WO2007049561A1 - Polyester-based artificial hair - Google Patents

Polyester-based artificial hair Download PDF

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Publication number
WO2007049561A1
WO2007049561A1 PCT/JP2006/321069 JP2006321069W WO2007049561A1 WO 2007049561 A1 WO2007049561 A1 WO 2007049561A1 JP 2006321069 W JP2006321069 W JP 2006321069W WO 2007049561 A1 WO2007049561 A1 WO 2007049561A1
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WO
WIPO (PCT)
Prior art keywords
polyester
artificial hair
flame retardant
weight
parts
Prior art date
Application number
PCT/JP2006/321069
Other languages
French (fr)
Japanese (ja)
Inventor
Toshiyuki Masuda
Original Assignee
Kaneka Corporation
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Publication date
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Publication of WO2007049561A1 publication Critical patent/WO2007049561A1/en

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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • A—HUMAN NECESSITIES
    • A41—WEARING APPAREL
    • A41G—ARTIFICIAL FLOWERS; WIGS; MASKS; FEATHERS
    • A41G3/00—Wigs
    • A41G3/0083—Filaments for making wigs
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments

Definitions

  • the present invention relates to a polyester-based artificial hair formed from polyethylene terephthalate and polytrimethylene terephthalate.
  • polyester fiber when polyester fiber is used as an artificial hair material, the polyester fiber has high rigidity, and when it is made to have a fineness close to that of human hair, it becomes bristles that are as if a wire is implanted. In order to ensure moderate softness, it is necessary to use with a finer fineness. However, since the thickness differs from that of human hair, there is a difference in appearance from human hair.
  • Polyester fiber has the advantage of being able to be freely styled by hairdressing heat appliances such as hair irons due to its excellent heat resistance, and because it has rigidity as a characteristic of polyester, when it is made into a wig, The advantage of being easy to form a hairstyle with is there.
  • hairdressing heat appliances such as hair irons due to its excellent heat resistance
  • the advantage of being easy to form a hairstyle with is there.
  • frizziness, tandals and frits are relatively easy to occur, and it was necessary to repair the frizziness and frits that occurred by using beauty heat appliances themselves or in a professional hair salon. .
  • nylon fibers have low rigidity, so that wigs using nylon fibers become cat hair (soft and not bulky hair), and it is not possible to form hairstyles that have a trendy mass among young people in recent years. It also has the problem of
  • Patent Document 1 International Publication WO2005Z010247
  • the object of the present invention is to solve the conventional problems as described above, maintain fiber properties such as heat resistance and high elongation of polyester fiber, have excellent curl characteristics, and have a soft touch close to human hair. It is intended to provide polyester-based artificial hair that is less prone to tandals and frits at the ends.
  • the inventors of the present invention maintain the physical properties of ordinary polyester fibers such as heat resistance and high elongation by mixing polyethylene terephthalate and polytrimethylene terephthalate at a specific ratio and spinning them, and curl characteristics. It has been found that a polyester-based artificial hair that is excellent in hair, has a soft tactile feel similar to human hair, is less likely to cause tandals and frits on the ends of the hair, and is produced.
  • the present invention relates to the following artificial hair.
  • Polyester artificial hair according to (1) having an intrinsic viscosity of polyethylene terephthalate ( ⁇ ) of 0.6 to 1.2 dlZg.
  • polyester-based artificial hair according to (1) which has an intrinsic viscosity of polytrimethylene terephthalate (B) of 0.6 to 1.5 dlZg.
  • a composition containing 5 to 30 parts by weight of a bromine-containing flame retardant (C) was further formed for a total of 100 parts by weight of polyethylene terephthalate (A) and polytrimethylene terephthalate (B) (1) ⁇ (3) V, polyester artificial hair according to any of the above.
  • Bromine-containing flame retardant (C) is brominated aromatic flame retardant, bromine-containing phosphate ester flame retardant, brominated polystyrene flame retardant, brominated benzaryl acrylate flame retardant, brominated epoxy Group flame retardant, brominated phenoxy flame retardant, brominated polycarbonate flame retardant, tetrabromobisphenol A derivative, bromine-containing triazine compound and bromine-containing isocyanuric acid compound
  • the polyester-based artificial hair according to (4) which is a flame retardant.
  • the antimony compound (D) is at least one antimony compound selected from the group consisting of antimony trioxide, antimony tetraacid, antimony tetraacid, antimony pentoxide and sodium antimonate (6 ) The polyester-based artificial hair described.
  • the polyester-based artificial hair according to (8) which is a compound having at least one of a modified wax, polydimethylsilicone, and modified silicone resin.
  • the polyester according to (10), wherein the organic fine particles (F) are at least one selected from the group force consisting of polyarylate, polyamide, fluorine resin, silicone resin, bridged acrylic resin, and crosslinked polystyrene. Artificial hair.
  • the fiber properties such as heat resistance and high elongation of the polyester fiber are maintained, excellent in the roll characteristics, soft touch close to human hair, Polyester-based artificial hair that is unlikely to occur can be obtained.
  • the polyester-based human hair of the present invention also has excellent transparency (color development)!
  • the polyester-based artificial hair of the present invention has polyethylene terephthalate as the polyester.
  • polyethylene terephthalate is used as a polyester by using a mixture of polyethylene terephthalate (A) and polytrimethylene terephthalate (B).
  • a soft texture and a tactile sensation can be obtained from the low elastic modulus of polytrimethylene terephthalate (B).
  • (Ii) is a copolymerized polyester mainly containing polyethylene terephthalate or polytrimethylene terephthalate (containing 80 mol% or more) in addition to polyethylene terephthalate and polytrimethylene terephthalate, and containing a small amount of a copolymer component. Is also included.
  • 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, Ethylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, 1,6-hexanediol, neopentyl glycol, 1,4-cyclohexanedimethanol, diethylene glycol, polyethylene glycol , Trimethylol mouthpiece, pentaerythrito Le, 4-hydroxybenzoic acid, ⁇ - force Purorataton the like.
  • sulfonic acid salts such as 5-sodium sulfoisophthalic acid, dihydroxyethyl 5-sodium sulfoiso
  • the copolyester is usually prepared by reacting a polymer of terephthalic acid and Z or its derivative (for example, methyl terephthalate) as a main component with an alkylene glycol and containing a small amount of a copolymer component. Although it is preferable to produce it by the stability and ease of operation, a small amount of co-polymer is added to the mixture of the main terephthalic acid and Z or its derivative (for example, methyl terephthalate) and alkylene glycol.
  • the polymerization component may be produced by polymerizing a monomer or oligomer component.
  • the copolymer polyester is not particularly limited in the way of copolymerization, in which the copolymer component is polycondensed to the main chain and Z or side chain of polyethylene terephthalate or polytrimethylene terephthalate as a main component. There is no.
  • the intrinsic viscosity of the polyethylene terephthalate (A) used in the present invention is preferably 0.6 to 1.2 dlZg, more preferably 0.65-1.ldlZg, more preferably 0.7 to 1. OdlZg. Even better.
  • the intrinsic viscosity of polyethylene terephthalate (A) is less than 0.6 dlZg, the mechanical strength tends to decrease, and when it comes into contact with a flame, it tends to melt and drip easily.
  • the intrinsic viscosity of polyethylene terephthalate (A) exceeds 1.2 dl / g, yarn breakage tends to occur during melt spinning, and the touch tends to be hard.
  • the intrinsic viscosity of the polytrimethylene terephthalate (B) used in the present invention is 0.6 to 1.5 dlZg, more preferably 0.7 to 1.4 dlZg, and still more preferably 0.8 to 1. It is 3dlZg.
  • the intrinsic viscosity of polytrimethylene terephthalate (B) is less than 0.6 dlZg, the mechanical strength tends to decrease, or when it comes into contact with a flame, it tends to melt and drip easily.
  • the intrinsic viscosity of polytrimethylene terephthalate (B) exceeds 1.5 dlZg, yarn breakage tends to occur during melt spinning, and the tactile sensation tends to become hard.
  • the present invention for the purpose of improving safety when used as artificial hair, it is preferable to add flame retardant to impart flame retardancy.
  • a bromine-containing flame retardant (C) as the flame retardant used because it can impart excellent flame retardancy to artificial hair.
  • the bromine-containing flame retardant (C) used in the present invention is not particularly limited, and any bromine-containing flame retardant generally used can be used.
  • Specific examples of the bromine-containing flame retardant (C) in the present invention include bromine-containing phosphate ester flame retardant, brominated polystyrene flame retardant, and fluorination, which can impart excellent flame retardancy to artificial hair.
  • Benzyl acrylate flame retardant brominated epoxy flame retardant, brominated phenoxy resin flame retardant, brominated polycarbonate flame retardant, tetrabromobisphenol A derivative, bromine-containing triazine compound, bromine-containing isocyanuric acid Bromine-containing phosphate ester flame retardant, brominated epoxy flame retardant, brominated phenoxy resin, which can impart excellent fiber properties and heat resistance to compounds and artificial hair, and can provide excellent processing stability during fiber production -Based flame retardants.
  • bromine-containing flame retardant (C) in the present invention include, for example, pentabromotoluene, hexabromobenzene, decabromodiphenyl, decabromodiphenyl ether, and bis (tribromophenoxy).
  • Bromine-containing phosphate esters such as ethane, tetrabromophthalic anhydride, ethylene bis (tetrabromophthalimide), ethylene bis (pentabromophenol), otatabromotrimethylphenolindane, tris (tribromoneopentyl) phosphate, bromine Polystyrenes, brominated polybenzyl acrylates, fluorinated epoxy oligomers, brominated phenoxy resins, brominated polycarbonate oligomers, tetrabromobisphenol A, tetrabromobisphenol A-bis (2,3-dibu Lomopropyl ether), Tetrabromobisphenol A-bis (aryl ether), tetrabromobisphenol A-bis (hydroxyethyl ether) and other tetrabromobisphenol A derivatives, and bromine-containing triazine compounds such as tris (tripromophenoxy) triazine And bromine-containing is
  • the amount of bromine-containing flame retardant (C) used in the present invention is preferably 5 to 30 parts by weight with respect to a total of 100 parts by weight of polyethylene terephthalate (A) and polytrimethylene terephthalate (B). 25 to 5 parts by weight is more preferred 7 to 20 parts by weight is even more preferred. If the amount of bromine-containing flame retardant (C) used is less than 5 parts by weight, the flame retardant effect tends to be difficult to obtain, and if it exceeds 30 parts by weight, the mechanical properties, heat resistance, and drip resistance of the resulting fiber There is a tendency to damage.
  • the flame retardancy is expressed by including the bromine-containing flame retardant (C) in the composition, but the flame retardant is expressed by including the antimony compound (D).
  • the effect can be remarkably improved.
  • the antimony compound (D) used in the present invention is not particularly limited. Specific examples of the antimony compound (D) include antimony triacid, antimony tetraacid, antimony tetraacid, antimony pentaacid, sodium antimonate and the like. Of these, sodium antimonate is preferred from the viewpoint of the spinnability of the composition.
  • the average particle size of the antimony compound (D) in the present invention is preferably 0.015 to 15 ⁇ m.
  • the antimony compound (D) 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.
  • the amount of antimony compound (D) used in the present invention is preferably 0.5 to: LO parts by weight with respect to 100 parts by weight of the total of polyethylene terephthalate (A) and polytrimethylene terephthalate (B). 6-9 parts by weight is more preferred 0.7-7 parts by weight is even more preferred.
  • the amount of the antimony compound (D) used is less than 0.5 parts by weight, the improvement of the flame retardancy tends to be small, and when it exceeds 10 parts by weight, the processing stability, appearance and transparency are low. There is a tendency to be damaged.
  • the dispersion state of the antimony compound (D) is improved by further containing the dispersant (E) in the composition, so that the spinning stability is improved and the fiber surface is protected. Disappears. Further, the dispersant (E) can impart slipperiness to the fiber surface, and a filament with good combing can be obtained.
  • a plasticizer or a lubricant can be used as the dispersant (E) used in the present invention.
  • the plasticizer or lubricant is not particularly limited, and any plasticizer or lubricant can be used as long as it is generally used.
  • dispersant (E) in the present invention include, for example, phthalates, adipates, polyester plasticizers, acrylic oligomer plasticizers, montanic waxes, and montanic esters.
  • montanic acid-based wax, montanic acid ester-based wax, partially-kenned montanic acid-based wax, montanic acid metal salt, polyethylene-based wax, polyethylene oxide-based wax, polytetrafluoroethylene, fluorine-modified Wax, polydimethylsilicone, and modified silicone resin have an influence on fiber properties such as dispersibility, flame retardancy, and heat resistance of antimony compounds. These compounds may be used alone or as a mixture of two or more.
  • the amount of the dispersant (E) used in the present invention is preferably 0.05 to 3 parts by weight with respect to 100 parts by weight of the total of polyethylene terephthalate (A) and polytrimethylene terephthalate (B), and 0.1 to 0.1 parts by weight. ⁇ 2.5 parts by weight is more preferred 0.15 to 2 parts by weight is even more preferred.
  • the amount of the dispersant (E) used is less than 0.05 parts by weight, the antimony compound particles (D) are partially agglomerated, and there is a tendency that yarn breakage occurs during the spinning process and the tactile feel of the fiber surface is reduced. There is. If it exceeds 3 parts by weight, the spinning stability will be lowered and yarn breakage will occur, and mechanical properties, heat resistance, flame resistance and drip resistance will tend to be impaired.
