CN1826436A - Flame-retardant polyester fibers for artificial hair - Google Patents
Flame-retardant polyester fibers for artificial hair Download PDFInfo
- Publication number
- CN1826436A CN1826436A CN200480021076.7A CN200480021076A CN1826436A CN 1826436 A CN1826436 A CN 1826436A CN 200480021076 A CN200480021076 A CN 200480021076A CN 1826436 A CN1826436 A CN 1826436A
- Authority
- CN
- China
- Prior art keywords
- artificial hair
- flame
- fiber
- retardant polyester
- polyester fibers
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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- 230000001052 transient effect Effects 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
- NSBGJRFJIJFMGW-UHFFFAOYSA-N trisodium;stiborate Chemical compound [Na+].[Na+].[Na+].[O-][Sb]([O-])([O-])=O NSBGJRFJIJFMGW-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a flame-retardant polyester fiber for artificial hair which is produced by melt-spinning a composition comprising 100 parts by weight of at least one polyester (A) selected from among polyalkylene terephthalates and copolyesters comprising polyalkylene terephthalates as the main component and 5 to 30 parts by weight of a brominated epoxy flame retardant (b). Further, the invention relates to a flame-retardant polyester fiber for artificial hair as described above which has at least one modified cross section; a flame-retardant polyester fiber for artificial hair as described above which is a mixed fiber having a mixing ratio of circular cross section to modified cross section of 8 : 2 to 1 : 9; and a flame-retardant polyester fiber for artificial hair which is produced by making a hydrophilic fiber treatment adhere to the above polyester fiber and is excellent in smoothness to the touch, combing properties, and flame retardance.
Description
Technical field
The present invention relates to flame-retardant polyester fibers for artificial hair with polyester and the formation of bromination epoxy flame retardant.More particularly, relate to the fibrous physical property that keeps anti-flammability, heat resistance, intensity, elongation etc.; Constancy, the transparency, devitrification resistance, the artificial hair fiber that cardability is good.
In addition, the present invention relates to profiled fibre, more particularly, relate to as the hair of wig, plait, headwear wig (extension hair) etc. and decorate the artificial hair used etc. different in nature cross-section fibers, reach the artificial hair fiber of this profiled fibre of use with the gloss with similar human hair of fiber, form and aspect, feel, bulkiness.
In addition, the invention still further relates to smooth sense of touch, the comb general character, artificial hair fiber that antistatic behaviour is good.
Background technology
Polyethylene terephthalate or based on the fiber of the polyester of polyethylene terephthalate, owing to have high-melting-point, high elastic modulus and excellent heat resistance, chemical-resistant, thus widely at the bottom of curtain, cushion, dress material, blanket, cover, aspect uses such as tablecloth, loose cover cloth, wall decoration material, artificial hair, automobile interior trim material, outdoor supporting material, safety net.
On the other hand, the hair product end user hair of past wig, headwear wig, postiche head, hair band, Doll hair etc. or artificial hair (modification acrylonitrile fiber, polyvinyl chloride fibre) etc.But the human hair is provided difficulty, and the importance that the old friend makes hair is increasing.As the artificial hair material, though use the modification acrylonitrile fiber who utilizes flame retardancy characteristics mostly, the heat resistance aspect is insufficient.
In recent years, proposed to use the polyester of the polyethylene terephthalate representative of good heat resistance to be the artificial hair scheme of the fiber of main component.Yet, owing to the polyester fiber that from polyethylene terephthalate is representative is a combustible material, so flame resistance is insufficient.
The crowd knows, has carried out the exploration of various raising polyester fiber flame resistances in the past, for example makes the method for fiber by the polyester of the anti-flammability monomer copolymerization that contains phosphorus atoms, or makes method that contains fire retardant in the polyester fiber etc.
As the former method that makes the anti-flammability monomer copolymerization, for example proposed to make phosphorus atoms to become the method (special public clear 55-41610 communique) that makes the phosphorus compound copolymerization of good thermal stability behind the ring composition, also proposed to make the method (special public clear 53-13479 communique) of carboxy phosphonic acid copolymerization, made the scheme of phosphorus compound and the method (spy opens flat 11-124732 communique) that contains the polyethylene terephthalate copolymer of polyarylate etc.
Use the scheme of aforementioned fire-retardantization technology as artificial hair, for example proposed to make the polyester fiber (spy opens flat 3-27105 communique, and the spy opens flat 5-339805 communique etc.) of phosphorus compound copolymerization.
Yet, the demanding anti-flammability of artificial hair, so artificial hair will use these copolymerization of polyester fiber, must increase its copolymerization amount, the result reduces the heat resistance of polyester significantly, the melt spinning difficulty that becomes, though or, burning missing of ignition near the occasion of flame, produce fusion, drip the problem of dropping down and so on other.In addition, the occasion that cooperates aforementioned phosphorus flame retardant, present anti-flammability and must strengthen the caused sense of being clamminess of its addition except increasing to, under the condition that is subjected to thermal process or high humidity, also exist the artificial hair make gained polyester fiber system easily to produce the situation of apparent problem of the fiber of devitrification and so on.
In addition,, proposed the method (special fair 3-57990 communique) that makes polyester fiber contain the halogenation loop chain hydride compounds of particulate, contained the method schemes such as (special fair 1-24913 communiques) of brominated alkyl cyclohexane as the latter's the method that contains fire retardant.Yet, make polyester fiber contain the method for fire retardant, in order to obtain sufficient anti-flammability, existence must make and contain treatment temperature and become high temperature more than 150 ℃, maybe must make and contain the processing time and become long-time or must use the problem of a large amount of fire retardant and so on, the problem that produces that fibrous physical property reduces or production efficiency reduces, production cost increases etc.
Therefore, also can not get keeping the fibrous physical property of the anti-flammability, heat resistance, intensity, elongation etc. of polyester fiber in the past in fact at present, constancy, devitrification resistance, viscosity reduce good artificial hair.
Generally, the synthetic fiber as Hair grooming uses have acrylic fibre, vinyl chloride fibers, vinylidene chloride fiber, polyester fiber, nylon fiber, polyamide fiber etc.So far, though use these fiber process to become the artificial hair commodity of wig, plait, headwear wig etc., but since these fibers do not possess simultaneously heat resistance, crimpiness, sense of touch etc. as artificial hair with fiber necessary complete characteristic, when therefore making head decoration product, can not satisfy the goods of various characteristics with a kind of fiber manufacturing, just make the goods that meet each fiber properties and use, and, repeating to study the cross sectional shape that improves the fiber that is suitable for extensive stock.
For example, can enumerate the longest partial L in the cocoon shape cross sectional shape, the length of the diameter W of the circular portion at two ends and the wide C of central portion venturi portion is limited to wig in the particular range with long filament (reality is opened clear 48-13277 communique), maximum gauge (L) by center of gravity in the fiber cross section is limited to the interior artificial hair of prescribed limit synthetic fiber (special public clear 53-6253 communique), the cross section is into circular or the oval-shaped four unit long filament of unit long filament with respect to one to be had other three unit long filament uniformly-spaced to be radial adjacent cross section Y font, the wig that the unit long filament contact each other of adjacency connects with the width that is substantially equal to this unit long filament radius and plait are with long filament (reality is opened clear 63-78026 communique), has the overlapping cross sectional shape in flat circular portion ground that makes at least 2, to the ratio L/W of the length L of the length W of its minor axis and major axis, in the heart distance C in 2 adjacent flat circles, and to connect in 2 flat circles in the heart straight line and the wig of the qualifications such as angle that become of the major axis of flat circle with long filament (spy opens clear 55-51802 communique) etc.
But, as the fiber of developing with fiber as above-mentioned artificial hair in the past, have by the length of the numerical definiteness all fibres cross sectional shape of the limit or the special shape of angle, except may not making easily, using as plait or the headwear wig occasion of using, good feel may not be arranged, too pay attention to the maintenance or the up rightness of hair style, often become the fiber of hard sense of touch.In addition, also insufficient aspect the easy operability of handwork.In addition, flat fiber extensively uses in the pile purposes so far, and as dummy head's hair fiber of wig etc., because the too many soft feeling of not liked etc. are estimated to be not suitable for as the purposes of artificial hair with fiber.
In addition, make polyester fiber contain the method for fire retardant, in order to obtain sufficient anti-flammability, must make in addition contain treatment temperature be more than 150 ℃ high temperature, maybe must make and contain the processing time for long-time or must use the problem of a large amount of fire retardants, produce that fibrous physical property reduces or the problem of production efficiency reduction, production cost increase etc.
In order to give flexibility, smooth sense of touch etc., provide various polysiloxane series finishing agents to the synthetic fiber of described anti-flammability/non-anti-flammability.For example, restorative in order to give flexibility, wrinkle resistance, elastic force and compression, use dimethyl polysiloxane, methylhydrogenpolysi,oxane, two terminal hydroxy group dimethyl polysiloxanes contain the organopolysiloxane of vinyl, contain the epoxy radicals organopolysiloxane, contain amino organopolysiloxane, contain the ester group organopolysiloxane, contain the organopolysiloxane of polyoxygenated alkene etc.In addition, the finishing agent that constitutes of the combination of known alkoxy silane and/or polyacrylamide resin or catalyst etc.
