubishi Igaku Co., Ltd.

* 3 Polybutylene terephthalate, manufactured by KOLON

* 4 Melamine cyanurate, manufactured by Nissan Chemical Co., Ltd.

* 8 Phosphate-treated calcium carbonate, average particle size 9 μm, manufactured by Maruo Calcium Co., Ltd.

* 9 Melamine resin Z-silica composite, average particle size 1.9 ^ πι, manufactured by Nissan Chemical Industries, Ltd.

(Production Examples 9-12) (Preparation of flame retardant finishing agent) A mill (Immettas Co., Ltd., vertical wet type) mixed with flame retardant, surfactant, antifoaming agent, and ion-exchanged water, and filled with glass beads with a diameter of 0.8 mm in the types and mixing ratios shown in Table 3. In the medium agitating mill (1TSG), after pulverizing until the average particle size reaches 1.5-3.O / xm, the non-volatile content becomes 40% by weight when dried at 120 ° C for 20 minutes. As described above, a flame retardant was obtained by diluting with ion exchange water.

[0122] [Table 3]

[0123] * 10 Organic cyclic phosphorus compound, Sanko Co., Ltd., SANKO— BCA

(Examples 1 to 10)

Using the polyester fiber for artificial hair obtained in Production Examples 1 to 4, a tow filament having a length of 30 cm and a total fineness of 100,000 dtex was produced. On the other hand, a treatment liquid was prepared by diluting the flame retardant caloric agent obtained in Production Examples 7 to 10 to 10% omf.

[0124] Using a combination of the filament type and flame retardant processing agent type shown in Table 4, using a high-pressure dyeing machine (manufactured by Osaka Co., Ltd., LLC type) at a treatment liquid temperature of 130 ° C, Under the pressure of 0.274 MPa, the tow filaments were immersed in a treatment solution having a bath ratio of 1:20, and the amount of each flame retardant exhausted was adjusted to 10% by weight by adjusting the immersion time.

[0125] [Table 4] Examples Comparative examples

1 2 3 4 5 6 7 S 9 1 0 1 2 Flamen tt tt Example ~ 1 ○ ○

a Production example 2 O 0

Production example 3 O O o o 〇〇 O Production example 4 〇

Chicks «Processing agent production example 9 O

Species Production example 10 0 o

»Example 1 1 o o O O O O o saw 12 〇 o

: '»* KFM (min) 60 60 60 60 60 60 60 Z0 90 60 10 1 20

It burned up (%> 10 10 10 10 10 10 1 0 3 18 1 0 1 30

[0126] With respect to the obtained filament, the amount of KRE-05, KRE-08 and KRE-101 as fiber treatment agents was 0.15% omf, 0.05% omf and 0.1% omf, respectively. Thus, it was made to adhere by the dipping method to obtain flame-retardant polyester artificial hair.

[0127] Table 5 shows the results of evaluating the strength, flame retardancy, gloss, feel, combing and ironing properties of the obtained flame-retardant polyester artificial hair.

[0128] [Table 5]

[0129] (Comparative Examples 1 and 2)

As shown in Table 4, the examples were the same except that the amount of flame retardant exhausted was adjusted to 1% by weight (Comparative Example 1) or 30% by weight (Comparative Example 2) by adjusting the immersion time. The same operation as As a result, flame retardant polyester artificial hair was obtained.

Table 5 shows the results of evaluation of iron setability using the obtained flame-retardant polyester-based artificial hair, with high elongation, flame retardancy, gloss, touch, and comb.

[0130] (Examples 11 to 17 and Example 20)

A wrinkle having a diameter of about 40 cm was prepared using 120 g of polyester fiber for artificial hair obtained in Production Examples 5-8. On the other hand, a treatment liquid was prepared by mixing the flame retardant processing agent obtained in Production Examples 7 to 10 with the dyeing liquid prepared by dye receiving as shown in Table 6 so that the flame retardant was 10% owf.

[0131] [Table 6]

[0132] * 10 Disperse dye, manufactured by Dystar Co., Ltd.

* 11 Dispersant, manufactured by Meisei Chemical Co., Ltd.