  • the fiber for flame-retardant polyester-based artificial hair of the present invention further comprises organic fine particles in the composition.
  • fine protrusions By mixing (F) and Z or inorganic fine particles (G), fine protrusions can be formed on the surface of the resulting fiber, and the gloss and gloss of the fiber surface can be adjusted.
  • the organic fine particles (F) in the present invention may be any organic resin having a structure that is incompatible with or partially incompatible with polyethylene terephthalate (A) and Z or polytrimethylene terephthalate (B). Can be used.
  • examples of the organic fine particles (F) include polyarylate, polyamide, fluorine resin, silicone resin, crosslinked acrylic resin, and crosslinked polystyrene. These may be used alone or in combination of two or more. Among these, cross-linked polyester particles and cross-linked acrylic particles having excellent heat resistance and dispersibility that can stably impart a gloss adjusting effect are preferred.
  • the inorganic fine particles (G) used in the present invention include polyethylene terephthalate (A) and Z or polytrimethylene terephthalate (B Those having a refractive index close to that of) are preferred.
  • Examples of the inorganic fine particles (G) include calcium carbonate, silicon oxide, titanium oxide, aluminum oxide, zinc oxide, talc, strong iron, montmorillonite, bentonite, and my strength. These may be used alone or in combination of two or more.
  • particles close to a spherical shape are preferably composite particles mainly composed of silicon oxide and acid hydride, which have a higher gloss adjustment effect.
  • the inorganic fine particles (G) 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.
  • the average particle size of the organic fine particles (F) and Z or inorganic fine particles (G) used in the present invention is preferably 0.1 to 15 m force, more preferably 0.2 to 10 m force, and 0.5 to 8 111 Power ⁇ Preferred ⁇ ⁇ ⁇ .
  • the average particle size of organic fine particles (F) and Z or inorganic fine particles (G) is smaller than 0.1 ⁇ m, the gloss adjustment effect tends to be small. There is a tendency to break down or to break yarn.
  • the amount of organic fine particles (F) and Z or inorganic fine particles (G) used in the present invention is not particularly limited, but a total of 100 parts by weight of polyethylene terephthalate (A) and polytrimethylene terephthalate HB). On the other hand, 0.1 to 5 parts by weight is preferable, 0.2 to 3 parts by weight is more preferable, and 0.3 to 2 parts by weight is more preferable.
  • the amount of organic fine particles (F) and Z or inorganic fine particles (G) used is less than 0.1 part by weight, the fine protrusions formed on the fiber surface are reduced, and the gloss adjustment effect on the fiber surface tends to be small.
  • the amount exceeds 5 parts by weight appearance, hue, and color developability tend to be impaired.
  • Polyester artificial hair obtained by the present invention includes, for example, polyethylene terephthalate (A), polytrimethylene terephthalate (B), bromine-containing flame retardant (C), antimony compound (D), dispersant (E ), Organic fine particles (F), inorganic fine particles (G), etc. are dry blended, and then the polyester composition obtained by melt kneading using various general kneaders is used with a single screw extruder. And can be obtained by melt spinning.
  • Examples of the kneader used in the production of the rosin composition include, for example, a single screw extruder, a twin screw extruder, a roll, a Banbury mixer, and an ader.
  • a twin screw extruder is preferable from the viewpoint of adjusting the kneading degree and ease of operation.
  • the barrel set temperature is 260 to 300.
  • the mixture is melt-kneaded at a discharge temperature of 50 to 150 kgZhr and a screw rotation speed of 150 to 200 rpm, the strand is taken out of the die, water-cooled, and then pelletized using a strand cutter to obtain the polyester-based artificial hair of the present invention.
  • a composition to be produced can be obtained.
  • the polyester-based artificial hair of the present invention has, for example, a temperature of 270 to 310 ° C such as an extruder, a gear pump, and a die, melt-spun, and passes the spun yarn through a heating tube, and then has a glass transition point. It can be obtained by cooling to below and taking it off at a speed of 50 to 5000 mZ. 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 the cooling air, the temperature of the cooling water tank, the cooling time, and the take-up speed can be appropriately adjusted according to the discharge amount and the number of holes in the base.
  • the polyester-based artificial hair of the present invention comprises polyethylene terephthalate (A) and polytrimethylene terephthalate (B), bromine-containing flame retardant (C), antimony compound (D), dispersant (E ), Organic fine particles (F), inorganic fine particles (G), etc. are dry blended using a twin screw extruder equipped with a gear pump and a spinning nozzle or a single screw extruder using a screw having kneading ability.
  • the resin composition can be obtained by melt spinning without taking out the resin composition.
  • the obtained spun yarn is heat-stretched.
  • Stretching is a two-step method in which the spun yarn is wound and then stretched, and continuously stretched without winding. Any of direct spinning and drawing methods may be used.
  • Hot stretching is performed by a single-stage stretching method or a multi-stage stretching method having two or more stages.
  • 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 together as appropriate.
  • the polyester-based artificial hair of the present invention may contain various additives such as a heat-resistant agent, a light stabilizer, a fluorescent agent, an antioxidant, an antistatic agent, and a pigment as necessary.
  • the fineness of the polyester-based artificial hair of the present invention obtained as described above is usually 10 to: LO Odtex, more preferably 20 to 90 dtex. Suitable for artificial hair.
  • the artificial hair has heat resistance capable of using a beauty heat instrument (hair iron) at 160 to 200 ° C., and preferably has self-extinguishing properties that are difficult to ignite.
  • the polyester-based artificial hair of the present invention can be used after being colored by dyeing or priming. When coloring by dyeing, it can be dyed under the same conditions as ordinary polyester fibers.
  • an original attachment fiber can be obtained by melt-kneading the pigment used for normal polyester fiber.
  • the pigment, dye, auxiliary agent and the like used for dyeing those having good weather resistance and flame retardancy are preferable.
  • the polyester-based artificial hair of the present invention is excellent in curl setting using a beauty heat instrument (hair iron) and excellent in curl retention. Moreover, the surface of the fiber is moderately erased by the irregularities on the fiber surface, and can be used as artificial hair.
  • oil agents such as fiber surface treatment agents and softeners can be used to provide a feeling of touch and texture, making it closer to human hair.
  • the flame-retardant polyester artificial hair of the present invention may be used in combination with other artificial hair materials such as modacrylic fiber, polysalt fiber fiber, nylon fiber, etc., or in combination with human hair. May be.
  • the characteristic value measurement method is as follows.
  • the tensile strength and elongation of the filaments were measured using a tensile / compression tester (INTESCO Model 201, manufactured by Intescone Earth).
  • a 20 mm long sample was prepared by taking one filament with a length of 40 mm, sandwiching 10 mm of both ends of the filament with a backing paper (thin paper) to which a double-sided adhesive tape was applied, and air-dried overnight.
  • a sample was attached to the tester, and the test was performed at a temperature of 24 ° C, humidity of 80% or less, an initial load of lZ30gF X fineness (denier), and a tensile speed of 20mmZ, and the tensile strength and elongation at break were measured.
  • the test was repeated 10 times under the same conditions, and the average value was defined as the filament elongation.
  • the 10% stretch elastic recovery rate of the filament was measured. Take one filament with a length of 40 mm, and sandwich 10 mm of both ends of the filament with a backing paper (thin paper) to which a double-sided tape with glue is attached. A 20 mm long sample was made by air drying overnight. A sample was mounted on the testing machine, and after 10% elongation at a temperature of 24 ° C, humidity of 80% or less, and a tensile speed of 200 mmZmin, it was immediately recovered at the same speed.
  • INTESCO Model 201 manufactured by Intescone Earth
  • Tensile recovery curve force The elongation (B%) with respect to the initial length of the sample when it became the same as the initial load at the time of recovery was read, and the 10% elongation elastic recovery rate was obtained by the following formula.
  • the 10% stretch elastic recovery rate can be evaluated as an index of the likelihood of the occurrence of frits at the ends of the hair, and the greater the stretch elastic recovery rate, the less likely that the frits occur.
  • the thermal contraction rate of the filament was measured using SSC5200H thermal analysis TMAZSS150C manufactured by Seiko Denshi Kogyo. Ten filaments were tied to the fixture so that the distance between chucks was 10 mm. 5. A 55mgZdtex load was applied, the heat shrinkage rate was measured in the range of 30 to 280 ° C at a temperature increase rate of 3 ° CZ, and the heat shrinkage rate at 180 ° C was defined as the heat shrinkage rate.
  • a tow filament having a length of 30 cm and a total fineness of 100,000 dtex was visually evaluated under sunlight.
  • a sensory evaluation was performed by a professional hairdresser and evaluated in three stages.
  • ⁇ A soft texture similar to human hair
  • a comb (made by Delrin Sabah) was passed through a tow filament with a length of 30 cm and a total fineness of 100,000 dtex, and the ease of combing was evaluated.
  • a filament with a fineness of about 50 dtex was cut into a length of 150 mm, 0.7 g was bundled, one end was sandwiched between clamps, fixed to a stand, and hung vertically.
  • a 20 mm flame was indirectly flamed for 3 seconds in a fixed filament with an effective length of 120 mm and burned to evaluate the combustibility.
  • Bundle one hand of a tow filament with a length of 30 cm and a total fineness of 100,000 dtex, hold it with your hand, shake it ten times with strength that makes the tow fall apart, pass the comb (made of Delrin resin), The condition (ease of combing) was evaluated.
  • the comb can be passed through without the pulling force of the hair (most resistance! /)
  • the composition shown in Table 1 is dried to a water content of lOOppm or less, dry blended, supplied to a twin-screw extruder (manufactured by Nippon Steel Co., Ltd., TEX44), and melted at a barrel set temperature of 260 ° C. After melt-kneading and pelletizing, it was 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 rectangular cross-section nozzle hole with a barrel setting temperature of 260 ° C and an aspect ratio of 1.4: 1.
  • the obtained unstretched yarn was stretched 4 times using a heat roll heated to 85 ° C, heat-treated using a heat roll heated to 190 ° C, wound at a speed of 30 mZ, and A polyester fiber (multifilament) having a fiber fineness of about 65 dtex was obtained.
  • KWC-Q Random copolymer polyether of ethylene oxide propylene oxide; manufactured by Maruhishi Oil Chemical Co., Ltd.
  • Z Carochemical 29 cationic surfactant
  • the solution was adhered so that the liquid content was 25% with respect to the tow weight, and dried at 120 ° C. for 10 minutes using a hot air dryer.
  • Table 1 shows.
  • Polyester fibers having a single fiber fineness of around 65 dtex were obtained in the same manner as in the Examples with compositions having the blending ratios shown in Table 1. Using the obtained fiber,
  • Table 1 shows the results of evaluation of 10% stretch elastic recovery, heat shrinkability, transparency, touch, combing, flame retardancy, tidal properties of hair ends, and iron set properties.
  • Table 1 shows the results of evaluation of 10% stretch elastic recovery, heat shrinkability, transparency, touch, combing, flame retardancy, tidal properties of hair ends, and iron set properties.
  • the artificial hair fiber of the present invention has a soft tactile sensation similar to human hair while maintaining the mechanical properties and thermal properties of polyester, compared to conventional artificial hair fibers, and the tandals of the hair ends. It was confirmed that it can be effectively used as polyester-based artificial hair, which is less likely to cause frits.
  • the polyester-based artificial hair of the present invention maintains the physical properties of polyester fibers such as heat resistance and high elongation, is excellent in transparency (color development) and curling characteristics, and has a soft touch close to human hair. , Tendall of hair ends, Fritz is unlikely to occur. Therefore, it is useful in the artificial hair industry.

Abstract

It is intended to provide a polyester-based artificial hair which sustains the fiber properties inherent to polyester fibers (for example, a high heat resistance and a high elongation), is excellent in transparency (color development performance) and curling characteristics, has a soft texture similar to the human hair and suffers from little hair tip tangling or flitting. This object can be achieved by providing a polyester-based artificial hair which is obtained by blending polyethylene terephthalate with polytrimethylene terephthalate at a specific ratio and then melt-spinning the obtained blend. By further using a bromine-containing flame retardant agent, it becomes possible to provide a polyester-based artificial hair which has flame retardancy in addition to the characteristics as described above.

Description

明 細 書  Specification
ポリエステル系人工毛髪  Polyester artificial hair
技術分野  Technical field
[0001] 本発明は、ポリエチレンテレフタレートおよびポリトリメチレンテレフタレートから形成 されるポリエステル系人工毛髪に関する。  The present invention relates to a polyester-based artificial hair formed from polyethylene terephthalate and polytrimethylene terephthalate.
背景技術  Background art
[0002] かつら、ヘアーウイッグ、付け毛、ヘアーバンド、ドールヘアーなどの頭髪製品にお いては、従来、人毛や人工毛髪 (モダクリル繊維、ポリ塩ィ匕ビニル繊維)などが使用さ れてきている。しかし、人毛の提供は困難になってきており、人工毛髪の重要性が高 まってきている。人工毛髪素材として、難燃性の特長を生力してモダクリルが多く使用 されてきたが、耐熱温度の点では不十分であった。近年になり、特許文献 1に開示さ れているように耐熱性に優れるポリエチレンテレフタレートに代表されるポリエステル を主成分とする繊維を用いた人工毛髪繊維が提案されるようになってきた。  In hair products such as wigs, hair wigs, furs, hair bands, doll hairs, human hair and artificial hair (modacrylic fibers, polyvinyl chloride and vinyl fibers) have been used in the past. Yes. However, the provision of human hair has become difficult, and the importance of artificial hair has increased. Modacrylic has been widely used as an artificial hair material due to its flame-retardant characteristics, but it was insufficient in terms of heat-resistant temperature. In recent years, as disclosed in Patent Document 1, artificial hair fibers using fibers mainly composed of polyester typified by polyethylene terephthalate having excellent heat resistance have been proposed.