For example, disclose and utilized organopolysiloxane that contains at least 2 epoxy radicals in per 1 molecule and the finishing agent that contains amino organopolysiloxane formation, two terminal hydroxy group organopolysiloxanes, the organopolysiloxane that contains amino and alkoxyl in 1 molecule, and/or the method for its partial hydrolystate and the finishing agent (the public clear 53-36079 communique of spy) of condensation product formation.
In addition, also put down in writing finishing agent (the special public clear 53-197159 communique that the organopolysiloxane that contains epoxy radicals and aminoalkyl trialkoxy silane constitute, special public clear 53-19716 communique), contain the diorganopolysiloxanecompositions that two amino more than 2 ends are three organic siloxies (special public clear 53-98499 communique) in 1 molecule.In addition, also proposed to use the method for the finishing agent (special public clear 58-17310 communique) that the alkoxy silane that contains more than 2 amino amino silicones and the reactive base that contains amino more than 1, epoxy radicals etc. in 1 molecule constitutes.
In addition, also disclose and adopted the method that contains more than 2 finishing agent (spy opens clear 55-152864 communique) that the diorganopolysiloxanecompositions that contains at least 2 above ester bonds in two amino organosiloxanes and 1 molecule constitutes in 1 molecule at least, contained the method for amino polysiloxanes, terminal hydroxyl polysiloxanes and the finishing agent (spy opens clear 58-214585 communique) that contains reactive basic alkylalkoxy silane formation.In addition, also disclose and adopted organopolysiloxane, amino silane compounds that contains epoxy radicals and the method for solidifying the finishing agent (spy opens clear 59-144683 communique) that constitutes with catalyst, has adopted the method for the finishing agent (spy opens clear 60-94680 communique) of the organopolysiloxane that contains at least 2 epoxy radicals in 1 molecule and polyacrylamide resin formation.
Yet these adhesions contain the fiber of polysiloxane fibers finishing agent, though smooth sense of touch, cardability etc. improve because the polysiloxane series fibre finish itself is an inflammability, so the problem that has the anti-flammability of anti-flammability synthetic fiber obviously to reduce.
Summary of the invention
The present invention relates to the flame-retardant polyester fibers for artificial hair that forms by bromination epoxy flame retardant (B) 5～30 weight portions that contain the polyester more than a kind (A) 100 weight portions of copolyester that polyalkylene terephthalates or polyalkylene terephthalates are main body and general formula (1) expression, preferably (A) composition is to be selected from polyethylene terephthalate, at least a kind polymer system polyester of polytrimethylene terephthalate and polybutylene terephthalate (PBT), (B) composition is at least a kind the fire retardant that is selected from the bromination epoxies of general formula (α)～(γ) expression.
(in the formula, m represents 0～150)
(in the formula, n represents 0～150)
(in the formula, p represents 0～150, and y represents 0～5)
Preferred above-mentioned flame-retardant polyester fibers for artificial hair, in (A) and (B) composition, mix organic fine particles (C) and/or inorganic particles (D) again, form fine projection at fiber surface, (C) composition is at least a kind that is selected from polyarylate, polyamide, fluororesin, silicones, crosslinked acrylic resin, the crosslinked polystyrene, and (D) composition is at least a kind that is selected from calcium carbonate, silica, titanium oxide, aluminium oxide, zinc oxide, talcum, kaolin, montmorillonite, bentonite, mica, the antimony based compound.
In addition, the present invention adheres to the fiber for artificial hair that the aliphatic poly ether compound is hydrophilic fibre finishing agent (E) system of main component on aforementioned flame-retardant polyester fiber.Providing flame-retardant polyester fiber, anti-flaming polypropylene fiber, fire-resistant polyamide fiber etc. is purpose to improve smooth sense of touch or feel etc., do not cause that the anti-flammability when similar use polysiloxane series fibre finish is handled reduces, have the anti-flammability fiber for artificial hair of smooth sense of touch equal when using the polysiloxane series finish to handle, cardability, antistatic behaviour, good flame resistance.
In addition, the present invention can make the cross sectional shape of polyester fiber become specific odd-shaped cross section, has the ellipse of being selected from, intersect circular, cocoon shape, big tripe shape, dog bone shape, band shape, 3～8 is leaf, the artificial hair polyester fiber of at least a kind odd-shaped cross section shape of star, the circle or the flat circular portion ground that relate to the fibre section and be more than 2 are overlapping, or the shape of joining each other, or the fibre section is 3～8 leaf, the degree of profile of formula (1) expression is at the profiled fibre of 1.1～8 scopes, and, the aspect ratio that also relates to the fibre section is 1.2～4 artificial hair polyester fiber, also relate to as circular with, be selected from ellipse, intersect circular, cocoon shape, big tripe shape, dog bone shape, band shape, 3～8 is leaf, the artificial hair polyester fiber of the blended fiber of at least a kind odd-shaped cross section shape in the star, wherein circular cross-section: the mixing ratio of odd-shaped cross section is 8: 2～1: 9.
Preferred above-mentioned flame-retardant polyester fibers for artificial hair is a non-crimping raw silk shape, solution dyeing, and the filament fiber number is 30～80dtex.
Description of drawings
Fig. 1～10th, the schematic diagram in the polyester fiber cross section of expression composition system of the present invention, each accompanying drawing is corresponding with following figure.
Fig. 1: crossed-circle tee section figure
Fig. 2: intersect flat circular section figure
Fig. 3: dog bone tee section figure
Fig. 4: 3 leaf sectional views
Fig. 5: 5 leaf sectional views
Fig. 6: 7 leaf sectional views
Fig. 7: the aspect ratio key diagram of odd-shaped cross section
Fig. 8: special-shaped nozzle 1
Fig. 9: special-shaped nozzle 2
Figure 10: special-shaped nozzle 3
The preferred plan that carries out an invention
Flame-retardant polyester fibers for artificial hair of the present invention carries out the fiber that melt spinning makes by containing the polyester of forming more than a kind (A) of copolyester that polyalkylene terephthalates or polyalkylene terephthalates are main body and the composition of bromination epoxy flame retardant (B).Polyalkylene terephthalates that contains in the polyester (A) that uses as the present invention or polyalkylene terephthalates are the copolyester of main body, for example can enumerate the polyalkylene terephthalates of polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate (PBT) etc. and/or based on these polyalkylene terephthalates, contain the copolyester of minor amounts of copolymerized composition.Aforementioned so-called main body is meant and contains 80 moles more than the %.
As aforementioned copolymer composition, for example, can enumerate M-phthalic acid, phthalic acid, naphthalene dicarboxylic acids, to the penylene dicarboxylic acids, trimellitic acid, Pyromellitic Acid, butanedioic acid, glutaric acid, adipic acid, suberic acid, azelaic acid, decanedioic acid, the polybasic carboxylic acid of dodecanedioic acid etc., the derivative of these polybasic carboxylic acids, 5-sulfoisophthalic acid sodium, 5-sulfoisophthalic acid sodium dihydroxy ethyl ester etc. contains the dicarboxylic acids of sulfonate, the derivative of these dicarboxylic acids, 1, the 2-propylene glycol, 1, ammediol, 1, the 4-butanediol, 1, the 6-hexylene glycol, neopentyl glycol, 1,4 cyclohexane dimethanol, diethylene glycol, polyethylene glycol, trimethylolpropane, pentaerythrite, the 4-hydroxybenzoic acid, 6-caprolactone etc.
Consider from the viewpoint of security, ease-to-operate, usually preferred aforementioned copolyester makes by making polymer as the terephthalic acid (TPA) of main body and/or its derivative (for example terephthalic acid (TPA) methyl esters) and aklylene glycol contain a spot of copolymer composition reaction, but also can make with the mixture of aklylene glycol, monomer or the polymerization of oligomer mixture of ingredients that contains as the minor amounts of copolymerized composition again by making terephthalic acid (TPA) and/or its derivative (for example terephthalic acid (TPA) methyl esters) as main body.
Aforementioned copolyester so long as the polycondensation on as the main chain of the polyalkylene terephthalates of main body and/or side chain of aforementioned copolymer composition gets final product, to method of copolymerization etc., does not have particular determination.
Concrete example as aforementioned copolyester based on polyalkylene terephthalates, for example can enumerate polyethylene terephthalate is the polyester that main body, copolymerization have the glycol ether of bisphenol-A, copolymerization has polyester, the copolymerization of 1,4 cyclohexane dimethanol that polyester of 5-sulfoisophthalic acid sodium dihydroxy ethyl ester etc. is arranged.
