KR101109304B1 - Method for manufacturing cation dyeable polyamide yarn - Google Patents

Method for manufacturing cation dyeable polyamide yarn Download PDF

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KR101109304B1
KR101109304B1 KR1020090035452A KR20090035452A KR101109304B1 KR 101109304 B1 KR101109304 B1 KR 101109304B1 KR 1020090035452 A KR1020090035452 A KR 1020090035452A KR 20090035452 A KR20090035452 A KR 20090035452A KR 101109304 B1 KR101109304 B1 KR 101109304B1
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KR20100116830A (en
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이용완
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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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/02Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
    • C08G69/08Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
    • C08G69/14Lactams
    • 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
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/08Melt spinning methods
    • D01D5/098Melt spinning methods with simultaneous stretching
    • 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
    • D01F1/04Pigments
    • 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
    • D01F1/06Dyes
    • 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
    • D03D15/54Woven 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 coloured
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/02Material containing basic nitrogen
    • D06P3/04Material containing basic nitrogen containing amide groups
    • D06P3/24Polyamides; Polyurethanes
    • D06P3/241Polyamides; Polyurethanes using acid dyes
    • 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
    • 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
    • D10B2401/14Dyeability

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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)
  • Health & Medical Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Artificial Filaments (AREA)

Abstract

본 발명은 카치온(cation) 가염형 폴리아미드 섬유의 제조방법에 관한 것으로, 더욱 상세하게는 ε-카프로락탐과 5-SSIPA(sodiosulfo isophthalic acid) 중합체에 염료 또는 안료를 블렌딩하여 고속 방사함으로써 견뢰도 및 보형성이 우수한 폴리아미드 섬유를 제조하는 방법 및 본 발명의 방법에 의하여 제조된 폴리아미드 섬유를 포함하는 직물의 제조방법에 관한 것이다The present invention relates to a method for producing a cation salted polyamide fiber, and more particularly, fastness and stability by blending a dye or a pigment in ε-caprolactam and 5-SSIPA (sodiosulfo isophthalic acid) polymer The present invention relates to a method for producing a polyamide fiber having excellent formation and a method for producing a fabric including the polyamide fiber produced by the method of the present invention.

염색견뢰도, 보형성, 심색성, 이형성, 카치온 가염형 섬유, 폴리아미드, 카프로락탐. Color fastness, shape retention, deep colorability, release property, cationic salted fiber, polyamide, caprolactam.

Description

카치온 가염형 폴리아미드 섬유의 제조방법{METHOD FOR MANUFACTURING CATION DYEABLE POLYAMIDE YARN} Manufacturing method of cationic salt type polyamide fiber {METHOD FOR MANUFACTURING CATION DYEABLE POLYAMIDE YARN}

본 발명은 카치온(cation) 가염형 폴리아미드 섬유의 제조방법에 관한 것으로, 더욱 상세하게는 ε-카프로락탐과 5-SSIPA(sodiosulfo isophthalic acid) 중합체에 염료 또는 안료를 블렌딩하여 고속 방사함으로써 견뢰도 및 보형성이 우수한 폴리아미드 섬유를 제조하는 방법 및 본 발명의 방법에 의하여 제조된 폴리아미드 섬유를 포함하는 직물의 제조방법에 관한 것이다.The present invention relates to a method for producing a cation salted polyamide fiber, and more particularly, fastness and stability by blending a dye or a pigment in ε-caprolactam and 5-SSIPA (sodiosulfo isophthalic acid) polymer The present invention relates to a method for producing a polyamide fiber having excellent formation and a method for producing a fabric comprising the polyamide fiber produced by the method of the present invention.

종래 카치온 가염형 폴리아미드 섬유의 제조방법으로는, 일본 공개특허 제2001-200054호에 개시된 바와 같이 술폰산나트륨염 등 카치온 가염형 관능기를 포함하는 화학물질을 중합단계에서 나이론 6의 주원료인 ε-카프로락탐과 반응시켜 카치온 가염형 고분자 중합물을 제조하고 이를 용융, 고속 방사하여 카치온 염료에 의하여 염색이 가능한 폴리아미드 섬유를 제조하는 방법이 알려져 있다. As a conventional method for producing a cationic salt polyamide fiber, as disclosed in Japanese Patent Laid-Open No. 2001-200054, a chemical substance containing a cationic salt type functional group such as sodium sulfonate salt is polymerized in the polymerization step of epsilon -capro It is known to prepare a polyamide fiber which can be dyed with a cationic dye by reacting with a lactam to produce a cationic salt type polymer polymer, and melting and spinning it at high speed.