[0003] し力しながら、ポリエステル繊維を人工毛髪素材として使用した場合、ポリエステル 繊維は、剛性が強いため、人毛に近い繊度にすると、まるで針金を植毛したような剛 毛となる。適度な柔ら力さを確保するためには、細い繊度にして使用する必要がある 。しかし、人毛との太さが異なってくるため、外観上、人毛との差異が生じ、不自然に なると 、う問題を有して ヽた。  [0003] However, when polyester fiber is used as an artificial hair material, the polyester fiber has high rigidity, and when it is made to have a fineness close to that of human hair, it becomes bristles that are as if a wire is implanted. In order to ensure moderate softness, it is necessary to use with a finer fineness. However, since the thickness differs from that of human hair, there is a difference in appearance from human hair.
[0004] また、人工毛髪を使ったかつらを着用、使用していると、人工毛髪に用いられてい る材料によっては、人工毛髪の主として毛先等に縮れ、タンダル (毛先の絡み)ゃフリ ッッ（毛先の折れ曲がり）が発生する。このような縮れ、タンダル、フリッツが発生すると 、人工毛髪の自然観が著しく損なわれ、一見してかつらであることが判明してしまうと いう不具合が生じる。このため、かつらの着用者は定期的に人工毛髪の修正を行なう 力 交換する必要があった。  [0004] In addition, when wearing and using a wig made of artificial hair, depending on the material used in the artificial hair, the artificial hair may be shrunk mainly into the hair tip, etc. (Bending of the hair ends) occurs. When such shrinkage, tandals and frits occur, the natural view of artificial hair is remarkably impaired, and at first glance it becomes clear that it is a wig. For this reason, wig wearers had to exchange force to periodically correct artificial hair.
[0005] ポリエステル繊維は、その優れた耐熱性により、ヘアーアイロンなどの美容熱器具 により、自由にスタイリングすることができるという長所やポリエステルの特性として剛 性があるため、かつらに仕立てたとき、量感のある髪型を形成しやすいという長所が ある。しかし縮れ、タンダル、フリッツが比較的発生し易いという短所があり、発生した 縮れやフリッツは、自ら美容熱器具を使用して修復したり、専門のへアサロンにおい て修復することが必要であった。 [0005] Polyester fiber has the advantage of being able to be freely styled by hairdressing heat appliances such as hair irons due to its excellent heat resistance, and because it has rigidity as a characteristic of polyester, when it is made into a wig, The advantage of being easy to form a hairstyle with is there. However, there is a disadvantage that frizziness, tandals and frits are relatively easy to occur, and it was necessary to repair the frizziness and frits that occurred by using beauty heat appliances themselves or in a professional hair salon. .
[0006] それに対し、このような縮れが比較的発生し難 、繊維として、ナイロン繊維がある。  [0006] On the other hand, such a crimp is relatively difficult to occur, and there is a nylon fiber as a fiber.
しかし、ナイロン繊維を使用した人工毛髪は、ナイロンの持つ特質により、工場出荷 時に熱処理によって所望の形にー且整えると、後から例えばカールを掛けたいなどと 思っても、一旦形成された形を変更することはできない。また、ナイロン繊維は、剛性 が低いため、ナイロン繊維を使用したかつらが猫毛 (柔らかぐ嵩高くない毛髪）にな りやすぐ近年、若者の間に流行の量感のある髪型を形成することができないという 問題も有している。  However, artificial hair using nylon fibers, due to the nature of nylon, once formed into a desired shape by heat treatment at the time of shipment from the factory, even if you later want to curl it, for example, it will once form. It cannot be changed. Nylon fibers have low rigidity, so that wigs using nylon fibers become cat hair (soft and not bulky hair), and it is not possible to form hairstyles that have a trendy mass among young people in recent years. It also has the problem of
[0007] また、塩ィ匕ビニルゃモダアクリルは、高熱で容易に分解または変質してしまう特質を 有しているため、経時変化により縮れが発生しても、かつらに高熱を用いることができ ず、縮れの修復が困難であると 、う問題を有して 、る。  [0007] Since vinyl chloride modacrylic has the property of being easily decomposed or altered by high heat, even if it shrinks due to aging, high heat cannot be used for the wig. However, if it is difficult to repair frizz, it has a problem.
[0008] このように、耐熱性、カール特性に優れ、人毛に近いソフトな触感を有し、毛先のタ ンダル、フリッツの起こり難い人工毛髪は、いまだ得られていない。 [0008] As described above, artificial hair that is excellent in heat resistance and curling characteristics, has a soft tactile sensation similar to human hair, and is difficult to generate tandals and frits on the ends of hairs has yet been obtained.
特許文献 1：国際公開 WO2005Z010247号公報  Patent Document 1: International Publication WO2005Z010247
発明の開示  Disclosure of the invention
発明が解決しょうとする課題  Problems to be solved by the invention
[0009] 本発明の目的は、前述のごとき従来の問題を解決し、ポリエステル繊維の耐熱性、 強伸度など繊維物性を維持し、カール特性に優れ、人毛に近いソフトな触感を有し、 毛先のタンダル、フリッツの起こり難い、ポリエステル系人工毛髪を提供することであ る。 [0009] The object of the present invention is to solve the conventional problems as described above, maintain fiber properties such as heat resistance and high elongation of polyester fiber, have excellent curl characteristics, and have a soft touch close to human hair. It is intended to provide polyester-based artificial hair that is less prone to tandals and frits at the ends.
課題を解決するための手段  Means for solving the problem
[0010] 本発明者らは、ポリエチレンテレフタレートとポリトリメチレンテレフタレートを特定の 比率で混合し、溶融紡糸することにより、通常のポリエステル繊維の耐熱性、強伸度 など繊維物性を維持し、カール特性に優れ、人毛に近いソフトな触感を有し、毛先の タンダル、フリッツの起こり難い、ポリエステル系人工毛髪が得られることを見いだした 。さらには、臭素含有難燃剤、アンチモンィ匕合物、可塑剤および/または滑剤、有機 微粒子および zまたは無機微粒子を含んでなる組成物を溶融紡糸することにより、 前記の特性を維持したまま、難燃性に優れ、より人毛に近い光沢感を有するポリエス テル系人工毛髪が得られることを見出した。 [0010] The inventors of the present invention maintain the physical properties of ordinary polyester fibers such as heat resistance and high elongation by mixing polyethylene terephthalate and polytrimethylene terephthalate at a specific ratio and spinning them, and curl characteristics. It has been found that a polyester-based artificial hair that is excellent in hair, has a soft tactile feel similar to human hair, is less likely to cause tandals and frits on the ends of the hair, and is produced. In addition, bromine-containing flame retardants, antimony compounds, plasticizers and / or lubricants, organic By melt spinning a composition comprising fine particles and z or inorganic fine particles, polyester-based artificial hair having excellent flame retardancy and glossiness closer to human hair can be obtained while maintaining the above-mentioned properties. I found out.
すなわち、本発明は次の人工毛髪に関する。  That is, the present invention relates to the following artificial hair.
(1)ポリエチレンテレフタレート (A)およびポリトリメチレンテレフタレート（B)から形成 されるポリエステル系人工毛髪であって、ポリエチレンテレフタレート (A)およびポリト リメチレンテレフタレート（B)の比率が、質量比で、 (A) / (B) = 90Z10〜40Z60 であることを特徴とするポリエステル系人工毛髪。  (1) Polyester artificial hair formed from polyethylene terephthalate (A) and polytrimethylene terephthalate (B), wherein the ratio of polyethylene terephthalate (A) to polytrimethylene terephthalate (B) is A) / (B) = 90Z10-40Z60 Polyester artificial hair, characterized in that
(2)ポリエチレンテレフタレート (Α)の固有粘度力 0. 6〜1. 2dlZgである、（1)に 記載のポリエステル系人工毛髪。  (2) Polyester artificial hair according to (1), having an intrinsic viscosity of polyethylene terephthalate (Α) of 0.6 to 1.2 dlZg.
(3)ポリトリメチレンテレフタレート（B)の固有粘度力 0. 6〜1. 5dlZgである、 （1)に 記載のポリエステル系人工毛髪。  (3) The polyester-based artificial hair according to (1), which has an intrinsic viscosity of polytrimethylene terephthalate (B) of 0.6 to 1.5 dlZg.
(4)ポリエチレンテレフタレート (A)およびポリトリメチレンテレフタレート（B)の合計 10 0重量部に対し、さらに臭素含有難燃剤 (C) 5〜30重量部を含有する組成物力 形 成された（1)〜（3) V、ずれかに記載のポリエステル系人工毛髪。  (4) A composition containing 5 to 30 parts by weight of a bromine-containing flame retardant (C) was further formed for a total of 100 parts by weight of polyethylene terephthalate (A) and polytrimethylene terephthalate (B) (1) ~ (3) V, polyester artificial hair according to any of the above.
(5)臭素含有難燃剤 (C)が、臭素化芳香族系難燃剤、臭素含有リン酸エステル系難 燃剤、臭素化ポリスチレン系難燃剤、臭素化べンジルアタリレート系難燃剤、臭素化 エポキシ系難燃剤、臭素化フエノキシ系難燃剤、臭素化ポリカーボネート系難燃剤、 テトラブロモビスフエノール A誘導体、臭素含有トリアジン系化合物および臭素含有ィ ソシァヌル酸系化合物よりなる群力も選ばれた少なくとも 1種の難燃剤である、（4)に 記載のポリエステル系人工毛髪。  (5) Bromine-containing flame retardant (C) is brominated aromatic flame retardant, bromine-containing phosphate ester flame retardant, brominated polystyrene flame retardant, brominated benzaryl acrylate flame retardant, brominated epoxy Group flame retardant, brominated phenoxy flame retardant, brominated polycarbonate flame retardant, tetrabromobisphenol A derivative, bromine-containing triazine compound and bromine-containing isocyanuric acid compound The polyester-based artificial hair according to (4), which is a flame retardant.
(6)ポリエチレンテレフタレート (A)およびポリトリメチレンテレフタレート（B)の合計 10 0重量部に対し、さらにアンチモン系化合物（D)を 0. 5〜： LO重量部含有する組成物 から形成された、（4)〜（5)の 、ずれかに記載のポリエステル系人工毛髪。  (6) formed from a composition containing 0.5 to LO parts by weight of antimony compound (D) with respect to a total of 100 parts by weight of polyethylene terephthalate (A) and polytrimethylene terephthalate (B), The polyester-based artificial hair according to any one of (4) to (5).
(7)アンチモン系化合物（D)が、三酸ィ匕アンチモン、四酸ィ匕アンチモン、五酸化アン チモンおよびアンチモン酸ナトリウムよりなる群力 選ばれた少なくとも 1種のアンチモ ン化合物である、（6)記載のポリエステル系人工毛髪。  (7) The antimony compound (D) is at least one antimony compound selected from the group consisting of antimony trioxide, antimony tetraacid, antimony tetraacid, antimony pentoxide and sodium antimonate (6 ) The polyester-based artificial hair described.
(8)ポリエチレンテレフタレート (A)およびポリトリメチレンテレフタレート（B)の混合物 合計 100重量部に対し、さらに分散剤 (E)を 0. 05〜3重量部含有する組成物から形 成された、 (1)〜（7)の 、ずれかに記載のポリエステル系人工毛髪。 (8) Mixture of polyethylene terephthalate (A) and polytrimethylene terephthalate (B) The polyester-based artificial hair according to any one of (1) to (7), formed from a composition further containing 0.05 to 3 parts by weight of the dispersant (E) with respect to 100 parts by weight in total.
(9)分散剤（E) 1S モンタン酸系ワックス、モンタン酸エステル系ワックス、部分ケン化 モンタン酸系ワックス、モンタン酸金属塩、ポリエチレン系ワックス、酸化ポリエチレン 系ワックス、ポリテトラフルォロエチレン、フッ素変性ワックス、ポリジメチルシリコーンお よび変性シリコーンレジンの 1種以上力もなる化合物である、 (8)記載のポリエステル 系人工毛髪。  (9) Dispersant (E) 1S Montanic acid wax, montanic acid ester wax, partial saponification Montanic acid wax, montanic acid metal salt, polyethylene wax, polyethylene oxide wax, polytetrafluoroethylene, fluorine The polyester-based artificial hair according to (8), which is a compound having at least one of a modified wax, polydimethylsilicone, and modified silicone resin.
(10)ポリエチレンテレフタレート (A)およびポリトリメチレンテレフタレート（B)の混合 物合計 100重量部に対し、さらに有機微粒子 (F)および Zまたは無機微粒子 (G)を 0. 1〜5重量部含有する組成物から形成された、（1)〜（9)のいずれかに記載のポリ エステル系人工毛髪。  (10) 0.1 to 5 parts by weight of organic fine particles (F) and Z or inorganic fine particles (G) are further added to 100 parts by weight of the total mixture of polyethylene terephthalate (A) and polytrimethylene terephthalate (B). The polyester-based artificial hair according to any one of (1) to (9), which is formed from a composition.
