KR101495919B1 - Method of manufacturing aromatic polyamide filament and a aromatic polyamide filament by the same - Google Patents

Method of manufacturing aromatic polyamide filament and a aromatic polyamide filament by the same Download PDF

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KR101495919B1
KR101495919B1 KR20080135825A KR20080135825A KR101495919B1 KR 101495919 B1 KR101495919 B1 KR 101495919B1 KR 20080135825 A KR20080135825 A KR 20080135825A KR 20080135825 A KR20080135825 A KR 20080135825A KR 101495919 B1 KR101495919 B1 KR 101495919B1
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aromatic polyamide
wholly aromatic
polyamide filament
spinning
filament
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KR20100077785A (en
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장세훈
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주식회사 효성
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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
    • D01F6/60Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • D01F6/605Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides from aromatic polyamides
    • 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
    • D01D10/00Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/02Heat treatment
    • 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
    • D01D10/00Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/06Washing or drying
    • 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
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/44Yarns or threads characterised by the purpose for which they are designed
    • D02G3/442Cut or abrasion resistant yarns or threads
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/44Yarns or threads characterised by the purpose for which they are designed
    • D02G3/446Yarns or threads for use in automotive applications
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F41WEAPONS
    • F41HARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
    • F41H1/00Personal protection gear
    • F41H1/02Armoured or projectile- or missile-resistant garments; Composite protection fabrics
    • 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
    • D10B2331/02Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyamides
    • D10B2331/021Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyamides aromatic polyamides, e.g. aramides
    • 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
    • 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
    • D10B2401/062Load-responsive characteristics stiff, shape retention
    • 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
    • D10B2401/063Load-responsive characteristics high strength

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)

Abstract

본 발명의 구현예들은 전방향족 폴리아미드 필라멘트의 제조방법 및 그에 의하여 제조된 전방향족 폴리아미드 필라멘트에 관한 것으로서, 보다 구체적으로는 전방향족 폴리아미드 중합체를 포함하는 방사도프를 방사노즐을 통하여 응고액조로 방사하여 전방향족 폴리아미드 필라멘트를 제조함에 있어서, 방사노즐 하부와 응고액조 사이에 60~120℃로 가열된 질소 유체층을 통과하여 방사하는 전방향족 폴리아미드 필라멘트의 제조방법 및 그에 의하여 제조된 전방향족 폴리아미드 필라멘트에 관한 것이다. Embodiments of the present invention are directed to a method for producing wholly aromatic polyamide filaments and to wholly aromatic polyamide filaments produced thereby, and more particularly, to a method for producing wholly aromatic polyamide filaments by spinning a spinning dope containing a wholly aromatic polyamide polymer through a spinning nozzle A method for producing wholly aromatic polyamide filaments by spinning through a nitrogen fluid layer heated to a temperature of 60 to 120 DEG C between a lower part of a spinning nozzle and a coagulating solution tank, To an aromatic polyamide filament.

전방향족 폴리아미드 필라멘트, 질소 유체층     A wholly aromatic polyamide filament, a nitrogen fluid layer

Description

전방향족 폴리아미드 필라멘트의 제조방법 및 그에 의하여 제조된 전방향족 폴리아미드 필라멘트{METHOD OF MANUFACTURING AROMATIC POLYAMIDE FILAMENT AND A AROMATIC POLYAMIDE FILAMENT BY THE SAME}TECHNICAL FIELD The present invention relates to a method for producing a wholly aromatic polyamide filament, and to a wholly aromatic polyamide filament produced by the method and a method for producing the wholly aromatic polyamide filament.

본 발명의 구현예들은 전방향족 폴리아미드 필라멘트의 제조방법 및 그에 의하여 제조된 전방향족 폴리아미드 필라멘트에 관한 것이다. Embodiments of the present invention are directed to a process for producing wholly aromatic polyamide filaments and to wholly aromatic polyamide filaments produced thereby.

전방향폭 폴리아미드 필라멘트는 방향족 디아민 화합물과 방향족 디에시드클로라이드 화합물을 중합시켜 얻은 전방향족 폴리아미드 중합체로부터 얻어지며, 기계적 강신도가 크고, 내열성이 우수하며 전기적 절연성이 우수하여, 고강신도, 고탄성율이 요구되어지는 우주항공 분야, 자동찬 산업 분야, 방탄 및 방화와 같은 안전 및 소방분야, 고기능성 필라멘트 산업 분야 등 전산업 분야에 걸쳐 그 적용 범위가 넓다. The omni-directional width polyamide filaments are obtained from a wholly aromatic polyamide polymer obtained by polymerizing an aromatic diamine compound and an aromatic diacid chloride compound, and have high mechanical strength, excellent heat resistance, excellent electrical insulation, high strength elongation and high modulus Its applications range from aerospace to automotive, fire safety and fire protection such as bulletproof and fire protection, and high-performance filament industry.