그러나 이러한 방법으로 제조되는 카치온 가염형의 폴리아미드 섬유는 중농 색 이상의 고발색성을 띠도록 제조하기가 어려우며, 특히 단사섬도가 0.1~2.0데니어급 원사를 제조하는 경우에는 염색견뢰도 측면에서 더욱 불리하다. However, the cationic salt polyamide fibers produced by this method are difficult to be produced to have a high color development of more than a medium color, especially in the case of producing a single yarn fineness 0.1 ~ 2.0 denier yarn is more disadvantageous in terms of color fastness.

한편, 심색성 및 염색견뢰도를 개선하기 위하여 나트륨술폰산염의 첨가량을 증가시켜 카치온 염착좌의 수를 증가시키는 경우에는 방사공정성 저하 및 강도, 신도 등 섬유의 기계적 물성 측면에서의 저하를 야기시킬 수 있다. 따라서 이러한 공정으로 제조된 카치온 가염형 폴리아미드는 카페트 등 비의류용 소재에서 다색성 구현을 위해 일반적인 폴리아미드계 폴리머를 용융방사하여 제조된 나이론 소재등과 혼섬하여 사용되는 등의 제한된 용도로만 사용되어 왔다.On the other hand, in order to improve the color depth and color fastness, increasing the amount of sodium sulfonate added to increase the number of cationic salt deposits may cause a decrease in the spinability and mechanical properties of the fiber, such as strength, elongation. Therefore, the cationic salt polyamide prepared by this process has been used only for limited purposes such as being mixed with a nylon material prepared by melt spinning a general polyamide-based polymer for multicoloring in non-clothing materials such as carpet. .

또한, 직물을 제조함에 있어 드레이프성 또는 보형기능성을 높이기 위하여 일반 폴리에스터 섬유 대비 장쇄의 길이가 긴 폴리프로필렌테레프탈레이트 또는 폴리부틸렌테레프탈레이트 폴리머를 용융방사하여 원사를 제조한 후 직물을 구성하는 경위사로 적용하는 예가 알려져 있다. 그러나, 이 경우에는 고압하에서 염색해야 하며, 밝은 색상 구현이 어렵고 균일성 있는 보형기능의 발현이 어렵다는 단점이 있었다.In addition, in order to improve the drape or prosthetic functionality in fabric, the fabric of the yarn after melt spinning a polypropylene terephthalate or polybutylene terephthalate polymer having a longer chain length compared to general polyester fiber Examples of application to yarns are known. However, in this case, it has to be dyed under high pressure, and it is difficult to realize bright colors and difficult to express uniform prosthetic functions.

본 발명은 상기와 같은 종래 기술의 문제점을 해결하기 위한 것으로, 본 발명의 하나의 목적은 중색 이상의 심색에서도 견뢰도가 우수하며 드레이프성 및 보형성이 우수한 카치온 가염형 폴리아미드 섬유의 제조방법을 제공하는 것이다.The present invention is to solve the problems of the prior art as described above, one object of the present invention is to provide a method for producing a cationic salted polyamide fiber excellent in color fastness and excellent drape and shape retention even in the deep color of the medium or more will be.

본 발명의 다른 목적은, 상기와 같은 본 발명의 제조방법에 의하여 제조되는 카치온 가염형 폴리아미드 섬유를 포함함으로써 카치온 가염성에 의해 이색성을 발휘함과 동시에 중색 이상의 심색에서도 높은 염색 견뢰효과를 가지며 동시에 드레이프성 및 보형성능이 우수한 직물의 제조방법을 제공하는 것이다.Another object of the present invention, by including the cationic salt type polyamide fiber prepared by the manufacturing method of the present invention as described above, exhibits the dichroism by the cationic saltability and at the same time has a high color fastness effect even in deep colors or more It is to provide a method for producing a fabric excellent in drape and moldability.