(11)有機微粒子 (F)が、ポリアリレート、ポリアミド、フッ素榭脂、シリコーン榭脂、架 橋アクリル榭脂および架橋ポリスチレンよりなる群力も選ばれた少なくとも 1種である、 (10)記載のポリエステル系人工毛髪。  (11) The polyester according to (10), wherein the organic fine particles (F) are at least one selected from the group force consisting of polyarylate, polyamide, fluorine resin, silicone resin, bridged acrylic resin, and crosslinked polystyrene. Artificial hair.
(12)無機微粒子 (G)が、炭酸カルシウム、酸化ケィ素、シリカ Zメラミン榭脂複合体 、酸化チタン、酸ィ匕アルミニウム、酸化亜鉛、タノレク、カオリン、モンモリロナイト、ベン トナイトおよびマイ力よりなる群力も選ばれた少なくとも 1種である、 (10)記載のポリエ ステル系人工毛髪。  (12) The group consisting of inorganic fine particles (G) consisting of calcium carbonate, silicon oxide, silica Z melamine resin complex, titanium oxide, acid aluminum, zinc oxide, tanorek, kaolin, montmorillonite, bentonite, and my strength The polyester-based artificial hair according to (10), which is at least one kind selected for its strength.
発明の効果  The invention's effect
[0012] 本発明によると、ポリエステル繊維の耐熱性、強伸度などの繊維物性を維持し、力 ール特性に優れ、人毛に近いソフトな触感を有し、毛先のタンダル、フリッツの起こり 難い、ポリエステル系人工毛髪を得ることができる。また、本発明のポリエステル系人 ェ毛髪はまたすぐれた透明性 (発色性)を有して!/ヽる。  [0012] According to the present invention, the fiber properties such as heat resistance and high elongation of the polyester fiber are maintained, excellent in the roll characteristics, soft touch close to human hair, Polyester-based artificial hair that is unlikely to occur can be obtained. The polyester-based human hair of the present invention also has excellent transparency (color development)!
発明を実施するための最良の形態  BEST MODE FOR CARRYING OUT THE INVENTION
[0013] 本発明のポリエステル系人工毛髪は、ポリエステルとしてポリエチレンテレフタレート  [0013] The polyester-based artificial hair of the present invention has polyethylene terephthalate as the polyester.
(A)とポリトリメチレンテレフタレート (B)の混合物を、溶融紡糸した繊維である。本発 明においては、ポリエステルとして、ポリエチレンテレフタレート (A)およびポリトリメチ レンテレフタレート（B)の混合物を用いることにより、ポリエチレンテレフタレートを用い た繊維に対して、ポリトリメチレンテレフタレート（B)の有する低弾性率に由来して、柔 らかい風合い、触感を得ることができる。また、ポリトリメチレンテレフタレート (B)の優 れた弹性回復率に由来して、人工毛髪の毛先のタンダル、フリッツの発生を抑制する ことができる。 A fiber obtained by melt spinning a mixture of (A) and polytrimethylene terephthalate (B). In the present invention, polyethylene terephthalate is used as a polyester by using a mixture of polyethylene terephthalate (A) and polytrimethylene terephthalate (B). A soft texture and a tactile sensation can be obtained from the low elastic modulus of polytrimethylene terephthalate (B). In addition, it is possible to suppress the occurrence of tandals and frits on the end of artificial hair due to the excellent recovery rate of polytrimethylene terephthalate (B).
[0014] 本発明において、ポリエチレンテレフタレート（A)とポリトリメチレンテレフタレート（B )との比率は、重量比で、（A)Z(B) =90Z10〜40Z60力好ましく、 85 15〜45 Ζ55がより好ましぐ 80Ζ20〜50Ζ50がさらに好ましい。ポリトリメチレンテレフタレ 一ト（Β)の比率が 10重量0 /0未満の場合には、ポリエチレンテレフタレートの高い弾性 率のため、柔らかな触感が発現され難くなる。また、ポリエチレンテレフタレートの低 い弾性回復率のため、人工毛髪として使用した場合に、フリッツやタンダルが起こり やすくなる傾向がある。また、ポリトリメチレンテレフタレート（Β)の比率が 60重量0 /0を 超える場合には、耐熱性の低下により、アイロンセット時に繊維の融着が発生したり、 力ール保持力が低下する傾向がある。 [0014] In the present invention, the ratio of polyethylene terephthalate (A) to polytrimethylene terephthalate (B) is preferably (A) Z (B) = 90Z10-40Z60, more preferably 85 15-45 to 55 by weight ratio. 80 to 20 to 50 to 50 is more preferable. If the ratio of the polytrimethylene terephthalate Ichito (beta) is less than 10 weight 0/0, due to the high modulus of polyethylene terephthalate, comprising soft touch is hardly expressed. Also, due to the low elastic recovery rate of polyethylene terephthalate, when used as artificial hair, there is a tendency for frits and tandals to occur. Further, when the ratio of polytrimethylene terephthalate (beta) is more than 60 weight 0/0, a tendency that the reduction of heat resistance, fusion may occur in the fibers during ironing set force Lumpur holding force decreases There is.
[0015] 本発明におけるポリエチレンテレフタレート (Α)およびポリトリメチレンテレフタレート  [0015] Polyethylene terephthalate (Α) and polytrimethylene terephthalate in the present invention
(Β)とは、それぞれ、ポリエチレンテレフタレートおよびポリトリメチレンテレフタレート の他に、ポリエチレンテレフタレートまたはポリトリメチレンテレフタレートを主体として（ 80モル％以上含有して）、少量の共重合成分を含有する共重合ポリエステルも含ま れる。  (Ii) is a copolymerized polyester mainly containing polyethylene terephthalate or polytrimethylene terephthalate (containing 80 mol% or more) in addition to polyethylene terephthalate and polytrimethylene terephthalate, and containing a small amount of a copolymer component. Is also included.
[0016] 前記共重合成分としては、例えば、イソフタル酸、オルトフタル酸、ナフタレンジカル ボン酸、パラフエ-レンジカルボン酸、トリメリット酸、ピロメリット酸、コハク酸、グルタル 酸、アジピン酸、スペリン酸、ァゼライン酸、セバシン酸、ドデカン二酸などの多価力 ルボン酸、それらの誘導体、 5—ナトリウムスルホイソフタル酸、 5—ナトリウムスルホイ ソフタル酸ジヒドロキシェチルなどのスルホン酸塩を含むジカルボン酸、その誘導体、 エチレングリコーノレ、 1, 2—プロパンジオール、 1, 3—プロパンジオール、 1, 4ーブ タンジオール、 1, 6—へキサンジオール、ネオペンチルグリコール、 1, 4ーシクロへ キサンジメタノール、ジエチレングリコール、ポリエチレングリコール、トリメチロールプ 口パン、ペンタエリスリトール、 4—ヒドロキシ安息香酸、 ε—力プロラタトンなどがあげ られる。 [0017] 前記共重合ポリエステルは、通常、主体となるテレフタル酸および Zまたはその誘 導体 (例えばテレフタル酸メチル）と、アルキレングリコールとの重合体に少量の共重 合成分を含有させて反応させることにより製造するのが、安定性、操作の簡便性の点 力も好ま 、が、主体となるテレフタル酸および Zまたはその誘導体 (例えばテレフタ ル酸メチル）と、アルキレングリコールとの混合物に、さらに少量の共重合成分である モノマーまたはオリゴマー成分を含有させたものを重合させることにより製造してもよ い。 [0016] 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, Ethylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, 1,6-hexanediol, neopentyl glycol, 1,4-cyclohexanedimethanol, diethylene glycol, polyethylene glycol , Trimethylol mouthpiece, pentaerythrito Le, 4-hydroxybenzoic acid, ε- force Purorataton the like. [0017] The copolyester is usually prepared by reacting a polymer of terephthalic acid and Z or its derivative (for example, methyl terephthalate) as a main component with an alkylene glycol and containing a small amount of a copolymer component. Although it is preferable to produce it by the stability and ease of operation, a small amount of co-polymer is added to the mixture of the main terephthalic acid and Z or its derivative (for example, methyl terephthalate) and alkylene glycol. The polymerization component may be produced by polymerizing a monomer or oligomer component.
[0018] 前記共重合ポリエステルは、主体となるポリエチレンテレフタレートまたはポリトリメチ レンテレフタレートの主鎖および Zまたは側鎖に前記共重合成分が重縮合していれ ばよぐ共重合の仕方などには特別な限定はない。  [0018] The copolymer polyester is not particularly limited in the way of copolymerization, in which the copolymer component is polycondensed to the main chain and Z or side chain of polyethylene terephthalate or polytrimethylene terephthalate as a main component. There is no.
[0019] 本発明に用いられるポリエチレンテレフタレート（A)の固有粘度としては、 0. 6〜1 . 2dlZgが好ましぐ 0. 65-1. ldlZgがより好ましぐ 0. 7〜1. OdlZgがさらに好 ましい。ポリエチレンテレフタレート (A)の固有粘度が 0. 6dlZg未満の場合、機械的 強度が低下したり、また、火炎に接触した場合に、溶融しやすくなり、ドリップが起こり やすくなる傾向がある。また、ポリエチレンテレフタレート (A)の固有粘度が 1. 2dl/ gを超えると、溶融紡糸時に糸切れが発生しやすくなつたり、触感が固くなる傾向があ る。  The intrinsic viscosity of the polyethylene terephthalate (A) used in the present invention is preferably 0.6 to 1.2 dlZg, more preferably 0.65-1.ldlZg, more preferably 0.7 to 1. OdlZg. Even better. When the intrinsic viscosity of polyethylene terephthalate (A) is less than 0.6 dlZg, the mechanical strength tends to decrease, and when it comes into contact with a flame, it tends to melt and drip easily. When the intrinsic viscosity of polyethylene terephthalate (A) exceeds 1.2 dl / g, yarn breakage tends to occur during melt spinning, and the touch tends to be hard.
[0020] 本発明に用いられるポリトリメチレンテレフタレート (B)の固有粘度としては、 0. 6〜 1. 5dlZg、より好ましくは、 0. 7〜1. 4dlZg、さらに好ましくは、 0. 8〜1. 3dlZgで ある。ポリトリメチレンテレフタレート (B)の固有粘度が 0. 6dlZg未満の場合、機械的 強度が低下したり、火炎に接触した場合に、溶融しやすくなり、ドリップが起こりやすく なる傾向がある。また、ポリトリメチレンテレフタレート（B)の固有粘度が 1. 5dlZgを 超えると、溶融紡糸時に糸切れが発生しやすくなつたり、触感が固くなる傾向がある。  [0020] The intrinsic viscosity of the polytrimethylene terephthalate (B) used in the present invention is 0.6 to 1.5 dlZg, more preferably 0.7 to 1.4 dlZg, and still more preferably 0.8 to 1. It is 3dlZg. When the intrinsic viscosity of polytrimethylene terephthalate (B) is less than 0.6 dlZg, the mechanical strength tends to decrease, or when it comes into contact with a flame, it tends to melt and drip easily. When the intrinsic viscosity of polytrimethylene terephthalate (B) exceeds 1.5 dlZg, yarn breakage tends to occur during melt spinning, and the tactile sensation tends to become hard.
[0021] 本発明においては、人工毛髪として使用する場合の安全性を高めることを目的とし て、難燃剤を配合して、難燃性を付与することが好ましい。この場合、使用する難燃 剤としては、人工毛髪に優れた難燃性を付与できるため、臭素含有難燃剤 (C)を用 いることが好ましい。本発明に用いられる臭素含有難燃剤 (C)には特に限定はなぐ 一般に用いられている臭素含有難燃剤であれば使用することができる。 [0022] 本発明における臭素含有難燃剤 (C)の具体例としては、人工毛髪に優れた難燃性 を付与できる、臭素含有リン酸エステル系難燃剤、臭素化ポリスチレン系難燃剤、臭 素化べンジルアタリレート系難燃剤、臭素化エポキシ系難燃剤、臭素化フエノキシ榭 脂系難燃剤、臭素化ポリカーボネート系難燃剤、テトラブロモビスフエノール A誘導体 、臭素含有トリアジン系化合物、臭素含有イソシァヌル酸系化合物や、人工毛髪に優 れた繊維物性、耐熱性を付与でき、繊維製造時に優れた加工安定性を付与できる 臭素含有リン酸エステル系難燃剤、臭素化エポキシ系難燃剤、臭素化フヱノキシ榭 脂系難燃剤をあげることができる。 [0021] In the present invention, for the purpose of improving safety when used as artificial hair, it is preferable to add flame retardant to impart flame retardancy. In this case, it is preferable to use a bromine-containing flame retardant (C) as the flame retardant used because it can impart excellent flame retardancy to artificial hair. The bromine-containing flame retardant (C) used in the present invention is not particularly limited, and any bromine-containing flame retardant generally used can be used. [0022] Specific examples of the bromine-containing flame retardant (C) in the present invention include bromine-containing phosphate ester flame retardant, brominated polystyrene flame retardant, and fluorination, which can impart excellent flame retardancy to artificial hair. Benzyl acrylate flame retardant, brominated epoxy flame retardant, brominated phenoxy resin flame retardant, brominated polycarbonate flame retardant, tetrabromobisphenol A derivative, bromine-containing triazine compound, bromine-containing isocyanuric acid Bromine-containing phosphate ester flame retardant, brominated epoxy flame retardant, brominated phenoxy resin, which can impart excellent fiber properties and heat resistance to compounds and artificial hair, and can provide excellent processing stability during fiber production -Based flame retardants.