Aforementioned polyalkylene terephthalates and copolyester thereof can use a kind, also can use mixing more than 2 kinds.Wherein, preferred polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate (PBT), (polyethylene terephthalate is the polyester that main body, copolymerization have the glycol ether of bisphenol-A to copolyester, copolymerization has 1, the polyester of 4-cyclohexanedimethanol, copolymerization have the polyester of 5-sulfoisophthalic acid sodium dihydroxy ethyl ester etc.), also preferred with these mixtures that mixes more than 2 kinds.
As the inherent viscosity of (A) composition, preferably 0.5～1.4, more preferably 0.5～1.0.Inherent viscosity is lower than at 0.5 o'clock, produces the tendency that the mechanical strength of gained fiber reduces, and surpasses at 1.4 o'clock, and along with the increase melt viscosity of molecular weight increases, the melt spinning difficulty that becomes produces the uneven tendency of fiber number.
The bromination epoxy flame retardant (B) that the present invention uses does not have particular determination, can use the bromination epoxy fire retardant of general use.
As the concrete example of (B) composition, the end that can enumerate general formula (α) expression that contains compound shown in the following formula is enclosed type bromination epoxy flame retardant not,
An endcapped type bromination epoxy based flame retardant etc. that contains general formula (β) expression of compound shown in the following formula,
The two end-sealed type bromination epoxy based flame retardants etc. that contain general formula (γ) expression of compound shown in the following formula,
These can use a kind, also can will be used in combination more than 2 kinds.
The use amount of above-mentioned (B) composition with respect to (A) composition 100 weight portions, is 5～30 weight portions.Wherein preferred 6～25 weight portions, preferred again 8～20 weight portions.When use amount is lower than 5 weight portions, be difficult to obtain flame retardant effect, during greater than 30 weight portions, destroy mechanical property, heat resistance, anti-dropping down property.
(B) number-average molecular weight of composition is preferably more than 20000, and more preferably 30000～80000.Number-average molecular weight is lower than at 20000 o'clock, and the dispersion territory that is dispersed in the fire retardant in the polyester is little, and the projection of fiber surface is little, and gloss strengthens.When molecular weight is too high, disperse the territory to become big, color development reduces.
As (C) composition, can use have with as (A) composition of principal component and/or (B) the organic resin composition of the incompatible or incompatible structure of part of composition, for example, preferably use polyarylate, polyamide, fluororesin, silicones, crosslinked acrylic resin, crosslinked polystyrene etc.These can use a kind, also can will be used in combination more than 2 kinds.
As (D) composition, have the transparency to fiber, the influence of color emissivity in mind, preferably have and approach (A) and/or (B) compound of the refractive index of the refractive index of composition, for example, can enumerate calcium carbonate, silica, titanium oxide, aluminium oxide, zinc oxide, talcum, kaolin, montmorillonite, bentonite, mica, antimony based compound etc.Wherein, the antimony based compound that uses as above-mentioned (D) composition does not have particular determination, as concrete example, can enumerate antimony trioxide compound, antimony pentaoxide compound, sodium antimonate.In addition, the particle diameter of these antimony based compounds does not have particular determination, but preferred 0.02～5 μ m, more preferably 0.02～3 μ m, preferred 0.02～2 μ m again.The antimony based compound that the present invention uses also can use epoxide, silane compound, isocyanate compound, titanate compound etc. to carry out surface treatment as required.
Use the occasion of antimony based compound, the use amount of antimony based compound does not have particular determination, but with respect to (A) composition 100 weight portions, 0.1～5 weight portion preferably, more preferably 0.1～3 weight portion, preferred again 0.2～2 weight portion.Use amount is during greater than 5 weight portions, and aesthetic appearance, form and aspect, color emissivity are destroyed, during less than 0.1 weight portion, because the micro crowning that fiber surface forms tails off, so the adjusting of the gloss of fiber surface is insufficient.In addition, also can with other (D) composition and usefulness, but as total use amount of (D) composition of this moment, preferably below 5 weight portions.
Use the occasion of antimony based compound as (D) composition, because performance that not only can the controlling fiber surface but also can improve the flame retardant effect of fiber self and preferred the use.
The hydrophilic fibre finishing agent (E) that the present invention uses does not have particular determination, can be to be selected from polyoxygenated alkene alkyl ether, polyoxyalkylene hydrocarbon chain alkene ether, polyoxygenated alkene aryl ether, polyoxygenated alkene alkyl aryl ether, these random copolymerization polyethers, polyoxygenated alkene Arrcostab, polyoxyalkylene hydrocarbon chain alkenyl esters, at least a in the polyoxygenated alkene alkyl aryl ester, with polyoxygenated alkene alkylamine, N, N-dihydroxy ethyl alkylamide, polyoxygenated alkene alkylamide, fatty glyceride, fatty acid polyglycerol ester, fatty acid pentaerythritol ester, polyoxygenated alkene pentaerythrite Arrcostab, sorbitan fatty acid ester, polyoxygenated alkene sorbitan fatty acid ester, fatty acid cane sugar ester, polyoxygenated alkene sucrose fatty ester, polyoxygenated alkene, alkylamine salt, alkylammonium salt, the alkyl aralkyl ammonium salt, Fixanol, alkyl picoline salt, soap, rosinate, sulphation soap, alkylsulfonate, alkylbenzenesulfonate, alkylnaphthalene sulfonate, the alkyl sulfo fatty acid ester salt, the dialkyl sulfosuccinate succinate salt, polyoxygenated alkene alkyl ether sulfosuccinic acid monoesters salt, polyoxyalkylene hydrocarbon chain alkene ether sulfosuccinic acid monoesters salt, polyoxygenated alkene aryl ether sulfosuccinic acid monoesters salt, alkyl diphenyl ether disulfonate, sulfated oil, sulfated fatty acid ester salt, alkyl sulfate salt, the alkenyl sulfuric acid, polyoxygenated alkene alkyl ether sulphate salts, polyoxygenated alkene alkyl ether carboxy acid salt, polyoxyalkylene hydrocarbon chain alkene ether sulfuric acid, polyoxygenated alkene aryl ether sulfuric acid, alkyl phosphate salt, polyoxygenated alkene alkyl ether phosphate salt, polyoxyalkylene hydrocarbon chain alkene ether phosphate ester salt, the general mixture that contains ether fibre finish and the general ionic surfactant who contains ether fibre finish and general use who uses that uses such as polyoxygenated alkene aryl ether phosphate ester salt, but because when containing constituent based on the polysiloxanes composition, anti-flammability reduces significantly, so must not contain the compound of polysiloxanes composition.In addition, hydrophilic fibre finishing agent (E) is to be selected from the polyethers based compound, the fatty acid ester based compound, organic amine, organic amide, the organic fatty acid esters, organic amine salt, organic ammonium salt, organic pyridinium salt, organic picoline salt, the organic fatty hydrochlorate, rosinate, organic sulfonate, organic succinate salt, organic succinic monoester salt, organic carboxylate, at least a in the organo-sulfate salt, or the mixture that mixes more than two kinds, the special random copolymerization polyethers (molecular weight Mw15000～50000) that preferably is selected from poly(ethylene oxide)-poly(propylene oxide), poly(ethylene oxide) (molecular weight 100～1000), at least a in the poly(propylene oxide) (molecular weight 100～1000).In order to give smooth sense of touch, cardability, antistatic behaviour etc., can add up to 0.01%～1% by weight fiber is adhered to hydrophilic fibre finishing agent (E).The addition of hydrophilic fibre finishing agent (E) is 0.01% when following, can not obtain sufficient cardability, and smooth sense of touch is also not enough.Otherwise be 1% when above, during contact tow long filament, finish is bonded on hand, and is because hand is clamminess or finish itself also is an easy firing, not preferred so might cause the anti-flammability reduction of fiber.Good for smooth sense of touch, cardability, present sufficient antistatic behaviour, preferably the random copolymerization polyethers of epoxy ethane-epoxy propane: the combination of cationic surfactant=50: 50, but the invention is not restricted to this combination.Adhesion method to fiber can adopt the stretching that continues, heat treated continuous processing to carry out, and also can adopt batch process to carry out.
In addition, can make the cross sectional shape of polyester fiber become specific odd-shaped cross section.
Fibre section of the present invention is shown in ((Fig. 1)～(Fig. 3)) (major axis a is a/b=1.2～4 with the ratio of minor axis b among the figure), overlapping or the shape of joining in circle more than 2 or flat circular portion ground, the wherein partly overlapping or circle more than 2 that joins or flat circle be side by side state on straight line preferably, about preferred symmetry.
Fibre section of the present invention is in 3～8 leaf occasions, in exemplifying ((Fig. 4)～(Fig. 6) (among the figure, the ratio of external diameter of a circle D and the diameter d of inscribed circle, D/d=1.1～8)), the degree of profile of following formula (1) expression is 1.1～8 scope, more preferably 1.3～6 scope preferably.Degree of profile surpasses at 8 o'clock, and sense of touch, cardability reduce, and are lower than at 1.1 o'clock, and the tendency of sense of touch hardening is arranged.And if become more than 9 leaves, then the difference with positive circular section diminishes, the tendency that has effect of the present invention to diminish.
