KR20090072480A - Process for preparing para-aramid fiber - Google Patents

Process for preparing para-aramid fiber Download PDF

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Publication number
KR20090072480A
KR20090072480A KR1020070140610A KR20070140610A KR20090072480A KR 20090072480 A KR20090072480 A KR 20090072480A KR 1020070140610 A KR1020070140610 A KR 1020070140610A KR 20070140610 A KR20070140610 A KR 20070140610A KR 20090072480 A KR20090072480 A KR 20090072480A
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South Korea
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para
spinning
polyvinyl alcohol
pva
aramid fiber
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KR1020070140610A
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Korean (ko)
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남지훈
박성호
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주식회사 효성
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Priority to KR1020070140610A priority Critical patent/KR20090072480A/en
Publication of KR20090072480A publication Critical patent/KR20090072480A/en

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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
    • D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • D01F6/605—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides from aromatic polyamides
    • 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
    • D01D5/06—Wet spinning methods
    • 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
    • D01F1/06—Dyes
    • 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
    • D01F1/10—Other agents for modifying properties
    • D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/44—Yarns or threads characterised by the purpose for which they are designed
    • D02G3/441—Yarns or threads with antistatic, conductive or radiation-shielding properties
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/02—Material containing basic nitrogen
    • D06P3/04—Material containing basic nitrogen containing amide groups
    • D06P3/24—Polyamides; Polyurethanes
    • D06P3/242—Polyamides; Polyurethanes using basic dyes
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/02—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyamides
    • D10B2331/021—Fibres 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
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00—Physical properties
    • D10B2401/06—Load-responsive characteristics
    • D10B2401/063—Load-responsive characteristics high strength
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00—Physical properties
    • D10B2401/14—Dyeability
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00—Physical properties
    • D10B2401/22—Physical properties protective against sunlight or UV radiation

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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)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)

Abstract

A manufacturing method of para-typed aramid fiber is provided to offer excellent tensile strength, dyeability and UV stability than conventional aramid fiber by absorbing PVA to PPTA fiber. A manufacturing method of para-typed aramid fiber comprises the following steps of: manufacturing spinning dope by dissolving a polyparaphenylene terephthalamide polymer in sulfuric acid; spinning the spinning dope with an air-gap spinning process; coagulating spun liquid on a polyvinyl alcohol solution; and manufacturing the para-typed aramid fiber in which polyvinyl alcohol is absorbed.

Description

파라형 아라미드 섬유의 제조방법{Process for preparing para-aramid fiber} Process for preparing para-aramid fiber

본 발명은 폴리파라페닐렌테레프탈아미드(이하, 'PPTA'라 한다.) 중합체를 황산에 용해시켜 방사도프를 제조한 다음, 상기 방사도프를 기격 습식방사법으로 방사 시, 폴리비닐알코올(Polyvinylalcohol, 이하, 'PVA'라 한다.) 수용액에서 응고시켜 PVA가 흡착된 파라형 아라미드 섬유를 제조하는 방법에 관한 것이다. In the present invention, polyparaphenylene terephthalamide (hereinafter, referred to as 'PPTA') is prepared by dissolving a polymer in sulfuric acid to prepare a spinning dope, and then spinning the spinning dope by a blow wet spinning method, polyvinyl alcohol (Polyvinylalcohol, hereinafter). The present invention relates to a method of preparing para-aramid fibers adsorbed by PVA by coagulation in an aqueous solution.

본 발명의 파라형 아라미드 섬유는 PPTA 방사도프를 기격 방사 시, 수용성 고분자인 폴리비닐알코올(polyvinylalcohol,PVA) 수용액을 응고욕으로 사용함으로써, PPTA와 PVA의 강한 결합력에 의해 PPTA 섬유에 PVA가 흡착되어 기존 파라-아라미드 섬유보다 인장강도, 염색성 및 UV 안정성이 우수하며 복합재로 사용 시 고무와의 접착력이 향상되는 특성이 있다.The para-aramid fiber of the present invention is a water-soluble polymer polyvinyl alcohol (polyvinylalcohol, PVA) as a coagulation bath during the spinning of the PPTA spinning dope, PVA is adsorbed to the PPTA fiber by the strong bonding strength of PPTA and PVA Tensile strength, dyeability and UV stability is superior to the existing para-aramid fibers, and when used as a composite material, the adhesive strength with rubber is improved.