[0023] 本発明における臭素含有難燃剤 (C)のさらに詳細な具体例としては、例えば、ペン タブロモトルエン、へキサブロモベンゼン、デカブロモジフエ-ル、デカブロモジフエ -ルエーテル、ビス（トリブロモフエノキシ）ェタン、テトラブロモ無水フタル酸、ェチレ ンビス（テトラブロモフタルイミド）、エチレンビス（ペンタブロモフエ-ル）、オタタブロモ トリメチルフエ-ルインダン、トリス（トリブロモネオペンチル）ホスフェートなどの臭素含 有リン酸エステル類、臭素化ポリスチレン類、臭素化ポリベンジルアタリレート類、臭 素化エポキシオリゴマー類、臭素化フヱノキシ榭脂、臭素化ポリカーボネートオリゴマ 一類、テトラブロモビスフエノール A、テトラブロモビスフエノール A—ビス（2, 3—ジブ ロモプロピルエーテル）、テトラブロモビスフエノール A—ビス（ァリルエーテル）、テトラ ブロモビスフエノール A—ビス（ヒドロキシェチルエーテル）などのテトラブロモビスフエ ノール A誘導体、トリス（トリプロモフエノキシ）トリァジンなどの臭素含有トリアジン系化 合物、トリス（2, 3—ジブロモプロピル)イソシァヌレートなどの臭素含有イソシァヌル 酸系化合物などが挙げられる。これらは 1種で用いてもよぐ 2種以上を組み合わせて 用いてもよい。  [0023] More specific specific examples of the bromine-containing flame retardant (C) in the present invention include, for example, pentabromotoluene, hexabromobenzene, decabromodiphenyl, decabromodiphenyl ether, and bis (tribromophenoxy). Bromine-containing phosphate esters such as ethane, tetrabromophthalic anhydride, ethylene bis (tetrabromophthalimide), ethylene bis (pentabromophenol), otatabromotrimethylphenolindane, tris (tribromoneopentyl) phosphate, bromine Polystyrenes, brominated polybenzyl acrylates, fluorinated epoxy oligomers, brominated phenoxy resins, brominated polycarbonate oligomers, tetrabromobisphenol A, tetrabromobisphenol A-bis (2,3-dibu Lomopropyl ether), Tetrabromobisphenol A-bis (aryl ether), tetrabromobisphenol A-bis (hydroxyethyl ether) and other tetrabromobisphenol A derivatives, and bromine-containing triazine compounds such as tris (tripromophenoxy) triazine And bromine-containing isocyanuric acid compounds such as tris (2,3-dibromopropyl) isocyanurate. These may be used alone or in combination of two or more.
[0024] 本発明における臭素含有難燃剤 (C)の使用量は、ポリエチレンテレフタレート (A) およびポリトリメチレンテレフタレート (B)の合計 100重量部に対し、 5〜30重量部が 好ましぐ 6〜25重量部がより好ましぐ 7〜20重量部がさらに好ましい。臭素含有難 燃剤 (C)の使用量が 5重量部未満では、難燃効果が得られにくい傾向があり、 30重 量部を超えると、得られる繊維の機械的特性、耐熱性、耐ドリップ性が損なわれる傾 向がある。 [0025] 本発明においては、組成物中に臭素含有難燃剤 (C)を含有することにより、難燃性 は発現されるが、アンチモンィ匕合物 (D)を含有することにより、難燃効果を著しく向上 させることができる。本発明に用いられるアンチモンィ匕合物（D)には、特に限定はな い。アンチモンィ匕合物（D)の具体例としては、三酸ィ匕アンチモン、四酸ィ匕アンチモン 、五酸ィ匕アンチモン、アンチモン酸ナトリウムなどがあげられる。これらのなかでは、組 成物の紡糸加工性の点から、アンチモン酸ナトリウムが好ましい。 [0024] The amount of bromine-containing flame retardant (C) used in the present invention is preferably 5 to 30 parts by weight with respect to a total of 100 parts by weight of polyethylene terephthalate (A) and polytrimethylene terephthalate (B). 25 to 5 parts by weight is more preferred 7 to 20 parts by weight is even more preferred. If the amount of bromine-containing flame retardant (C) used is less than 5 parts by weight, the flame retardant effect tends to be difficult to obtain, and if it exceeds 30 parts by weight, the mechanical properties, heat resistance, and drip resistance of the resulting fiber There is a tendency to damage. [0025] In the present invention, the flame retardancy is expressed by including the bromine-containing flame retardant (C) in the composition, but the flame retardant is expressed by including the antimony compound (D). The effect can be remarkably improved. The antimony compound (D) used in the present invention is not particularly limited. Specific examples of the antimony compound (D) include antimony triacid, antimony tetraacid, antimony tetraacid, antimony pentaacid, sodium antimonate and the like. Of these, sodium antimonate is preferred from the viewpoint of the spinnability of the composition.
[0026] 本発明におけるアンチモン化合物（D)の平均粒子径は、 0. 02-15 μ mが好まし [0026] The average particle size of the antimony compound (D) in the present invention is preferably 0.015 to 15 μm.
0. 1〜12 /z mがより好ましぐ 0. 2〜： LO /z mがさらに好ましい。本発明におけるァ ンチモンィ匕合物（D)は、必要に応じて、エポキシ化合物、シランィ匕合物、イソシァネ ート化合物、チタネート化合物等で表面処理されてもよい。  0.1 to 12 / z m is more preferable 0.2 to: LO / z m is more preferable. The antimony compound (D) 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.
[0027] 本発明におけるアンチモン化合物（D)の使用量は、ポリエチレンテレフタレート (A) およびポリトリメチレンテレフタレート (B)の合計 100重量部に対し、 0. 5〜： LO重量部 が好ましぐ 0. 6〜9重量部がより好ましぐ 0. 7〜7重量部がさらに好ましい。アンチ モンィ匕合物（D)の使用量が 0. 5重量部未満では、難燃効果の向上が小さくなる傾 向があり、 10重量部を超えると、加工安定性、外観性、透明性が損なわれる傾向が ある。 [0027] The amount of antimony compound (D) used in the present invention is preferably 0.5 to: LO parts by weight with respect to 100 parts by weight of the total of polyethylene terephthalate (A) and polytrimethylene terephthalate (B). 6-9 parts by weight is more preferred 0.7-7 parts by weight is even more preferred. When the amount of the antimony compound (D) used is less than 0.5 parts by weight, the improvement of the flame retardancy tends to be small, and when it exceeds 10 parts by weight, the processing stability, appearance and transparency are low. There is a tendency to be damaged.
[0028] 本発明においては、組成物中に分散剤 (E)をさらに含有することにより、アンチモン 化合物 (D)の分散状態が改善されるため、紡糸安定性が向上し、繊維表面のがさつ きがなくなる。さらに、分散剤 (E)は繊維表面にすべり性を付与することができ、くし通 りの良いフィラメントを得ることができる。本発明に用いられる分散剤 (E)としては、可 塑剤または滑剤を使用することができる。可塑剤または滑剤としては特に限定はなく 、一般に用いられているものであれば、使用することができる。  [0028] In the present invention, the dispersion state of the antimony compound (D) is improved by further containing the dispersant (E) in the composition, so that the spinning stability is improved and the fiber surface is protected. Disappears. Further, the dispersant (E) can impart slipperiness to the fiber surface, and a filament with good combing can be obtained. As the dispersant (E) used in the present invention, a plasticizer or a lubricant can be used. The plasticizer or lubricant is not particularly limited, and any plasticizer or lubricant can be used as long as it is generally used.
[0029] 本発明における分散剤 (E)の具体例としては、例えば、フタル酸エステル類、アジ ピン酸エステル類、ポリエステル系可塑剤、アクリルオリゴマー系可塑剤、モンタン酸 系ワックス、モンタン酸エステル系ワックス、部分ケン化モンタン酸系ワックス、モンタ ン酸金属塩、炭化水素系ワックス、エチレン 酢酸ビュル共重合ワックス、酸化ェチ レン 酢酸ビュル共重合ワックス、ポリエチレン系ワックス、酸化ポリエチレン系ヮック ス、ポリプロピレン系ワックス、アクリル系高分子ワックス、アミド系ワックス、アミド変性 ワックス、ポリテトラフルォロエチレン、フッ素変性ワックス、脂肪酸エステル、グリセリン エステル、ソルビタンエステル、脂肪酸アマイド、脂肪族ポリエステル、ポリジメチルシ リコーン、変性シリコーンレジンなどが挙げられる。 [0029] Specific examples of the dispersant (E) in the present invention include, for example, phthalates, adipates, polyester plasticizers, acrylic oligomer plasticizers, montanic waxes, and montanic esters. Wax, partially saponified montanic acid wax, metal montanate, hydrocarbon wax, ethylene acetate butyl copolymer wax, ethylene oxide butyl acetate copolymer wax, polyethylene wax, polyethylene oxide wax, polypropylene Wax, acrylic polymer wax, amide wax, amide modification Examples thereof include wax, polytetrafluoroethylene, fluorine-modified wax, fatty acid ester, glycerin ester, sorbitan ester, fatty acid amide, aliphatic polyester, polydimethyl silicone, and modified silicone resin.
[0030] これらの中では、モンタン酸系ワックス、モンタン酸エステル系ワックス、部分ケンィ匕 モンタン酸系ワックス、モンタン酸金属塩、ポリエチレン系ワックス、酸化ポリエチレン 系ワックス、ポリテトラフルォロエチレン、フッ素変性ワックス、ポリジメチルシリコーン、 変性シリコーンレジンが、アンチモン化合物の分散性、難燃性、耐熱性などの繊維物 性への影響力 S小さい点力も好ましい。これらの化合物は、単独で使用してもよぐまた 、 2種以上を混合して使用してもよい。  [0030] Among these, montanic acid-based wax, montanic acid ester-based wax, partially-kenned montanic acid-based wax, montanic acid metal salt, polyethylene-based wax, polyethylene oxide-based wax, polytetrafluoroethylene, fluorine-modified Wax, polydimethylsilicone, and modified silicone resin have an influence on fiber properties such as dispersibility, flame retardancy, and heat resistance of antimony compounds. These compounds may be used alone or as a mixture of two or more.
[0031] 本発明における分散剤 (E)の使用量は、ポリエチレンテレフタレート (A)およびポリ トリメチレンテレフタレート (B)の合計 100重量部に対し、 0. 05〜3重量部が好ましく 、0. 1〜2. 5重量部がより好ましぐ 0. 15〜2重量部がさらに好ましい。分散剤 (E) の使用量が 0. 05重量部未満では、アンチモン化合物粒子 (D)が部分的に凝集し、 紡糸加工時の糸切れが発生したり、繊維表面の触感ががさついたりする傾向がある 。 3重量部を超えると、紡糸安定性が低下して糸切れが発生したり、機械的特性、耐 熱性、難燃性、耐ドリップ性が損なわれる傾向がある。  [0031] The amount of the dispersant (E) used in the present invention is preferably 0.05 to 3 parts by weight with respect to 100 parts by weight of the total of polyethylene terephthalate (A) and polytrimethylene terephthalate (B), and 0.1 to 0.1 parts by weight. ~ 2.5 parts by weight is more preferred 0.15 to 2 parts by weight is even more preferred. When the amount of the dispersant (E) used is less than 0.05 parts by weight, the antimony compound particles (D) are partially agglomerated, and there is a tendency that yarn breakage occurs during the spinning process and the tactile feel of the fiber surface is reduced. There is. If it exceeds 3 parts by weight, the spinning stability will be lowered and yarn breakage will occur, and mechanical properties, heat resistance, flame resistance and drip resistance will tend to be impaired.
[0032] 本発明の難燃性ポリエステル系人工毛髪用繊維は、組成物中にさらに有機微粒子  [0032] The fiber for flame-retardant polyester-based artificial hair of the present invention further comprises organic fine particles in the composition.
(F)および Zまたは無機微粒子 (G)を混合することにより、得られる繊維の表面に微 細な突起を形成し、繊維表面の光沢、つやを調整することができる。  By mixing (F) and Z or inorganic fine particles (G), fine protrusions can be formed on the surface of the resulting fiber, and the gloss and gloss of the fiber surface can be adjusted.
[0033] 本発明における有機微粒子 (F)としては、ポリエチレンテレフタレート (A)および Z またはポリトリメチレンテレフタレート（B)と相溶しないか、部分的に相溶しない構造を 有する有機榭脂であれば使用することができる。有機微粒子 (F)としては、例えば、 ポリアリレート、ポリアミド、フッ素榭脂、シリコーン榭脂、架橋アクリル榭脂、架橋ポリス チレンなどが挙げられる。これらは 1種で用いてもよぐ 2種以上を組み合わせて用い てもよい。これらのなかでは、安定的に光沢調整効果を付与できる、優れた耐熱性お よび分散性を有する、架橋ポリエステル粒子および架橋アクリル粒子が好ま ヽ。  [0033] The organic fine particles (F) in the present invention may be any organic resin having a structure that is incompatible with or partially incompatible with polyethylene terephthalate (A) and Z or polytrimethylene terephthalate (B). Can be used. Examples of the organic fine particles (F) include polyarylate, polyamide, fluorine resin, silicone resin, crosslinked acrylic resin, and crosslinked polystyrene. These may be used alone or in combination of two or more. Among these, cross-linked polyester particles and cross-linked acrylic particles having excellent heat resistance and dispersibility that can stably impart a gloss adjusting effect are preferred.
