KR100454497B1 - Manufacturing method of polyester fiber having excellent hygroscopicity and antistatic property by blending polyamide ingredient showing fibril structure by difference of miscibility - Google Patents

Manufacturing method of polyester fiber having excellent hygroscopicity and antistatic property by blending polyamide ingredient showing fibril structure by difference of miscibility Download PDF

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KR100454497B1
KR100454497B1 KR1019970034748A KR19970034748A KR100454497B1 KR 100454497 B1 KR100454497 B1 KR 100454497B1 KR 1019970034748 A KR1019970034748 A KR 1019970034748A KR 19970034748 A KR19970034748 A KR 19970034748A KR 100454497 B1 KR100454497 B1 KR 100454497B1
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polyester
antistatic property
polyester fiber
miscibility
antistatic
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KR1019970034748A
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Korean (ko)
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KR19990011602A (en
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박성윤
박성균
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주식회사 휴비스
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    • 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
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/02Preparation of spinning solutions
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/08Melt spinning methods
    • 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
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/09Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • 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
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)

Abstract

PURPOSE: A manufacturing method of polyester fiber having excellent hygroscopicity and antistatic property without deterioration of physical properties is characterized by blending a polyamide ingredient showing fibril structure by difference of miscibility. CONSTITUTION: Polyester fiber having excellent hygroscopicity and antistatic property is obtained by the steps of: preparing denatured polyester type copolymerized or mixed polyethylene terephthalate or a third ingredient; including 1-15wt.% of polyalkylene oxide glycol and 0.1-1.0wt.% of a sulphonates anion surfactant(formula 1) into the denatured polyester type; blending 1-20wt.% of polyamide having miscibility being different from the polyester type in melt-spinning; and then post-finishing the blended polyester to show fibril structure. In the formula 1, R1 is C12-C18 of hydrocarbon; M is Na, K or Li.

Description

흡수성 및 제전성이 우수한 폴리에스테르 섬유의 제조방법Manufacturing method of polyester fiber excellent in water absorption and antistatic property

본 발명은 제전성 폴리에스테르에 피브릴 구조를 발현시키는 비상용성 폴리머의 일종인 폴리아마이드 성분을 블렌드 용융방사하여 제조하는 흡수성 및 제전성이 우수한 폴리에스테르 섬유에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polyester fiber excellent in absorbency and antistatic properties prepared by blend melt spinning a polyamide component, which is a kind of incompatible polymer that expresses a fibril structure in an antistatic polyester.

폴리에스테르 섬유는 기계적 강도 및 물리 화학적 성질이 우수하여 의류용 및 산업용으로 널리 사용되고 있는 반면에 용융방사법에 의한 제조를 하기 때문에 일반적으로 섬유 표면이 평활하고, 미끈거리는 느낌과 뻣뻣한 감을 주는 결점을 가지고 있다. 또한, 폴리에스테르 자체가 소수성이기 때문에 천연섬유인 면, 마 등과 비교하여 볼때 정전기 발생 및 낮은 흡수성으로 인한 사용상의 문제점 들이 지적되고 있다.Polyester fibers are widely used in clothing and industrial applications because of their excellent mechanical strength and physicochemical properties, while they are generally manufactured by melt spinning, which generally has a smooth, slippery and stiff feeling. . In addition, since the polyester itself is hydrophobic, problems in use due to the generation of static electricity and low water absorption are pointed out in comparison with cotton and hemp which are natural fibers.

지금까지 알려진 흡수성 및 제전성 폴리에스테르 섬유의 대표적인 제조 기술로는 SiO2등의 무기입자를 함유한 폴리에스테르 섬유에서 무기입자를 알카리 수용액을 사용하여 용출 제거하여 섬유표면에 미세한 요철을 형성시키는 방법과 제전성능을 가지는 화합물과 공극 생성성 화합물을 기존의 폴리에스테르에 블렌드 또는공중합하여 폴리에스테르 중공 섬유를 제조한 다음 전자와 마찬가지로 용해 추출 함으로써 섬유축과 수평방향으로 중공의 내부와 연통하는 미세공은 발현시키는 방법이 있다.Representative techniques for producing absorbent and antistatic polyester fibers known to date include methods of eluting and removing inorganic particles from polyester fibers containing inorganic particles such as SiO 2 by using an aqueous alkali solution to form fine irregularities on the surface of the fiber; A polyester hollow fiber is prepared by blending or co-polymerizing a compound having an antistatic performance and a pore-forming compound with existing polyester, and dissolving and extracting the same as the former to express micropores communicating with the inside of the hollow in the fiber axis and the horizontal direction. There is a way to.

