CN1147627C - Polyester yarn and method for production thereof - Google Patents

Polyester yarn and method for production thereof

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Publication number
CN1147627C
CN1147627C CNB008022550A CN00802255A CN1147627C CN 1147627 C CN1147627 C CN 1147627C CN B008022550 A CNB008022550 A CN B008022550A CN 00802255 A CN00802255 A CN 00802255A CN 1147627 C CN1147627 C CN 1147627C
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China
Prior art keywords
polyester filament
dtex
yarn
modulus
preparation
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Expired - Fee Related
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CNB008022550A
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Chinese (zh)
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CN1327492A (en
Inventor
¿
望月克彦
菅埜幸治
ƽ
前田裕平
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Toray Industries Inc
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Toray Industries Inc
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Publication of CN1327492A publication Critical patent/CN1327492A/en
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    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/40Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the structure of the yarns or threads
    • D03D15/41Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the structure of the yarns or threads with specific twist
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G1/00Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
    • D02G1/02Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02JFINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J1/00Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
    • D02J1/08Interlacing constituent filaments without breakage thereof, e.g. by use of turbulent air streams
    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/20Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
    • D03D15/283Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads synthetic polymer-based, e.g. polyamide or polyester fibres
    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/50Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads
    • D03D15/567Shapes or effects upon shrinkage
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2331/00Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/04Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00Physical properties
    • D10B2401/04Heat-responsive characteristics
    • D10B2401/046Shape recovering or form memory
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00Physical properties
    • D10B2401/06Load-responsive characteristics
    • D10B2401/061Load-responsive characteristics elastic

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Artificial Filaments (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Woven Fabrics (AREA)

Abstract

The present invention relates to polyester yarn which is characterized in that it is a multifilament yarn substantially comprising polytrimethylene terephthalate, and as well as the strength from the stress-strain curve being at least 3 cN/dtex and the Young's modulus being no more than 25 cN/dtex, the minimum value of the differential Young's modulus at 3-10% extension is no more than 10 cN/dtex and the elastic recovery following 10% elongation is at least 90%. Furthermore, said polyester yarn can be obtained by a method of producing polyester yarn which is characterized in that multifilament yarn obtained by the melt spinning of polymer substantially comprising polytrimethylene terephthalate of intrinsic viscosity eta at least 0.7 is hauled-off at a spinning rate of at least 2000 m/min and, without winding up, subjected to drawing and heat-treatment, after which it is continuously subjected to a relaxation heat treatment at a relaxation factor of 6 to 20% and wound up as a package. Moreover, the present invention also relates to a woven material of outstanding soft-stretchability which is characterized in that the aforesaid polyester yarn is used as the warp yarn and/or the weft yarn in the form of twisted yarn of twist coefficient 10,000 to 20,000. In this way, it is possible to produce yarn stably at a high yarn production rate without package tightening occurring, and, as well as there being little variation in properties in the fibre lengthwise direction, when made into fabric, said fabric stretches at low modulus so there is little sense of tightness, and it is possible to provide polyester yarn and woven materials with a soft handle.

Description

Polyester Filament, its preparation method and the fabric that uses it
Invention field
The present invention relates to Polyester Filament that forms by polytrimethylene terephthalate and preparation method thereof, relate to Polyester Filament that has following feature and preparation method thereof in detail, promptly in high speed throwing process, do not have lock seam, throwing stably is because the rerum natura deviation of fiber on vertically is little, meanwhile, flexible during the system cloth and silk with low modulus, so fastening sense is little, have soft hand feeling.
Background of invention
Resilience excellence behind the polytrimethylene terephthalate elongate fiber, Young's modulus are low, have soft flexural property, and meanwhile, dyeability is good, chemically has and the same stable properties of polyethylene terephthalate.Therefore, as at United States Patent (USP) the 3rd, 584, seen in No. 103 communiques and the 3rd, 681, No. 188 communiques of United States Patent (USP) etc., very early since just research used as the material of clothes.
But because raw material 1, the ammediol price is higher, does not use so be made into synthetic fiber as yet.
In recent years, disclosed in No. 691 specifications etc. as United States Patent (USP) the 5th, 304, owing to found 1 of cheapness, the synthetic method of ammediol is so the price of polytrimethylene terephthalate fiber can be estimated again.
But, work through the inventor, find that the polytrimethylene terephthalate fiber directly adopts when normally used two step method prepares in the dacron fibre, after the spinning, internal structure changes immediately, cause the different of internal structure change amount in tow internal layer and the skin by the effect that is called so-called lock seam phenomenon, cause the difference of rerum natura, so can not make stay-in-grade fiber.
In addition, as the method that addresses this problem, the spy opens and has proposed in the clear 52-8123 communique spinning process and stretching process are carried out continuously, adopts the method for fibrous inner structure being carried out the DSD of heat fixation before coiling.But,, can not control the lock seam phenomenon fully even adopted this method.