* 12 Nonionic surfactant, manufactured by Daiichi Kogyo Co., Ltd.

A combination of polyester fiber and flame retardant processed material shown in Table 7 using a high-pressure dyeing machine (manufactured by Osaka Co., Ltd., LLC type) at a treatment liquid temperature of 130 ° C and a pressure of 0.274 MPa Below, it was immersed in the treatment solution having a bath ratio of 1:20 for 60 minutes to treat each flame retardant exhaust amount at 10% by weight and the dye concentration at 1% by weight. Next, using the reducing solution shown in Table 6 and using the reducing solution under reducing conditions, dyed filaments were obtained.

[0133] [Table 7] Examples Comparative examples

1 1 12 13 14 1 5 1 6 17 1 8 19 20 3 4 Filament production example 5 O o

Species Production example 6 O 〇

Manufacturing example 7 〇〇 O O O O o Manufacturing example S O

Burning agent production example S 〇

Species Production example 10 o o

Manufacturing example 1 1 ο o o O 〇〇〇 Manufacturing example 1 2 〇〇

: ¾¾ hour M (min) 60 60 60 60 60 60 60 20 90 60 10 1 20 Burning agent exhaust amount (¾) 10 10 10 1 0 10 10 10 3 1 & 10 1 30

[0134] For the obtained filaments, the amount of KRE-05, KRE-08, and KRE-101 as the fiber treatment agents becomes 0.15% omf, 0.05% omf, and 0.1% omf, respectively. Thus, it was made to adhere by the immersion method, and the flame-retardant polyester type artificial hair was obtained.

[0135] Table 8 shows the results of evaluating the strength, flame retardancy, gloss, hue, touch, combing, and iron set properties of the obtained flame-retardant polyester artificial hair.

[0136] [Table 8]

[Examples 18 to 19]

As shown in Table 7, the examples were the same except that the amount of flame retardant exhausted was adjusted to 3% by weight (Example 18) and 18% by weight (Example 19) by adjusting the immersion time. the same as In this way, a flame-retardant polyester artificial hair was obtained.

Table 8 shows the results of evaluating the strength, flame retardancy, gloss, hue, touch, combing, and iron setting properties of the obtained flame-retardant polyester artificial hair.

[0138] (Comparative Examples 3 to 4)

As shown in Table 7, the examples were the same except that the amount of flame retardant exhausted was adjusted to 1% by weight (Comparative Example 1) and 30% by weight (Comparative Example 2) by adjusting the immersion time. In the same manner as described above, a flame-retardant polyester artificial hair was obtained.

[0139] (Comparative Example 5)

100 parts by weight of polyethylene terephthalate (BK-2180, manufactured by Mitsubishi Chemical Corporation) dried to a water content of lOOppm or less, 10 parts by weight of pentabromotoluene, sodium antimonate (SA-A, manufactured by Nippon Seiko Co., Ltd.) 2 parts by weight Parts, cross-linked acrylic fine particles (MX—180TA, manufactured by Soken Chemical Co., Ltd.) 1 part by weight and black pigment masterbatch (carbon black content 20% by weight, PESM22367BLACK, manufactured by Dainichi Seiki Kogyo Co., Ltd.) 3 parts by weight Were dry blended, supplied to a twin-screw extruder (manufactured by Nippon Steel Works, TEX44), melt-kneaded at a barrel setting temperature of 280 ° C., pelletized, and dried to a water content of lOOppm or less.

Next, using a melt spinning machine (SV30, manufactured by Shinko Machinery Co., Ltd.), the molten polymer is discharged from a spinneret having a round cross-section nozzle hole with a cylinder diameter of 280 ° C and a nozzle diameter of 0.5 mm. It was cooled in a 50 ° C water bath installed at a position of 30 mm, and wound at a speed of lOOmZ to obtain an undrawn yarn. The undrawn yarn obtained was drawn in a hot water bath at 80 ° C to make a 4-fold drawn yarn, wound using a heat roll heated to 200 ° C at a speed of lOOmZ, and heat-treated. A polyester fiber (multifilament) having a single fiber fineness of about 50 dtex was obtained.