무기 입자를 사용한 전자의 방법은 기존의 폴리에스테르 섬유에 비하여 흡수기능은 상승되지만 고분자 자체의 친수성이 떨어지기 때문에 충분한 수분의 흡수는 기대하기 어려워 수분에 의한 끈적거리는 느낌을 주는 결점이 있다.The former method using inorganic particles has a drawback that the absorption function is higher than that of the existing polyester fiber, but the hydrophilicity of the polymer itself is inferior.

한편, 블렌드 및 공중합을 통하여 폴리머 자체를 개질한 후 미세공을 발현시키는 후자의 방법에 있어서도 공극 생성성 화합물로 인한 섬유의 물리적 성질의 저하를 가져오는 단점으로 인하여 충분히 만족할 만한 정도의 흡수성을 가지지 못하는 문제점이 있다.On the other hand, the latter method of expressing micropores after modifying the polymer itself through blending and copolymerization does not have sufficient satisfactory absorbency due to the disadvantage of lowering the physical properties of the fiber due to the pore-forming compound. There is a problem.

한국특허공보 제 86-1224에는 폴리에스테르 중합단계에서 디메틸테레프탈레이트(DMT)에 대해 SiO2가 0.3∼1.2 중량 % 함유된 폴리에스테르를 직물상태에서 알카리 감량처리하여 무기입자를 용출시킨 후 미세다공성 섬유를 제조하는 방법이 제시되고 있으며, 한국특허공보 제 86-397에는 폴리에스테르 중공사에 공극 생성성 화합물로 설페이트계 화합물을 첨가하여 제직, 제편 전후에 용출시키는 방법이 소개되어 있으나 상기의 단점으로 인하여 실용화하는데 문제점이 있었다.Korean Patent Publication No. 86-1224 discloses that a polyester containing 0.3 to 1.2% by weight of SiO 2 relative to dimethyl terephthalate (DMT) in the polyester polymerization step is subjected to alkali weight loss treatment in a textile state to elute inorganic particles, and then fine porous fibers. The method for preparing the present invention has been proposed, and Korean Patent Publication No. 86-397 introduces a method of eluting before and after weaving and weaving by adding a sulfate-based compound as a pore-forming compound to polyester hollow fiber. There was a problem in practical use.

따라서 본 발명에서는 제전 성능을 가지는 폴리에스테르 섬유에 폴리머 상용성의 차이에 의하여 피브릴 구조를 발현시키는 폴리아마이드 성분을 블렌드하며,최종적으로는 섬유의 물리적 성질의 저하 없이 흡수성능과 더불어 제전 성능을 향상시킨 폴리에스테르 섬유의 제조방법을 제공하는 것을 목적으로 하고 있다.Therefore, the present invention blends a polyamide component expressing a fibril structure due to a difference in polymer compatibility to polyester fibers having antistatic performance, and finally improves antistatic performance and antistatic performance without degrading the physical properties of the fiber. It aims at providing the manufacturing method of a polyester fiber.

본 발명은 폴리에틸렌테레프탈레이트 혹은 제3성분을 공중합 또는 혼합시킨 변성 폴리에스테르류에 폴리알킬렌옥사이드글리콜과 하기 일반식(1)의 술폰산염 음이온 계면활성제 화합물을 함유시키고, 폴리에스테르류와는 비상용성을 가지는 나일론6, 나일론66등의 폴리아마이드류를 용융방사시 블렌드하여 후가공시 피브릴 구조를 발현시키는 흡수성 및 제전성이 우수한 폴리에스테르 섬유의 제조방법에 관한 것이다.The present invention comprises a polyalkylene oxide glycol and a sulfonate anion surfactant compound of the following general formula (1) in a modified polyester obtained by copolymerizing or mixing polyethylene terephthalate or a third component, and are incompatible with polyesters. The present invention relates to a method for producing a polyester fiber having excellent absorbency and antistatic property, in which polyamides such as nylon 6 and nylon 66 having a blend are melt-blended during melt spinning to express a fibril structure during post-processing.