Goal of the invention
The purpose of this invention is to provide does not have lock seam, makes stay-in-grade tow in silk producing procedures, meanwhile, in the resilience scope, Polyester Filament of low, the soft elasticity of Young's modulus, flexibility excellence and preparation method thereof.
Disclosure of the Invention
For solving aforesaid problem, Polyester Filament of the present invention has following composition.The Polyester Filament that promptly the present invention relates to comes down to the compound silk that formed by polytrimethylene terephthalate, this has following feature, promptly be more than the 3cN/dtex in the intensity on the load-deformation curve, Young's modulus is below the 25cN/dtex, meanwhile, percentage elongation is that the minimum of a value of 3~10% differential Young's modulus is that 10cN/dtex is following, the rebound degree after 10% elongation is more than 90%.In addition, this Polyester Filament can be made by the manufacture method with following feature, being about to inherent viscosity [η] is that polymer more than 0.7, that come down to be made up of polytrimethylene terephthalate carries out melt spinning, divide above spinning speed traction with the compound silk that obtains with 2000m/, then do not reel and after continuously elongated, the heat treatment, the heat treatment that relaxes continuously of relaxation rate with 6~20% is wound into package.
Have, fabric of the present invention has following structure again.That is, it is 10000~20000 twist yarn that above-mentioned Polyester Filament is twisted with the fingers into the twist, makes gauze and/or weft yarn comes usefulness, has excellent gentle flexible fabric as feature.
The accompanying drawing summary
Fig. 1: be the schematic diagram of spin-drawing device one example that makes Polyester Filament usefulness of the present invention.
Fig. 2: be another the routine schematic diagram of spin-drawing device that makes Polyester Filament usefulness of the present invention.
Fig. 3: the load-deformation curve and the differential Young's modulus-strain curve of the present invention's (embodiment 1) Polyester Filament.
Fig. 4: the load-deformation curve of the Polyester Filament of (comparative example 4) and differential Young's modulus-strain curve beyond the present invention.
Symbol description
1: spinning-nozzle
2: ventilator
3: the oiling guide groove
4: the first hot-rollings
5: the second hot-rollings
6: cold roller
7: spinnerets interweaves
8: winder
Detailed Description Of The Invention
Polyester capillaries of the present invention is in fact the composite filament that is formed by PTT.
Among the present invention, consist of the polyester of polyester capillaries, its Component units at least 90mol% is take terephthalic acid (TPA) as main acid constituents, the PTT (PTT made in following brief note) that the diol component take 1,3-PD as the master makes. Here, also can contain 10mol%, preferably contain the copolymer composition that other following ester bond of 6mol% forms. But can enumerate such as glycols such as omega-dicarboxylic acids, ethylene glycol, diethylene glycol (DEG), dipropylene glycol, butanediol, neopentyl glycol, cyclohexanedimethanol, polyethylene glycol, polypropylene glycol such as M-phthalic acid, succinic acid, cyclohexane cyclohexanedimethanodibasic, adipic acid, cannabinoid acid, decanedioic acid, 5-sodium sulfonate M-phthalic acids as the compound of copolymerization, but, be not limited to these. In addition, also can add as required TITANIUM DIOXIDE DELUSTRANT, lubricant silica and/or alumina particulate, antioxidant ヒ Application ダ one De phenol derivatives, coloring pigment etc.
In addition, the intensity of polyester capillaries of the present invention is very important more than the 3cN/dtex. If intensity below 3cN/dtex, then will cause the phenomenons such as fluffing, broken string in the senior manufacturing procedures such as the system of knitting, the goods tearing strength that makes simultaneously is low.
Elongation at break with knit the frequency relation of being inversely proportional to that fluffing occurs when processed, elongation at break more can satisfy the intensity of practicality, then more can suppress the generation of fluffiness. For this reason, residual percentage elongation be more than 40% for good, be preferably more than 45%.
Polyester Filament of the present invention, Young's modulus are below the 25cN/dtex, and percentage elongation is that the minimum of a value of 3~10% o'clock differential Young's modulus is very important below the 10cN/dtex.These characteristics are all closely related with tensile properties, the resilience of elasticity cloth and silk, and in order to satisfy the gentle elasticity of requirement of the present invention, above-mentioned no matter which kind of characteristic is got low value for well.That is, owing to satisfied above-mentioned characteristic fully, so when making cloth and silk, the initial stage stretches easy (low Young's modulus).In addition, owing to can unhinderedly stretch (low differential Young's modulus) in the scope of 3~10% percentage elongation of in actual use stretching resilience, so can make gentle elasticity cloth and silk comfortable and easy to wear.
The flexural rigidity of Young's modulus and cloth and silk is also proportional, and Young's modulus is low more, and soft hand feeling is just arranged more.For this reason, Young's modulus with below the 22cN/dtex for well, serving as better below the 20cN/dtex.