상기와 같은 목적을 달성하기 위한 본 발명의 하나의 양상은, ε-카프로락탐 100 중량부에 대하여 5-SSIPA 0.5~3.0 중량부를 첨가하여 중합체를 중합하는 단계 및 상기 중합체 100중량부에 대하여 염료 또는 안료를 0.5~2.0중량부 블렌딩하여 고속 방사하는 단계를 포함하는 것을 특징으로 하는 카치온 가염형 폴리아미드 섬유의 제조방법에 관한 것이다. One aspect of the present invention for achieving the above object is a step of polymerizing a polymer by adding 0.5 to 3.0 parts by weight of 5-SSIPA based on 100 parts by weight of ε-caprolactam and dyes or It relates to a method for producing a cationic salt polyamide fiber comprising the step of high-speed spinning by blending the pigment 0.5 to 2.0 parts by weight.

본 발명의 일 구현예에 따른 상기 카치온 가염형 폴리아미드 섬유의 제조방법은, 방사 속도가 4000 m/min. 이상인 것을 특징으로 한다.In the method for preparing the cationic salt polyamide fiber according to one embodiment of the present invention, the spinning speed is 4000 m / min. It is characterized by the above.

본 발명의 일 구현예에 따른 따른 상기 카치온 가염형 폴리아미드 섬유의 제조방법은, 단사섬도가 0.5-2.0데니어인 것을 특징으로 한다.The method for preparing the cationic salt type polyamide fiber according to the embodiment of the present invention is characterized in that the single yarn fineness is 0.5-2.0 denier.

상기와 같은 목적을 달성하기 위한 본 발명의 다른 양상은, 상기 본 발명에 따른 제조방법에 의하여 제조된 카치온 가염형 폴리아미드 섬유를 직물의 경사, 또는 위사, 또는 경위사로 적용하여 직물을 제직한 후, 80~98℃ 범위에서 카치온 염료로 염색하고, 100~140℃ 범위에서 열처리하여 건조시키는 직물의 제조방법에 관한 것이다.Another aspect of the present invention for achieving the above object, after weaving the fabric by applying the cationic salted polyamide fiber prepared by the manufacturing method according to the present invention as the warp, weft, or theft weft of the fabric. , Dyeing with a cationic dye in the range of 80 ~ 98 ℃, heat treatment in the range of 100 ~ 140 ℃ relates to a fabrication method of the fabric.

본 발명에 따른 카치온 가염형 폴리아미드 섬유의 제조방법에 의하여 제조된 카치온 가염형 폴리아미드 섬유 및 이를 포함하는 직물은, 소량의 카치온 염료로도 고발색성을 발현함과 동시에 우수한 습윤견뢰도를 갖으며 드레이프성 및 보형성능면에서도 종래의 나이론직물 및 폴리프로필렌테레프탈레이트 직물에 비하여 우수한 성능을 보인다.The cationic salt polyamide fiber and the fabric comprising the same are produced by the method for preparing the cationic salt polyamide fiber according to the present invention, while exhibiting high color development even with a small amount of cationic dye, and having excellent wet fastness and drape. In terms of performance and formability, it shows superior performance compared to conventional nylon and polypropylene terephthalate fabrics.

또한 본 발명에 따른 카치온 가염형 폴리아미드 섬유의 제조방법은, 폴리아미드 중합물을 방사속도 4,000m/min이상의 고속으로 용융방사함에 있어서 사절이나 곡사를 발생시키지 않고 방사작업성이 양호하게 제조할 수 있으며, 제조된 카치온 가염형 폴리아미드 섬유는 단면균일성이 양호한 효과가 있다.In addition, the method of manufacturing the cationic salt polyamide fiber according to the present invention, it is possible to produce a good spinning workability without the generation of trimming or twisting in melt spinning the polyamide polymer at a high speed of more than 4,000m / min spinning speed , The prepared cationic salt polyamide fibers have an effect of good cross-sectional uniformity.

이하에서 실시예 등을 참고하여 본 발명에 대하여 더욱 상세하게 설명한다. 다만 이는 본 발명을 구체적으로 설명하기 위한 목적일 뿐, 본 발명이 여기에 제한 되는 것으로 해석되어서는 아니 된다. 또한, 본 발명을 설명함에 있어서 관련된 공지의 범용적인 기능 또는 구성에 대한 상세한 설명은 생략한다.Hereinafter, the present invention will be described in more detail with reference to Examples. However, this is only for the purpose of illustrating the present invention in detail, it should not be construed that the present invention is limited thereto. In addition, in the description of the present invention, detailed descriptions of well-known general functions or configurations will be omitted.

