KR19980056773A - Manufacturing method of polyamide monofilament with excellent flexibility - Google Patents
Manufacturing method of polyamide monofilament with excellent flexibility Download PDFInfo
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- KR19980056773A KR19980056773A KR1019960076043A KR19960076043A KR19980056773A KR 19980056773 A KR19980056773 A KR 19980056773A KR 1019960076043 A KR1019960076043 A KR 1019960076043A KR 19960076043 A KR19960076043 A KR 19960076043A KR 19980056773 A KR19980056773 A KR 19980056773A
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- polyamide
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- polyamide monofilament
- excellent flexibility
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- 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
- D01D5/04—Dry spinning methods
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
- D01F6/80—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyamides
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- 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
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- 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
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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)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Polyamides (AREA)
Abstract
본 발명은 ε-카프로락탐 30 내지 50 중량% 아디프산과 헥사메틸렌디아민의 혼합염 10 내지 30 중량%를 사용한 중합물에 2-메틸펜타메틸렌디아민과 이소프탈릭산으로 이루어진 염 10 내지 30 중량%, 라우르락탐 10 내지 20 중량% 첨가하여 폴리아미드 중합물을 제조하고 압출하여 폴리아미드 모노필라멘트를 제조하는 것으로서, 중·고온영역에서도 강성이 양호하게 유지되고 투명성과 유연성이 우수한 폴리아미드 모노필라멘트를 얻을 수 있다.The present invention relates to 10 to 30% by weight of a salt consisting of 2-methylpentamethylenediamine and isophthalic acid in a polymer using 30 to 50% by weight of a mixed salt of ε-caprolactam 30 to 50% by weight of a mixed salt of adipic acid and hexamethylenediamine. Polyamide monofilament is prepared by adding 10 to 20% by weight of uractam to prepare a polyamide polymer and extruding it to obtain a polyamide monofilament having excellent rigidity and excellent transparency and flexibility even in a medium to high temperature region. .
Description
본 발명은 유연성이 우수한 폴리아미드 모노필라멘트의 제조방법에 관한 것으르 더욱 상세하게는, 기존의 폴리아미드 중합물에 제 3의 물질을 첨가하여 공중합 함으로써 중, 고온 영역에서도 강성이 양호하게 유지되고 투명성과 유연성이 매우 우수한 폴리아미드 모노필라멘트의 제조방법을 제공하는 것이다.The present invention relates to a method for producing polyamide monofilament having excellent flexibility. More specifically, by adding a third material to the existing polyamide polymer and copolymerizing it, the rigidity is maintained well in the medium and high temperature ranges and the transparency and It is to provide a method for producing a polyamide monofilament with excellent flexibility.
폴리아미드 모노필라멘트(mono-filment) 는 1본 (本) 의 굵은 단섬유로 된것을 의미하는 것으로써 어망, 브러시(brush) 강모, 배드민턴, 테니스 라켓의 거트(gut)등에 주로 사용되는데 직선강도 이외에도 높은 결절강도 및 우수한 투명성이 요구된다.Polyamide monofilament (mono-filment) means a single thick coarse fiber, mainly used in fishing nets, brush bristles, badminton, gut of tennis rackets, etc. High nodule strength and good transparency are required.
상기와 같은 목적의 폴리아미드 모노필라멘트의 제조는 용융 폴리아미드를 압출 급냉 후 제 1단계로 3 내지 4배 연신하고 높은 온도에서 2단계 연신을 한 다음에 열고정을 하는 방법으로 제조하였고, 아울러 투명성을 좋게하기 위해서 용융압출된 폴리아미드를 방사노즐로 부터 냉각장치에 도달할 때까지의 시간을 통상 0.3초 전후로 짧게하여 급냉하는 방법을 사용하였다. 그러나 이렇게 제조된 폴리아미드 모노필라멘트는 투명성은 양호하나 반면에 투명성에 비하여 유연성 측면에서는 충분하지 못한 결점이 있었다.The polyamide monofilament for the above purpose was prepared by extrusion molten polyamide 3 to 4 times in the first step after extrusion quenching, heat drawing in two stages at high temperature and then heat setting, and transparency In order to improve the efficiency, the method of rapidly cooling the melt-extruded polyamide from the spinning nozzle to the cooling device was generally shortened to about 0.3 seconds. However, the polyamide monofilaments thus prepared have good transparency, but have insufficient defects in terms of flexibility compared to transparency.