Equally, percentage elongation be 3~10% o'clock the differential Young's modulus minimum of a value with below the 8cN/dtex for good, with below the 5cN/dtex for better.
It is more than 90% that Polyester Filament of the present invention extends 10% later rebound degree.If rebound degree less than 90%, then after the elongation, the part of residual part plastic deformation down can produce the shortcoming that is called " loose twist ", therefore, and the decline of the grade of fabric.The rebound degree of elongation after 10% more than 95% for well, then better more than 98%.
The silk resilience that is formed by PTT well mainly results from its molecular structure.In the crystalline texture of PTT, the methylene chain of alkylene glycol part is a domination left and right sides structure arranged, because phenyl ring overlaps each other and interact to reduce and density reduces, flexible raising, so, can make strand extend easily, bounce back by the turning effort of the methylene chain of aforementioned alkylene glycol part.
In addition, in the inventor's experiment as can be known: degree of crystallinity is high more, and resilience is high more.Therefore, degree of crystallinity with more than 30% for well, better more than 35%.Here, the mensuration of degree of crystallinity is pressed the density tapering pipe method of JISL1013 (chemical fiber filament test method) 7.14.2, is tried to achieve by density.
Polyester Filament boiling water shrinkage of the present invention is 3~15%, and the maximum of shrinkage stress is below the 0.3cN/dtex, and the temperature when showing the shrinkage stress maximum is for good more than 120 ℃.
Boiling water shrinkage is design one of most important factor during cloth and silk, and boiling water shrinkage is set in 3% when above, and the shape stability in senior operation is relatively good, is set at 15% when following, and can make does not have cloth and silk coarse hard sense, soft.Equally, if thermal shrinkage stress is too high, the superfluous contraction then arranged, just the feel of coarse hard sense is arranged.Therefore, for obtain not have coarse hard sense, soft hand feeling, the maximum of shrinkage stress is that 0.3cN/dtex is following for good, with 0.15~0.25cN/dtex for better.In addition, in order to formalize easily and to improve senior processing such as bulk, the temperature when showing the shrinkage stress maximum to be being good more than 120 ℃, with more than 130 ℃ for better.
Polyester Filament of the present invention, the continuous shrinkage factor CV% on the draw direction of silk with below 5% for well.Shrinkage factor CV% is one of index of reflection silk homogenieity disadvantage on draw direction continuously, and this value is more little, quality is high more.In order to make high-quality cloth and silk, CV% with below 5% for well, serving as better below 4%.
Polyester Filament of the present invention is carried out interleaving treatment, and the CF value is good in 1~30 scope.The CF value is fixed to more than 1, when carrying out throwing, silk processing and knitting system, can suppress the fracture of monofilament.In addition, make the monofilament bar, mix when fine as the combined yarn that the shrinkage difference will be arranged, good in order to make animal migration, with CF value calmly to below 30 for well.It is then better that the CF value is controlled at 5~25 scope.
Constitute the section configuration of Polyester Filament fiber of the present invention, no matter be garden section, triangular cross-section, leafy shape section, flat partially section, X type section or other well-known section all can, without any restriction, can do suitable selection as required.
Flexibility when making fabric in order to improve, filament fiber number are that 5dtex is following for good, with below the 3dtex for better.
Polyester Filament of the present invention has very confidential relation between twist multiplier and the elasticity, if when twist multiplier surpasses a certain value, then elasticity has the tendency that is increased sharply.In fact, be about 5000 the fabric made of silk with twist multiplier, rebound degree is about 5%, and still, twist multiplier is 10000 o'clock, and rebound degree is about 15%, and twist multiplier is 14000 o'clock, rebound degree then brings up to about 30%.Therefore, though even the Polyester Filament no twist that makes among the present invention also can use,, it is then better to be by twist multiplier that high twist yarn is made in 10000~20000 middle twisted filament.
Twist multiplier is represented with following formula:
Twist multiplier K=T * U 0.5
T: the twisting count of every 1m filament length.D: the fiber number of strand
Here, the twisting count T of so-called every 1m filament length is meant with electronic inspection twister 90 * 10 -3Backtwisting under the loading of cN/dtex, the ratio value representation of separating filament length behind twisting count and the backtwisting when using up complete solution and twisting with the fingers.
Cloth and silk form of the present invention has fabric, compiles thing, nonwoven fabric and padded coaming etc., can do suitable selection according to the purposes difference, can be suitable for to make men's shirt, blouse, pants, suit, Block Le ゾ Application etc.
Enumerate a Polyester Filament preparation method's of the present invention example below.
Preparation method as the main raw material PTT of Polyester Filament of the present invention can directly use well-known method.Stringiness when improving spinning makes the silk with practical intensity, and the inherent viscosity of used PTT [η] is very important more than 0.7, is preferably more than 0.8.