Figure pat00002
Figure pat00002

상기에서 R1은 탄소수 12∼18의 탄화수소이고, M은 Na 또는 K 또는 LiR 1 is a hydrocarbon having 12 to 18 carbon atoms, and M is Na or K or Li

상기와 같이 제전성을 나타내기 위해 폴리알킬렌옥사이드글리콜과 술폰산염 음이온 계면활성제가 함유된 폴리에스테르에 흡수성 발현의 목적을 달성하기 위하여 폴리에스테르류와는 비상용성을 가지는 나일론6, 나일론66 등의 폴리아마이드류를 용융방사시 블렌드하여 섬유로 방사하고 연신한 후 직물 또는 편물의 형태로 만든다.In order to achieve the purpose of absorbent expression in the polyester containing polyalkylene oxide glycol and sulfonate anionic surfactant to exhibit antistatic properties as described above, nylon 6, nylon 66 and the like which have incompatibility with polyesters Polyamides are blended during melt spinning, spun into fibers, elongated and then in the form of woven or knitted fabrics.

최종적으로 직물 또는 편물은 알카리 감량의 후가공 공정을 통하여 섬유의 물리적 성질의 저하 없이 흡수성능과 더불어 우수한 제전 성능을 가지는 폴리에스테르 섬유로 제조 되어진다.Finally, the fabric or knitted fabric is made of polyester fiber having excellent antistatic performance and absorbing performance without deterioration of the physical properties of the fiber through the post processing process of reducing the alkali.

본 발명의 제전성 폴리에스테르와 비상용성을 가지는 폴리아마이드외 블렌드 용융방사에 의해 섬유의 내, 외부에 균일하게 형성된 피브릴 구조는 기존의 무기 입자 또는 공극 생성성 화합물을 사용하였을 경우보다 흡습성능을 더욱 향상시키는 작용를 하게될 뿐만 아니라 레이온조의 독특한 촉감과 dry한 느낌을 가지는 섬유를 제공한다.Fibrillated structure uniformly formed inside and outside the fibers by melt spinning with polyamide and other blends having incompatibility with the antistatic polyester of the present invention provides better hygroscopic performance than conventional inorganic particles or pore-generating compounds. Not only does it improve further, it also provides the unique feel and dryness of the rayon bath.

한편, 폴리에스테르류에 함유된 제전 성분인 폴리알킬렌옥사이드글리콜과 상기 일반식(1)의 술폰산염 음이온 계면활성제 화합물은 섬유내에서 우수한 제전 성능을 발휘하게 된다.On the other hand, polyalkylene oxide glycol which is an antistatic component contained in polyester and the sulfonate anionic surfactant compound of the general formula (1) exhibit excellent antistatic performance in fibers.

본 발명에 있어서 폴리에스테르에 제전성능을 부여하는 화합물이 되는 폴리알킬렌옥사이드글리콜로는 폴리에틸렌글리콜, 폴리(1,2-프로필렌옥사이드)글리콜, 폴리(1,3-프로필렌옥사이드)글리콜, 폴리테트라메틸렌옥사이드글리콜, 폴리헥사메틸렌옥사이드글리콜, 에틸렌옥사이드와 프로필렌옥사이드의 블록 또는 랜덤 공중합체 및 에틸렌옥사이드와 테트라하이드로퓨란의 블록 또는 랜덤 공중합체 등이 사용되어질 수 있다. 본 발명에 있어서는 폴리에틸렌글리콜이 주로 사용되어졌다.In the present invention, polyalkylene oxide glycol serving as a compound for imparting antistatic performance to polyester is polyethylene glycol, poly (1,2-propylene oxide) glycol, poly (1,3-propylene oxide) glycol, polytetramethylene Oxide glycol, polyhexamethylene oxide glycol, a block or random copolymer of ethylene oxide and propylene oxide, and a block or random copolymer of ethylene oxide and tetrahydrofuran may be used. In the present invention, polyethylene glycol is mainly used.

폴리알킬렌옥사이드글리콜의 분자량은 1,000∼100,000, 특히 4,000∼40,000 의 범위가 더욱 바람직하며, 수평균 분자량이 1,000 미만에서는 얻어진 폴리에스테르의 공극 생성성과 제전성능이 미약하게 되고, 40,000을 넘는 경우에 있어서는 생성된 공극의 크기가 과도하게 클 뿐만아니라 상용성면에서도 바람직하지 못하다.The molecular weight of the polyalkylene oxide glycol is more preferably in the range of 1,000 to 100,000, particularly in the range of 4,000 to 40,000. When the number average molecular weight is less than 1,000, the pore formation and the antistatic performance of the obtained polyester become weak, and in the case of exceeding 40,000, The size of the resulting pores is not only too large but also undesirable in terms of compatibility.