일반적으로 파라형 아라미드 단독 섬유는 펼쳐진 사슬구조에 기인하여 사슬들 사이의 수소결합과 낮은 반데르발스력 이외에는 강한 면 결합을 형성하는 힘이 없다. 이로 인해 피브릴화가 나타나며 압축강도가 낮아지며 또한 모우가 발생하는 단점을 지니고 있다.In general, para-aramid alone fibers have no force to form strong cotton bonds except hydrogen bonds and low van der Waals forces between the chains due to the unfolded chain structure. As a result, fibrillation occurs, the compressive strength is lowered, and also has the disadvantage of generating a moor.

기격습식방사(dry jet wet spinning)는 습식방사의 한 방법으로 특히, 아라미드 섬유 제조 시 유용하게 이용되고 있다. 파라형 아라미드 섬유의 제조에서 방사구금(Spinneret)을 통과해 나온 방사 용액은 1~10mm 의 공기층을 통과해 응고액을 지나면서 용매가 추출되며 섬유형태를 나타내게 된다. 응고욕의 요건으로 방사 용매와 혼화성(miscibility)이 있어야 하는데, 일반적으로 순수한 물이 응고액으로 사용된다. Dry jet wet spinning is one method of wet spinning, and is particularly useful when preparing aramid fibers. In the production of para-aramid fibers, the spinning solution passed through the spinneret passes through the air layer of 1 to 10 mm, passes through the coagulating solution, and the solvent is extracted to form a fiber. The requirement for the coagulation bath should be miscibility with the spinning solvent, in which pure water is usually used as the coagulant.

한편 응고액으로 수용성 폴리머를 함유한 물을 사용함으로 최종 섬유 물성 또는 가공성의 향상이 나타나게 되는데 1995년 4월 28일자로 허여된 스티븐(Steven D)의 미합중국 특허 제5,393,477호에는 방향족 폴리아미드 섬유 제조시 폴리에틸렌옥시드 수용액을 응고욕으로 사용한 섬유의 제조방법이 개시되어있다.On the other hand, the use of water containing a water-soluble polymer as a coagulant improves final fiber properties or processability. US Patent No. 5,393,477 to Steven D, issued April 28, 1995, describes the production of aromatic polyamide fibers. Disclosed is a method for producing fibers using an aqueous polyethylene oxide solution as a coagulation bath.

본 발명은 파라 아라미드 섬유를 제조함에 있어 낮은 온도의 응고욕에 PVA를 첨가함으로써, 기존의 방사 공정에서 필터의 막힘, 물성의 불균일 및 PVA의 분해를 방지할 수 있고, 응고과정 중에 파라형 아라미드 표면에 PVA의 흡착을 최대화시켜 기존 파라-아라미드 단독 섬유보다 인장강도, 염색성 및 UV 안정성이 우수하며, 복합재로 사용 시 고무와의 접착력이 향상된 파라형 아라미드를 제조하는 것을 목적으로 한다.In the present invention, by adding PVA to a low temperature coagulation bath in the preparation of para-aramid fibers, it is possible to prevent clogging of the filter, non-uniformity of physical properties and decomposition of PVA in the existing spinning process, and the para-aramid surface during the coagulation process. The purpose of the present invention is to prepare para-aramid, which has superior tensile strength, dyeability and UV stability than conventional para-aramid single fiber by maximizing adsorption of PVA, and has improved adhesion to rubber when used as a composite material.

상기 과제를 해결하기 위하여 본 발명의 적절한 실시 형태에 따르면, 폴리파라페닐렌테레프탈아미드 중합체를 황산에 용해시켜 방사도프를 제조하는 단계; 상기 방사도프를 기격 습식방사법으로 방사하는 단계; 방사된 용액를 응고욕인 폴리비닐알콜 수용액에서 응고시켜 폴리비닐알콜이 흡착된 파라형 아라미드 섬유를 제조하는 단계를 포함하는 파라형 아라미드섬유의 제조방법을 제공한다.In order to solve the above problems, according to a preferred embodiment of the present invention, dissolving a polyparaphenylene terephthalamide polymer in sulfuric acid to prepare a spinning dope; Spinning the spinning dope by a wet wet spinning method; It provides a method for producing para-aramid fibers comprising the step of coagulating the spun solution in a polyvinyl alcohol aqueous solution as a coagulation bath to produce para-aramid fibers adsorbed polyvinyl alcohol.

본 발명의 다른 적절한 실시 형태에 따르면, 상기 폴리비닐알콜의 분자량이 13,000 내지 146,000인 것을 특징으로 한다.According to another suitable embodiment of the present invention, the polyvinyl alcohol has a molecular weight of 13,000 to 146,000.