In addition, Polyester Filament of the present invention, both direct spinning stretching carried out so-called continuous polymerization spinning behind the polymerizable, and also can cutting into slices, the back is dry, spin-drawing.
During melt spinning, for the spray silk that makes the nozzle place stable, spinning temperature than the fusing point of PTT high 10~60 ℃ for good, than fusing point high 20~50 ℃ better.In order to suppress separating out of oligomer in the spinning, improve spinnability, also can cartridge heater, suction device be set as required, for preventing the polymer oxidative degradation or preventing that nozzle from polluting the also generator of inert gases such as available air, water vapour, nitrogen at 2~20cm place under the nozzle.
In addition, when preparing Polyester Filament of the present invention, the most important thing is spinning after, the drawing process of the direct fabrics that stretch is immediately adopted in then not rolling.
By the undrawn yarn that PTT forms, as previously mentioned, its internal structure just begins to change after spinning, produces so-called lock seam phenomenon, and this becomes the reason that causes tow ectonexine poor properties.For this reason, in order to suppress the generation of this lock seam phenomenon, the inventor studies, know, after dividing above spinning speed to stretch with 2000m/, then not rolling and after the continuously elongated heat treatment, the heat treatment that relaxes continuously of the relaxation rate with 5~20% is effective.Adopt this method, can improve edge-curl phenomenon greatly, the difference of the inside and outside layer of tow is minimum, makes high-quality silk.In addition, also find the heat treatment that relaxes under high relaxation rate, then the Young's modulus in stretching resilience field is low, can make the gentle elastic yarn of easy stretching.
The strand inhomogeneities is little in order to make, the homogeneous silk of the shortcoming such as inhomogeneous that is difficult to occur to dye, and it is very important more than dividing that spinning speed is controlled at 2000m/.Improve spinning speed, also improved spinning tension, because of being difficult to be subjected to the influence of external interference, so the refinement operation is stable.For this reason, divide above speed spinning then better with 3000m/.In order further to guarantee stable stringiness, preferably spinning speed is controlled at below the 6000m/ branch.
Stretching ratio is set in and makes residual percentage elongation is for well more than 40%.
In order to make target polyesters silk of the present invention, it is 6~20% very important that the relaxation rate during with the lax heat treatment after stretching is controlled at.After the stretching, carry out the lax heat treatment more than 6%,,, can suppress edge-curl phenomenon and take place so the delay slack of permanent set diminishes because the deformation of fibrous inside can relax rapidly.As previously mentioned,, in the elongation range (percentage elongation is below 10%) of practicality, stretch easily, also can give excellent gentle elasticity owing to passed through lax heat treatment.Be more preferably relaxation rate more than 8%.On the other hand, in order to ensure the stability of tow operation in the silk producing procedures, relaxation rate is controlled at 20% below to well, and being controlled at below 18% is better.
Here, with Fig. 1 and Fig. 2 the heat-treating methods that relaxes is described.
Fig. 1 is in the lax heat treatment process, adopts the schematic diagram of cold roller method.By the tow of spinning-nozzle 1 ejection, after ventilator 2 coolings, refuel convergence in the guide groove 3, give finish after, after 4 tractions of the 1st hot-rolling, heating up, between the 1st hot-rolling 4 and the 2nd hot-rolling 5, stretch, HEAT SETTING.After the drawn operation, utilize the heat of the 2nd hot-rolling 5 again, the heat treatment that relaxes between the 2nd hot-rolling 5 and cold roller 6 is by winder 8 rollings.For the heat treatment that more effectively relaxes, between the 2nd hot-rolling 5 and cold roller 6, adopt with hot-air and/or steam as the annealing device of thermal medium or the 3rd hot-rolling is set, carrying out the second step relaxation processes also is the effective ways that reach the object of the invention.
Fig. 2 is the schematic diagram that adopts the method for the spinnerets that interweaves in the lax heat treatment process, and the spinnerets 7 that interweaves plays a part control tow cooling device and tension gradient.That is, owing to, the tow tension before interweaving is descended, so the shrinkage stress that utilization is produced by the effect of the heat of second hot-rolling 5 can and interweave at second hot-rolling 5 and carry out hot relaxation processes between the spinnerets 7 through interleaving treatment.At this moment, relaxation rate can be controlled by the interweave air pressure of spinnerets action of change.In addition, at the 2nd hot-rolling 5 with interweave between the spinnerets 7 also and can carry out the second step relaxation processes by adopting with hot-air and/or steam as the annealing device of thermal medium or the 3rd hot-rolling is set.
These methods are all controlled relaxation rate easily, are the desirable methods of preparation Polyester Filament of the present invention.