본 발명에 사용된 폴리알킬렌옥사이드글리콜은 그대로도 양호한 내열성을 보이지만, 힌더드 페놀계 화합물을 블렌드 또는 공중합시 병용하면 특히 내열성이 향상되어진다. 여기에서 힌더드 페놀계 화합물로는 페놀계 수산기의 인접위치에 입체장해를 가진 치환기를 가진 페놀 유도체로, 예를들면 테르라키스[메틸렌-3-(3,5-디-제3부틸-4-하이드록시페닐)프로피오네이트]메탄 (상품명; 이가녹스 1010) 등이 사용되어질 수 있다.The polyalkylene oxide glycol used in the present invention shows good heat resistance as it is, but especially when the hindered phenol compound is used in blend or copolymerization, heat resistance is improved. Herein, the hindered phenolic compound is a phenol derivative having a substituent having steric hindrance in the adjacent position of the phenolic hydroxyl group, for example, terakis [methylene-3- (3,5-di-tertbutyl-4-). Hydroxyphenyl) propionate] methane (trade name; Iganox 1010) and the like can be used.

이때 첨가되어지는 힌더드 페놀계 화합물의 첨가량은 폴리알킬렌옥사이드글리콜 성분에 대해 0.5 중량% ~ 3.0 중량% 가 바람직하다. 만약 0.5 중량% 미만일 경우에는 목적하는 내열성의 효과를 얻기 힘들고, 3.0 중량%를 초과 하게되면 방사 작업성 및 원사물성, 특히 원사강도가 저하된다.In this case, the amount of the hindered phenol compound added is preferably 0.5% by weight to 3.0% by weight based on the polyalkylene oxide glycol component. If it is less than 0.5% by weight, it is difficult to obtain the desired heat resistance effect, and if it exceeds 3.0% by weight, spinning workability and yarn properties, in particular, yarn strength are lowered.

폴리알킬렌옥사이드글리콜은 방사 또는 중합말기에 블렌드할 수도 있으며, 중합시 공단량체로 첨가하여 공중합할 수도 있다. 블렌드 하는 예로는 폴리알킬렌옥사이드글리콜과 통상의 폴리에틸렌테레프탈레이트 칩을 블렌드하여 블렌드물 중의 폴리알킬렌옥사이드글리콜의 성분량이 최종 목적하는 중량%가 되도록 하여 방사하는 방법이 있고, 공중합 하는 예로는 테레프탈산과 에틸렌글리콜을 에스테르화 반응시켜 얻은 비스-베타-하이드록시에틸렌테레프탈레이트 구조의 올리고머와 폴리알킬렌옥사이드글리콜을 반응기에 넣고 아연아세테이트, 삼산화안티몬 등의 중축합 촉매의 존재하에서 220℃에서 260℃, 상압하에서 에스테르 교환반응 시킨 후, 감압하여 진공하에서 반응시키는 방법이 있다.The polyalkylene oxide glycol may be blended at the end of spinning or polymerization, or may be copolymerized by adding a comonomer during polymerization. An example of blending is a method of blending polyalkylene oxide glycol and a conventional polyethylene terephthalate chip so that the component amount of polyalkylene oxide glycol in the blend is the final desired weight% and spinning is carried out as an example of copolymerization with terephthalic acid. The oligomer of the bis-beta-hydroxyethylene terephthalate structure obtained by esterification of ethylene glycol, and polyalkylene oxide glycol were put into a reactor, and 220 degreeC at 260 degreeC and atmospheric pressure in presence of polycondensation catalysts, such as zinc acetate and antimony trioxide, After transesterification under a reduced pressure, there is a method of reacting under reduced pressure.

본 발명에 사용하는 폴리알킬렌옥사이드글리콜은 블렌드 하거나 공중합 하는 방법에 있어서 임의의 단계에서 투입해도 좋으나 공중합시에는 에스테르화 반응말기 중축합 반응전에 투입하는 것이 더욱 좋다.The polyalkylene oxide glycol used in the present invention may be added at any stage in the method of blending or copolymerizing, but it is more preferable to add the polyalkylene oxide glycol before the final polycondensation reaction at the time of copolymerization.