따라서, 본 발명은 상기의 문제점을 해결하기 위하여 투명성이 우수하면서 높은 연신비로 연신하여도 유연성이 우수한 폴리아미드 모노필라멘트의 제조방법을 제공하는 것으로, 본 발명에 사용되는 폴리아미드는 아디프산과 헥사메틸렌 디아민으로 이루어지는 혼합염과 ε-카프로락탐으로 이루어지는 기존의 중합물에 제3의 물질인 2-메틸펜타메틸렌디아민과 이소프탈릭산으로 이루어진 염 그리고 라우르락탐 중합물을 첨가하여 공중합 한 것으로써 중, 고온 영역에서도 강성이 양호하게 유지되고, 직경이 큰 모노필라멘트에서도 유연성이 매우 우수한 폴리아미드 모노필라멘트의 제조를 가능하게 한다.Accordingly, the present invention provides a method for producing a polyamide monofilament having excellent transparency and excellent flexibility even at a high draw ratio in order to solve the above problems, the polyamide used in the present invention is adipic acid and hexamethylene Copolymerization by adding a mixed salt consisting of diamine and an existing polymer consisting of ε-caprolactam, adding a third material, a salt consisting of 2-methylpentamethylenediamine and isophthalic acid, and a laulactam polymer to copolymerize them. The stiffness is maintained well at even and enables the production of polyamide monofilaments having excellent flexibility even in large diameter monofilaments.
이하 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.
본 발명에서는 보다 높은 투명성과 유연성을 확보하기 위하여 ε-카프로락탐을 전체원료의 30 내지 50 중량% 로 하고, 아디프산과 헥사메틸렌디아민의 혼합염을 10 내지 30 중량% 사용한 중합물에 2-메틸펜타메틸렌 디아민과 이소프탈릭산으로 이루어진 염 10 내지 30 중량%, 라우르락탐은 10 내지 20 중량%, 더욱바람직하게는 10 중량%를 첨가하여 제조하는 것을 특징으로 한다. 여기서 라우르락탐은 탄소수12개의 긴체인을 제공함으르써 비결정성에 영향을 주어 유연성을 극대 시키는 효과가 있으나, 고가이며 라우르락탐만을 첨가하여 제조된 공중합물은 서로 달라붙는 현상을 보이므로 본 발명에서는 2 -메틸펜타메틸렌 디아민 과 이소프탈릭산을 첨가함으로써 이를 해결하였다. 이와같이 공중합된 폴리아미드에는 통상의 활제, 염료, 안료등의 착색제 혹은 내후성 향상을 위한 첨가제 등을 함유시킬 수 있다.In the present invention, in order to ensure higher transparency and flexibility, 2-methylpenta is used in a polymer using ε-caprolactam as 30 to 50% by weight of the total raw material and 10 to 30% by weight of a mixed salt of adipic acid and hexamethylenediamine. 10 to 30% by weight of a salt consisting of methylene diamine and isophthalic acid, laulactam is characterized in that it is prepared by adding 10 to 20% by weight, more preferably 10% by weight. Wherein laulactam has a long chain of 12 carbon atoms to affect the amorphousness has the effect of maximizing flexibility, but the copolymer produced by adding only laulactam is expensive and shows the phenomenon of sticking together Eg solved this by adding 2-methylpentamethylene diamine and isophthalic acid. The polyamide copolymerized in this way may contain ordinary lubricants, dyes, colorants such as pigments, additives for improving weather resistance, and the like.
상기의 폴리아미드는 통상 펠렛(Pellet)의 형태로 공급되고, 용융된 후 공경(孔徑) 10mm이상의 방사 노즐에서 압출된다.The polyamide is usually supplied in the form of pellets, melted and extruded in a spinning nozzle having a pore size of 10 mm or more.