일반적으로 전방향족 폴리아미드 필라멘트는 방향족 디아민과 방향족 디에시드클로라이드를 N-메틸-2-피롤리돈을 포함하는 중합용매 중에서 중합시켜 전방향 족 폴리아미드 중합체를 제조하는 공정과, 상기 중합체를 농황산 용매에 용해시켜 방사원액을 제조하는 공정과, 상기 방사원액을 방사 구금으로부터 방사하여 방사된 방사물을 비응고성 유체층을 통해 응고액 욕조내로 통과시켜 필라멘트를 형성하는 공정과, 상기 필라멘트를 수세, 건조 및 열처리하는 공정 들을 거쳐 제조된다. Generally, wholly aromatic polyamide filaments are prepared by polymerizing an aromatic diamine and an aromatic diacid chloride in a polymerization solvent containing N-methyl-2-pyrrolidone to prepare an allophanic polyamide polymer, A step of producing a fiberizable liquid by spinning the fiberizable liquid from a spinneret and passing the irradiated radiation through a non-compatible fluid layer into a coagulating bath to form filaments; and washing and drying the filament And heat treatment.

이 때, 방사구금을 통해 방사된 방사물을 공기 등과 같은 비응고성 유체층을 통해 응고액 욕조내로 통과시키는 경우, 방사물의 표면과 내부의 물성이 불균일해질 수 있다. In this case, when the radiation emitted through the spinneret is passed through the non-aggressive fluid layer such as air or the like into the coagulating bath, the physical properties of the surface and the interior of the radiation may become uneven.

본 발명의 구현예들은 전방향족 폴리아미드 필라멘트를 제조함에 있어서, 방사 노즐로부터 방사된 방사물을 60~120℃로 가열된 질소(dry nitrogen) 유체층에 통과시켜 방사물의 표면과 내부가 균일하게 응고된 전방향족 폴리아미드 필라멘트의 제조방법을 제공하는 것이다. In embodiments of the present invention, when manufacturing the wholly aromatic polyamide filaments, the radiation emitted from the spinning nozzle is passed through a dry nitrogen fluid layer heated to 60 to 120 ° C., And a method for producing a coagulated wholly aromatic polyamide filament.

본 발명의 구현예들은 상기 제조방법에 의해 제조되는 강신도 및 탄성율이 우수한 전방향족 폴리아미드 필라멘트를 제공하는 것이다. Embodiments of the present invention provide a wholly aromatic polyamide filament having excellent strength and elasticity, which is produced by the above-mentioned production method.

본 발명의 하나의 양상은One aspect of the present invention is

전방향족 폴리아미드 중합체를 농황산 용매에 용해시켜 제조한 방사도프를 방사노즐을 통하여 응고액조로 방사하여 전방향족 폴리아미드 필라멘트를 제조함에 있어서, 방사노즐 하부와 응고액조 사이에 형성된 60~120℃로 가열된 질소 (dry nitrogen) 유체층을 통과하여 방사하는 전방향족 폴리아미드 필라멘트의 제조방법에 관한 것이다. In preparing a wholly aromatic polyamide filament by spinning a spinning dope prepared by dissolving a wholly aromatic polyamide polymer in a concentrated sulfuric acid solvent through a spinning nozzle into a coagulating solution tank, To a method for producing wholly aromatic polyamide filaments that radiate through a heated nitrogen fluid layer.

본 발명의 다른 양상은 상기 제조방법에 의해 제조되는 전방향족 폴리아미드 필라멘트에 관한 것이다. Another aspect of the present invention relates to a wholly aromatic polyamide filament produced by the above method.

본 발명의 구현예들에 의한 전방향족 폴리아미드 필라멘트는 수분과의 반응속도가 늦추어지므로 방사도프를 균일하게 응고시켜 보다 향상된 강신도 및 탄성율을 나타낸다. The wholly aromatic polyamide filaments according to the embodiments of the present invention slow down the reaction rate with moisture, and therefore, the spinning dope uniformly coagulates to exhibit improved strength and elasticity.