[0034] 本発明に用いられる無機微粒子 (G)としては、繊維に透明性および発色性を付与 できるポリエチレンテレフタレート (A)および Zまたはポリトリメチレンテレフタレート（B )の屈折率に近い屈折率を有するものが好ましい。無機微粒子 (G)としては、例えば 、炭酸カルシウム、酸化ケィ素、酸化チタン、酸ィ匕アルミニウム、酸化亜鉛、タルク、力 ォリン、モンモリロナイト、ベントナイト、マイ力などがあげられる。これらは 1種で用いて もよぐ 2種以上を組み合わせて用いてもよい。これらのなかでは、球形に近い微粒 子の方が光沢調整効果は高ぐ酸化ケィ素、酸ィヒケィ素を主体とした複合粒子など が好ましい。本発明に用いられる無機微粒子 (G)は、必要に応じてエポキシィ匕合物 、シランィ匕合物、イソシァネートイ匕合物、チタネートイ匕合物等で表面処理されてもよい [0034] The inorganic fine particles (G) used in the present invention include polyethylene terephthalate (A) and Z or polytrimethylene terephthalate (B Those having a refractive index close to that of) are preferred. Examples of the inorganic fine particles (G) include calcium carbonate, silicon oxide, titanium oxide, aluminum oxide, zinc oxide, talc, strong iron, montmorillonite, bentonite, and my strength. These may be used alone or in combination of two or more. Among these, particles close to a spherical shape are preferably composite particles mainly composed of silicon oxide and acid hydride, which have a higher gloss adjustment effect. The inorganic fine particles (G) 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.
[0035] 本発明に用いられる有機微粒子 (F)および Zまたは無機微粒子 (G)の平均粒子 径は、 0. 1〜15 m力好ましく、 0. 2〜10 m力より好ましく、 0. 5〜8 111力 ^さらに 好ま ヽ。有機微粒子 (F)および Zまたは無機微粒子 (G)の平均粒子径が 0. 1 μ m より小さい場合には、光沢調整効果が小さくなる傾向があり、 より大きい場合 には、光沢調整効果力 、さくなる、または、糸切れが発生する傾向がある。 [0035] The average particle size of the organic fine particles (F) and Z or inorganic fine particles (G) used in the present invention is preferably 0.1 to 15 m force, more preferably 0.2 to 10 m force, and 0.5 to 8 111 Power ^ Preferred さ ら に. When the average particle size of organic fine particles (F) and Z or inorganic fine particles (G) is smaller than 0.1 μm, the gloss adjustment effect tends to be small. There is a tendency to break down or to break yarn.
[0036] 本発明に用いられる有機微粒子 (F)および Zまたは無機微粒子 (G)の使用量は、 特に限定されないが、ポリエチレンテレフタレート (A)およびポリトリメチレンテレフタレ 一 HB)の合計 100重量部に対し、 0. 1〜5重量部が好ましぐ 0. 2〜3重量部がより 好ましぐ 0. 3〜2重量部がさらに好ましい。有機微粒子 (F)および Zまたは無機微 粒子 (G)の使用量が 0. 1重量部未満では、繊維表面に形成される微細な突起が少 なくなるため、繊維表面の光沢調整効果が小さくなる傾向があり、 5重量部を超えると 、外観性、色相、発色性が損なわれる傾向がある。  [0036] The amount of organic fine particles (F) and Z or inorganic fine particles (G) used in the present invention is not particularly limited, but a total of 100 parts by weight of polyethylene terephthalate (A) and polytrimethylene terephthalate HB). On the other hand, 0.1 to 5 parts by weight is preferable, 0.2 to 3 parts by weight is more preferable, and 0.3 to 2 parts by weight is more preferable. When the amount of organic fine particles (F) and Z or inorganic fine particles (G) used is less than 0.1 part by weight, the fine protrusions formed on the fiber surface are reduced, and the gloss adjustment effect on the fiber surface tends to be small. When the amount exceeds 5 parts by weight, appearance, hue, and color developability tend to be impaired.
[0037] 本発明で得られるポリエステル系人工毛髪は、例えば、ポリエチレンテレフタレート（ A)およびポリトリメチレンテレフタレート（B)さらには臭素含有難燃剤 (C)、アンチモ ン化合物 (D)、分散剤 (E)、有機微粒子 (F)、無機微粒子 (G)などをドライブレンドし た後、種々の一般的な混練機を用いて溶融混練して得られたポリエステル系組成物 を、単軸押出機を用いて溶融紡糸して得ることができる。  [0037] Polyester artificial hair obtained by the present invention includes, for example, polyethylene terephthalate (A), polytrimethylene terephthalate (B), bromine-containing flame retardant (C), antimony compound (D), dispersant (E ), Organic fine particles (F), inorganic fine particles (G), etc. are dry blended, and then the polyester composition obtained by melt kneading using various general kneaders is used with a single screw extruder. And can be obtained by melt spinning.
[0038] 榭脂組成物の製造に用いられる前記混練機の例としては、例えば、一軸押出機、 二軸押出機、ロール、バンバリ一ミキサー、エーダーなどがあげられる。これらのうち では、二軸押出機が、混練度の調整、操作の簡便性の点から好ましい。 [0039] 例えば、スクリュー径 45mmの二軸押出機を用いて、バレル設定温度を 260〜300[0038] Examples of the kneader used in the production of the rosin composition include, for example, a single screw extruder, a twin screw extruder, a roll, a Banbury mixer, and an ader. Among these, a twin screw extruder is preferable from the viewpoint of adjusting the kneading degree and ease of operation. [0039] For example, using a twin screw extruder with a screw diameter of 45 mm, the barrel set temperature is 260 to 300.
°Cとし、吐出量 50〜150kgZhr、スクリュー回転数 150〜200rpmで溶融混練し、ダ イスよりストランドを引取、水冷した後に、ストランドカッターを用いてペレツトイ匕して、本 発明のポリエステル系人工毛髪を製造する組成物を得ることができる。 The mixture is melt-kneaded at a discharge temperature of 50 to 150 kgZhr and a screw rotation speed of 150 to 200 rpm, the strand is taken out of the die, water-cooled, and then pelletized using a strand cutter to obtain the polyester-based artificial hair of the present invention. A composition to be produced can be obtained.
[0040] 本発明のポリエステル系人工毛髪は例えば、押出機、ギアポンプ、口金などの温度 を 270〜310°Cとし、溶融紡糸し、紡出糸条を加熱筒に通過させた後、ガラス転移点 以下に冷却し、 50〜5000mZ分の速度で引き取ることにより得ることができる。また 、紡出糸条を冷却用の水を入れた水槽で冷却し、繊度のコントロールを行なうことも 可能である。加熱筒の温度や長さ、冷却風の温度や吹付量、冷却水槽の温度、冷却 時間、引取速度は、吐出量および口金の孔数によって適宜調整することができる。  [0040] The polyester-based artificial hair of the present invention has, for example, a temperature of 270 to 310 ° C such as an extruder, a gear pump, and a die, melt-spun, and passes the spun yarn through a heating tube, and then has a glass transition point. It can be obtained by cooling to below and taking it off at a speed of 50 to 5000 mZ. 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 the cooling air, the temperature of the cooling water tank, the cooling time, and the take-up speed can be appropriately adjusted according to the discharge amount and the number of holes in the base.
[0041] また、本発明のポリエステル系人工毛髪はポリエチレンテレフタレート (A)およびポ リトリメチレンテレフタレート (B)、さらには臭素含有難燃剤 (C)、アンチモンィ匕合物（ D)、分散剤 (E)、有機微粒子 (F)、無機微粒子 (G)などをドライブレンドした組成物 を、ギアポンプおよび紡糸ノズルを備えた二軸押出機または混練能を有するスクリュ 一を使用した単軸押出機を用いて、一且榭脂組成物を取り出すことなぐ溶融紡糸し て得ることができる。  [0041] The polyester-based artificial hair of the present invention comprises polyethylene terephthalate (A) and polytrimethylene terephthalate (B), bromine-containing flame retardant (C), antimony compound (D), dispersant (E ), Organic fine particles (F), inorganic fine particles (G), etc. are dry blended using a twin screw extruder equipped with a gear pump and a spinning nozzle or a single screw extruder using a screw having kneading ability. The resin composition can be obtained by melt spinning without taking out the resin composition.
[0042] 本発明においては、得られた紡出糸条は熱延伸される力 延伸は紡出糸条をー且 巻き取ってから延伸する 2工程法および、巻き取ることなく連続して延伸する直接紡 糸延伸法のいずれの方法によってもよい。熱延伸は、 1段延伸法または 2段以上の 多段延伸法で行なわれる。熱延伸における加熱手段としては、加熱ローラ、ヒートプ レート、スチームジェット装置、温水槽などを使用することができ、これらを適宜併用 することちでさる。  [0042] In the present invention, the obtained spun yarn is heat-stretched. Stretching is a two-step method in which the spun yarn is wound and then stretched, and continuously stretched without winding. Any of direct spinning and drawing methods may be used. 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 together as appropriate.
[0043] 本発明のポリエステル系人工毛髪には、必要に応じて、耐熱剤、光安定剤、蛍光 剤、酸化防止剤、静電防止剤、顔料などの各種添加剤を含有させることができる。  [0043] The polyester-based artificial hair of the present invention may contain various additives such as a heat-resistant agent, a light stabilizer, a fluorescent agent, an antioxidant, an antistatic agent, and a pigment as necessary.
[0044] このようにして得られる本発明のポリエステル系人工毛髪の繊度は、通常、 10〜： LO Odtex、さらには 20〜90dtexであるの力 人工毛髪に適している。また、人工毛髪と しては、 160〜200°Cで美容熱器具 (ヘアーアイロン）が使用できる耐熱性を有して おり、着火しにくぐ自己消火性を有していることが好ましい。 [0045] 本発明のポリエステル系人工毛髪は染色または原着により着色して使用することが できる。染色により着色する場合には、通常のポリエステル系繊維と同様の条件で染 色することができる。また、原着の場合には、通常のポリエステル系繊維に用いられる 顔料を溶融混練することにより、原着繊維を得ることができる。染色に使用される顔料 、染料、助剤などとしては、耐候性および難燃性のよいものが好ましい。 [0044] The fineness of the polyester-based artificial hair of the present invention obtained as described above is usually 10 to: LO Odtex, more preferably 20 to 90 dtex. Suitable for artificial hair. In addition, the artificial hair has heat resistance capable of using a beauty heat instrument (hair iron) at 160 to 200 ° C., and preferably has self-extinguishing properties that are difficult to ignite. [0045] The polyester-based artificial hair of the present invention can be used after being colored by dyeing or priming. When coloring by dyeing, it can be dyed under the same conditions as ordinary polyester fibers. Moreover, in the case of original attachment, an original attachment fiber can be obtained by melt-kneading the pigment used for normal polyester fiber. As the pigment, dye, auxiliary agent and the like used for dyeing, those having good weather resistance and flame retardancy are preferable.
[0046] 本発明のポリエステル系人工毛髪は、美容熱器具 (ヘアーアイロン)を用いたカー ルセット性に優れ、カールの保持性にも優れる。また、繊維表面の凹凸により、適度 に艷消されており、人工毛髪として使用することができる。さらに、繊維表面処理剤、 柔軟剤などの油剤を使用し、触感、風合を付与して、より人毛に近づけることができる  [0046] The polyester-based artificial hair of the present invention is excellent in curl setting using a beauty heat instrument (hair iron) and excellent in curl retention. Moreover, the surface of the fiber is moderately erased by the irregularities on the fiber surface, and can be used as artificial hair. In addition, oil agents such as fiber surface treatment agents and softeners can be used to provide a feeling of touch and texture, making it closer to human hair.
[0047] また、本発明の難燃性ポリエステル系人工毛髪は、モダアクリル繊維、ポリ塩ィ匕ビ- ル繊維、ナイロン繊維など、他の人工毛髪素材と併用してもよいし、人毛と併用しても よい。 [0047] The flame-retardant polyester artificial hair of the present invention may be used in combination with other artificial hair materials such as modacrylic fiber, polysalt fiber fiber, nylon fiber, etc., or in combination with human hair. May be.
実施例  Example
[0048] 次に、本発明を実施例に基づいてさらに具体的に説明するが、本発明はこれらに 限定されるものではない。なお、特性値の測定法は、以下のとおりである。  [0048] Next, the present invention will be more specifically described based on examples, but the present invention is not limited thereto. The characteristic value measurement method is as follows.