본 발명의 일 구현예에 따른 카치온 가염형 폴리아미드 섬유의 제조방법은, ε-카프로락탐 100 중량부에 대하여 5-SSIPA (sodiosulfo isophthalic acid) 0.5~3.0 중량부를 첨가하여 중합체를 중합하는 단계 및 상기 중합체 100중량부에 대하여 염료 또는 안료를 0.5~2.0중량부 블렌딩하여 고속 방사하는 단계를 포함한다. Cationic salt polyamide fiber production method according to an embodiment of the present invention, the step of polymerizing the polymer by adding 0.5 to 3.0 parts by weight of 5-SSIPA (sodiosulfo isophthalic acid) based on 100 parts by weight of ε-caprolactam and the Blending 0.5 to 2.0 parts by weight of the dye or pigment with respect to 100 parts by weight of the polymer;

즉, 본 발명의 일 구현예에 따른 제조방법은 카치온 가염형 폴리아미드 중합물을 제조함에 있어 술폰산나트륨염을 함유한 5-SSIPA를 ε -카프로락탐의 중량 대비 0.5~3.0중량부가 되도록 첨가하여 카치온 가염형 중합물을 제조하고, 이를 방사속도 4,000m/min이상의 고속으로 용융 방사함에 있어서 상기 카치온 가염형 폴리아미드 중합물의 중량대비0.5~2.0중량부의 염료 또는 안료를 첨가하여 방사하는 것을 특징으로 한다. That is, in the preparation method according to the embodiment of the present invention, in preparing the cationic salt type polyamide polymer, 5-SSIPA containing sodium sulfonate salt is added so as to be 0.5 to 3.0 parts by weight based on the weight of ε-caprolactam. It is characterized by producing a type polymer, and spinning by melt spinning at a high speed of 4,000m / min or more spinning rate by adding 0.5 to 2.0 parts by weight of a dye or pigment relative to the weight of the cationic salt polyamide polymer.

본 발명을 더욱 구체적으로 설명하면, 직접방사법으로 단사섬도가 0.1 ~ 2.0데니어인 이염성 나일론 극세 제균섬유를 제조함에 있어서, 중합물의 구성은 ε-카프로락탐 100 중량부에 대하여 5-SSIPA 0.5 ~ 3.0중량부의 조성으로 이루어진다. The present invention will be described in more detail. In the preparation of the dibasic nylon microbacterial fiber having a single yarn fineness of 0.1 to 2.0 denier by direct spinning, the composition of the polymer is 5-SSIPA 0.5 to 3.0 with respect to 100 parts by weight of ε-caprolactam. It is composed of parts by weight.

이때, 5-SSIPA의 함량이 0.5중량부 미만이면 카치온 가염성능이 발현되지 못하며, 3.0 중량부 이상이면 방사작업성의 저하 및 염색견뢰도 저하의 문제가 발생되며 초기탄성률의 저하와 함께 원단제조시 적절하지 못한 굽힘 회복성이 나타나게 된다. At this time, if the content of 5-SSIPA is less than 0.5 parts by weight, the cationic salting performance is not expressed, and if it is 3.0 parts by weight or more, problems of deterioration of spinning workability and dyeing fastness occur. Poor bend recovery is seen.

이어서, 상기와 같이 제조된 이염성 폴리아미드 중합물 100 중량부에 대하여 0.5~2.0중량부의 안료 또는 염료를 첨가하여 블렌딩하고, 건조한 후 압출기를 통하여 압출함으로써 섬유를 제조한다. 이때, 안료 또는 염료의 투입량이 2.0 중량부 이상일 경우는 방사작업시 사절의 증가와 함께 기계적 물성의 저하가 야기되며, 0.5 중량부 미만의 경우는 심색효과 및 견뢰도 향상효과를 기대하기 힘들다. 본 발명의 제조방법에 있어서 상기 안료 또는 염료로는 카본블랙 등 당업계에서 사용되는 공지의 안료 또는 염료를 제한없이 사용할 수 있다.Subsequently, 0.5 to 2.0 parts by weight of pigment or dye is added to 100 parts by weight of the dibasic polyamide polymer prepared as described above, blended, dried and extruded through an extruder to prepare a fiber. At this time, when the amount of the pigment or dye is more than 2.0 parts by weight, the increase in the number of trimming during the spinning operation causes a decrease in mechanical properties, less than 0.5 parts by weight it is difficult to expect the effect of improving the deep color and fastness. As the pigment or dye in the production method of the present invention, known pigments or dyes used in the art such as carbon black can be used without limitation.