이하, 첨부 도면을 참조하여 본 발명의 구현예들에 대하여 더욱 상세하게 설명한다. 본 발명의 하나의 양상은 전방향족 폴리아미드 중합체를 농황산 용매에 용해시켜 제조한 방사도프를 방사노즐을 통하여 응고액조로 방사하여 전방향족 폴리아미드 필라멘트를 제조함에 있어서, 방사노즐 하부와 응고액조 사이에 형성된60~120℃로 가열된 질소 유체층을 통과하여 방사하는 전방향족 폴리아미드 필라멘트의 제조방법에 관계한다. Hereinafter, embodiments of the present invention will be described in more detail with reference to the accompanying drawings. One aspect of the present invention relates to a method for producing a wholly aromatic polyamide filament by spinning a radial dope prepared by dissolving a wholly aromatic polyamide polymer in a concentrated sulfuric acid solvent through a spinning nozzle into a coagulating solution tank, And then radiating through a nitrogen fluid layer heated to 60-120 캜 formed in the reactor.

도 1은 본 발명의 일구현예에 의한 전방향족 폴리아미드 필라멘트를 제조하는 공정 개략도이다. 도 1을 참조하여 보다 구체적으로 설명하면, 본 발명의 일구현에에 의한 전방향족 폴리아미드 필라멘트를 제조하기 위하여 먼저 전방향족 폴리아미드 중합체를 농황산 용매에 용해시켜 방사도프를 제조한다. 중합체를 제조하는 한 가지 예로는 전체 원료 및 용매계의 합산에 대한 p-페닐렌디아민 및 테레프탈로일클로라이드의 비를 10.0 내지 13.0 wt% 로 하고, 당량비를 0.95 내지 1.01의 비율로 하여 N-메틸 피롤리돈(NMP)에 용해시킨 용액을 10℃ 이하의 온도에서 교반장치가 설치되어 있는 중합용 반응기 내에 투입한 후 교반하여 겔상의 중합체를 제조하고, 이를 분쇄, 중화, 수세 및 건조시켜 미세 분말상의 폴리(p-페닐렌테레프탈아미드) 중합체를 제조한다. 이와 같이 제조된 폴리(p-페닐렌테레프탈아미드) 중합체는 고유점도 5.5 내지 7.0 dL/g 범위를 갖는다.1 is a schematic view of a process for producing a wholly aromatic polyamide filament according to an embodiment of the present invention. More specifically, referring to FIG. 1, to prepare a wholly aromatic polyamide filament according to an embodiment of the present invention, a wholly aromatic polyamide polymer is first dissolved in a concentrated sulfuric acid solvent to prepare a spinning dope. One example of the preparation of the polymer is a method in which the ratio of p-phenylenediamine and terephthaloyl chloride to the total of the raw materials and the solvent system is adjusted to 10.0 to 13.0 wt% and the equivalence ratio is set to 0.95 to 1.01, (NMP) in a polymerization reactor equipped with a stirrer at a temperature of 10 ° C or lower and stirring the mixture to prepare a gel polymer. The polymer is pulverized, neutralized, washed, and dried to obtain a fine powder Of a poly (p-phenylene terephthalamide) polymer. The poly (p-phenylene terephthalamide) polymer thus prepared has an intrinsic viscosity ranging from 5.5 to 7.0 dL / g.

다음으로, 폴리(p-페닐렌테레프탈아미드) 중합체를 70 내지 90℃에서 농황산에 용해시켜 방사도프를 제조한다. Next, the radiation dope is prepared by dissolving the poly (p-phenylene terephthalamide) polymer in concentrated sulfuric acid at 70 to 90 占 폚.

상기 방사도프를 제조하는 공정에서 폴리(p-페닐렌테레프탈아미드) 중합체의 양은 방사 도프 전체에 대해 19.1 내지 19.9 wt%일 수 있다. The amount of poly (p-phenylene terephthalamide) polymer in the process of preparing the spinning dope may be from 19.1 to 19.9 wt% based on the total spin dope.

농황산 농도는 97 내지 101.1% 일 수 있고, 클로로황산이나 플루오로황산 등도 사용될 수 있다. The concentration of the concentrated sulfuric acid may be 97 to 101.1%, and chlorosulfuric acid, fluorosulfuric acid and the like may also be used.