(formula 1)
Degree of profile=(the external diameter of a circle in filament cross section)/(diameter of the inscribed circle in filament cross section)
The aspect ratio of the odd-shaped cross section of the present invention ratio of the length of minor axis (length of the major axis of cross sectional shape with), (among the figure, ratio x/y=1.2～4 of major axis x and minor axis y), preferably 1.2～4 scope, more preferably 1.5～2.5 scope shown in (Fig. 7).Aspect ratio can not obtain gloss, sense of touch near the human hair greater than 4 o'clock, less than 1.2 o'clock, the tendency of feel hardening was arranged.
Polyester fiber of the present invention as circular and oval, intersects circle, cocoon shape, greatly tripe shape, dog bone shape, be with the occasion of the blended fiber of at least a kind the odd-shaped cross section shape of selecting in shape, 3～8 leaf, the star, circular cross-section: the mixing ratio of odd-shaped cross section, preferably 8: 2～1: 9, more preferably 7: 3～2: 8.
Use as the fiber number of the occasion that above-mentioned profiled fibre of the present invention is used as artificial hair, be preferably the scope of 30～80dtex.In addition, can by by ratio arbitrarily with this profiled fibre and human hair's blend manufacturing hair style freely as the Hair grooming commodity.During blend, when the mixed proportion of profiled fibre of the present invention is too high, the sense of touch hardening, and the mixed proportion of profiled fibre can not be made hair style freely when too low.Because such reason, it is that 80～10 weight %, human hair are the scope of 20～80 weight % that blending ratio preferably makes profiled fibre.
In addition, profiled fibre of the present invention, except the human hair, the also artificial hair fiber of other that can use so far with aforementioned, for example, blend such as acrylic fibre, vinyl chloride fibers, vinylidene chloride fiber, polyester fiber, nylon fiber, polyolefin series fiber are used.
The flame-retardant polyester composition that the present invention uses, for example, can by in advance will (A) and (B) composition and (C) composition as required or (D) composition do mixed after, use various general mixing rolls to carry out melting mixing and make.As the example of aforementioned mixing roll, for example, can enumerate single screw extrusion machine, double screw extruder, cylinder, Banbury, kneader etc.Wherein, consider preferred double screw extruder from the adjusting of mixing degree, the viewpoint of ease-to-operate.
Flame-retardant polyester fibers for artificial hair of the present invention can make by adopting common melt spinning method that aforementioned flame-retardant polyester composition is carried out melt spinning.
That is, for example, the temperature of establishing extruder, gear pump, spinning head etc. is 270～310 ℃, carries out melt spinning, makes to spin strand by behind the cartridge heater, is cooled to below the glass transition temperature, draws by the speed that 50～5000m/ divides, and makes and spins strand.In addition, cooling spins strand in being added with the tank of cooling water, can carry out the control of fiber number.The temperature of the temperature of the temperature of cartridge heater or length, cooling air or the amount of blowing, bosh, cool time, hauling speed can utilize the hole count of spray volume and spinning head suitably to regulate.
The strand that spins that makes carries out hot-stretch, any method of the direct spinning stretching method that the two operation methods that stretching can be adopted temporary transient coiling to spin to stretch behind the strand stretch continuously with not reeling.Hot-stretch adopts 1 section extension or the multistage extension more than 2 sections to carry out.As the heater means in the hot-stretch, can use warm-up mill, hot plate, steam injection equipment, warm water tank etc., also can be suitably with these means and usefulness.
Flame-retardant polyester fibers for artificial hair of the present invention can contain the various additives of fire retardant beyond (B) composition, heat-resistant agent, light stabilizer, fluorescer, antioxidant, antistatic additive, pigment, plasticizer, lubricant etc. according to need.By containing pigment, can obtain dope-dyed fiber.
The flame-retardant polyester fibers for artificial hair of the present invention that makes like this is the fiber of non-crimping raw silk shape, and the fiber number of fiber is 30～80dtex and then be 35～75dtex normally, is suitable for artificial hair and uses.In addition,, preferably have and to be difficult to catch fire 160～200 ℃ of heat resistances of using beautifying heat utensil (hair waving pin) down, have from fire extinguishing property as the artificial hair fiber.
The occasion of flame-retardant polyester fiber solution dyeing of the present invention can directly be used, but the occasion of solution dyeing not, can with the same condition of common flame-retardant polyester fiber under dye.
The pigment that dyeing is used, dyestuff, auxiliary agent etc., the product of preferred weatherability and good flame resistance.
Flame-retardant polyester fibers for artificial hair of the present invention uses fixed volume youngster's property of beautifying heat utensil (hair waving pin) good, rolls up youngster's retentivity.In addition, by adding (C) composition or (D) composition as required, can give concavo-convexly to fiber surface, moderately delustring can be more suitable for using as artificial hair.In addition, use the finish of hydrophilic fibre finishing agent (E) composition, softener etc., give sense of touch, feel, can be more near the human hair.
In addition, flame-retardant polyester fibers for artificial hair of the present invention can with other artificial hair material and usefulness such as modification acrylonitrile fiber, polyvinyl chloride fibre, nylon fiber, also can and use with the human hair.
The human hair that the hair product of wig, headwear wig, postiche head etc. uses, generally carry out processing or the decolouring and the dyeing of epidermal area, owing to leading to fiber surface finishing agent, the softener that uses polysiloxane series in order to ensure sense of touch, comb, so it is different with untreated human hair, be flammable, but, show excellent flame-retardant performance by mixing human hair's ratio mixes flame-retardant polyester fibers for artificial hair of the present invention below 60% with the human hair occasion.
Embodiment
Below, according to embodiment the present invention is more specifically described, but the present invention is not subjected to these qualification.
Moreover the determination method of characteristic value is as follows.
＜comb is logical 〉
Make the tow long filament adhering fibre surface conditioning agent of length 30cm, total fiber number 100,000 dtex.The tow long filament that makes processing is estimated the easiness by comb by comb (polyformaldehyde (Derlin) resin system).
Zero: do not have resistance (gently) basically
△: some resistances (weight) are arranged
*: quite big resistance is arranged or tangle halfway.
(intensity and elongation)
Use INTESCO corporate system INTESCO Model 201 types, measure TENSILE STRENGTH, the elongation of long filament.Get 1 threads of length 40mm, use the cardboard (thin paper) post the two sides adhesive tape of sticking with paste adhesive to clamp the two ends 10mm of long filament, at an air-dry night, make the sample of length 20mm.Sample is contained on the testing machine, divides down at 24 ℃ of temperature, humidity below 80%, loading 0.034cN * fiber number (dtex), draw speed 20mm/ and test, mensuration intensity, elongation.Adopt the same terms to repeat 10 tests, with intensity and the elongation of mean value as long filament.
(anti-flammability)
Long filament is cut into the length of 150mm, ties up 0.7g, use clamp clamps one end, be fixed on the bearing support, vertically hang down.In 3 seconds of flame that make the fixed length wire connection of effective long 120mm touch 20mm, make its burning.
Flammability
◎: 0 second residual flame time (missing of ignition)
Zero: less than 3 seconds
△: 3～10 seconds
*: more than 10 seconds
Anti-dropping down property
◎: a number that goes out up to fire is 0
Below zero: 5
△：6～10
*: more than 11
(gloss)
The tow long filament of visual valuation length 30cm, total fiber number 100,000 dtex under sunshine.
◎: gloss can be transferred to the level that is equal to the human hair
Zero: gloss is transferred to appropriateness
△: some gloss are too many, and perhaps some gloss very little
*: gloss is too many, or gloss is very little
(transparency)
The tow long filament of visual valuation length 30cm, total fiber number 100,000 dtex under sunshine.
Zero: transparent feel is arranged, the coloured depth (distinctness)
△: some opaque senses (muddiness) are arranged
*: opaque sense is arranged, do not have the depth of color
(devitrification resistance)
After the tow long filament of length 10cm, total fiber number 100,000 dtex carried out steam processing (120 ℃, relative humidity 100% time 1 hour), intensive drying at room temperature.Gloss before and after the contrast steam processing, the variation of form and aspect change greatly more, and then devitrification resistance is poor more.
◎: gloss, the equal no change of form and aspect
Zero: gloss no change, form and aspect have some variations
△: gloss, form and aspect all have some variations
*: gloss, form and aspect all have obvious variation
(sense of touch)
Be clamminess
After leaving standstill 3 hours in thermostatic constant wet chamber's (23 ℃, relative humidity 55%), use the tow long filament of length 30cm, total fiber number 100,000 dtex right hand thumb, forefinger, middle finger to estimate.
Zero: do not have the sense of being clamminess
△: some senses of being clamminess are arranged
*: the sense of being clamminess is arranged
Smooth property
After leaving standstill 3 hours in thermostatic constant wet chamber's (23 ℃, relative humidity 55%), use the tow long filament of length 30cm, total fiber number 100,000 dtex right hand thumb, forefinger, middle finger to estimate.