본 발명의 일 구현예에 따른 카치온 가염형 폴리아미드 섬유의 제조방법에서, 방사속도는 4,000m/min이상으로 하는 것이 좋으며, 필요에 따라서 연신 및 열처리를 한 후 권취하는 것도 좋다. In the method for producing a cationic salt type polyamide fiber according to an embodiment of the present invention, the spinning speed is preferably set to 4,000 m / min or more, and may be wound after stretching and heat treatment as necessary.

이상과 같은 방법에 의하여 제조된 카치온 가염형 폴리아미드 섬유는 적은 양의 카치온염료를 사용하여도 심색발현이 가능함과 동시에 우수한 견뢰도를 발현하며 우수한 드레이프성 및 보형성을 갖게 된다.The cationic salt type polyamide fiber prepared by the above method is capable of deep color expression using a small amount of cationic dye and at the same time, expresses excellent fastness and has excellent drape and shape retention.

본 발명의 또 다른 양상은, 상기 본 발명에 따른 제조방법에 의하여 제조된 카치온 가염형 폴리아미드 섬유를 직물의 경사, 또는 위사, 또는 경위사로 적용하여 직물을 제직한 후, 80~98℃ 범위에서 카치온 염료로 염색하고, 100~140℃ 범위에서 열처리하여 건조시키는 직물의 제조방법에 관한 것이다.Another aspect of the present invention, after weaving the fabric by applying the cationic salt-coated polyamide fiber prepared by the manufacturing method according to the present invention as the warp, weft, or theodolite of the fabric, in the range of 80 ~ 98 ℃ Dyeing with a cationic dye, and relates to a method for producing a fabric which is dried by heat treatment in the range of 100 ~ 140 ℃.

이를 보다 구체적으로 설명하면, 전술한 바와 같이 ε-카프로락탐 100 중량부에 대하여 5-SSIPA 0.5 ~ 3.0중량부를 첨가하여 카치온 가염형 폴리아미드 중합체를 제조후, 상기 중합체100 중량부에 대하여0.5~2.0 중량부의 카본블랙을 첨가하 여 통상의 용융방사법으로 원사를 제조한다.More specifically, as described above, 0.5 to 3.0 parts by weight of 5-SSIPA is added to 100 parts by weight of ε-caprolactam to prepare a cationic salt polyamide polymer, and then 0.5 to 2.0 based on 100 parts by weight of the polymer. By weight of carbon black is added to prepare a yarn by a conventional melt spinning method.

즉, 안료를 함유시킨 카치온 가염형 폴리아미드 중합물을 용융 압출시키고 냉각, 고화 후 유제를 부여한 후 필요에 따라 고압공기에 의해 교락을 부여하면서 권취하여 0.5~2.0데니어의 의료용 폴리아미드 원사를 제조한다.That is, the cationic salt polyamide polymer containing the pigment is melt-extruded, cooled and solidified, and then emulsified, and then wound while applying entanglement by high pressure air to prepare a medical polyamide yarn having 0.5 to 2.0 denier.

이어서, 드레이프성 및 보형성능이 우수한 직물의 제조를 위하여 상기와 같은 공정으로 제조된 폴리아미드 원사에 꼬임을 부여하여 위사 또는 경사 또는 경위사 모두로 적용하여 직물을 제조한다. 이어서 상기와 같이 제조된 직물을 80~98℃의 염욕하에서 카치온 염료로 염색한후 100~140℃의 온도에서 열처리하여 세팅하면 드레이프성 및 보형성능이 우수한 카치온 가염형 직물을 제조하게 된다. Subsequently, the fabric is fabricated by applying twist to the polyamide yarn prepared in the above-described process to produce a fabric having excellent drape and moldability, and applying both weft or warp or warp yarns. Subsequently, the fabric prepared as described above is dyed with a cationic dye under a salt bath of 80 to 98 ° C., and then heat-set at a temperature of 100 to 140 ° C. to prepare a cationic salt-type fabric having excellent drape and moldability.

방사공정 중 유제의 부여는 1회 또는 2회 이상으로 실시하는데, 첫 번째 유제 부여는 고속방사에 의해 수반된 기류의 영향을 줄이기 위하여 계량급유방식으로 하는 것이 바람직하며, 2번째 이상에서는 로울러 급유방식으로 하는 것이 좋다. During the spinning process, the oil is added once or twice or more, and the first oil is preferably metered and lubricated to reduce the effects of airflow caused by high-speed spinning. It is good to do.