[0049] (強度および伸度）  [0049] (Strength and elongation)
引張圧縮試験機 (インテスコネ土製、 INTESCO Model201型）を用いて、フィラメン トの引張強伸度を測定した。長さ 40mmのフィラメント 1本をとり、フィラメントの両端 10 mmを、接着剤を糊付けした両面テープを貼り付けた台紙 (薄紙)で挟み、一晩風乾 させて、長さ 20mmの試料を作製した。試験機に試料を装着し、温度 24°C、湿度 80 %以下、初期荷重 lZ30gF X繊度 (デニール）、引張速度 20mmZ分で試験を行 ない、破断時の引張強度および伸度を測定した。同じ条件で試験を 10回繰り返し、 平均値をフィラメントの強伸度とした。  The tensile strength and elongation of the filaments were measured using a tensile / compression tester (INTESCO Model 201, manufactured by Intescone Earth). A 20 mm long sample was prepared by taking one filament with a length of 40 mm, sandwiching 10 mm of both ends of the filament with a backing paper (thin paper) to which a double-sided adhesive tape was applied, and air-dried overnight. A sample was attached to the tester, and the test was performed at a temperature of 24 ° C, humidity of 80% or less, an initial load of lZ30gF X fineness (denier), and a tensile speed of 20mmZ, and the tensile strength and elongation at break were measured. The test was repeated 10 times under the same conditions, and the average value was defined as the filament elongation.
[0050] (10%伸張弾性回復率）  [0050] (10% stretch elastic recovery)
引張圧縮試験機 (インテスコネ土製、 INTESCO Model201型）を用いてフィラメント の 10%伸張弾性回復率を測定した。長さ 40mmのフィラメント 1本をとり、フィラメント の両端 10mmを、接着剤を糊付けした両面テープを貼り付けた台紙 (薄紙)で挟み、 一晩風乾させて、長さ 20mmの試料を作製した。試験機に試料を装着し、温度 24°C 、湿度 80%以下、引張速度 200mmZminで 10%伸張後、ただちに同速度で回復 させた。伸張回復曲線力 回復時の初期荷重と同じになった時のサンプル初期長に 対する伸び率 (B%)を読み取り、下記式で、 10%伸張弾性回復率を求めた。 10% 伸張弾性回復率は、毛先のフリッツの起こり易さの指標として評価でき、伸張弾性回 復率の大き 、方が、フリッツが起こりにくいことを示して 、る。 Using a tensile and compression tester (INTESCO Model 201, manufactured by Intescone Earth), the 10% stretch elastic recovery rate of the filament was measured. Take one filament with a length of 40 mm, and sandwich 10 mm of both ends of the filament with a backing paper (thin paper) to which a double-sided tape with glue is attached. A 20 mm long sample was made by air drying overnight. A sample was mounted on the testing machine, and after 10% elongation at a temperature of 24 ° C, humidity of 80% or less, and a tensile speed of 200 mmZmin, it was immediately recovered at the same speed. Tensile recovery curve force The elongation (B%) with respect to the initial length of the sample when it became the same as the initial load at the time of recovery was read, and the 10% elongation elastic recovery rate was obtained by the following formula. The 10% stretch elastic recovery rate can be evaluated as an index of the likelihood of the occurrence of frits at the ends of the hair, and the greater the stretch elastic recovery rate, the less likely that the frits occur.
10%伸張弾性回復率 (％) = { (10-B) /10} X 100  10% elastic recovery (%) = {(10-B) / 10} X 100
[0051] (熱収縮性）  [0051] (Heat shrinkability)
セイコー電子工業 (株）製、 SSC5200H熱分析 TMAZSS150Cを用いて、フィラメ ントの熱収縮率を測定した。チャック間距離が 10mmになるように 10本のフィラメント を固定治具に結びつけた。 5. 55mgZdtexの荷重をかけ、昇温速度 3°CZ分で 30 〜280°Cの範囲で熱収縮率を測定し、 180°Cでの熱収縮率を熱収縮率とした。  The thermal contraction rate of the filament was measured using SSC5200H thermal analysis TMAZSS150C manufactured by Seiko Denshi Kogyo. Ten filaments were tied to the fixture so that the distance between chucks was 10 mm. 5. A 55mgZdtex load was applied, the heat shrinkage rate was measured in the range of 30 to 280 ° C at a temperature increase rate of 3 ° CZ, and the heat shrinkage rate at 180 ° C was defined as the heat shrinkage rate.
[0052] (透明性）  [0052] (Transparency)
長さ 30cm、総繊度 10万 dtexのトウフィラメントを太陽光のもと、目視により評価した。  A tow filament having a length of 30 cm and a total fineness of 100,000 dtex was visually evaluated under sunlight.
◎:透明感があり、色の深み (鮮やかさ）がある  ◎: Transparency, color depth (brightness)
〇：若干不透明感があるが、色の深み (鮮やかさ）は低下して 、な 、 〇: There is a slight opacity, but the color depth (brightness) decreases.
△：不透明感 (曇り）があり、若干色の深み (鮮やかさ）が低下して 、るΔ: Opaque (cloudy), slightly reduced color depth (brightness)
X：不透明感があり、色の深みがない X: Opaque and no color depth
[0053] (触感） [0053] (feel)
専門美容師による官能評価を行い、 3段階で評価した。  A sensory evaluation was performed by a professional hairdresser and evaluated in three stages.
◎：人毛と同等の非常に柔らかな風合 、  ◎: Very soft texture equivalent to human hair
〇：人毛に似たに柔らかな風合い  ◯: A soft texture similar to human hair
△:人毛に比べ、やや硬い風合い  Δ: Slightly harder texture than human hair
X：人毛に比べ、硬い風合い  X: Harder than human hair
[0054] (くし通り） [0054] (Combination street)
長さ 30cm、総繊度 10万 dtexのトウフィラメントに、くし (デルリン榭脂製)を通し、くし の通り易さを評価した。  A comb (made by Delrin Sabah) was passed through a tow filament with a length of 30 cm and a total fineness of 100,000 dtex, and the ease of combing was evaluated.
◎：全く抵抗ない (非常に軽い） 〇：ほとんど抵抗ない (軽い） A: No resistance at all (very light) 〇: Almost no resistance (light)
△:若干抵抗がある（重い）  Δ: Some resistance (heavy)
X：かなり抵抗がある、または、タンダル、フリッツがあり途中で引つ力かる  X: There is a lot of resistance, or there are tandals and fritzs, and you can pull along the way
[0055] (難燃性） [0055] (Flame retardancy)
繊度約 50dtexのフィラメントを 150mmの長さに切り、 0. 7gを束ね、一方の端をクラ ンプで挟んでスタンドに固定して垂直に垂らした。有効長 120mmの固定したフィラメ ントに 20mmの炎を 3秒間接炎させ、燃焼させて燃焼性を評価した。  A filament with a fineness of about 50 dtex was cut into a length of 150 mm, 0.7 g was bundled, one end was sandwiched between clamps, fixed to a stand, and hung vertically. A 20 mm flame was indirectly flamed for 3 seconds in a fixed filament with an effective length of 120 mm and burned to evaluate the combustibility.
燃焼性  Combustion quality
◎：残炎時間が 0秒 (着火しな！、）  ◎: Afterflame time 0 seconds (Do not ignite!)
〇:残炎時間が 3秒未満  〇: After flame time is less than 3 seconds
：残炎時間が3〜10秒  : After flame time 3 to 10 seconds
X：残炎時間が 10秒以上  X: Afterflame time is 10 seconds or more
[0056] (アイロンセット性） [0056] (Iron set property)
ヘアーアイロンによるカールセットのしゃすさ、カール形状の保持性の指標である。フ イラメントを 180°Cに加熱したヘアーアイロンにかるく挟み、 3回扱き予熱した。このと きのフィラメント間の融着、櫛通り、フィラメントの縮れ、糸切れを目視評価した。つぎ に、予熱したフィラメントをヘアーアイロンに捲きつけ、 10秒間保持し、アイロンを引き 抜く。このときの抜きやすさ (ロッドアウト性)、抜いたときのカールの保持性を目視評 価し 7こ。  It is an indicator of curling set by hair iron and curling shape retention. The filament was pinched between hair irons heated to 180 ° C and preheated 3 times. At this time, fusion between filaments, combing, filament shrinkage, and thread breakage were 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 it is removed.
フィラメント間の融着ー  Fusion between filaments
〇：融着なし  ○: No fusion
△:わずかな融着がある  Δ: Slight fusion
X：融着あり  X: Fusion
縮れ Z糸切れ  Crimp Z thread breakage
〇：縮れ、糸切れがない  ○: No shrinkage or thread breakage
わずかに縮れ、糸切れがある  Slightly curled and has thread breakage
X：縮れ、糸切れがある  X: There is a shrinkage or thread breakage
ロッドアウト 〇：アイロンロッドがスムーズに抜ける Rod out ○: Iron rod comes out smoothly
△：アイロンロッドが若干抜け難 ヽ  Δ: Slightly difficult to remove iron rod ヽ
X：アイロンロッドが抜け難い  X: Iron rod is hard to come off
—セット性—  —Set characteristics—
〇：カールの形状が維持される  ○: The shape of the curl is maintained
△：わずかにカールの形状が崩れる  Δ: Slightly collapsed curl shape
X：カールの形状が崩れる  X: The shape of the curl is broken
[0057] (毛先のタングル性） [0057] (Tangled hair end)
長さ 30cm、総繊度 10万 dtexのトウフィラメントの一方を束ねて手でつかみ、トウがバ ラバラになるような強さで 10回振り、くし (デルリン榭脂製)を通し、毛先の絡み具合 (く しの通り易さ）を評価した。  Bundle one hand of a tow filament with a length of 30 cm and a total fineness of 100,000 dtex, hold it with your hand, shake it ten times with strength that makes the tow fall apart, pass the comb (made of Delrin resin), The condition (ease of combing) was evaluated.
◎：毛先が引つ力からずにくしを通せる（抵抗がほとんどな!/、）  ◎: The comb can be passed through without the pulling force of the hair (most resistance! /)
〇：毛先が若干引つかかる (抵抗が少しある）  〇: The hair tip is pulled slightly (there is a little resistance)
△:毛先が引つ力かる力 くしを通せる (抵抗がある）  △: The pulling force of the hair tip can pass through the comb (there is resistance)
X：毛先が引つかかり、くしが通らない  X: The tip of the hair is pulled and the comb does not pass
[0058] 本実施例および比較例において使用した原料は、以下のとおりである。 [0058] The raw materials used in the examples and comparative examples are as follows.
ポリエチレンテレフタレート（A)：  Polyethylene terephthalate (A):
'ポリエチレンテレフタレート、三菱化学 (株)製、 BK- 2180  'Polyethylene terephthalate, manufactured by Mitsubishi Chemical Corporation, BK-2180
ポリトリメチレンテレフタレート（B)：  Polytrimethylene terephthalate (B):
'ポリトリメチレンテレフタレート、 Shell社製、コノレテラ CP509200  'Polytrimethylene terephthalate, manufactured by Shell, Conoleterra CP509200
ポリブチレンテレフタレート：  Polybutylene terephthalate:
'ポリブチレンテレフタレート、三菱エンジニアリングプラスチックス (株)製、ノバデユラ ン 5010R5  'Polybutylene terephthalate, manufactured by Mitsubishi Engineering Plastics Co., Ltd., Novade Yuran 5010R5
臭素含有難燃剤 (C)：  Bromine-containing flame retardant (C):
•臭素化エポキシ系難燃剤、阪本薬品工業 (株)製、 SR-T20000  • Brominated epoxy flame retardant, Sakamoto Pharmaceutical Co., Ltd., SR-T20000
アンチモン化合物（D) :  Antimony compounds (D):
'アンチモン酸ナトリウム、 日本精鉱 (株)製、 SA— A、平均粒子径 2. 4 m 分散剤 (E)： 'モンタン酸エステル系ワックス、クラリアントジャパン（株）製、 LicowaxE 無機微粒子 (F) : 'Sodium antimonate, manufactured by Nippon Seiko Co., Ltd., SA—A, average particle size 2.4 m Dispersant (E): 'Montanate ester wax, manufactured by Clariant Japan KK, LicowaxE inorganic fine particles (F):
'微粒シリカ、富士シリシァ化学 (株)製、サイリシァ 310P、平均粒子径 2. Ι μ να 顔料：  'Fine silica, manufactured by Fuji Silicon Chemical Co., Ltd., Silicia 310P, average particle size 2. Ι μ να Pigment:
'顔料マスタバッチ、カーボンブラック 20wt%含有、大日精ィ匕工業 (株)製、 PESM2 2367BLACK  'Pigment master batch, carbon black 20wt%, manufactured by Dainichi Seisaku Kogyo Co., Ltd., PESM2 2367BLACK
[0059] (実施例 1〜12)  [0059] (Examples 1 to 12)
表 1に示す配合比率の組成物を、水分量 lOOppm以下に乾燥し、ドライブレンドし、 二軸押出機（日本製鋼所 (株)製、 TEX44)に供給し、バレル設定温度 260°Cで溶 融混練し、ペレット化した後に、水分量 lOOppm以下に乾燥させた。次いで、溶融紡 糸機 (シンコーマシナリー (株)製、 SV30)を用いて、バレル設定温度 260°Cで扁平 比が 1. 4 : 1の繭形断面ノズル孔を有する紡糸口金より溶融ポリマーを吐出し、 20°C の冷却風により空冷し、 lOOmZ分の速度で巻き取って未延伸糸を得た。得られた 未延伸糸に対し、 85°Cに加熱したヒートロールを用いて 4倍に延伸し、 190°Cに加熱 したヒートロールを用いて熱処理を行い、 30mZ分の速度で巻き取り、単繊維繊度が 65dtex前後のポリエステル系繊維（マルチフィラメント）を得た。  The composition shown in Table 1 is dried to a water content of lOOppm or less, dry blended, supplied to a twin-screw extruder (manufactured by Nippon Steel Co., Ltd., TEX44), and melted at a barrel set temperature of 260 ° C. After melt-kneading and pelletizing, it was 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 rectangular cross-section nozzle hole with a barrel setting temperature of 260 ° C and an aspect ratio of 1.4: 1. Then, it was air-cooled with a cooling air of 20 ° C. and wound at a speed of lOOmZ to obtain an undrawn yarn. The obtained unstretched yarn was stretched 4 times using a heat roll heated to 85 ° C, heat-treated using a heat roll heated to 190 ° C, wound at a speed of 30 mZ, and A polyester fiber (multifilament) having a fiber fineness of about 65 dtex was obtained.