혼합물은 폴리알킬렌옥사이드글리콜의 첨가량이 폴리에스테르 성분에 대해 1∼15 중량%의 범위가 되도록 하는 것이 바람직하다. 혼합물중 폴리에스테르 성분에 대한 폴리알킬렌옥사이드글리콜의 첨가량이 15 중량%를 초과할 경우에는 방사시에 사절 및 강신도 저하, 착색 등의 피해를 발생시키고 1 중량% 미만인 경우에는 제전성 발휘 효과가 불충분하다.The mixture is preferably such that the amount of polyalkylene oxide glycol added is in the range of 1 to 15% by weight based on the polyester component. When the amount of the polyalkylene oxide glycol added to the polyester component in the mixture exceeds 15% by weight, damages such as trimming and elongation, coloring, etc. occur during spinning, and when the amount is less than 1% by weight, the effect of exhibiting antistatic properties is insufficient. Do.

상기 일반식(1)의 화합물은 섬유 고분자쇄의 비결정부 생성 증대 및 대전 방지 성능 향상을 위해 중합 또는 방사시에 폴리에스테르 중합물과 균일 혼합하여 용융방사 함이 바람직 하며 투입량은 중합체 대비 0.1∼1.0 중량% 사용함을 특징으로 한다. 0.1 중량% 미만이면 제전효과를 얻기 어렵고 1.0 중량%를 초과하면 사절과 황변현상을 나타나는 단점이 있다.The compound of the general formula (1) is preferably melt-spun by homogeneous mixing with the polyester polymer during polymerization or spinning in order to increase the formation of amorphous portions of the fiber polymer chain and to improve the antistatic performance, and the dosage is 0.1 to 1.0 weight of the polymer. % Use. If it is less than 0.1% by weight, it is difficult to obtain an antistatic effect. If it exceeds 1.0% by weight, there is a disadvantage in that trimming and yellowing occur.

후가공 공정인 알카리 감량후 폴리에스테르와 비상용성에 의해 피브릴 구조를 발현시켜 우수한 흡수성과 촉감을 나타나게 하는 나일론6, 나일론66 등의 폴리아마이드류는 폴리에스테르 중합물과 균일 혼합하여 용융방사 함이 바람직 하며 투입량은 중합체 대비 1∼20 중량% 사용함을 특징으로 한다. 1 중량% 미만이면 알카리 감량후 피브릴 발현효과를 얻기 어렵고 20 중량%를 초과하면 비상용성의 문제로 인하여 사절과 섬유물성 저하를 초래하게 된다.Polyamides, such as nylon 6 and nylon 66, which exhibit fibrillated structure by polyester and incompatibility after alkali reduction, which is a post-processing process, exhibit excellent water absorption and tactile feel, are preferably mixed by melt mixing with polyester polymer. It is characterized by using 1 to 20% by weight relative to the polymer. If it is less than 1% by weight, it is difficult to obtain the fibrils expression effect after reducing the alkali, and if it exceeds 20% by weight, it will cause trimming and deterioration of fiber properties due to incompatibility problems.

상기와 같은 방법으로 얻어진 폴리에스테르 섬유는 일반적인 제전성과 흡수성을 가지는 폴리에스테르 섬유가 중공섬유로 방사 되어지는 것과는 달리 통상의 노즐을 사용하여 방사하여도 우수한 제전성과 흡수성을 나타내는 장점을 가지기 때문에 제조 원가면에서 유리하다.The polyester fiber obtained by the above method has the advantage of exhibiting excellent antistatic property and absorbency even when spun using ordinary nozzles, unlike polyester fibers having general antistatic properties and water absorbency are spun into hollow fibers. Is advantageous in