실시예 1Example 1

5-SSIPA의 함량을 ε-카프로락탐 100 중량부에 대하여 3 중량부로 하여 카치온 가염형 폴리아미드 중합물을 제조하고 칩을 건조한 후, 카본블랙의 농도가 카치온 가염형 폴리아미드 중합물 100 중량부에 대하여 2 중량부가 되도록 블렌딩하였다. 이어서 상기 블렌딩을 압출용융후 직접방사법으로 섬도70데니어, 필라멘트수 68인 (단사섬도: 1.0데니어) 폴리아미드 섬유를 제조하였다. 방사공정에서 냉각풍의 속도는 0.5m/s로 하고, 방사구금 하부 100cm에서 필라멘트를 집속하고, 방사온 도는 265℃, 방사속도는 4,800m/min으로 하여 사를 제조하였다.The cationic salt polyamide polymer was prepared by using 5-SSIPA in an amount of 3 parts by weight based on 100 parts by weight of ε-caprolactam, and after drying the chip, the carbon black concentration was 2 parts by weight of 100 parts by weight of the cationic salt polyamide polymer. Blended to parts by weight. Subsequently, the blend was subjected to direct spinning after melt extrusion to prepare a polyamide fiber having a fineness of 70 deniers and a filament number of 68 (single fineness: 1.0 denier). In the spinning process, the speed of the cooling wind was 0.5 m / s, the filaments were focused at 100 cm below the spinneret, the spinning temperature was 265 ° C., and the spinning speed was 4,800 m / min.

이어서, 상기 공정으로 제조된 원사에 500TM의 꼬임을 부여하여 연사한 후, 폴리아미드70데니어 34필라멘트의 경사에 위사로 적용하여 제직하였다. 이어서, 90 ℃의 온도에서 30분간 0.5%의 Rifa cationic Black 2GH(이화염료 社)를 투입하여 염색한후, 140℃에서 건조후 견뢰도 및 심색성을 평가하고 관능평가에 의해 직물의 보형성을 평가하였으며 그 결과를 표 1에 나타내었다.Subsequently, the yarn prepared by the above process was twisted and twisted with 500TM, and then woven by applying a weft to the warp of polyamide 70 denier 34 filament. Subsequently, after dyeing with 0.5% Rifa cationic Black 2GH (Phosphorescence Dyestuff Co., Ltd.) at a temperature of 90 ° C. for 30 minutes, the fastness and color depth after drying at 140 ° C. were evaluated and the shape retention of the fabric was evaluated by sensory evaluation. The results are shown in Table 1.

실시예 2Example 2

중합물 제조시 ε-카프로락탐 100 중량부에 대하여 0.5 중량부의 5-SSIPA를 첨가하여 중합물을 제조하고, 상기 중합물 100 중량부에 대하여 0.5 중량부의 카본블랙을 첨가 블렌딩한 것을 제외하고는 실시예 1과 동일하게 사를 제조하고 제균성 및 방사작업성을 평가하였으며, 그 결과를 표 1에 나타내었다.Example 1 except that 0.5 parts by weight of 5-SSIPA was added to 100 parts by weight of ε-caprolactam to prepare a polymer, and 0.5 parts by weight of carbon black was added and blended to 100 parts by weight of the polymer. The yarns were prepared in the same manner and the bactericidal and radioworkability were evaluated, and the results are shown in Table 1.

비교예 1Comparative Example 1

카치온 가염형 중합물을 사용하여 방사시 카본블랙 등의 염료나 안료를 블렌딩하지 않고 제사, 제직, 염가공을 진행한 후 견뢰도 및 보형성능을 평가하였으며, 그 결과를 표 1에 나타내었다. 염가공시 카치온 염료의 농도는 섬유 100 중량부에 대하여 2.0 중량부로 하였다.After the spinning, weaving, and salt processing were performed without blending dyes or pigments such as carbon black using spinning cationic salt type polymers, the fastness and formability were evaluated, and the results are shown in Table 1. The concentration of the cationic dye during salting was 2.0 parts by weight based on 100 parts by weight of the fiber.

비교예 2Comparative Example 2

염가공시 카치온 염료의 농도를 섬유 100 중량부에 대하여 4.0 중량부로 한 것 이외에는 비교예 1과 동일하게 진행후 견뢰도 및 직물의 보형성능을 평가하였다.The fastness and the shape retaining ability of the fabric were evaluated in the same manner as in Comparative Example 1 except that the concentration of the cationic dye was 4.0 parts by weight based on 100 parts by weight of the fiber during dyeing.

