KR20010056222A - Low temperature dyeable polyester fiber and preparation thereof - Google Patents
Low temperature dyeable polyester fiber and preparation thereof Download PDFInfo
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- KR20010056222A KR20010056222A KR1019990058862A KR19990058862A KR20010056222A KR 20010056222 A KR20010056222 A KR 20010056222A KR 1019990058862 A KR1019990058862 A KR 1019990058862A KR 19990058862 A KR19990058862 A KR 19990058862A KR 20010056222 A KR20010056222 A KR 20010056222A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/098—Melt spinning methods with simultaneous stretching
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/04—Pigments
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Abstract
Description
본 발명은 폴리에스테르사에 관한 것으로서, 보다 구제적으로는 폴리에틸렌테레프탈레이트와 폴리트리메틸렌테레프탈레이트의 블랜드 방사에 의한 저온 염색성 및 소프트니스가 우수한 폴리에스테르 섬유 및 그 제조방법에 관한 것이다.The present invention relates to a polyester yarn, and more particularly, to a polyester fiber having excellent low temperature dyeability and softness by blend spinning of polyethylene terephthalate and polytrimethylene terephthalate, and a method of manufacturing the same.
폴리에스테르 섬유의 대표적인 예인 폴리에틸렌테레프탈레이트 섬유는 130℃가 상용의 염색온도이나, 이와 같은 온도로 염색을 행하게 되면 섬유의 열화가 발생하여 촉감이 까칠하게 되므로 의류용, 특히 인너웨어 용도로의 사용에 제한이 있는 것이다.Polyethylene terephthalate fiber, which is a typical example of polyester fiber, has a normal dyeing temperature of 130 ° C., but if it is dyed at such a temperature, the fiber deteriorates and the touch becomes rough. There is a limit.
이 때문에 폴리에틸렌테레프탈레이트 섬유의 저온 가염화의 시도로서 고속 방사하는 방법(예를 들면, 미국 특허 제4,134,883호)과 공중합에 의한 개질방법(예를 들면, 일본특원소 61-226510호 공보) 등이 제안되어 있다.For this reason, as a method of low temperature salting of polyethylene terephthalate fiber, a method of high-speed spinning (for example, U.S. Patent No. 4,134,883) and a reforming method by copolymerization (for example, Japanese Patent Application No. 61-226510) It is proposed.
고속 방사 폴리에틸렌테레프탈레이트 섬유는 염색온도가 낮아지기는 한 것이나 짙은 색의 염색에 110∼120℃의 염색온도가 요구되고, 이러한 염색온도에서는섬유의 촉감이 까칠하게 되어 인너웨어의 용도로는 부적합하다.The high-speed spinning polyethylene terephthalate fiber has a low dyeing temperature, but a dyeing temperature of 110-120 ° C. is required for dark dyeing, and at this dyeing temperature, the texture of the fiber becomes rough, which is not suitable for inner wear.
한편,공중합 폴리에틸렌테레프탈레이트 섬유는 염색의 내광견뢰도가 통상의 폴리에틸렌테레프탈레이트 보다 낮고,염료 선택에 제약이 있다. 또한 이러한 섬유는 저온염색성이 있으나 짙은 색의 염색에는 105℃ 이상의 고온이 필요하고 염색된 섬유는 촉감이 까칠하게 되어 인너웨어의 용도로는 부적합하게 된다.On the other hand, the co-polymerized polyethylene terephthalate fiber has a low light fastness of dyeing than a conventional polyethylene terephthalate, there is a restriction in dye selection. In addition, these fibers have a low temperature dyeing, but the dyeing of the dark color requires a high temperature of 105 ° C. or higher, and the dyed fibers become hard to touch, making them unsuitable for inner wear.
따라서 본 발명은 상기한 바와 같은 선행기술의 제반 문제점을 감안하여 저온에서 염색가능하고 개선된 소프트니스를 갖는 폴리에스테르 섬유를 제공하는 것을 기술적 과제로 한다.It is therefore an object of the present invention to provide a polyester fiber which can be dyed at low temperatures and has improved softness in view of the above-mentioned problems of the prior art.
상기한 과제를 해결하기 위한 본 발명자의 연구에서 폴리에틸렌테레프탈레이트와 폴리트리메틸렌테레프탈레이트를 블랜드하여 방사하면 이염성 및 소프트니스가 우수하고 염색균일성이 우수한 폴리에스테르 섬유를 제조할 수 있게 된다는 사실을 알게 되었고, 그 결과 본 발명을 완성하게 된 것이다.In the study of the present inventors for solving the above problems, blending and spinning polyethylene terephthalate and polytrimethylene terephthalate can produce polyester fibers having excellent dyeing and softness and excellent dyeing uniformity. As a result, the present invention has been completed.