Immerse the filaments so that the amount of KRE-05, KRE-08, and KRE-101 as the fiber treatment agent is 0.15% omf, 0.05% omf, and 0.10% omf, respectively. It was made to adhere by the method to obtain a flame-retardant polyester artificial hair.

Using the resulting artificial hair, strong elongation, flame retardancy, gloss, hue, touch, comb, iron Table 8 shows the results of evaluation of setability.

As shown in the table, the flame retardant exhausting process and the flame retardant exhausting process and dyeing are performed at the same time, resulting in excellent elongation, flame retardancy, gloss, touch, combing, and setability. It was confirmed that it was possible to obtain a flame-retardant artificial hair fiber.

Claims

The scope of the claims

[1] Polyalkylene terephthalate or one or more copolyesters mainly composed of polyalkylene terephthalate (A) 100 parts by weight of polyester (A), flame retardant aid (B) 0 to 10 parts by weight, Organic fine particles (C) and Z or inorganic fine particles (D) O. Flame retardant obtained by exhausting a flame retardant to a polyester filament formed from a resin composition containing 1 to 5 parts by weight. Flame retardant polyester artificial hair, wherein the exhaust amount of the flame retardant (E) is 2 to 20% by weight based on the polyester filament.

[2] A flame-retardant polyester artificial hair obtained by dyeing the flame-retardant polyester artificial hair according to claim 1 simultaneously with the flame retardant exhaust process.

[3] Polyester (A) strength The flame-retardant polyester artificial hair according to claim 1 or 2, wherein the polyester (A) strength is at least one polymer selected from the group strength consisting of polyethylene terephthalate, polypropylene terephthalate and polybutylene terephthalate.

[4] Flame Retardant (B) 1S Group power consisting of melamine cyanurate, antimony triacid, antimony tetraacid, antimony pentaoxide, and sodium antimonate. The flame-retardant polyester artificial hair according to any one of 1 to 3.

[5] The organic fine particles (C) are at least one selected from the group consisting of polyarylate, polyamide, fluorine resin, silicone resin, crosslinked acrylic resin, and crosslinked polystyrene. Fire retardant polyester artificial hair as described in Kakko.

[6] The inorganic fine particles (D) are at least one selected from the group consisting of calcium carbonate, silicon oxide, titanium oxide, aluminum oxide, zinc oxide, talc, kaolin, montmorillonite, bentonite and my strength. The flame-retardant polyester artificial hair according to any one of claims 1 to 5.

[7] Flame retardant (E) used for flame retardant exhaust processing is phosphorus flame retardant, bromine-containing phosphorus flame retardant, brominated aliphatic flame retardant, brominated aromatic flame retardant, brominated Polystyrene flame retardant, brominated benzyl acrylate, flame retardant, brominated epoxy flame retardant, brominated poly-bonate flame retardant, tetrabromobisphenol A derivative, bromine-containing triazine compound and bromine-containing Group power consisting of isocyanuric acid compounds at least one selected The flame-retardant polyester artificial hair according to claims 1 to 6, which is a flame retardant

[8] The flame retardant polyester artificial hair according to claim 7, wherein the flame retardant (E) used for the flame retardant exhaust processing has a melting point of 160 ° C or higher.

[9] The molecular weight of the flame retardant (E) used in the flame retardant exhaust processing is 200 to 4000.

7. Flame-retardant polyester artificial hair according to 7.

[10] Dyeing to a polyester filament and flame retardant exhaustion processing power are simultaneously performed at a temperature of 90 to 150 ° C., and the polyester artificial hair contains 0.1% by weight or more of the dye. 9. Flame retardant polyester-based artificial hair as described in the article.

[11] The flame-retardant polyester artificial hair according to any one of claims 1 to 10, wherein the flame-retardant polyester fiber has a non-crimped raw silk shape.

[12] The flame-retardant polyester-based artificial hair fiber according to any one of claims 1 or 3 to 9, wherein the fiber is flame-retardant polyester-based fiber.

[13] The flame retardant polyester artificial hair according to any one of claims 1 to 12, wherein the single fiber fineness is 10 to: LOOdtex.