비교예 3Comparative Example 3

일반 나일론 중합물을 사용하여 카본블랙등 염료나 안료를 블렌딩하지 않고 비교예 1과 같은 공정으로 제사, 제직, 염가공을 진행한후 견뢰도 및 직물의 보형성능을 평가하였으며, 그 결과를 표 1에 나타내었다. 염가공시 산성염료 Neurilan Black LDH (요크셔 사)의 농도는 섬유 100 중량부에 대하여 4.0 중량부로 염색하였다.After weaving, weaving, and dyeing in the same manner as in Comparative Example 1 without blending dyes or pigments such as carbon black using general nylon polymer, the fastness and formability of the fabric were evaluated, and the results are shown in Table 1. It was. During dyeing, the concentration of acid dye Neurilan Black LDH (Yorkshire) was dyed at 4.0 parts by weight based on 100 parts by weight of fibers.

비교예 4Comparative Example 4

폴리프로필렌테레프탈레이트 중합물을 사용하여 방사한 75데니어 72필라멘트의 원사로 제직후 분산염료 Kayalon Polyester Black RV-SF (일본화약) 섬유 100 중량부에 4.0 중량부로 120℃에서 염색후 140℃로 건조하여 견뢰도 및 보형성능을 평가하였다.After weaving with 75 denier 72 filament yarn spun using polypropylene terephthalate polymer, 100 parts by weight of disperse dye Kayalon Polyester Black RV-SF fiber was dyed at 120 ° C. at 4.0 parts by weight and dried to 140 ° C. And prosthetic capacity was evaluated.

표 1. 염색견뢰도 및 보형기능성 평가 Table 1. Dyeing fastness and prosthetic functional evaluation

구분division 세탁견뢰도
(변퇴색)
Color fastness
(Fading)
오염pollution 보형기능Prosthetic function 심색성 (L값)Deep color (L value)
Nylon오염Nylon pollution Cotton오염Cotton pollution 실시예1Example 1 44 44 44 OO 1313 실시예2Example 2 3-43-4 3-43-4 44 OO 1717 비교예1Comparative Example 1 33 33 33 OO 1818 비교예2Comparative Example 2 2-32-3 22 2-32-3 OO 1515 비교예3Comparative Example 3 44 44 44 XX 1313 비교예4Comparative Example 4 44 3-43-4 44 1414

① 세탁견뢰도: KS K 1902 A-1 방법으로 측정① Fastness to washing: measured by KS K 1902 A-1 method

② 보형기능 : 숙련된 평가자 10명의 관능평가결과 종합하여 평가함② Prosthetic function: The sensory evaluation results of 10 experienced evaluators are evaluated.

양호 O, 중간 △, 나쁨 X               Good O, Medium △, Bad X

③ 심색성 : 색도분광측정기로 *L*a*b 값을 측정 L 값으로 Black color 심색성 평가.③ Deep color: Measure * L * a * b value with chromatic spectrophotometer Evaluate black color deep color with L value.

본 발명의 방법에 의하여 제조된 카치온 가염형 폴리아미드 섬유 및 직물은 상기 표 1에서 보는 바와 같이 종래기술에서와 같이 원사제조 단계에서 염료나 안료를 첨가하지 않고 제조한 카치온 가염형 폴리아미드 섬유의 경우 보형기능성은 유지하나 비교예 1과 같이 염색견뢰도, 특히 오염견뢰도 측면에서 불리한 점이 있으며, 심색성 발현을 위해 염료의 농도를 증가시킬 경우 견뢰도의 저하는 더욱 뚜렷해진다. 반면, 비교예 3 및 4에서와 같이 일반 나일론이나 보형기능성 면에서 뛰어나다고 알려진 폴리프로필렌테레프탈레이트 섬유를 이용했을 경우에는 염색견뢰도 및 심색성 측면에서는 우수하나 보형기능성은 다소 떨어지는 단점을 보인다.The cationic salt polyamide fiber and the fabric produced by the method of the present invention is as shown in Table 1 in the case of the cationic salt polyamide fiber prepared without the addition of dyes or pigments in the yarn manufacturing step as in the prior art as shown in Table 1 Prosthetic functionalities are maintained but disadvantageous in terms of staining fastness, especially staining fastness, as in Comparative Example 1, and the decrease in the fastness becomes more pronounced when the concentration of the dye is increased for deep color expression. On the other hand, when using polypropylene terephthalate fibers known to be excellent in general nylon or prosthetic functional properties as in Comparative Examples 3 and 4, the dyeing fastness and deep colorability is excellent but the prosthetic functionality is somewhat inferior.