◎: level and smooth sense is arranged, very smooth
Zero: level and smooth sense is arranged, smooth
△: smooth but slightly heavy
*: be difficult to smooth
(surface roughness)
Use laser microscope (キ one エ Application ス makes VK-9500) to measure.Calculate by the multiplying power of 3000 times (20 times on 150 times * interior dress lens of object lens) according to the calculating formula of the definition (JIS B0601-1994) of surface roughness regulation fiber side and fiber axis are measured 10 images that obtain concurrently.
(scalding qualitative)
The easy degree of using the fixing volume of hair waving pin youngster is the index of volume youngster shape retention.Long filament is clipped in the hair waving pin that is heated to 180 ℃ lightly, friction preheating 3 times, fusion, the comb between visual valuation long filament this moment is logical, curling, the fracture of wire of long filament.Then, the long filament of preheating is wrapped on the hair waving pin, kept for 10 seconds, extract hair waving pin.Visual valuation easily pulling out property (withdrawing from property of bar), the volume retentivity when pulling out at this moment.
(rolling up youngster's property surely)
The long filament that forms straw formula hair is wrapped on the pipe of diameter 32mm, under 110 ℃ temperature, rolled up youngster surely 60 minutes, at room temperature aging after 60 minutes, an end of the fixing long filament that curls, suspend in midair, visual valuation is rolled up youngster's easy degree, volume youngster's stability surely.
Zero: form volume youngster fully, stability might as well
△: form the volume youngster, but poor stability
*: form the volume youngster deficiently
(embodiment 1～15)
In the composition of the table 1 that the polyethylene terephthalate below being dried to amount of moisture 100ppm, bromination epoxy flame retardant, organic fine particles, inorganic particles are formed and ratio shown in the table 2; add painted with polyester granulate PESM 6100BLACK (Dainichiseika Color Chem's system; content of carbon black 30%; polyester is contained in (A) composition) 2 parts do and mix; supply with double screw extruder; after 280 ℃ of following melting mixings, granulating, be dried to below the amount of moisture 100ppm.Then, use melt spinning machine spinneret ejection molten polymer by the circular section spray orifice with nozzle diameter 0.5mm under 280 ℃, air cooling is pressed the speed coiling that 100m/ divides, and obtains spinning strand.In 80 ℃ tepidarium, the strand that spins that obtains is stretched, become 4 times of drawn yarns, use is heated to 200 ℃ hot-rolling, press the speed coiling that 30m/ divides, heat-treat, (CATION is a surfactant for adhering fibre finishing agent KWC-Q (epoxy ethane-epoxy propane random copolymerization polyethers, ball water chestnut oiling Co., Ltd. system) and KRE-103 respectively, Matsumoto Yushi-Seiyaku Co., Ltd.'s system) 0.20%omf makes the polyester fiber (multifilament) about filament fiber number 50dtex.
Table 1
| Embodiment | |||||||||
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | |
| EFG-85A *1 | 100 | 100 | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
| EP-200 *2 | 10 | ||||||||
| EC-200 *2 | 10 | ||||||||
| EPC-15 *2 | 10 | 15 | |||||||
| YDB-412 *3 | 10 | 15 | |||||||
| SR-T2000 *4 | 15 | ||||||||
| SR-T5000 *4 | 10 | ||||||||
| SR-T7040 *4 | 10 | ||||||||
| UPOLYMERU-100 *5 | 2 | ||||||||
| イ ペ one Network CR-60 *6 | 0.2 | 0.2 | 0.2 | ||||||
| PKP-53 *7 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | ||||
* 1: polyethylene terephthalate, clock are spun fine Co., Ltd. system of closing
* 2: end-blocking/end-sealed type bromination epoxy flame retardant not, Dainippon Ink. ﹠ Chemicals Inc's system
* 3: end-sealed type bromination epoxy flame retardant not, Toto Kasei KK's system
* 4: end-blocking/end-sealed type bromination epoxy flame retardant not, this pharmaceutical industries of slope Co., Ltd. system
* 5: polyarylate, You Niqika Co., Ltd. system
* 6: titanium oxide, Ishihara Sangyo Kaisha, Ltd.'s system
* 7: talcum, talcum Co., Ltd. of Fuji system
Table 2
| Embodiment | ||||||
| 10 | 11 | 12 | 13 | 14 | 15 | |
| EFG-85A *1 | 100 | 100 | 100 | 100 | 100 | 100 |
| XAC-4965 *9 | 15 | |||||
| SR-T20000 *10 | 12 | 16 | ||||
| YPB-43M *11 | 5 | 10 | 15 | |||
| UPOLYMERU-100 *5 | 2 | |||||
| PKP-53 *7 | 0.6 | 0.6 | ||||
* 1: polyethylene terephthalate, clock are spun fine Co., Ltd. system of closing
* 9: end-sealed type bromination epoxy flame retardant not, Asahi Chemical Industry Co., Ltd's system
* 10: end-sealed type bromination epoxy flame retardant not, number-average molecular weight 30000, this pharmaceutical industries of slope Co., Ltd. system
* 11: end-sealed type bromination epoxy flame retardant not, number-average molecular weight 40000, Toto Kasei KK's system
* 5: polyarylate, You Niqika Co., Ltd. system
* 7: talcum, talcum Co., Ltd. of Fuji system
The estimation of fibres intensity that use is made, elongation, anti-flammability, gloss, the transparency, devitrification resistance, comb are logical, sense of touch, surface roughness, scald result qualitative, that roll up youngster's property surely and be illustrated in table 3, table 4.
Table 3
| Comparative example | ||||||||
| 1 | 2 | 3 | 4 | 5 | ||||
| Nozzle form | Just round | Just round | Just round | Just round | Just round | |||
| Fiber number (dtex) | 52 | 48 | 47 | 47 | 50 | |||
| Fibre finish adhesion amount (%omf) | KWC-Q | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | ||
| KRE-103 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | |||
| Intensity (cN/dtex) | 2.2 | 2.0 | 1.9 | 2.9 | 2.6 | |||
| Elongation (%) | 68 | 63 | 42 | 52 | 47 | |||
| Anti-flammability | Flammability | △ | △ | ○ | ◎ | ◎ | ||
| Anti-dropping down property | × | × | × | ◎ | ◎ | |||
| Gloss | × | △ | △ | ◎ | × | |||
| The transparency | △ | △ | △ | × | △ | |||
| Devitrification resistance | △ | △ | × | △ | △ | |||
| Comb is logical | × | × | △ | △ | × | |||
| Sense of touch | Be clamminess | × | × | × | ○ | × | ||
| Smooth property | × | × | × | ○ | × | |||
| Surface roughness | Arithmetic average roughness (μ m) | 0.1 | 0.6 | 0.5 | 1.2 | 0.1 | ||
| 10 mean roughness (μ m) | 0.1 | 0.4 | 0.4 | 0.5 | 0.4 | |||
| Scald fixed (180 ℃) | Fusion | ○ | ○ | ○ | ○ | ○ | ||
| Curl/fracture of wire | ○ | ○ | ○ | ○ | ○ | |||
| Bar withdraws from | ○ | ○ | ○ | ○ | ○ | |||
| Constancy | ○ | ○ | ○ | ○ | ○ | |||
| Surely roll up youngster's property (110 ℃) | ○ | ○ | ○ | ○ | ○ | |||
Table 4
| Comparative example | ||||||||
| 1 | 2 | 3 | 4 | 5 | ||||
| Nozzle form | Just round | Just round | Just round | Just round | Just round | |||
| Fiber number (dtex) | 52 | 48 | 47 | 47 | 50 | |||
| Fibre finish adhesion amount (%omf) | KWC-Q | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | ||
| KRE-103 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | |||
| Intensity (cN/dtex) | 2.2 | 2.0 | 1.9 | 2.9 | 2.6 | |||
| Elongation (%) | 68 | 63 | 42 | 52 | 47 | |||
| Anti-flammability | Flammability | △ | △ | ○ | ◎ | ◎ | ||
| Anti-dropping down property | × | × | × | ◎ | ◎ | |||
| Gloss | × | △ | △ | ◎ | × | |||
| The transparency | △ | △ | △ | × | △ | |||
| Devitrification resistance | △ | △ | × | △ | △ | |||
| Comb is logical | × | × | △ | △ | × | |||
| Sense of touch | Be clamminess | × | × | × | ○ | × | ||
| Smooth property | × | × | × | ○ | × | |||
| Surface roughness | Arithmetic average roughness (μ m) | 0.1 | 0.6 | 0.5 | 1.2 | 0.1 | ||
| 10 mean roughness (μ m) | 0.1 | 0.4 | 0.4 | 0.5 | 0.4 | |||
| Scald fixed (180 ℃) | Fusion | ○ | ○ | ○ | ○ | ○ | ||
| Curl/fracture of wire | ○ | ○ | ○ | ○ | ○ | |||
| Bar withdraws from | ○ | ○ | ○ | ○ | ○ | |||
| Constancy | ○ | ○ | ○ | ○ | ○ | |||
| Surely roll up youngster's property (110 ℃) | ○ | ○ | ○ | ○ | ○ | |||
(comparative example 1～5)
Shown in the table 5 that polyethylene terephthalate below being dried to amount of moisture 100ppm, bromination epoxy flame retardant, inorganic particles are formed in the composition of ratio; add painted with polyester granulate PESM 6100 BLACK (Dainichiseika Color Chem's system; content of carbon black 30%; polyester is contained in (A) composition) 2 parts do and mix; supply with double screw extruder; at 280 ℃ of following melting mixings, after the granulating, be dried to below the amount of moisture 100ppm.Then, use melt spinning machine at 280 ℃ of spinneret ejection molten polymers by the circular section spray orifice with nozzle diameter 0.5mm, air cooling is pressed the speed coiling that 100m/ divides, and obtains spinning strand.In 80 ℃ tepidarium, the strand that spins that obtains is stretched, become 4 times of drawn yarns, use is heated to 200 ℃ hot-rolling, press the speed coiling that 30m/ divides, heat-treat, adhering fibre finishing agent KWC-Q (epoxy ethane-epoxy propane random copolymerization polyethers, ball water chestnut oiling Co., Ltd. system) and KRE-103 (CATION is a surfactant, Matsumoto Yushi-Seiyaku Co., Ltd.'s system) 0.20%omf make the polyester fiber (multifilament) about filament fiber number 50dtex respectively.