得られたポリエステル系繊維に、親水性繊維処理剤である KWC— Q (エチレンォキ サイド プロピレンオキサイドのランダム共重合ポリエーテル；丸菱油化 (株)製) Zカロ 工剤 29 (カチオン性界面活性剤;丸菱油化 (株)製） =0. 20/0. 20%omfとなるよ うに、それぞれの純分を 0. 80%含む水溶液を調製し、総繊度 10万 dtexのトウフイラ メントに、トウ重量に対して含液率 25%になるように溶液を付着させ、熱風乾燥機を 用いて 120°Cにて 10分間乾燥させた。得られた繊維を用いて、強伸度、 10%伸張 弾性回復率、熱収縮性、透明性、触感、くし通り、難燃性、毛先のタンダル性、アイ口 ンセット性を評価した結果を、表 1に示す。  To the obtained polyester fiber, KWC-Q (Random copolymer polyether of ethylene oxide propylene oxide; manufactured by Maruhishi Oil Chemical Co., Ltd.) Z Carochemical 29 (cationic surfactant) ; Manufactured by Maruhishi Oil & Chemical Co., Ltd.) = 0/20/0. Prepare an aqueous solution containing 0.88% of each pure so that it becomes 20% omf, and tow filament with a total fineness of 100,000 dtex, The solution was adhered so that the liquid content was 25% with respect to the tow weight, and dried at 120 ° C. for 10 minutes using a hot air dryer. Using the obtained fibers, the results of evaluating the strength, 10% elongation, elastic recovery, heat shrinkability, transparency, touch, combing, flame retardancy, tandals of hair ends, and eye opening properties are shown. Table 1 shows.
[0060] [表 1]
Figure imgf000018_0001
[0060] [Table 1]
Figure imgf000018_0001
[0061] (比較例 1〜7) [0061] (Comparative Examples 1 to 7)
表 1に示す配合比率の組成物を、実施例と同様にして、単繊維繊度が 65dtex前後 のポリエステル系繊維 (マルチフィラメント）を得た。得られた繊維を用いて、強伸度、 Polyester fibers (multifilaments) having a single fiber fineness of around 65 dtex were obtained in the same manner as in the Examples with compositions having the blending ratios shown in Table 1. Using the obtained fiber,
10%伸張弾性回復率、熱収縮性、透明性、触感、くし通り、難燃性、毛先のタンダル 性、アイロンセット性を評価した結果を表 1に示す。表 1に示したように、比較例に対し 、実施例では、ポリトリメチレンテレフタレートを使用することにより、透明性 (発色性）、 カール特性に優れ、人毛に近いソフトな触感を有し、毛先のタンダル、フリッツの起こ り難いことが確認された。従って本発明の人工毛髪用繊維は、従来の人工毛髪用繊 維に比べ、ポリエステルの機械的特性、熱的特性を維持したまま、人毛に近いソフト な触感を有し、毛先のタンダル、フリッツの起こり難い、ポリエステル系人工毛髪として 有効に用いることが可能となることを確認した。 Table 1 shows the results of evaluation of 10% stretch elastic recovery, heat shrinkability, transparency, touch, combing, flame retardancy, tidal properties of hair ends, and iron set properties. As shown in Table 1, in contrast to the comparative example, in the example, by using polytrimethylene terephthalate, it has excellent transparency (color development), curl characteristics, and soft touch close to human hair, It was confirmed that tundals and frits on the hair tips were unlikely to occur. Therefore, the artificial hair fiber of the present invention has a soft tactile sensation similar to human hair while maintaining the mechanical properties and thermal properties of polyester, compared to conventional artificial hair fibers, and the tandals of the hair ends. It was confirmed that it can be effectively used as polyester-based artificial hair, which is less likely to cause frits.
産業上の利用可能性  Industrial applicability
[0062] 本発明のポリエステル系人工毛髪はポリエステル繊維の耐熱性、強伸度などの繊維 物性を維持し、透明性 (発色性)、カール特性に優れ、人毛に近いソフトな触感を有 し、毛先のタンダル、フリッツの起こり難い。従って、人工毛髪産業において有用であ る。 [0062] The polyester-based artificial hair of the present invention maintains the physical properties of polyester fibers such as heat resistance and high elongation, is excellent in transparency (color development) and curling characteristics, and has a soft touch close to human hair. , Tendall of hair ends, Fritz is unlikely to occur. Therefore, it is useful in the artificial hair industry.

Claims

請求の範囲 The scope of the claims
[1] ポリエチレンテレフタレート (A)およびポリトリメチレンテレフタレート（B)から形成され るポリエステル系人工毛髪であって、ポリエチレンテレフタレート (A)およびポリトリメ チレンテレフタレート（B)の比率力 質量比で、 （A)Z(B) =90Z10〜40Z60であ ることを特徴とするポリエステル系人工毛髪。  [1] Polyester artificial hair formed from polyethylene terephthalate (A) and polytrimethylene terephthalate (B), wherein the specific force mass ratio of polyethylene terephthalate (A) and polytrimethylene terephthalate (B) is (A) Polyester artificial hair, characterized in that Z (B) = 90Z10-40Z60.
[2] ポリエチレンテレフタレート (Α)の固有粘度力 0. 6〜1. 2dlZgである、請求項 1に 記載のポリエステル系人工毛髪。  [2] The polyester-based artificial hair according to claim 1, which has an intrinsic viscosity of polyethylene terephthalate (Α) of 0.6 to 1.2 dlZg.
[3] ポリトリメチレンテレフタレート（B)の固有粘度力 0. 6〜1. 5dlZgである、請求項 1 に記載のポリエステル系人工毛髪。  [3] The polyester-based artificial hair according to claim 1, which has an intrinsic viscosity of polytrimethylene terephthalate (B) of 0.6 to 1.5 dlZg.
[4] ポリエチレンテレフタレート（A)およびポリトリメチレンテレフタレート（B)の合計 100重 量部に対し、さらに臭素含有難燃剤 (C) 5〜30重量部を含有する組成物から形成さ れた請求項 1〜3のいずれかに記載のポリエステル系人工毛髪。  [4] Claims formed from a composition containing 5 to 30 parts by weight of a bromine-containing flame retardant (C) with respect to a total of 100 parts by weight of polyethylene terephthalate (A) and polytrimethylene terephthalate (B). The polyester-based artificial hair according to any one of 1 to 3.
[5] 臭素含有難燃剤 (C)が、臭素化芳香族系難燃剤、臭素含有リン酸エステル系難燃 剤、臭素化ポリスチレン系難燃剤、臭素化べンジルアタリレート系難燃剤、臭素化工 ポキシ系難燃剤、臭素化フエノキシ系難燃剤、臭素化ポリカーボネート系難燃剤、テ トラブロモビスフエノール A誘導体、臭素含有トリアジン系化合物および臭素含有イソ シァヌル酸系化合物よりなる群カゝら選ばれた少なくとも 1種の難燃剤である、請求項 4 に記載のポリエステル系人工毛髪。  [5] Bromine-containing flame retardant (C) is a brominated aromatic flame retardant, bromine-containing phosphate ester flame retardant, brominated polystyrene flame retardant, brominated benzaryl acrylate flame retardant, brominated At least selected from the group consisting of a poxy flame retardant, a brominated phenoxy flame retardant, a brominated polycarbonate flame retardant, a tetrabromobisphenol A derivative, a bromine-containing triazine compound and a bromine-containing isocyanuric acid compound. The polyester-based artificial hair according to claim 4, which is a kind of flame retardant.
[6] ポリエチレンテレフタレート (A)およびポリトリメチレンテレフタレート（B)の合計 100重 量部に対し、さらにアンチモン系化合物（D)を 0. 5〜 10重量部含有する組成物から 形成された、請求項 4〜5のいずれか〖こ記載のポリエステル系人工毛髪。  [6] It is formed from a composition containing 0.5 to 10 parts by weight of an antimony compound (D) with respect to 100 parts by weight of the total of polyethylene terephthalate (A) and polytrimethylene terephthalate (B). Item 5. The polyester-based artificial hair according to any one of Items 4 to 5.
[7] アンチモン系化合物（D) 1S 三酸ィ匕アンチモン、四酸ィ匕アンチモン、五酸化アンチ モンおよびアンチモン酸ナトリウムよりなる群力 選ばれた少なくとも 1種のアンチモン 化合物である、請求項 6に記載のポリエステル系人工毛髪。  [7] The antimony compound (D) 1S is at least one antimony compound selected from the group consisting of 1S antimony trioxide, 1 antimony tetraacid, antimony pentoxide, and sodium antimonate. The polyester-based artificial hair described.
[8] ポリエチレンテレフタレート (A)およびポリトリメチレンテレフタレート（B)の混合物合 計 100重量部に対し、さらに分散剤 (E)を 0. 05〜3重量部含有する組成物から形成 された、請求項 1〜7のいずれか〖こ記載のポリエステル系人工毛髪。  [8] A composition comprising 0.05 to 3 parts by weight of dispersant (E) with respect to 100 parts by weight of the total mixture of polyethylene terephthalate (A) and polytrimethylene terephthalate (B). Item 8. The polyester-based artificial hair according to any one of Items 1 to 7.
[9] 分散剤（E) 1S モンタン酸系ワックス、モンタン酸エステル系ワックス、部分ケン化モ ンタン酸系ワックス、モンタン酸金属塩、ポリエチレン系ワックス、酸化ポリエチレン系 ワックス、ポリテトラフルォロエチレン、フッ素変性ワックス、ポリジメチルシリコーンおよ び変性シリコーンレジンの 1種以上力もなる化合物である、請求項 8記載のポリエステ ル系人工毛髪。 [9] Dispersant (E) 1S Montanic acid wax, montanic acid ester wax, partially saponified rubber An tannic acid-based wax, a metal salt of montanic acid, a polyethylene-based wax, a polyethylene oxide-based wax, a polytetrafluoroethylene, a fluorine-modified wax, a polydimethylsilicone, and a modified silicone resin. Item 9. Polyester artificial hair according to Item 8.
[10] ポリエチレンテレフタレート (A)およびポリトリメチレンテレフタレート（B)の混合物合 計 100重量部に対し、さらに有機微粒子 (F)および Zまたは無機微粒子 (G)を 0. 1 〜5重量部含有する組成物力 形成された、請求項 1〜9のいずれかに記載のポリエ ステル系人工毛髪。  [10] 0.1 to 5 parts by weight of organic fine particles (F) and Z or inorganic fine particles (G) are further added to 100 parts by weight of the total mixture of polyethylene terephthalate (A) and polytrimethylene terephthalate (B). The polyester artificial hair according to any one of claims 1 to 9, wherein the composition is formed.
[11] 有機微粒子 (F)が、ポリアリレート、ポリアミド、フッ素榭脂、シリコーン榭脂、架橋ァク リル榭脂および架橋ポリスチレンよりなる群力も選ばれた少なくとも 1種である、請求 項 10記載のポリエステル系人工毛髪。  [11] The organic fine particles (F) according to claim 10, wherein the organic fine particles (F) are at least one selected from the group consisting of polyarylate, polyamide, fluorine resin, silicone resin, crosslinked acryl resin and crosslinked polystyrene. Polyester artificial hair.
[12] 無機微粒子 (G)が、炭酸カルシウム、酸化ケィ素、シリカ Zメラミン榭脂複合体、酸ィ匕 チタン、酸ィ匕アルミニウム、酸化亜鈴、タルク、カオリン、モンモリロナイト、ベントナイト およびマイ力よりなる群力も選ばれた少なくとも 1種である、請求項 10記載のポリエス テル系人工毛髪。  [12] Inorganic fine particles (G) are composed of calcium carbonate, silicon oxide, silica Z melamine resin complex, acid titanium, acid aluminum, dumbbell, talc, kaolin, montmorillonite, bentonite and my strength 11. The polyester-based artificial hair according to claim 10, wherein the group strength is at least one selected.
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KR102285778B1 (en) * 2016-04-13 2021-08-03 덴카 주식회사 Resin composition for artificial hair and molded article thereof
KR20190004304A (en) * 2016-04-28 2019-01-11 덴카 주식회사 Artificial hair fiber
US20190090565A1 (en) * 2016-04-28 2019-03-28 Denka Company Limited Fiber for artificial hair
US10856598B2 (en) * 2016-04-28 2020-12-08 Denka Company Limited Fiber for artificial hair
KR102286437B1 (en) * 2016-04-28 2021-08-04 덴카 주식회사 artificial hair fiber

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