In addition, double as stretches, HEAT SETTING reaches lax heat treated warm-up mill (the 2nd hot-rolling in Fig. 1, Fig. 2 example), and the most handy surface roughness is the wrinkle roller of 1.5S~8S.Surface roughness is the fragmentation value of the maximum height (Rmax) put down in writing among the JIS B0601, and in fact 1.5S~8S is equivalent to the fragmentation value of 1.6S, 3.2S, 6.3S.Its maximum height surpasses 0.8 μ m, corresponding with below the 6.3 μ m.This Roughness Surface on Control more than 1.5S, because the coefficient of friction between tow and the roller descends significantly, is had moderately and skids, so even under high relaxation rate, tow can warp, stably throwing on warm-up mill yet.When surface roughness is high, though tow can stably move in lax operation,, if surpass 8S, because tow surface excessive friction, so cause intensity decreases.The optimal surface roughness of warm-up mill is 3.2S~6.3S (Rmax:1.7~6.3 μ m).The mensuration of surface roughness is pressed the regulation of JIS B 0601, measures with the ホ Application メ Le テ ス -T1000 type instrument of ホ Application メ Le corporate system and asks for maximum height Rmax.
In order there not to be fracture of wire, stably carry out throwing, draft temperature (temperature of the 1st hot-rolling) is advisable for high 10~50 ℃ to be controlled at than the glass transition temperature of PTT, and it is then better to stretch under the temperature of glass transition temperature+20~40 ℃.HEAT SETTING and lax heat treated temperature (the 2nd heat roller temperature) are though can be in 90~180 ℃ temperature range, set according to desirable percent thermal shrinkage, but, in order not have uneven silk and to make the residual deformation that causes by stretching lax, be controlled in 105~180 ℃ of scopes temperature then better.
Spinning oil will contain flatting agent, emulsifying agent and antistatic agent etc.Specifically can enumerate mineral oil such as atoleine, octyl palmitate, laurel oleate, fatty acid esters such as stearic acid isotridecyl ester, dioleyl adipate, binary acid dibasic esters such as di-n-octyl sebacate, trimethylolpropane trilaurate, coconut wet goods polyol ester, aliphatic such as dilauryl thiodipropionate contain thioesters, polyoxyethylene oleyl ether, Emulsifier EL-60 base ether, the polyoxyethylene nonylplenyl ether, non-ionic surface active agents such as trimethylolpropane trilaurate, alkylsulfonate, anion surfactants such as the slaine of alkylphosphonic etc. or amine salt, Sodium docusate salt, oxolane/ethylene oxide copolymers such as sodium alkanesulfonate salt, expoxy propane/ethylene oxide copolymer etc., be throwing, warping, knit in each operation of system, when particularly knitting system, for improving reed, the trafficability characteristic of harness cord and the prescription that adopts.As required, also can with rust inhibitor, antiseptic, antioxidant, bleeding agent, surface tension reducer, commutation viscosity reducers, anti-abrasion agent, other modifier etc. and use.
The adhesion amount of finish for tow, is controlled at 0.3~1.2 weight %, and this is being favourable aspect senior operation trafficability characteristic.
Embodiment
Introduce the present invention in more detail below by embodiment.Each characteristic value among the embodiment is measured in the following method.
A. inherent viscosity [η]
Sample polymer is dissolved in the o-chlorphenol (following slightly note is made OCP), under 25 ℃, asks the relative viscosity η of plurality of points with Ostwald viscosimeter r, the concentration when it is extrapolated to infinite dilution is tried to achieve inherent viscosity.
B. TENSILE STRENGTH, Young's modulus (TENSILE STRENGTH at initial stage)
With the TENS ILON UCT-100 of sample, under the constant speed stretching condition shown in the JIS L1013 (chemical fiber filament test method(s)), measure with ォ リ ェ Application テ ッ Network corporate system.Extension at break is asked for by the elongation at the maximum weighted point place shown on the S-S curve.
In addition, Young's modulus be JIS L 1013 (chemical fiber filament test method(s)) 7.10 the joint in the expression initial stage tensile strength condition under measure.
C. differential Young's modulus
The stress of each point on the S-S curve that obtains in the B item is tried to achieve the percentage elongation differential.
D. rebound degree
Adopting the TENSILON UCT-100 of ォ リ ェ Application テ ッ Network corporate system, is 20cm in the clamping spacing, and draw speed is under the condition of 10cm/ branch, the stretching sample, make sample be stretched to 10% of clamping spacing, it is heavy to go down in identical speed immediately then, asks for rebound degree by the hysteresis curve of record.
Rebound degree (%)=(beta/alpha) * 100
α: the elongation that stretched 10% o'clock
β: the resilience elongation when stress equates with initial load
E. shrinkage stress
Adopt the thermal stress analyzer of カ ネ ボ ウ ェ Application ジ ニ ァ リ Application グ corporate system, under the condition of 2.4 ℃/second of programming rates, measure.Sample is made the ring of 10cm * 2, and initial stage tension force is made as fiber number (dtex) * 0.9 * (1/30) gf.