The estimation of fibres intensity that use is made, elongation, anti-flammability, gloss, the transparency, devitrification resistance, comb are logical, sense of touch, surface roughness, scald qualitative, roll up the table 6 that the results are shown in of youngster's property surely.
Table 5
| Comparative example | |||||
| 1 | 2 | 3 | 4 | 5 | |
| EFG-85A *1 | 100 | 100 | 100 | 100 | |
| Triphenyl phosphate | 10 | ||||
| PX-200 *12 | 10 | ||||
| ハイムRH-416 *13 | 100 | ||||
| パイロチエツク68PB *14 | 6 | ||||
| FR-1808 *15 | 10 | ||||
| イ ペ one Network CR-60 *6 | 1 | ||||
* 1: polyethylene terephthalate, clock are spun fine Co., Ltd. system of closing
* 12: condensed phosphoric acid esters flame retardant, Daihachi Chemical Industry Co., Ltd.'s system
* 13: phosphorus flame retardant copolymerized type polyester, Toyo Boseki K.K's system
* 14: brominated Polystyrene flame retardant, daily output Off エ ロ one Co., Ltd.'s system
* 15: eight bromine trimethylphenyl indanes, Block ロ system ケ system Off ア one イ one ス ト (strain) system
* 6: titanium oxide, Ishihara Sangyo Kaisha, Ltd.'s system
Table 6
| Comparative example | ||||||||
| 1 | 2 | 3 | 4 | 5 | ||||
| Nozzle form | Just round | Just round | Just round | Just round | Just round | |||
| Fiber number (dtex) | 52 | 48 | 47 | 47 | 50 | |||
| Fibre finish adhesion amount (%omf) | KWC-Q | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | ||
| KRE-103 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | |||
| Intensity (cN/dtex) | 2.2 | 2.0 | 1.9 | 2.9 | 2.6 | |||
| Elongation (%) | 68 | 63 | 42 | 52 | 47 | |||
| Anti-flammability | Flammability | △ | △ | ○ | ◎ | ◎ | ||
| Anti-dropping down property | × | × | × | ◎ | ◎ | |||
| Gloss | × | △ | △ | ◎ | × | |||
| The transparency | △ | △ | △ | × | △ | |||
| Devitrification resistance | △ | △ | × | △ | △ | |||
| Comb is logical | × | × | △ | △ | × | |||
| Sense of touch | Be clamminess | × | × | × | ○ | × | ||
| Smooth property | × | × | × | ○ | × | |||
| Surface roughness | Arithmetic average roughness (μ m) | 0.1 | 0.6 | 0.5 | 1.2 | 0.1 | ||
| 10 mean roughness (μ m) | 0.1 | 0.4 | 0.4 | 0.5 | 0.4 | |||
| Scald fixed (180 ℃) | Fusion | ○ | ○ | ○ | ○ | ○ | ||
| Curl/fracture of wire | ○ | ○ | ○ | ○ | ○ | |||
| Bar withdraws from | ○ | ○ | ○ | ○ | ○ | |||
| Constancy | ○ | ○ | ○ | ○ | ○ | |||
| Surely roll up youngster's property (110 ℃) | ○ | ○ | ○ | ○ | ○ | |||
Shown in table 3 and table 4, opposite with comparative example, confirm that anti-flammability, gloss, the transparency, devitrification resistance, the comb among the embodiment is logical, sense of touch, scald qualitative, to roll up youngster's property surely good.Therefore, the artificial hair fiber of current use bromination epoxy flame retardant, compare with fiber with the artificial hair that uses phosphonium flame retardant in the past, affirmation can be effectively as mechanical property, the thermal characteristics of still keeping polyester, anti-flammability, gloss, the transparency, constancy, devitrification resistance, the logical improved artificial hair of comb.
(embodiment 16～22)
Shown in the table 7 that polyethylene terephthalate below being dried to amount of moisture 100ppm, bromination epoxy flame retardant, inorganic particles are formed in the composition of ratio; add painted with polyester granulate PESM 6100 BLACK (Dainichiseika Color Chem's system; content of carbon black 30%; polyester is contained in (A) composition) 2 parts do and mix; supply with double screw extruder; after 280 ℃ of melting mixings, granulating, be dried to below the amount of moisture 100ppm.Then, use melt spinning machine at 280 ℃ of spinning heads ejection molten polymers by spray orifice with the cross sectional shape that becomes Fig. 8～10, air cooling, the speed of dividing by 100m/ is reeled to make and is spun strand.In 80 ℃ tepidarium, the strand that spins that makes is stretched, become 4 times of drawn yarns, use is heated to 200 ℃ hot-rolling, press the speed coiling that 30m/ divides, heat-treat, (CATION is a surfactant for adhering fibre finishing agent KWC-Q (epoxy ethane-epoxy propane random copolymerization polyethers, ball water chestnut oiling Co., Ltd. system) and KRE-103 respectively, Matsumoto Yushi-Seiyaku Co., Ltd.'s system) 0.20%omf makes the polyester fiber (multifilament) about filament fiber number 60～70dtex.
Table 7
| Embodiment | |||||||
| 16 | 17 | 18 | 19 | 20 | 21 | 22 | |
| EFG-85A *1 | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
| SR-T20000 *10 | 10 | 10 | 10 | 10 | 10 | ||
| YPB-43M *11 | 15 | 15 | |||||
| PKP-53 *7 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | ||
| イムシルA-8 *16 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | ||
* 1: polyethylene terephthalate, clock are spun fine Co., Ltd. system of closing
* 10: end-sealed type bromination epoxy flame retardant not, number-average molecular weight 30000, this pharmaceutical industries of slope Co., Ltd. system
* 11: end-sealed type bromination epoxy flame retardant not, number-average molecular weight 40000, Toto Kasei KK's system
* 7: talcum, talcum Co., Ltd. of Fuji system
* 16: silica, UNIMIN corporate system
(in (Fig. 8), A is 0.9mm, and B is 0.4mm)
(in (Fig. 9), A is 1.0mm, and B is 0.35mm, and C is 0.25mm)
(in (Figure 10), R is 0.6mm, and r is 0.4mm)
The estimation of fibres intensity that use is made, elongation, anti-flammability, gloss, the transparency, devitrification resistance, comb are logical, sense of touch, surface roughness, scald qualitative, roll up the table 8 that the results are shown in of youngster's property surely.
Table 8
| Embodiment | ||||||||||
| 16 | 17 | 18 | 19 | 20 | 21 | 22 | ||||
| Nozzle form | Abnormity 1 | Abnormity 2 | Abnormity 3 | Abnormity 1/ is circle=67/33 just | Abnormity 1/ just justifies 50/50 | Abnormity 1 | Abnormity 2 | |||
| Fiber number (dtex) | 67 | 65 | 68 | 62 | 59 | 70 | 68 | |||
| Fibre finish adhesion amount (%omf) | KWC-Q | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | ||
| KRE-103 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | |||
| Intensity (cN/dtex) | 2.5 | 2.2 | 1.8 | 2.7 | 2.9 | 2.4 | 2.2 | |||
| Elongation (%) | 68 | 53 | 38 | 59 | 52 | 53 | 48 | |||
| Anti-flammability | Flammability | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ | ||
| Anti-dropping down property | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ | |||
| Gloss | ○ | ○ | ○ | ○ | ○ | ◎ | ◎ | |||
| The transparency | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |||
| Devitrification resistance | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |||
| Comb is logical | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |||
| Sense of touch | Be clamminess | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ||
| Smooth property | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ | |||
| Surface roughness | Arithmetic average roughness (μ m) | 1.0 | 1.0 | 1.1 | 1.0 | 1.1 | 1.4 | 1.3 | ||
| 10 mean roughness (μ m) | 0.8 | 0.9 | 0.8 | 0.7 | 0.8 | 1.1 | 1.1 | |||
| Scald fixed (180 ℃) | Fusion | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ||
| Curl/fracture of wire | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |||
| Bar withdraws from | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |||
| Constancy | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |||
| Surely roll up youngster's property (110 ℃) | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |||
(embodiment 23～29)
Shown in the table 9 that polyethylene terephthalate below being dried to amount of moisture 100ppm, bromination epoxy flame retardant, inorganic particles are formed in the composition of ratio; add painted with polyester granulate PESM 6100 BLACK (Dainichiseika Color Chem's system; content of carbon black 30%; polyester is contained in (A) composition) 2 parts do and mix; supply with double screw extruder; at 280 ℃ of melting mixings, after the granulating, be dried to below the amount of moisture 100ppm.Then, use melt spinning machine 280 ℃ by spinneret ejection molten polymer with the spray orifice that becomes Fig. 8,9 cross sectional shape, air cooling press the speed coiling that 100m/ divides, and makes and spins strand.In 80 ℃ tepidarium, the strand that spins that makes is stretched, become 4 times of drawn yarns, use the hot-rolling that is heated to 200 ℃, press the speed coiling that 30m/ divides, heat-treat, adhere to the fibre finish shown in the table 10 respectively, make the polyester fiber (multifilament) about filament fiber number 70dtex.