그러므로 본 발명에 의하면 고유점도 0.60∼0.65의 폴리에틸렌테레프탈레이트(PET) 70∼95중량%와 고유점도 0.80∼1.0의 폴리트리메틸렌테레프탈레이트(PTT) 30∼5중량%를 함유하는 블랜드를 방사하는 것에 의해 제조되며, 90∼100℃에서 염색가능하며, 영율이 400∼700㎏/㎟, 신도가 40% 미만인 것을 특징으로 하는 저온염색성 폴리에스테르 섬유가 제공된다.Therefore, according to the present invention, it is possible to spin a blend containing 70 to 95% by weight of polyethylene terephthalate (PET) having an intrinsic viscosity of 0.60 to 0.65 and 30 to 5% by weight of polytrimethylene terephthalate (PTT) having an intrinsic viscosity of 0.80 to 1.0. It is produced by, is dyed at 90 ~ 100 ℃, provides a low-temperature dyeing polyester fiber characterized in that the Young's modulus is 400 ~ 700kg / ㎜, elongation is less than 40%.
이하, 본 발명을 보다 상세하게 설명하기로 한다.Hereinafter, the present invention will be described in more detail.
본 발명은 폴리에스테르 섬유가 낮은 온도에서 염색가능하고, 균일하게 염색되며, 소프트니스가 양호하고 저신도의 특성을 갖게 하기 위하여, 소재를 고유점도 0.60∼0.65의 폴리에틸렌테레프탈레이트 70∼95중량%와 고유점도 0.80∼1.0의 폴리트리메틸렌테레프탈레이트 30∼5중량%를 함유하는 폴리머 블랜드로 설계한다. 만일 폴리머 블랜드중 폴리트리메틸렌테레프탈레이트의 비율이 5중량% 보다 적은 양으로 함유되는 경우에는 원하는 정도의 염색온도, 염색균일성 및 소프트니스를 얻을 수 없게 되고, 30중%를 초과하는 경우에는 융점이 지나치게 낮아지거나 또는 융점이 사라지게 되어 (즉, 비결정화되어) 섬유로서의 폴리에틸렌테레프탈레이트의 우수한 특성이 상실되므로 부적합하게 된다. 그러나 본 발명에 따라 압출방사되는 폴리머 블랜드중 폴리트리메틸렌테레프탈레이트의 비율이 5∼30중량%이면 섬유로서의 폴리에틸렌테레프탈레이트의 우수한 특성을 적정수준으로 유지하면서도 원하는 정도의 염색온도, 바람직하게 90∼100℃, 염색균일성, 우수한 소프트니스, 바람직하게 영율 400∼700㎏/㎟, 낮은 신도, 바람직하게 40% 미만, 특히 25∼35%의 신도를 만족하는 폴리에스테르 섬유의 제조를 가능하게 한다. 또한 사용되는 폴리에틸렌테레프탈레이트의 고유점도는 0.60∼0.65이고 폴리트리메틸렌테레프탈레이트의 고유점도는 0.80∼1.0이어야 한다. 만일 각각의 고유점도가 상기한 범위를 벗어나면 동일온도에서 점도의 차이가 커져서 방사성이 불량하게 되므로 원하는 물성의 섬유를 제조하는 것이 곤란하게 된다.The present invention is made of 70-95% by weight of polyethylene terephthalate having an intrinsic viscosity of 0.60 to 0.65 so that polyester fibers can be dyed at low temperatures, are dyed uniformly, have good softness and have low elongation. It is designed as a polymer blend containing 30 to 5% by weight of polytrimethylene terephthalate having an intrinsic viscosity of 0.80 to 1.0. If the proportion of polytrimethylene terephthalate in the polymer blend is contained in an amount of less than 5% by weight, the desired degree of dyeing temperature, dyeing uniformity and softness will not be obtained. This becomes too low or the melting point disappears (i.e., crystallized), which makes the polyethylene terephthalate's excellent properties as a fiber unsuitable. However, when the ratio of polytrimethylene terephthalate in the polymer blend extruded according to the present invention is 5 to 30% by weight, the excellent properties of the polyethylene terephthalate as a fiber are maintained at an appropriate level, and the desired dyeing temperature is preferably 90 to 100. It is possible to produce polyester fibers which satisfies a degree of dyeing uniformity, good softness, preferably a Young's modulus of 400 to 700 kg / mm 2, low elongation, preferably less than 40%, in particular 25 to 35%. In addition, the intrinsic viscosity of the polyethylene terephthalate used is 0.60 to 0.65 and the intrinsic viscosity of the polytrimethylene terephthalate should be 0.80 to 1.0. If each intrinsic viscosity is out of the above range, the difference in viscosity becomes large at the same temperature, so that the spinning is poor, it is difficult to manufacture the fiber of the desired physical properties.