본 발명에 의해 제조된 섬유를 통상의 방사 노즐을 사용하여 제사한 후, 직물 또는 편물의 형태로 만들고, 이때 얻어진 직물 또는 편물은 후가공 공정중 알카리 감량 가공을 거치게 된다. 피브릴 발현 주변부분의 용출에 사용되는 알카리 수용액으로는 NaOH나 KOH를 농도 0.5%∼15%, 더욱 바람직하기로는 1%∼10%로 하여 사용하며, 처리온도는 70℃∼130℃, 더욱 바람직하기로는 80℃∼120℃로 하여 감량율 1%∼70%, 더욱 바람직하기로는 5%∼50%로 하여 사용하게 되며, 최종적으로 흡수성이 우수한 폴리에스테르 제전 섬유가 얻어지게 된다.After the fiber produced by the present invention is sacrificed using a conventional spinning nozzle, it is made into the form of a woven fabric or knitted fabric, and the obtained woven fabric or knitted fabric is subjected to alkali reduction during the post processing process. As an aqueous alkali solution used for elution of fibrils, the concentration of NaOH or KOH is 0.5% to 15%, more preferably 1% to 10%, and the treatment temperature is 70 ° C to 130 ° C. In the following, the reduction ratio is 1% to 70%, more preferably 5% to 50%, and finally a polyester antistatic fiber having excellent water absorption is obtained.

이하 본 발명을 실시예 및 비교예에 의거하여 구체적으로 설명한다.Hereinafter, the present invention will be specifically described based on Examples and Comparative Examples.

실시예 1Example 1

테레프탈산과 에틸렌글리콜을 에스테르화 반응시켜 얻은 폴리에틸렌테레프탈레이트 올리고머에 대해 제전 성능을 가지는 폴리에틸렌글리콜(분자량 20,000) 성분을 4.0 중량%, 도데실벤젠술폰산 나트륨은 0.4 중량% 첨가한다. 한편, 중축합 반응은 아연아세테이트 0.01 중량%를 첨가하여 250℃에서 1시간 에스테르 교환반응을 시킨 후, 중합촉매인 삼산화안티몬 0.014 중량%를 첨가하여 0.1∼0.2 mmHg로 감압하면서 285℃까지 승온하여 2시간 동안 진행 시킨다. 이때 얻어진 중합체의 고유점도는 0.72 이었다. 이렇게 얻어진 폴리에스테르 칩을 열풍건조기에서 125℃에서 8시간 건조한 후 4.0 중량%의 나일론6(분자량 21,500, 용융점 229℃)와 균일 혼할하여 용융방사 하였다. 용융방사는 통상의 75데니어/36필라멘트 노즐을 사용하였고, 방사온도 280℃, 권취속도 1000m/min에서 방사하여 미연신사를 얻었다. 이 미연신사를 연신배율 3.7으로 연신하여 얻어진 폴리에스테르 섬유로 편직물을 제조하였다. 이 편직물을 4% NaOH 수용액으로 감량처리하여 흡수성과 제전성을 측정하였으며 그 결과는 표 1과 같다.To the polyethylene terephthalate oligomer obtained by esterifying terephthalic acid and ethylene glycol, 4.0 wt% of polyethylene glycol (molecular weight 20,000) having antistatic performance and 0.4 wt% of sodium dodecylbenzenesulfonate are added. On the other hand, the polycondensation reaction was added 0.01% by weight of zinc acetate and subjected to transesterification at 250 ° C for 1 hour, then 0.014% by weight of antimony trioxide, a polymerization catalyst, was added and heated up to 285 ° C under reduced pressure to 0.1-0.2 mmHg. Proceed for hours. The intrinsic viscosity of the polymer obtained at this time was 0.72. The polyester chip thus obtained was dried at 125 ° C. for 8 hours in a hot air dryer, and then melt mixed with 4.0 wt% of nylon 6 (molecular weight 21,500, melting point 229 ° C.) for uniform mixing. Melt spinning used a conventional 75 denier / 36 filament nozzle, spinning at a spinning temperature of 280 ℃, winding speed 1000m / min to obtain an undrawn yarn. The knitted fabric was manufactured from the polyester fiber obtained by extending | stretching this undrawn yarn to draw ratio 3.7. This knitted fabric was reduced in 4% aqueous NaOH solution to measure absorbency and antistatic properties. The results are shown in Table 1 below.

실시예 2∼3, 비교예 1∼4Examples 2-3 and Comparative Examples 1-4

다음 표 1과 같이 폴리에틸렌테레프탈레이트 올리고머에 대한 폴리에틸렌글리콜의 함량, 도데실벤젠술폰산 나트륨의 함량 및 나일론6의 함량을 달리하는 것외에는 실시예 1과 동일한 방법으로 실시 하였다. 4% NaOH 수용액으로 감량가공한 후 측정한 흡수성과 제전성 측정 결과는 표 1과 같다.As shown in Table 1, except that the polyethylene glycol content, the sodium dodecylbenzene sulfonate content and the nylon 6 content of the polyethylene terephthalate oligomer were changed in the same manner as in Example 1. Absorption and antistatic properties measured after the weight loss process with 4% NaOH aqueous solution are shown in Table 1.