Table 9
| Embodiment | |||||||
| 23 | 24 | 25 | 26 | 27 | 28 | 29 | |
| EFG-85A *1 | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
| SR-T20000 *10 | 16 | 16 | 16 | 16 | 16 | ||
| YPB-43M *11 | 15 | 15 | |||||
| PKP-53 *7 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | ||
* 1: polyethylene terephthalate, clock are spun fine Co., Ltd. system of closing
* 10: end-sealed type bromination epoxy flame retardant not, number-average molecular weight 30000, this pharmaceutical industries of slope Co., Ltd. system
* 11: end-sealed type bromination epoxy flame retardant not, number-average molecular weight 40000, Toto Kasei KK's system
* 7: talcum, talcum Co., Ltd. of Fuji system
Table 10
| Embodiment | ||||||||||
| 23 | 24 | 25 | 26 | 27 | 28 | 29 | ||||
| Nozzle form | Abnormity 1 | Abnormity 1 | Abnormity 1 | Abnormity 1 | Abnormity 1 | Abnormity 2 | Abnormity 2 | |||
| Fiber number (dtex) | 70 | 70 | 70 | 70 | 70 | 68 | 68 | |||
| Fibre finish adhesion amount (%omf) | KWC-Q *17 | 0.1 | 0.2 5 | 0.1 5 | 0.1 | |||||
| KRE-103 *18 | 0.1 | 0.1 | ||||||||
| KRE-102 *19 | 0.2 | 0.1 | ||||||||
| KRE-15 *20 | 0.2 | 0.1 | 0.1 | |||||||
| KRE-16 *21 | 0.1 4 | 0.0 7 | 0.0 7 | |||||||
| KRE-17 *22 | 0.0 6 | 0.0 3 | 0.0 3 | |||||||
| Intensity (cN/dtex) | 2.5 | 2.5 | 2.5 | 2.5 | 2.5 | 2.4 | 2.4 | |||
| Elongation (%) | 54 | 54 | 54 | 54 | 54 | 48 | 48 | |||
| Anti-flammability | Flammability | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ | ||
| Anti-dropping down property | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ | |||
| Gloss | ○ | ○ | ○ | ○ | ○ | ◎ | ◎ | |||
| The transparency | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |||
| Devitrification resistance | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |||
| Comb is logical | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |||
| Sense of touch | Be clamminess | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ||
| Smooth property | ○ | ◎ | ○ | ◎ | ○ | ○ | ○ | |||
| Surface roughness | Arithmetic average roughness (μ m) | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.4 | 1.4 | ||
| 10 mean roughness (μ m) | 0.8 | 0.8 | 0.8 | 0.8 | 0.8 | 1.1 | 1.1 | |||
| Scald fixed (180 ℃) | Fusion | ○ | ○ | ○ | ○ | ○ | ○ | ○ | ||
| Curl/fracture of wire | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |||
| Bar withdraws from | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |||
| Constancy | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |||
| Surely roll up youngster's property (110 ℃) | ○ | ○ | ○ | ○ | ○ | ○ | ○ | |||
In addition, shown in table 8 and table 10, by with fibre section shape heteromorphosis or use specific fibre finish, confirm to make rerum natura, artificial hair fiber that the quality balance is good again.
The possibility of utilizing on the industry
The object of the invention is to solve aforementioned problem in the past, the fibrous physical properties such as the heat resistance of keeping common polyester fiber, intensity, elongation are provided, the desired anti-flammability of artificial hair, constancy, anti-dropping down property, the transparency, devitrification resistance, be clamminess, comb and have friendly relations, again the controlled flame-retardant polyester fibers for artificial hair of the gloss of fiber as requested.
In addition, above-mentioned polyester fiber is the artificial hair polyester fiber that at least a kind of odd-shaped cross section shape is arranged, that the fibre section is the composite fibre of odd-shaped cross section shape, it is 8: 2～1: 9 artificial hair polyester fiber by the mixing ratio of using circular cross-section/odd-shaped cross section, make the fibrous physical property of the heat resistance of keeping polyester fiber, intensity, elongation etc., improve the shortcoming of volume youngster characteristic, the artificial hair polyester fiber that gloss, sense of touch and comb are had friendly relations.
In addition, to improve smooth sense of touch or feel etc. as purpose, do not cause that the anti-flammability when similar use polysiloxane series fibre finish is processed reduces, and the anti-flammability artificial hair fiber with smooth sense of touch equal when using the polysiloxane series finish to process, cardability, good flame resistance is provided.
Claims (23)
1. flame-retardant polyester fibers for artificial hair, it is formed by polyester (A) 100 weight portions and bromination epoxy flame retardant (B) 5～30 weight portions, and it is a kind of copolyester of main body or more kinds of that described polyester (A) contains polyalkylene terephthalates or polyalkylene terephthalates.
2. the described flame-retardant polyester fibers for artificial hair of claim 1, wherein, (B) composition is the number-average molecular weight 20000 of following general formula (1) expression or higher bromination epoxy flame retardant (B1), at fiber surface fine projection is arranged.
3. the described flame-retardant polyester fibers for artificial hair of claim 1, wherein, (A) composition is the polyester that contains at least a kind of polymer that is selected from polyethylene terephthalate, polytrimethylene terephthalate and polybutylene terephthalate (PBT).
4. claim 1 or 3 described flame-retardant polyester fibers for artificial hair, wherein, (B) composition is at least a kind of fire retardant that is selected from the bromination epoxy flame retardant of general formula (2)～(4) expression,
In the formula, m represents 0～29,
In the formula, R
1Expression C
1-10Alkyl, n represents 0～100.
5. claim 1 or 2 described flame-retardant polyester fibers for artificial hair, wherein, (B1) composition is at least a kind of fire retardant that is selected from the bromination epoxy flame retardant of general formula (5)～(7) expression,
In the formula, m represents 30～150,
In the formula, R
1Expression C
1-10Alkyl, n represents 30～100,
In the formula, R
2Expression C
1-10Alkyl, p represents 30～100, y represents 0～5.
6. claim 2,3, any one described flame-retardant polyester fibers for artificial hair of 5, wherein, the projection on aforementioned fibers surface is unbodied.
7. claim 2,3,5, any one described flame-retardant polyester fibers for artificial hair of 6, wherein, the size of the projection on aforementioned fibers surface is the scope of major diameter 0.2～20 μ m, minor axis 0.1～10 μ m, high 0.1～2 μ m.
8. the described flame-retardant polyester fibers for artificial hair of any one of claim 1～7, wherein, by (A) with (B) composition, mix the fiber surface that composition that organic fine particles (C) and/or inorganic particles (D) obtain forms again fine projection arranged.
9. the described flame-retardant polyester fibers for artificial hair of claim 8, wherein, (C) composition is to be selected from polyarylate, polyamide, fluororesin, silicones, crosslinked acrylic resin, crosslinked polystyrene at least a kind.
10. the described flame-retardant polyester fibers for artificial hair of claim 8, wherein, (D) composition is to be selected from calcium carbonate, silica, titanium oxide, aluminium oxide, zinc oxide, talcum, kaolin, imvite, bentonite, mica at least a kind.
11. flame-retardant polyester fibers for artificial hair, wherein, the cross section of the described flame-retardant polyester fibers for artificial hair of any one of claim 1～10 have be selected from ellipse, intersect circle, cocoon shape, big tripe shape, dog bone shape, be with at least a kind of odd-shaped cross section shape of shape, 3～8 leaf, star.
12. the described artificial hair polyester fiber of claim 11, wherein, the fibre section is the shape that circle more than 2 or flat circular portion ground overlap or joins.