이어서 제조한 방사도프를 방사노즐(1)로 방사한 후 방사된 방사물을 질소 충전 장치(2)에 의해 형성된 60~120℃로 가열된 질소 유체층(3) 내로 통과시킨다. 이 때, 상기 질소 유체층의 높이는 5 내지50mm 인 것이 방사성이나 필라멘트의 물성 향상에 바람직하다. 이와 같이 방사노즐로 방사된 방사물이 가열된 질소 유체층을 통과함으로 인해 수분과의 반응속도가 늦추어져서 방사도프가 균일하게 응고되어 제조된 전방향족 폴리아미드 필라멘트의 강신력이 증가한다.  The radiant dope thus prepared is then radiated to the spinning nozzle 1 and the radiated radiation is passed into the nitrogen fluid layer 3 heated to 60-120 ° C. formed by the nitrogen-filling device 2. At this time, the height of the nitrogen fluid layer is preferably 5 to 50 mm for improving the physical properties of the radioactive or filament. As the radiation emitted by the spinning nozzle passes through the heated nitrogen fluid layer, the reaction rate with moisture is slowed and the spinning dope uniformly coagulates, thereby increasing the strength of the wholly aromatic polyamide filament.

다음으로 응고액이 담긴 응고액조(4)를 통과시킨 다음 수세, 건조 및 열처리하여 전방향족 폴리아미드 필라멘트를 얻을 수 있다. 응고액은 5 내지 15 wt% 황산 수용액으로 이루어질 수 있다. Next, the wholly aromatic liquid polyamide filaments can be obtained by passing the coagulating bath (4) containing the coagulating solution, followed by washing with water, drying and heat treatment. The coagulating solution may be composed of 5 to 15 wt% aqueous sulfuric acid solution.

본 발명의 다른 양상에 의하면, 상기 방사 노즐(1) 및 응고액조(4) 전체를 가열된 질소 분위기로 할 수 있다.  According to another aspect of the present invention, the entire spinning nozzle (1) and the coagulating solution tank (4) can be heated to a nitrogen atmosphere.

이와 같은 본 발명의 구현예들에 의하여 제조된 전방향족 폴리아미드 필라멘트는 강신도 및 탄성율이 우수하다. The wholly aromatic polyamide filaments produced by the embodiments of the present invention have excellent strength and elasticity.

이하, 구체적인 실시예를 가지고 본 발명의 구성 및 효과를 보다 상세히 설명하지만, 이들 실시예는 단지 본 발명을 보다 명확하게 이해시키기 위한 것일 뿐, 본 발명의 범위를 한정하고자 하는 것은 아니다. Hereinafter, the structure and effects of the present invention will be described in more detail with reference to specific examples. However, these examples are merely for the purpose of understanding the present invention more clearly and do not limit the scope of the present invention.

실시예 1: 전방향족 폴리아미드 필라멘트의 제조Example 1: Preparation of wholly aromatic polyamide filaments

P-페닐렌디아민 와 테레프탈로일클로라이드를 등몰량으로 저온 중합시켜 제조한 고유 점도 6.3 dL/g의 폴리(p-페닐렌테레프탈아미드) 중합체 19.5 중량%를 트윈 스크류 압출기에서 농도가 101.1%인 황산에 85℃ 로 용해시켜 광학적 비등방성 방사원액인 방사도프를 제조하였다.19.5 wt% of a poly (p-phenylene terephthalamide) polymer having an intrinsic viscosity of 6.3 dL / g, prepared by low-temperature polymerization of p-phenylenediamine and terephthaloyl chloride in an equimolar amount, was dissolved in a sulfuric acid At 85 占 폚 to prepare an optical anisotropic spinning dope, spinning dope.

다음으로, 제조된 방사도프를 도 1에 도시된 방사 구금을 통해 방사한 후, 방사된 방사물을 7mm 높이에 80 ℃ 로 가열된 질소(dry nitrogen) 유체층을 통과시킨 후, 3℃ 의 응고액의 담겨져 있는 응고액조 내로 통과시켜 필라멘트를 형성하였다.Next, the prepared spinning dope was radiated through the spinneret shown in Fig. 1, and then the spinning spinning was passed through a dry nitrogen fluid layer heated to 80 DEG C at a height of 7 mm, And passed through a coagulating bath containing a solid solution to form filaments.