[표 1]TABLE 1

Figure pat00003
Figure pat00003

* 흡수높이(mm/10min) 측정 방법* How to measure absorption height (mm / 10min)

2.5 20cm의 시험편을 5매이상 채취하여 각 시험편 하단 1cm를 증류수가 들어있는 용기의 물속에 침지한 후 10분이 경과하였을 때 모세관 현상으로 상승한 물의 높이를 측정하여 그 평균값을 표시한다.2.5 Collect 5 or more 20 cm specimens and immerse 1 cm of the lower end of each specimen in the water of a container containing distilled water. Measure the height of the water raised by capillary action when 10 minutes have elapsed.

* 제전성 측정 방법* How to measure antistatic

제전성 측정은 측정 시료를 5회 세탁후 건조하여 25℃, 40% 상대습도에서 24시간 방치한 후 마찰 대전압을 측정하였다.Antistatic measurement was measured after washing the sample 5 times, dried, and left for 24 hours at 25 ℃, 40% relative humidity and then measured the frictional electrification voltage.

본 발명은 물리적 성질의 저하 없이 흡수성능과 더불어 제전 성능을 향상시킨 폴리에스테르 섬유의 제조를 가능하게 함은 물론 본 발명의 섬유는 통상의 방사 노즐을 사용하였기 때문에 제조 원가면에서 유리한 장점을 가진다.The present invention enables the production of polyester fibers with improved water absorption performance and antistatic performance without deterioration of physical properties, as well as the fiber of the present invention has an advantageous advantage in terms of manufacturing cost because it uses a conventional spinning nozzle.

Claims (4)

폴리에틸렌테레프탈레이트 혹은 제 3성분을 공중합 또는 혼합시킨 변성 폴리에스테르류에 폴리알킬렌옥사이드글리콜과 하기 일반식(1)의 술폰산염 음이은 계면활성제 화합물을 함유시키고, 폴리에스테르류와는 비상용성을 가지는 폴리아마이드류를 용융방사시 블렌드하여 후가공시 피브릴 구조를 발현시키는 것을 특징으로 하는 흡수성 및 제전성이 우수한 폴리에스테르 섬유의 제조 방법.The modified polyesters obtained by copolymerizing or mixing polyethylene terephthalate or the third component contain polyalkylene oxide glycol and sulfonate salts of the following general formula (1), and have a surfactant compound, and have incompatibility with polyesters. A method for producing a polyester fiber having excellent water absorption and antistatic property, characterized by blending polyamides during melt spinning to express a fibril structure during post-processing.
Figure pat00004
Figure pat00004
상기에서 R1은 탄소수 12∼18의 탄화수소이고, M은 Na 또는 K 또는 LiR 1 is a hydrocarbon having 12 to 18 carbon atoms, and M is Na or K or Li
제 1항에 있어서, 폴리알킬렌옥사이드글리콜은 폴리에스테르 성분에 대하여 1∼ 15 중량% 첨가된 것을 특징으로 하는 흡수성 및 제전성이 우수한 폴리에스테르의 제조방법.The method for producing a polyester having excellent water absorption and antistatic property according to claim 1, wherein the polyalkylene oxide glycol is added in an amount of 1 to 15% by weight based on the polyester component. 제 1항에 있어서, 술폰산염 음이온 계면활성제는 폴리에스테르 성분에 대하여 0.1 ∼ 1.0 중량% 첨가된 것을 특징으로 하는 흡수성 및 제전성이 우수한 폴리에스테르 섬유의 제조방법.The method for producing a polyester fiber having excellent water absorption and antistatic property according to claim 1, wherein the sulfonate anionic surfactant is added in an amount of 0.1 to 1.0 wt% based on the polyester component. 제 1항에 있어서, 폴리아마이드는 폴리에스테르 성분에 대하여 1 ∼ 20중량%첨가된 것을 특징으로 하는 흡수성 및 제전성이 우수한 폴리에스테르 섬유의 제조방법.The method for producing a polyester fiber having excellent water absorption and antistatic property according to claim 1, wherein the polyamide is added in an amount of 1 to 20% by weight based on the polyester component.
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