폴리트리메틸렌테레프탈레이트는 테레프탈산 또는 테레프탈산 디메틸로 대표되는 테레프탈산의 저급 알코올 에스테르와 트리메틸렌 글리콜(1,3-프로판디올)을 중축합시키고 얻을 수 있는, 최근에야 비로서 상업적인 생산이 가능하게 된 고분자물질이다.Polytrimethylene terephthalate is a polymer that has only recently been commercially available for the production of polycondensates of lower alcohol esters of terephthalic acid and trimethylene glycol (1,3-propanediol) represented by terephthalic acid or dimethyl terephthalate. to be.
본 발명에 이용한 폴리트리메틸렌테레프탈레이트나 폴리에틸렌테레프탈레이트에는 필요에 따라 본 발명의 효과를 손상시키지 않는 범위에서 산 성분으로서 이소프탈산,호박산,아디핀산,2,6-나프탈렌디카르본산등이나,글리콜 성분으로서 에틸렌 글리콜,1,4-부탄디올,1,6-헥산디올,폴리옥시 알킬렌 글리콜등의 글리콜 성분이 공중합되고 있어도 좋다.또,필요에 따라 각종의 첨가제,예를 들면 무광택제,열 안정제,난연제,대전 방지제,소포제 등을 함유해도 좋다.Polytrimethylene terephthalate and polyethylene terephthalate used in the present invention, if necessary, isophthalic acid, succinic acid, adipic acid, 2,6-naphthalenedicarboxylic acid, or glycol as an acid component in a range that does not impair the effects of the present invention. As the component, glycol components such as ethylene glycol, 1,4-butanediol, 1,6-hexanediol, and polyoxyalkylene glycol may be copolymerized. In addition, various additives, for example, a matting agent and a heat stabilizer, may be required. It may contain a flame retardant, antistatic agent, antifoaming agent and the like.
이하 이러한 특성을 만족하는 폴리에스테르 섬유를 제조하기에 바람직한 방법의 일예를 들어 설명하면, 본 발명의 폴리에스테르 섬유는 고유점도 0.60∼0.65의 폴리에틸렌테레프탈레이트 70∼95중량%와 고유점도 0.80∼1.0의 폴리트리메틸렌테레프탈레이트 30∼5중량%로 되는 폴리머 블랜드를 준비하고, 이 블랜드를 스핀드로우 방식으로 익스트루더와 방사팩을 구비하는 방사기에서 방사하여 섬유를 제조하되, 방사온도 280∼290℃, 방사기내 체류시간 10∼20분, 제1고뎃롤러속도 1,000∼2,000mpm(m/min), 제2고뎃롤러속도 3,000∼5,000mpm, 제1고뎃롤러 온도 70∼120℃, 제2고뎃롤러온도 100∼150℃의 조건하에서 방사하여 제조할 수 있다. 상기 조건들중에서도 특히 방사기내 체류시간이 중요한데, 만일 방사기내 체류시간이 10분 미만이면 블랜드 효과가 미흡하게 되고, 20분을 초과하는 경우에는 열분해가 발생되어 제조되는 섬유의 물성을 손상시키게 되므로 상기한 범위로 유지시키는 것이 필요하다.Hereinafter, an example of a preferred method for producing a polyester fiber that satisfies these properties, the polyester fiber of the present invention is 70 to 95% by weight polyethylene terephthalate having an intrinsic viscosity of 0.60 to 0.65 and intrinsic viscosity of 0.80 to 1.0 Prepare a polymer blend of polytrimethylene terephthalate 30 to 5% by weight, and spin the blend in a spinning machine having an extruder and a spinning pack in a spin draw method to produce fibers, wherein the spinning temperature is 280 to 290 ° C, 10 to 20 minutes residence time in the spinning machine, 1st high speed roller speed 1,000 ~ 2,000mpm (m / min), 2nd high speed roller speed 3,000 ~ 5,000mpm, 1st high speed roller temperature 70 ~ 120 ℃, 2nd high speed roller temperature 100 It can manufacture by spinning on the conditions of -150 degreeC. Among these conditions, in particular, the residence time in the spinning machine is important. If the residence time in the spinning machine is less than 10 minutes, the blending effect is insufficient, and in the case of more than 20 minutes, pyrolysis occurs and the physical properties of the fabrics are damaged. It is necessary to keep it in a range.