F. silk vertically on continuous shrinkage factor CV%
Adopt the FTA500 of eastern レ ェ Application ジ ニ ァ リ Application グ corporate system, setting tension force is fiber number (dtex) * 0.9 * (1/60) gf, treatment temperature is that 100 ℃ (under water vapours), silk speed are long for measuring under the condition of 10m for 10m/min, sample, shrinkage factor is recorded on the record-paper, asks for silk continuous shrinkage factor CV% in the vertical.
The G.CF value
Condition by the interleaving degree shown in 7.13 of the JIS L1013 (chemical fiber filament test method(s)) is measured.Test number (TN) 50 times by the mean value L (mm) of weaving length, is asked for CF value (Coherence Factor) by following formula.
CF value=1000/L
H. degree of crystallinity
Measure density according to the density tapering pipe method among JIS L1013 (chemical fiber filament test method(s)) 7.14.2, ask degree of crystallinity by following formula.
Xc[%]={dc×(d-da))/{d×(dc-da))×100
Xc: degree of crystallinity (%)
D: the density of actual measurement silk
Dc: the density of complete crystalline portion
Da: the density of crystalline portion not fully
Here, dc 1.387g/cm 3, da 1.295g/cm 3
Embodiment 1
With the drawing-spinning machine shown in Fig. 1, it with inherent viscosity [η] 0.96 homopolymerization PTT fusion, under 265 ℃ of spinning temperatures, by the spinning in 24 holes mouth 1 ejection of disputing, cooling in ventilator 2, refuel bring together in the guide groove 3 give finish after, stretch with the speed that 3000m/ divides with the 1st hot-rolling 4, under 70 ℃, rotated for 5 weeks, after tow is heated up, stretch with the draw speed (1.6 times of stretching ratios) that 4800m/ divides, under 140 ℃, rotate and 5 weeks carried out HEAT SETTING with the 2nd hot-rolling 5, between the 2nd hot-rolling 5 and cold roller 6, be 10% to make it lax again with relaxation rate, then, with interlaced device 7, with the calm the anger condition of 0.2MPa of work, the interleaving treatment limit is carried out with the speed rolling of winder 8 with the 4220m/ branch in the limit, makes 54 dtexs, the drawn yarn of 24 long filaments.The 2nd hot-rolling 5 usefulness surface roughnesses are the wrinkle roller of 3.2S (Rmax:3 μ m).
Throwing is good, and fracture of wire, side volume phenomenon do not take place.The intensity of the Polyester Filament that makes in addition, be 3.6cN/dtex, Young's modulus (initial stage tensile strength) for 20.8cN/dtex, percentage elongation be that the minimum of a value of 3~10% o'clock differential Young's modulus is that rebound degree after 1.8cN/dtex, 10% elongation is 97.8%.Physics value is shown in Table 1, and load-deformation curve and differential Young's modulus-strain curve are shown among Fig. 3.
Again aforesaid compound silk is knitted 4 drillipgs of system with the longitude and latitude method, its result knits system property, fabric quality is all good, has slight elasticity.
Embodiment 2, embodiment 3
Except draw speed being set at 4350m/ branch (1.45 times of stretching ratios) (embodiment 2) and 5000m/ branch (1.67 times of stretching ratios) (embodiment 3), all the other are implemented under the condition identical with embodiment 1.The Polyester Filament of embodiment 2, its intensity are 3.3cN/dtex, and be also lower than embodiment 1, and still, other characteristic is good similarly to Example 1.In addition, the Polyester Filament of embodiment 3 and embodiment 1 compare, and the platform number of times that stops when knitting system increases by 2 times approximately, but other characteristic is good.
Embodiment 4, embodiment 5
Except the relaxation rate between the 2nd hot-rolling 5 and the cold roller 6 being set at 6% (embodiment 4) and 18% (embodiment 5), all the other are implemented under the condition identical with embodiment 1.The Polyester Filament of embodiment 4, embodiment 5 is the same with embodiment 1, and the quality of throwing, fabric is all good, and has slight elasticity.Particularly the fabric of embodiment 5 has more excellent flexibility than embodiment 1.
Comparative example 1
Except operating characteristic viscosity [η] was 0.68 homopolymerization PTT, all the other were implemented under the condition identical with embodiment 1.The Polyester Filament draftability of comparative example 1 is poor, the drawing zone fracture of wire is many, can't take a sample.
Comparative example 2
Except draw speed being set at 3900m/ branch (1.3 times of stretching ratios), all the other are implemented under the condition identical with embodiment 1.The Polyester Filament intensity of comparative example 2 is that 2.9cN/dtex, percentage elongation are 73.5%, and intensity is low, percentage elongation is big, and simultaneously, the 10% later rebound degree that stretches is also low, the practical poor durability behind the weaving cloth and silk.