13. the described artificial hair polyester fiber of claim 11, wherein, the fibre section is 3～8 leaf, and described fiber is the profiled fibre of the degree of profile of formula (1) expression in 1.1～8 scope.
Formula 1
Degree of profile=(the external diameter of a circle in filament cross section)/(diameter of the inscribed circle in filament cross section)
14. the described artificial hair polyester fiber of claim 11, wherein, the aspect ratio of fibre section is 1.2～4.
15. the described flame-retardant polyester fibers for artificial hair of claim 11, it is the blended fiber that the fibre section is selected from least a kind of odd-shaped cross section shape of circle, ellipse, intersection circle, cocoon shape, big tripe shape, dog bone shape, band shape, 3～8 leaf, star, and the mixing ratio of circular cross-section/odd-shaped cross section is 8: 2～1: 9.
16. flame-retardant polyester fibers for artificial hair adheres to hydrophilic fibre finishing agent (E) and obtains on the described flame-retardant polyester fibers for artificial hair of any one of its claim 1～15.
17. the described flame-retardant polyester fibers for artificial hair of claim 16, wherein, (E) composition is be selected from polyethers based compound, fatty acid ester based compound, organic amine, organic amide, organic fatty acid esters, organic amine salt, organic ammonium salt, organic pyridinium salt, organic ammonium salt, organic pyridinium salt, organic picoline salt, organic fatty hydrochlorate, rosinate, organic sulfonate, organic succinate salt, organic succinic monoester salt, organic carboxylate, organo-sulfate salt, organophosphorus ester salt at least a.
18. claim 1,2 and 16 described flame-retardant polyester fibers for artificial hair, wherein, (E) composition is to be selected from polyoxyalkylene alkyl, polyoxyalkylene alkenyl ether, polyoxyalkylene aryl ether, these random copolymerization polyethers, polyoxyalkylene alkyl aryl ether, polyoxyalkylene Arrcostab, polyoxyalkylene alkenyl ester, polyoxyalkylene alkyl aryl ester at least a.
19. the described flame-retardant polyester fibers for artificial hair of claim 16, wherein, (E) composition is at least a of the random copolymerization polyethers (molecular weight MW 15000～50000) that is selected from epoxy ethane-epoxy propane, poly(ethylene oxide) (molecular weight 100～1000), poly(propylene oxide) (molecular weight 100～1000).
20. the described flame-retardant polyester fibers for artificial hair of any one of claim 5 and claim 16～19 wherein, adheres to (E) composition to fiber, making it is 0.01%～1% by weight.
21. the described flame-retardant polyester fiber of any one of claim 1～20 is characterized in that, flame-retardant polyester fiber is a non-crimping raw silk shape.
22. the described flame-retardant polyester fibers for artificial hair of any one of claim 1～21 is characterized in that flame-retardant polyester fiber is a solution dyeing.
23. the described flame-retardant polyester fibers for artificial hair of any one of claim 1～22, wherein, the filament fiber number is 30～80dtex.
Applications Claiming Priority (9)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2003201875A JP2005042234A (en) | 2003-07-25 | 2003-07-25 | Flame-retardant polyester-based fiber for artificial hair |
| JP201875/2003 | 2003-07-25 | ||
| JP358314/2003 | 2003-10-17 | ||
| JP2003358314A JP2005120533A (en) | 2003-10-17 | 2003-10-17 | Polyester-based fiber for artificial hair |
| JP2003408325A JP2005171391A (en) | 2003-12-05 | 2003-12-05 | Artificial hair fiber |
| JP408325/2003 | 2003-12-05 | ||
| JP081033/2004 | 2004-03-19 | ||
| JP2004081033A JP2005264397A (en) | 2004-03-19 | 2004-03-19 | Flame-retardant polyester-based artificial hair fiber |
| PCT/JP2004/010740 WO2005010247A1 (en) | 2003-07-25 | 2004-07-20 | Flame-retardant polyester fibers for artificial hair |
Related Child Applications (5)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010156479A Division CN101864613A (en) | 2003-07-25 | 2004-07-20 | Hair product |
| CNA2008100930202A Division CN101250768A (en) | 2003-07-25 | 2004-07-20 | Flame retardant polyester fiber for artificial hair |
| CNA200810093019XA Division CN101250767A (en) | 2003-07-25 | 2004-07-20 | Flame retardant polyester fiber for artificial hair |
| CNA2008101315018A Division CN101358386A (en) | 2003-07-25 | 2004-07-20 | Flame-retardant polyester fibers for artificial hair |
| CNA2008100930185A Division CN101250766A (en) | 2003-07-25 | 2004-07-20 | Flame retardant polyester fiber for artificial hair |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1826436A true CN1826436A (en) | 2006-08-30 |
| CN1826436B CN1826436B (en) | 2010-06-16 |
Family
ID=34261807
Family Applications (5)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100930202A Pending CN101250768A (en) | 2003-07-25 | 2004-07-20 | Flame retardant polyester fiber for artificial hair |
| CN2004800210767A Expired - Lifetime CN1826436B (en) | 2003-07-25 | 2004-07-20 | Flame-retardant polyester fibers for artificial hair |
| CNA200810093019XA Pending CN101250767A (en) | 2003-07-25 | 2004-07-20 | Flame retardant polyester fiber for artificial hair |
| CNA2008101315018A Pending CN101358386A (en) | 2003-07-25 | 2004-07-20 | Flame-retardant polyester fibers for artificial hair |
| CNA2008100930185A Pending CN101250766A (en) | 2003-07-25 | 2004-07-20 | Flame retardant polyester fiber for artificial hair |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100930202A Pending CN101250768A (en) | 2003-07-25 | 2004-07-20 | Flame retardant polyester fiber for artificial hair |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200810093019XA Pending CN101250767A (en) | 2003-07-25 | 2004-07-20 | Flame retardant polyester fiber for artificial hair |
| CNA2008101315018A Pending CN101358386A (en) | 2003-07-25 | 2004-07-20 | Flame-retardant polyester fibers for artificial hair |
| CNA2008100930185A Pending CN101250766A (en) | 2003-07-25 | 2004-07-20 | Flame retardant polyester fiber for artificial hair |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JP2005042234A (en) |
| CN (5) | CN101250768A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101376690B (en) * | 2007-08-30 | 2011-06-15 | 中国石化上海石油化工股份有限公司 | Preparation of flame-retardant polyester for preparing fiber |
| CN102732982A (en) * | 2012-06-21 | 2012-10-17 | 精源(南通)化纤制品有限公司 | Microbending treatment method for polytrimethylene terephthalate (PTT) protofilament for artificial hair |
| CN103501647A (en) * | 2011-05-13 | 2014-01-08 | 电气化学工业株式会社 | Fiber for artificial hair, and hairpiece product |
| CN105263348A (en) * | 2013-06-06 | 2016-01-20 | 株式会社钟化 | Fiber for artificial hair, and head decoration article including same |
| CN108882764A (en) * | 2016-04-13 | 2018-11-23 | 电化株式会社 | Artificial hair resin combination and its formed body |
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| JP4742760B2 (en) * | 2004-09-07 | 2011-08-10 | 株式会社カネカ | Flame retardant polyester artificial hair |
| WO2006028102A1 (en) | 2004-09-07 | 2006-03-16 | Kaneka Corporation | Artificial hair made of flame-retardant polyester |
| JPWO2006107028A1 (en) * | 2005-04-04 | 2008-09-25 | 株式会社カネカ | Artificial hair |
| JP4679954B2 (en) * | 2005-04-26 | 2011-05-11 | 株式会社カネカ | Artificial hair fiber |
| WO2007049561A1 (en) * | 2005-10-28 | 2007-05-03 | Kaneka Corporation | Polyester-based artificial hair |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4732921A (en) * | 1986-12-05 | 1988-03-22 | Hoechst Celanese Corporation | Flame retardant polybutylene terephthalate |
-
2003
- 2003-07-25 JP JP2003201875A patent/JP2005042234A/en active Pending
-
2004
- 2004-07-20 CN CNA2008100930202A patent/CN101250768A/en active Pending
- 2004-07-20 CN CN2004800210767A patent/CN1826436B/en not_active Expired - Lifetime
- 2004-07-20 CN CNA200810093019XA patent/CN101250767A/en active Pending
- 2004-07-20 CN CNA2008101315018A patent/CN101358386A/en active Pending
- 2004-07-20 CN CNA2008100930185A patent/CN101250766A/en active Pending
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| CN101376690B (en) * | 2007-08-30 | 2011-06-15 | 中国石化上海石油化工股份有限公司 | Preparation of flame-retardant polyester for preparing fiber |
| CN103501647A (en) * | 2011-05-13 | 2014-01-08 | 电气化学工业株式会社 | Fiber for artificial hair, and hairpiece product |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN101250766A (en) | 2008-08-27 |
| CN101250767A (en) | 2008-08-27 |
| CN101250768A (en) | 2008-08-27 |
| CN1826436B (en) | 2010-06-16 |
| CN101358386A (en) | 2009-02-04 |
| JP2005042234A (en) | 2005-02-17 |
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