본 발명의 또 다른 적절한 실시 형태에 따르면, 상기 폴리비닐알콜 수용액은 폴리비닐알콜의 농도가 5 내지 10 중량%인 것을 특징으로 한다.According to another suitable embodiment of the present invention, the polyvinyl alcohol aqueous solution is characterized in that the concentration of polyvinyl alcohol is 5 to 10% by weight.

본 발명의 파라형 아라미드 섬유는 PPTA 방사도프를 기격 방사한 후, 수용성 고분자인 PVA 수용액을 응고욕으로 사용함으로써, PPTA와 PVA의 강한 결합력에 의해 PPTA 섬유에 PVA가 흡착되어 기존 파라-아라미드 섬유보다 인장강도, 염색성 및 UV 안정성이 우수하며 복합재로 사용 시 고무와의 접착력이 향상되는 특성이 있다.Para-aramid fibers of the present invention by spraying the PPTA spinning dope and then using a PVA aqueous solution of a water-soluble polymer as a coagulation bath, PVA is adsorbed to the PPTA fibers by the strong bonding strength of PPTA and PVA, compared to conventional para-aramid fibers Excellent tensile strength, dyeability and UV stability, and when used as a composite material has the property to improve the adhesion to rubber.

상기 목적을 달성하기 위하여 본 발명은 PPTA 중합체를 황산에 용해시켜 방사도프를 제조한 다음, 상기 방사도프를 기격 습식방사법으로 방사 시, PVA 수용액에서 응고시켜 파라형 아라미드 섬유에 PVA가 흡착되는 것을 특징으로 하는 파라형 아라미드섬유의 제조방법을 제공한다.In order to achieve the above object, the present invention is to prepare a spinning dope by dissolving the PPTA polymer in sulfuric acid, and then, the spinning dope is solidified in a PVA aqueous solution when spinning the spinning dope by a spinning wet spinning method to adsorb PVA to para-aramid fibers. It provides a method for producing para-aramid fibers.

본 발명에 사용된 PVA는 검화도가 98%이상이며, 분자량이 9,000내지 146,000의 범위인 PVA가 사용되며 바람직하게는 분자량이 13,000내지 146,000인 PVA가 적당하다. 분자량이 146,000 초과인 경우에는 PVA의 흡착이 낮아 물성 향상의 변화가 없었다.PVA used in the present invention has a saponification degree of 98% or more, a PVA having a molecular weight in the range of 9,000 to 146,000 is used, preferably a PVA having a molecular weight of 13,000 to 146,000. When the molecular weight was more than 146,000, the adsorption of PVA was low and there was no change in physical properties.

또한, 상기 PVA 수용액에서 PVA의 농도는 5 내지 10 중량%인 것이 바람직하다.In addition, the concentration of PVA in the PVA aqueous solution is preferably 5 to 10% by weight.

본 발명은 수용성 고분자인 PVA 수용액을 응고욕으로 하여 파라 아라미드 특히, PPTA 방사도프를 토출하여 PPTA와 PVA의 강한 결합력에 의해 PPTA 섬유에 PVA가 흡착되어 기존 파라-아라미드 단독 섬유보다 인장강도, 염색성 및 UV 안정성이 우수하며, 복합재로 사용 시 고무와의 접착력이 향상되는 특성이 있다.According to the present invention, PVA is adsorbed onto PPTA fibers by the strong bonding force of PPTA and PVA by discharging para aramid, especially PPTA spinning dope, using aqueous solution of PVA as a coagulation bath. Excellent UV stability, and when used as a composite material has the property of improving the adhesive strength with the rubber.

본 발명에서 제조된 섬유는 PPTA를 19.5%의 농도로 100%이상의 황산에 85℃에서 녹인 후 기격 습식방사법을 이용하여 PVA가 녹아있는 응고욕에 방사하였다.The fiber prepared in the present invention was dissolved in PPTA at 19.5% concentration in sulfuric acid of 100% or more at 85 ℃ and spun into a coagulation bath in which PVA is dissolved by using a wet wet spinning method.

아래에서 실시예를 들어 본 발명을 더욱 상세히 설명하나, 본 발명에 따른 실시예들은 여러 가지 다른 형태로 변형될 수 있으며, 본 발명의 범위가 아래에서 상술하는 실시예들에 한정되는 것으로 해석되어서는 안 된다.Hereinafter, the present invention will be described in more detail with reference to Examples, but embodiments according to the present invention can be modified in many different forms, and the scope of the present invention is construed as being limited to the embodiments described below. Can not be done.