Comparative example 3, comparative example 4
Except the relaxation rate between the 2nd hot-rolling 5 and the cold roller 6 is set at 22% and 3%, all the other are implemented under the condition identical with embodiment 1.Relaxation rate is set at the Polyester Filament of 22% comparative example 3, and strand rocks severity on the 2nd hot-rolling, and in addition, silk twists on the 2nd hot-rolling fracture of wire takes place.
Relaxation rate is 3% a comparative example 4 because the generation of edge-curl phenomenon, and difference appears in the rerum natura of the inside and outside layer of tow, and the tow end face occurs periodically that thickness changes, and then makes the quality of knitting system property variation, dyeing also bad.In addition, though in cloth and silk some elasticity,, shown the extremely difficult characteristic that stretches.Physics value is shown in Table 1, and load-deformation curve and differential Young's modulus-strain curve are shown among Fig. 4.
Comparative example 5
Except draw speed being set at 5250m/ branch (1.75 times of stretching ratios), unloading cold roller 6, relaxation rate is set at 0%, all the other are implemented under the condition identical with embodiment 1.The Polyester Filament of comparative example 5 is more severe than the edge-curl phenomenon of comparative example 4, and then the extremely difficult stretching of the cloth and silk that makes, and meanwhile flexibility is also poor.
Embodiment 6
Except the speed setting with the 1st hot-rolling 4 is that the speed setting of 1000m/ branch, the 2nd hot-rolling 5 is the 3500m/ branch (3.5 times of stretching ratios), all the other are implemented under the condition identical with embodiment 1.
The cloth and silk that is formed by the Polyester Filament of embodiment 6 is the same with embodiment 1, has shown better elastic, still, has formed the uneven dyeing that is caused by the silk inhomogeneity on stained clot-h.
Embodiment 7
Except the mirror roller of the 2nd hot-rolling 5 being used instead 0.8S (Rmax:0.8 μ m following), all the other are implemented under the condition identical with embodiment 1.Among the embodiment 7, the strand instability of relax zone operation between the 2nd hot-rolling and the cold roller 6 produces little sticking phenomenon on the 2nd hot-rolling, reverse, and fracture of wire is a lot.For this reason, the fracture of wire number of times is about 10 times of embodiment 1.
Embodiment 8
To the Polyester Filament that makes among the embodiment 1 carry out 2000t/m (the twist yarn COEFFICIENT K: the twist yarn of S/Z 14700), make warp and parallel, make 4 drillipgs again.It is pressed well-established law, 98 ℃ down lax concise, carrying out the intermediate heat typing under 160 ℃ after, decrement 15 weight % in 3% NaOH hydrothermal solution finalize the design after the dyeing at last.The cloth and silk flexibility and the excellent elasticity that make.
" relaxation rate " in the table is meant the relaxation rate between the 2nd hot-rolling and the cold roller 6, " differential Young's modulus " is meant that percentage elongation is the minimum of a value of 3~10% o'clock differential Young's modulus, " rebound degree " is meant the rebound degree after the elongation 10% "; " shrinkage stress " is meant the maximum of shrinkage stress; " peak temperature " is meant the temperature when shrinkage stress is maximum; " shrinkage factor CV% " is meant the continuous shrinkage factor CV% on tow is vertical, and " fabric quality " is meant the appearance of fabrics quality (sense organ by the people is estimated) after the dyeing.
The possibility of utilizing on the industry
Polyester Filament of the present invention and preparation method thereof can make does not have edge-curl phenomenon in silk producing procedures, stay-in-grade tow, meanwhile, can make the fabric of low, the gentle elasticity of Young's modulus, flexibility excellence in the resilience scope.