이어서, 제조된 필라멘트를 중화, 수세, 건조하여 1500 데니어의 원사를 권취하였다. 제조된 전방향족 폴리아미드 필라멘트의 물성을 평가하여 표 2에 나타내었다.Then, the produced filament was neutralized, washed with water and dried to obtain a yarn of 1500 denier. The properties of the prepared wholly aromatic polyamide filaments were evaluated and are shown in Table 2.

실시예 2-3: 전방향족 폴리아미드 필라멘트의 제조Example 2-3: Preparation of wholly aromatic polyamide filaments

질소 유체층의 높이와 온도를 표 1에 나타낸 바와 같이 변화시키면서 실시예 1과 동일한 방법으로 실험을 수행하여 전방향족 폴리아미드 필라멘트를 제조하였다.A wholly aromatic polyamide filament was prepared by conducting the same experiment as in Example 1 while changing the height and temperature of the nitrogen fluid layer as shown in Table 1.

제조된 전방향족 폴리아미드 필라멘트의 물성을 평가하여 표 2에 나타내었다.The properties of the prepared wholly aromatic polyamide filaments were evaluated and are shown in Table 2.

비교예 1: 전방향족 폴리아미드 필라멘트의 제조Comparative Example 1: Preparation of wholly aromatic polyamide filaments

질소 유체층의 높이와 온도를 표 1에 나타낸 바와 같이 변화시키면서 실시예 1과 동일한 방법으로 실험을 수행하여 전방향족 폴리아미드 필라멘트를 제조하였다.A wholly aromatic polyamide filament was prepared by conducting the same experiment as in Example 1 while changing the height and temperature of the nitrogen fluid layer as shown in Table 1.

제조된 전방향족 폴리아미드 필라멘트의 물성을 평가하여 표 2에 나타내었다.The properties of the prepared wholly aromatic polyamide filaments were evaluated and are shown in Table 2.

본 발명에 있어서, 강도 및 탄성율은 아래와 같은 방법으로 측정하였다.In the present invention, the strength and the modulus of elasticity were measured by the following methods.

강도burglar

인스트론(Instron) 5565(인스트론사제, 미국)를 이용하여, ASTM D 885의 규정에 따라 표준 상태(20℃, 65% 상대습도) 하에서 길이가 250mm인 샘플사를 이용하여 샘플사가 파단될 때의 강력(g)을 측정한 다음 이를 샘플사의 데니어로 나누어 강도를 구하였다. 상기 강도는 5회 테스트한 후 그 평균값으로 하였다 이때, 인장속도는 300mm/분으로 하였고, 80turns/m의 조건으로 측정하였다.When a sample yarn was broken using a sample yarn having a length of 250 mm under a standard state (20 ° C, 65% relative humidity) according to the specification of ASTM D 885 using Instron 5565 (manufactured by Instron, USA) The strength (g) of the sample was measured and then divided by the denier of the sample yarn to determine the strength. The strength was measured five times, and then the average value was obtained. At this time, the tensile speed was set to 300 mm / min and measured under the condition of 80 turns / m.

탄성률Elastic modulus

상기의 강도 측정 조건으로 샘플사의 응력-변형 곡선을 구한 다음, 상기 응력-변형율 곡선상의 기울기로부터 계산한다.The stress-strain curve of the sample yarn is obtained under the above-described conditions for measuring the strength, and is then calculated from the slope on the stress-strain curve.

[표 1][Table 1]

실시예 1Example 1 실시예 2Example 2 실시예 3Example 3 비교예 1Comparative Example 1 N2 유체층N 2 fluid layer 높이(mm)Height (mm) 77 1010 2020 1010 온도(℃)Temperature (℃) 8080 8080 100100 1515 응고액Huge sum 온도(℃)Temperature (℃) 33 33 33 33 방사 속도Spinning speed 속도(m/min)Speed (m / min) 350350 350350 500500 350350

[표 2][Table 2]

실시예 1Example 1 실시예 2Example 2 실시예 3Example 3 비교예 1Comparative Example 1 강도(g/d)Strength (g / d) 24.124.1 23.423.4 22.122.1 22.422.4 신도 (%)Shinto (%) 3.883.88 3.93.9 4.04.0 3.833.83 탄성율 (g/d)Modulus of elasticity (g / d) 580580 550550 520520 540540

이상에서 본 발명의 바람직한 구현예를 들어 본 발명에 대해서 상세하게 설명하였으나, 본 발명의 정신 및 범위를 벗어나지 않는 범위 내에서 본 발명이 다양하게 변경 또는 변형될 수 있음은 당업자에게 자명하므로, 이러한 모든 변경 및 변형예들도 본 발명의 보호범위에 포함되는 것으로 해석되어야 한다. It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit and scope of the invention as set forth in the appended claims. Modifications and variations are intended to be included within the scope of the present invention.