반면, 실시예 1 및 2와 같이 제조한 카치온 가염형 폴리 아미드 섬유의 경우에는 적은양의 염료로도 우수한 심색효과 발현이 가능하고 염색견뢰도, 특히 오염견뢰도 측면에서도 우수한 효과를 보이며, 우수한 보형기능성 효과를 가진다.On the other hand, in the case of the cationic salt type polyamide fiber prepared as in Examples 1 and 2, it is possible to express the deep color effect even with a small amount of dye, and also shows excellent effect in terms of color fastness, especially stain fastness, and excellent prosthetic functional effect. Has

이상에서 본 발명의 바람직한 구현예를 들어 본 발명을 상세하게 설명하였으나 본 발명은 상술한 구현예에 한정되지 않으며, 본 발명의 기술적 사상의 범위 내 에서 본 발명이 속하는 기술 분야의 당업자에 의해 많은 변형이 가능함은 자명할 것이다.Although the present invention has been described in detail with reference to preferred embodiments of the present invention, the present invention is not limited to the above-described embodiments, and many modifications are made by those skilled in the art to which the present invention pertains within the scope of the technical idea of the present invention. This possibility will be self-evident.

Claims (6)

삭제delete 삭제delete 삭제delete ε-카프로락탐 100 중량부에 대하여 5-SSIPA 0.5~3.0 중량부를 첨가하여 중합체를 중합하는 단계; 및 상기 중합체 100중량부에 대하여 염료 또는 안료를 0.5~2.0중량부 블렌딩하여 고속 방사하는 단계를 포함하여 제조되는 카치온 가염형 폴리아미드 섬유를 직물의 경사, 또는 위사, 또는 경위사로 적용하여 직물을 제직한 후, 80~98℃ 범위에서 카치온 염료로 염색하고, 100~140℃ 범위에서 열처리하여 건조시키는 것을 특징으로 하는 직물의 제조방법.polymerizing the polymer by adding 0.5 to 3.0 parts by weight of 5-SSIPA based on 100 parts by weight of ε-caprolactam; And blending 0.5 to 2.0 parts by weight of dyes or pigments with respect to 100 parts by weight of the polymer, and spinning the fabric by applying a cationic salt-containing polyamide fiber prepared as a warp, or weft or warp yarn of the fabric. After that, dyeing with a cationic dye in the 80 ~ 98 ℃ range, and a method of producing a fabric, characterized in that the heat treatment by drying in the range of 100 ~ 140 ℃. 제4항에 있어서, 상기 방사 속도는 4,000 m/min. 이상인 것을 특징으로 하는 직물의 제조방법.The method of claim 4, wherein the spinning speed is 4,000 m / min. The manufacturing method of the fabric characterized by the above. 제 4항에 있어서, 단사섬도는 0.5-2.0데니어인 것을 특징으로 하는 직물의 제조방법.The method of claim 4, wherein the single yarn fineness is 0.5-2.0 denier.
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KR101458293B1 (en) * 2013-01-18 2014-11-04 주식회사 효성 Method for preparing cation dyeable polyester/nylon composite fiber and cation dyeable polyester/nylon composite fiber prepared thereby

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KR20050016438A (en) * 2002-05-24 2005-02-21 인비스타 테크놀러지스 에스.에이.알.엘 Method and Apparatus for Producing Polyamide Filaments of High Tensile Strength by High Speed Spinning
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Publication number Priority date Publication date Assignee Title
KR970010717A (en) * 1995-08-03 1997-03-27 서곤 How to convert n-butene to isobutene
KR20050016438A (en) * 2002-05-24 2005-02-21 인비스타 테크놀러지스 에스.에이.알.엘 Method and Apparatus for Producing Polyamide Filaments of High Tensile Strength by High Speed Spinning
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KR20080061104A (en) * 2006-12-28 2008-07-02 주식회사 효성 Method of producing a multi-tone color polyamide fabric

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101458293B1 (en) * 2013-01-18 2014-11-04 주식회사 효성 Method for preparing cation dyeable polyester/nylon composite fiber and cation dyeable polyester/nylon composite fiber prepared thereby

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