Table 1
Embodiment Comparative example Embodiment
1 2 3 4 5 1 2 3 4 5 6 7
Inherent viscosity [η] 0.96 0.96 0.96 0.96 0.96 0.68 0.96 0.68 0.96 0.96 0.96 0.96
The 1st hot-rolling speed The m/ branch 3000 3000 3000 3000 3000 3000 3000 3000 3000 3000 1000 3000
The 2nd hot-rolling speed The m/ branch 4800 4350 5000 4800 4800 4800 3900 4800 4800 5250 3500 4800
Relaxation rate 10.0 10.0 10.0 6.0 18.0 10.0 10.0 22.0 3.0 0.0 10.0 10.0
Intensity cN/dtex 3.6 3.3 3.7 3.7 3.4 - 2.9 - 3.5 3.8 3.7 3.6
Percentage elongation 50.5 59.2 43.2 42.0 57.8 - 73.5 - 44.3 26.5 45.4 50.1
Young's modulus cN/dtex 20.8 19.4 21.5 21.7 19.8 - 18.9 - 21.5 28.6 21.0 20.8
The differential Young's modulus cN/dtex 1.8 1.5 2.5 6.6 1.4 - 1.4 - 11.2 14.4 3.2 2.0
Rebound degree 97.8 90.8 98.0 98.2 93.3 - 85.5 - 98.5 98.8 98.1 97.2
Degree of crystallinity 38 36 39 40 37 - 36 - 43 47 40 38
Boiling water shrinkage 6.7 6.2 7.5 8.0 6.5 - 5.8 - 8.7 10.0 7.3 6.6
Shrinkage stress cN/dtex 0.17 0.13 0.19 0.20 0.15 - 0.11 - 0.25 0.33 0.19 0.17
The peak temperature 168 169 170 170 167 - 167 - 17 1 171 172 167
Shrinkage factor CV% 2.8 3.7 3.0 3.8 3.2 - 4.2 - 7.6 7.9 5.2 4.5
The CF value 9.5 14.5 8.2 4.7 16.9 - 15.4 - 0.8 0.2 4.1 13.8
Fabric quality 4 grades of evaluations - - × ×
Elasticity 4 grades of evaluations - - × ×

Claims (23)

1. Polyester Filament, in fact it is the compound silk that is formed by polytrimethylene terephthalate, it is characterized in that, on load-deformation curve, intensity is more than the 3cN/dtex, and Young's modulus is below the 25cN/dtex, meanwhile, percentage elongation is that the minimum of a value of 3~10% o'clock differential Young's modulus is below the 10cN/dtex, and the rebound degree after 10% elongation is more than 90%.
2. the Polyester Filament of claim 1 is characterized in that, Young's modulus is below the 22cN/dtex.
3. the Polyester Filament of claim 1 is characterized in that, percentage elongation is that the minimum of a value of 3~10% o'clock differential Young's modulus is below the 5cN/dtex.
4. the Polyester Filament of claim 1 is characterized in that, residual percentage elongation is more than 45%.
5. the Polyester Filament of claim 1 is characterized in that, the rebound degree after 10% elongation is more than 95%.
6. the Polyester Filament of claim 1 is characterized in that, degree of crystallinity is more than 30%.
7. the Polyester Filament of claim 1 is characterized in that, the shrinkage factor in boiling water is 3~15%, and the maximum of shrinkage stress is below the 0.3cN/dtex, and the temperature when showing the shrinkage stress maximum is more than 120 ℃.
8. the Polyester Filament of claim 7 is characterized in that, the maximum of shrinkage stress is 0.15~0.25cN/dtex.
9. the Polyester Filament of claim 7 is characterized in that, the temperature when showing the shrinkage stress maximum is more than 130 ℃.
10. the Polyester Filament of claim 1 is characterized in that, the tow CV value of continuous shrinkage factor longitudinally is below 5%.
11. the Polyester Filament of claim 1 is characterized in that, the CF value is 1~30.
12. the Polyester Filament of claim 11 is characterized in that, the CF value is 5~25.
13. the Polyester Filament of claim 1 is characterized in that, the filamentary fiber number that constitutes Polyester Filament is below the 3dtex.
14. a fabric is characterized in that, it is 10000~20000 twist yarn that each the Polyester Filament in the claim 1~13 is made the twist yarn coefficient, makes organizine and/or tram again and uses.
15. the preparation method of a Polyester Filament, it is characterized in that, with inherent viscosity [η] is polymer melt spinning more than 0.7, that in fact formed by polytrimethylene terephthalate, make compound silk, dividing above spinning speed traction with 2000m/ again, then do not reel and after the continuously elongated heat treatment, is under 6~20% the condition at relaxation rate, carry out continuously lax heat treatment, be wound into package then.
16. the preparation method of the Polyester Filament of claim 15 is characterized in that, is that polytrimethylene terephthalate more than 0.8 carries out melt spinning with inherent viscosity [η].
17. the preparation method of the Polyester Filament of claim 15 is characterized in that, spinning temperature is higher 20~50 ℃ than the fusing point of polytrimethylene terephthalate.
18. the preparation method of the Polyester Filament of claim 15 is characterized in that dividing above spinning speed to draw with 3000m/.
19. the preparation method of the Polyester Filament of claim 15 is characterized in that, under 8~18% relaxation rate condition, heat treatment relaxes.
20. the preparation method of the Polyester Filament of claim 22 is characterized in that, uses the wrinkle roller of surface roughness as 1.5S~8S in the stretching heat treatment.
21. the preparation method of the Polyester Filament of claim 15 is characterized in that, uses the wrinkle roller of surface roughness as 3.2S~6.3S in the stretching heat treatment.
22. the preparation method of the Polyester Filament of claim 15 is characterized in that, draft temperature is elevated to higher 10~50 ℃ than the glass transition temperature of polytrimethylene terephthalate.
23. the preparation method of the Polyester Filament of claim 15 is characterized in that, carries out HEAT SETTING and lax heat treatment in 105~180 ℃ temperature range.
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