<인장 강도>Tensile Strength

필라멘트의 인장특성은 시험조건 하에서 14시간 이상 컨디셔닝 후에 21℃의 온도와 50-60%의 상대습도에서 측정하였다. 신장속도를 0.25cm/min으로 하고 게이지의 길이가 2.54cm인 것을 사용한다.Tensile properties of the filaments were measured at a temperature of 21 ° C. and a relative humidity of 50-60% after conditioning for at least 14 hours under test conditions. The elongation rate is 0.25cm / min and the gauge length is 2.54cm.

< < 실시예Example 1> 1>

p-페닐렌디아민과 테레프탈로일클로라이드를 등몰량 저온 중합시켜 제조한 고유 점도 6.3의 PPTA 중합체를 100% 황산에 19.5 중량%로 85℃에서 용해시킨 후, 기격(air gap) 습식방사법으로 방사하였다. 그리고 분자량이 31,000~50,000인 PVA가 5 중량%로 녹아있는 수용액에서 응고시켜 아라미드 섬유를 제조하였다. 이때 제조된 아라미드 섬유의 인장 강도는 24g/d이었고, 카티온 염료로 염색 시 염색성에 있어서 확연한 차이를 나타내었다.PPTA polymer having an intrinsic viscosity of 6.3 prepared by isothermally polymerizing p-phenylenediamine and terephthaloyl chloride was dissolved in 100% sulfuric acid at 19.5% by weight at 85 ° C, and then spun by air gap wet spinning. . And aramid fibers were prepared by solidifying in an aqueous solution in which PVA having a molecular weight of 31,000 to 50,000 was dissolved at 5% by weight. At this time, the tensile strength of the prepared aramid fiber was 24g / d, and showed a significant difference in the dyeability when dyed with a cation dye.

< < 실시예Example 2> 2>

p-페닐렌디아민과 테레프탈로일클로라이드를 등몰량 저온 중합시켜 제조한 고유 점도 6.3의 PPTA 중합체를 100% 황산에 19.5 중량%로 85℃에서 용해시킨 후, 기격(air gap) 습식방사법으로 방사하였다. 그리고 분자량이 31,000~50,000인 PVA가 10 중량%로 녹아있는 수용액에서 응고시켜 아라미드 섬유를 제조하였다. 이때 제조된 아라미드 섬유의 인장 강도는 25g/d이었고, 카티온 염료로 염색 시 염색성에 있어서 확연한 차이를 나타내었다.PPTA polymer having an intrinsic viscosity of 6.3 prepared by isothermally polymerizing p-phenylenediamine and terephthaloyl chloride was dissolved in 100% sulfuric acid at 19.5% by weight at 85 ° C, and then spun by air gap wet spinning. . And aramid fibers were prepared by coagulation in an aqueous solution in which PVA having a molecular weight of 31,000 to 50,000 was dissolved in 10% by weight. At this time, the tensile strength of the prepared aramid fiber was 25g / d, and showed a significant difference in the dyeability when dyed with a cation dye.

<  < 비교예Comparative example 1> 1>

p-페닐렌디아민과 테레프탈로일클로라이드를 등몰량 저온 중합시켜 제조한 고유 점도 6.3의 PPTA 중합체를 100% 황산에 19.5중량%로 85℃로 용해시킨 후, 기격(air gap) 습식방사법으로 방사하였다. 그리고 PVA가 녹아있지 않은 수용액에서 응고시켜 아라미드 섬유를 제조하였다. 이때 제조된 아라미드 섬유의 인장 강도는 22g/d이었고, 카티온 염료로 염색 시 염색이 되지 않았다.PPTA polymer having an intrinsic viscosity of 6.3 prepared by equimolarly low temperature polymerization of p-phenylenediamine and terephthaloyl chloride was dissolved in 19.5% by weight in 85% sulfuric acid at 85 ° C, and then spun by air gap wet spinning. . And aramid fibers were prepared by solidifying in an aqueous solution in which PVA is not dissolved. At this time, the tensile strength of the prepared aramid fiber was 22g / d, it was not dyed when dyed with a cation dye.