또한, 제1고뎃롤러 및 제2고뎃롤러의 속도는 섬유의 신도가 40% 미만이 되도록 조절하는 것이 필요하고, 제1고뎃롤러 및 제2고뎃롤러의 온도 역시 제조된 섬유가 균일한 염색성을 가지며 비수수축율이 8∼12%가 되도록 조절하는 것이 바람직하다.In addition, the speed of the first gourd roller and the second gourd roller needs to be adjusted so that the elongation of the fiber is less than 40%, and the temperature of the first gourd roller and the second gourd roller also has uniform dyeing property. It is preferable to adjust so that a specific contraction rate may be 8 to 12%.
폴리에틸렌테레프탈레이트와 폴리트리메틸렌테레프탈레이트의 블랜드는 예를 들어 로타리 건조기를 사용하여 준비하거나, 또는 별도의 칩 호퍼로부터 계량하여(예를 들어 로타리 밸브를 사용하여) 준비하거나, 또는 도우징 머신(dozing machine)을 사용하여 폴리트리메틸렌테레프탈레이트를 사이드 피딩하는 것으로 준비할 수 있다.Blends of polyethylene terephthalate and polytrimethylene terephthalate can be prepared, for example, using a rotary dryer, metered from a separate chip hopper (for example using a rotary valve), or a dozing machine. machine) to prepare the polytrimethylene terephthalate by side feeding.
이와 같은 본 발명에 의하여 제조되는 폴리에스테르 섬유는 보통 120∼130℃에 이루어지는 폴리에틸렌테레프탈레이트 섬유 보다 훨씬 낮은 온도인 90∼100℃의 온도에서 염색이 가능하고, 염색균일성도 우수하며, 소프트니스 또한 우수하게 된다. 의류용 폴리에틸렌테레프탈레이트 섬유는 보통 영율이 보통 1,000㎏/㎟ 정도인데 반하여 본 발명의 폴리에스테르 섬유는 이 보다 훨씬 낮은 400∼700㎏/㎟ 정도의 영율을 나타낸다.The polyester fiber prepared according to the present invention can be dyed at a temperature of 90 to 100 ° C., which is much lower than the polyethylene terephthalate fiber, which is usually formed at 120 to 130 ° C., and has excellent dyeing uniformity and excellent softness. Done. Polyethylene terephthalate fibers for garments usually have a Young's modulus of about 1,000 kg / mm 2, while the polyester fibers of the present invention exhibit a Young's modulus of about 400 to 700 kg / mm 2, much lower than this.
상술한 바와 같은 본 발명의 특징 및 기타의 장점은 후술되는 실시예로부터 보다 명백하게 될 것이다. 단, 본 발명은 하기 실시예로 한정되는 것은 아니다.Features and other advantages of the present invention as described above will become more apparent from the embodiments described below. However, the present invention is not limited to the following examples.
하기 실시예에서 제시되는 물성치들은 다음과 같은 방법으로 측정한 것이다.Physical properties presented in the following Examples are measured by the following method.
* 이염성 : 블루칼라(blue color)의 분산염료를 1.0 owf 사용하여 다양한 온도에서 30분간 염색한 후 측색기를 이용하여 630nm에서 K/S값을 측정하여 염착을 비교하였다. K/S값이 높을수록 염색이 잘되는 것이다.* Dyeing: After dyeing blue dye dispersion dye at 1.0 owf for 30 minutes at various temperatures, K / S values were measured at 630nm using a colorimeter to compare dyeing. The higher the K / S value, the better the dyeing.
* 영율(Young's modulus) : 만능시험기(UTM)를 사용하여 파지거리 200㎜, 크로스헤드(crosshead) 속도 400㎜/min의 조건하에서 측정.* Young's modulus: Measured under conditions of holding distance 200mm and crosshead speed 400mm / min using universal testing machine (UTM).
* 염색균일성 : 블루칼라의 분산염료를 사용하여 98℃에서 30분간 염색후 육안으로 균일과 불균일로 판정.* Dyeing uniformity: After dyeing at 98 ℃ for 30 minutes using blue dye dispersion dye, it is judged as uniformity and unevenness by naked eye.