도 1은 본 발명의 일구현예에 의한 전방향족 폴리아미드 필라멘트를 제조하는 공정 개략도이다.1 is a schematic view of a process for producing a wholly aromatic polyamide filament according to an embodiment of the present invention.

** 도면의 주요 부호에 대한 설명 ** Description of Reference Numerals in the Drawings

1: 방사노즐 2: 질소 충전 장치1: Spinning nozzle 2: Nitrogen charging device

3: 질소 유체층 4: 응고액조3: Nitrogen fluid layer 4: coagulating solution tank

Claims (8)

전방향족 폴리아미드 중합체를 농황산 용매에 용해시켜 제조한 방사도프를 방사노즐을 통하여 응고액조로 방사하여 전방향족 폴리아미드 필라멘트를 제조함에 있어서, 상기 방사노즐 하부와 상기 응고액조 사이에 형성된 80~120℃로 가열된 질소(dry nitrogen) 유체층을 통과하여 방사하고, 상기 방사 노즐 및 응고액조 전체를 가열된 질소 분위기로 하는 것을 특징으로 하는 전방향족 폴리아미드 필라멘트의 제조방법.A spinning dope prepared by dissolving a wholly aromatic polyamide polymer in a concentrated sulfuric acid solvent is spinned in a coagulating solution tank through a spinning nozzle to produce a wholly aromatic polyamide filament, Wherein the spinning nozzles and the coagulating solution tank are heated to a nitrogen atmosphere. The method according to any one of claims 1 to 3, 제1항에 있어서, 상기 질소 유체층의 높이는 5 내지50 mm인 전방향족 폴리아미드 필라멘트의 제조방법.The method of claim 1, wherein the nitrogen fluid layer has a height of 5 to 50 mm. 제 1항에 있어서, 상기 전방향족 폴리아미드 중합체의 고유점도가 5.5 내지 7.0 dL/g인 전방향족 폴리아미드 필라멘트의 제조방법.The method of producing a wholly aromatic polyamide filament according to claim 1, wherein the wholly aromatic polyamide polymer has an intrinsic viscosity of 5.5 to 7.0 dL / g. 제 1항에 있어서, 상기 농황산 용매내 황산농도가 97 내지 100%인 전방향족 폴리아미드 필라멘트의 제조방법.The method of producing a wholly aromatic polyamide filament according to claim 1, wherein the concentration of sulfuric acid in the concentrated sulfuric acid solvent is 97 to 100%. 제1항에 있어서, 상기 응고액조의 응고액은 5내지 15 wt%의 황산 수용액인 전방향족 폴리아미드 필라멘트의 제조방법.The method of producing a wholly aromatic polyamide filament according to claim 1, wherein the coagulating solution of the coagulating solution tank is an aqueous sulfuric acid solution of 5 to 15 wt%. 삭제delete 제 1항 내지 제 5항 중 어느 한 항에 의한 제조방법에 의해 제조된 전방향족 폴리아미드 필라멘트.A wholly aromatic polyamide filament produced by the process according to any one of claims 1 to 5. 제 7항에 있어서, 상기 전방향족 폴리아미드 필라멘트는 강도가 22g/d 이상인 전방향족 폴리아미드 필라멘트.The wholly aromatic polyamide filament according to claim 7, wherein the wholly aromatic polyamide filament has a strength of 22 g / d or more.
KR20080135825A 2008-12-29 2008-12-29 Method of manufacturing aromatic polyamide filament and a aromatic polyamide filament by the same KR101495919B1 (en)

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KR940004688B1 (en) * 1992-05-21 1994-05-27 주식회사 코오롱 Method of preparing aromatic polyamide line filament type long staple fibers and spinning nozzle of thats
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Publication number Priority date Publication date Assignee Title
KR940004688B1 (en) * 1992-05-21 1994-05-27 주식회사 코오롱 Method of preparing aromatic polyamide line filament type long staple fibers and spinning nozzle of thats
KR20080022832A (en) * 2006-09-08 2008-03-12 주식회사 코오롱 Aromatic polyamide filament and method of manufacturing the same

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