<   < 비교예Comparative example 2> 2>

p-페닐렌디아민과 테레프탈로일클로라이드를 등몰량 저온 중합시켜 제조한 고유 점도 6.3의 PPTA 중합체를 100% 황산에 19.5중량%로 85℃로 용해시킨 후, 기 격(air gap) 습식방사법으로 방사하였다. 그리고 분자량이 5,000인 PVA가 10 중량%로 녹아있는 수용액에서 응고시켜 아라미드 섬유를 제조하였다. 이때 제조된 아라미드 섬유의 인장 강도는 20g/d이었고, 카티온 염료로 염색 시 염색성에 있어서 큰 차이를 보이지 않았다.After dissolving p-phenylenediamine and terephthaloyl chloride in an equimolar amount at low temperature, PPTA polymer having an intrinsic viscosity of 6.3 was dissolved in 100% sulfuric acid at 19.5% by weight at 85 ° C, and then spun by air gap wet spinning. It was. And aramid fibers were prepared by solidifying in an aqueous solution in which PVA having a molecular weight of 5,000 is dissolved at 10% by weight. At this time, the tensile strength of the prepared aramid fiber was 20g / d, and did not show a significant difference in the dyeability when dyed with a cation dye.

<   < 비교예Comparative example 3> 3>

p-페닐렌디아민과 테레프탈로일클로라이드를 등몰량 저온 중합시켜 제조한 고유 점도 6.3의 PPTA 중합체를 100% 황산에 19.5중량%로 85℃로 용해시킨 후, 기격(air gap) 습식방사법으로 방사하였다. 그리고 분자량이 186,000인 PVA가 10 중량%로 녹아있는 수용액에서 응고시켜 아라미드 섬유를 제조하였다. 이때 제조된 아라미드 섬유의 인장 강도는 22g/d이었고, 카티온 염료로 염색 시 염색이 되지 않았다.PPTA polymer having an intrinsic viscosity of 6.3 prepared by equimolarly low temperature polymerization of p-phenylenediamine and terephthaloyl chloride was dissolved in 19.5% by weight in 85% sulfuric acid at 85 ° C, and then spun by air gap wet spinning. . Aramid fibers were prepared by coagulation in an aqueous solution in which PVA having a molecular weight of 186,000 was dissolved at 10% by weight. At this time, the tensile strength of the prepared aramid fiber was 22g / d, it was not dyed when dyed with a cation dye.

Claims (3)

파라형 아라미드 섬유의 제조방법에 있어서, In the manufacturing method of para-type aramid fiber, 폴리파라페닐렌테레프탈아미드 중합체를 황산에 용해시켜 방사도프를 제조하는 단계; Dissolving the polyparaphenylene terephthalamide polymer in sulfuric acid to prepare a spinning dope; 상기 방사도프를 기격 습식방사법으로 방사하는 단계;Spinning the spinning dope by a wet wet spinning method; 방사된 용액를 응고욕인 폴리비닐알콜 수용액에서 응고시켜 폴리비닐알콜이 흡착된 파라형 아라미드 섬유를 제조하는 단계를 포함하는 파라형 아라미드섬유의 제조방법.A method for producing para-aramid fibers comprising the step of coagulating the spun solution in a polyvinyl alcohol aqueous solution as a coagulation bath to prepare para-aramid fibers adsorbed to polyvinyl alcohol. 제 1항에 있어서, 상기 폴리비닐알콜의 분자량이 13,000 내지 146,000인 것을 특징으로 하는 파라형 아라미드 섬유의 제조방법.The method for producing para-aramid fibers according to claim 1, wherein the polyvinyl alcohol has a molecular weight of 13,000 to 146,000. 제 1항에 있어서, 상기 폴리비닐알콜 수용액은 폴리비닐알콜의 농도가 5 내지 10 중량%인 것을 특징으로 하는 파라형 아라미드 섬유의 제조방법.The method of claim 1, wherein the polyvinyl alcohol aqueous solution has a polyvinyl alcohol having a concentration of 5 to 10% by weight.
KR1020070140610A 2007-12-28 2007-12-28 Process for preparing para-aramid fiber KR20090072480A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101386429B1 (en) * 2012-12-28 2014-04-29 코오롱인더스트리 주식회사 Method of dry-spinning para-aramid fiber
WO2019208997A1 (en) * 2018-04-26 2019-10-31 한양대학교 산학협력단 Composite fibers including graphene fibers having coating film formed thereon, and method for preparing same

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101386429B1 (en) * 2012-12-28 2014-04-29 코오롱인더스트리 주식회사 Method of dry-spinning para-aramid fiber
JP2016505728A (en) * 2012-12-28 2016-02-25 コーロン インダストリーズ インク Dry spinning method for para-aramid fiber
WO2019208997A1 (en) * 2018-04-26 2019-10-31 한양대학교 산학협력단 Composite fibers including graphene fibers having coating film formed thereon, and method for preparing same

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