*신도 : UTM으로 측정Elongation: Measured by UTM
[실시예 및 비교예][Examples and Comparative Examples]
통상의 폴리에스테르 섬유제조용 스핀드로우 방사기에서 폴리에틸렌테레프탈레이트(PET)칩과 폴리트리메틸렌테레프탈레이트(PTT)칩을 진공식 회전 건조기에 투입하고 150℃에서 10시간동안 건조하면서 블랜딩하였다. 이때 상기 폴리에틸렌테레프탈레이트칩과 폴리트리메틸렌테레프탈레이트칩의 고유점도 및 블랜드 비은 하기 표 1과 같이 하였다.Polyethylene terephthalate (PET) chips and polytrimethylene terephthalate (PTT) chips were introduced into a vacuum rotary dryer in a conventional spin drawer for producing polyester fibers, and blended while drying at 150 ° C. for 10 hours. In this case, the intrinsic viscosity and blend ratio of the polyethylene terephthalate chip and the polytrimethylene terephthalate chip were as shown in Table 1 below.
이와 같이 건조된 블랜딩칩을 직경이 0.27㎜이고, 길이가 0.5㎜인 36홀의 방사노즐을 통하여 방사온도 285℃에서 방사한후, 속도가 1,500mpm이고 온도가 표 1과 같은 제1고뎃롤러 및 속도가 4,500mpm이고 온도가 120℃인 제2고뎃롤러를 사용하여 75데니어/36필라멘트의 신도가 35%인 폴리에스테르 섬유를 제조하였다.The dried blending chip was spun at a spinning temperature of 285 ° C. through a 36-hole spinneret having a diameter of 0.27 mm and a length of 0.5 mm, and then the speed was 1,500 mpm and the temperature was shown in Table 1. A polyester fiber having an elongation of 75 denier / 36 filaments of 35% was prepared using a second gourd roller having a temperature of 4,500 mpm and a temperature of 120 ° C.
방사기내 체류시간은 검정색의 원착칩을 방사중에 소량 투입하여 측정하였으며 그 결과는 표 1와 같다.The residence time in the spinning machine was measured by inserting a small amount of black chips into the spinning. The results are shown in Table 1.
제조된 폴리에스테르 섬유의 80℃, 90℃, 100℃ 및 110℃에서의 K/S값, 염색균일성, 영율 및 방사공정성을 측정 및 평가하여 표 2에 나타내었다.K / S values, dyeing uniformity, Young's modulus, and spinning processability at 80 ° C., 90 ° C., 100 ° C. and 110 ° C. of the prepared polyester fiber were measured and evaluated.
상기한 실시예 및 비교예의 결과들로부터 명백하게 되는 바와 같이, 본 발명의 폴리에스테르 섬유는 염색균일성이 우수하고, 소프트니스가 양호하며 저신도의 특성을 보유할 뿐만아니라, 낮은 온도에서 염색가능하므로 염색후에도 우수한 소프트니스를 보유하여 특히 인너웨어 용도로 매우 적합한 고부가가치의 섬유인 것이다.As will be apparent from the results of the above-described examples and comparative examples, the polyester fibers of the present invention are excellent in dyeing uniformity, have good softness, have low elongation properties, and can be dyed at low temperatures. It has high softness even after dyeing and is a high value added fiber which is very suitable especially for inner wear.
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KR20010112541A (en) * | 2000-06-08 | 2001-12-20 | 조 정 래 | Manufacturing of easily dyeable polyester fiber |
KR100365811B1 (en) * | 1999-12-03 | 2002-12-26 | 주식회사 코오롱 | Easy dyeable biaxially oriented polyester film |
KR100622204B1 (en) * | 2000-01-10 | 2006-09-07 | 주식회사 휴비스 | Polytrimethyleneterephthalate fiber and preparation thereof |
KR100783801B1 (en) * | 2007-02-05 | 2007-12-07 | 주식회사 새 한 | Manufacturing method of polytrimethylene terephthalate fiber by extracting easily soluble polymer for alkali and its product |
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KR20130136075A (en) | 2012-06-04 | 2013-12-12 | 현대자동차주식회사 | Eco friendly tufted carpet for vehicle having improved abrasion resistance |
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KR100587118B1 (en) * | 1999-12-18 | 2006-06-07 | 주식회사 휴비스 | Preparation of polyester fiber with tone effect |
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KR100365811B1 (en) * | 1999-12-03 | 2002-12-26 | 주식회사 코오롱 | Easy dyeable biaxially oriented polyester film |
KR100622204B1 (en) * | 2000-01-10 | 2006-09-07 | 주식회사 휴비스 | Polytrimethyleneterephthalate fiber and preparation thereof |
KR20010112541A (en) * | 2000-06-08 | 2001-12-20 | 조 정 래 | Manufacturing of easily dyeable polyester fiber |
KR100783801B1 (en) * | 2007-02-05 | 2007-12-07 | 주식회사 새 한 | Manufacturing method of polytrimethylene terephthalate fiber by extracting easily soluble polymer for alkali and its product |
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