직경이 3.0mm보다 큰 모노필라멘트를 얻기 위해서 공경이 10mm이상인 방사노즐에서 용융 폴리아미드를 압출할 매 통상의 경우에는 실의 흔들림이 일어나 인취가 불안정해지고 진원성이 나쁘게 되어 물성에 영향을 주지만 본 발명에 따라 공중합된 폴리아미드는 압출할때 용융물의 흐름성이 균일해 실의 흔들림을 방지할 수 있다.In order to extrude the molten polyamide from a spinning nozzle with a pore diameter of 10 mm or more to obtain a monofilament having a diameter larger than 3.0 mm, in general, the shaking of the thread occurs, leading to instability and poor roundness, thus affecting physical properties. The polyamide copolymerized according to the present invention can uniformly flow the melt during extrusion to prevent the shaking of the yarn.
상기한 바와같이 제조한 폴리아미드 모노필라멘트는 투명성과 유연성을 만족 시키기위하여 그 직경을 2.0 내지 4.0mm로 하는 것이 바람직한데 기존의 모노필라멘트보다 같은 굵기에서 상대적으로 우수한 유연성을 갖는 효과가 있다.Polyamide monofilament prepared as described above is preferably in the diameter of 2.0 to 4.0mm to satisfy the transparency and flexibility, there is an effect having a relatively excellent flexibility at the same thickness than the conventional monofilament.
이하 실시예 및 비교예를 들어 본 발명에 대하여 상세히 설명한다.Hereinafter, the present invention will be described in detail with reference to Examples and Comparative Examples.
[실시예1]Example 1
ε-카프로락탐 2880g과 헥사메틸렌디아민 디암모늄 아디페이트 1200g과 라우르락탐 750g, 2- 메틸펜타메틸렌디아민 830g과 이소프탈릭산 1150g을 같이 넣고 여기에 60 내지 70 % 용액이 되도록 증류수를 첨가한 후 중합한다. 이 중합물을 50mm압출기를 이용하여 공경 10mm의 노즐로 부터 압출하고 공기중에 유지한 후 급냉하고 다음에 연신처리를 한 다음 인취속도 20m/ 분 으로 직경이 3.5mm의 폴리아미드 모노 필라멘트를 제조한후 물성을 표.1에 나타내었다. 이 공중합물의 상대점도는 3.12이다.2880 g of ε-caprolactam, 1200 g of hexamethylenediamine diammonium adipate, 750 g of laulactam, 830 g of 2-methylpentamethylenediamine, and 1150 g of isophthalic acid are added together, and distilled water is added thereto to make a solution of 60 to 70%. do. The polymer was extruded from a nozzle with a diameter of 10 mm using a 50 mm extruder, held in air, quenched, then stretched, and prepared polyamide monofilament having a diameter of 3.5 mm with a pulling speed of 20 m / min. Is shown in Table 1. The relative viscosity of this copolymer is 3.12.
실시예2Example 2
ε- 카프로락탐 2255g과 헥사메틸렌디아민 디암모늄 아디페이트1100g과 라우르락탐 920g, 2-메틸펜타메틸렌디아민 700)g과 이소프탈릭산1002g을 같이 넣는다. 여기에 60 내지 70% 용액이 되도록 증류수를 첨가한 후 중합한다. 중합 및 모노필라멘트 제조방법은 실시예 1과 동일하게 행하고 그 결과를 표.1에 나타내었다. 이 공중합물의 상대점도는 3.12이다.2255 g of epsilon caprolactam, 1100 g of hexamethylenediamine diammonium adipate, 920 g of laulactam, 700) g of 2-methylpentamethylenediamine and 1002 g of isophthalic acid are added together. Distilled water is added here to make a solution of 60 to 70% and then polymerized. The polymerization and monofilament manufacturing methods were carried out in the same manner as in Example 1, and the results are shown in Table 1. The relative viscosity of this copolymer is 3.12.
[비교예1]Comparative Example 1
ε-카프로락탐 2100g과 헥사메틸렌디아민 수용액 980g, 그리고 아디프산 752g과 증류수 980g을 반응기에 넣고 260℃에서 반응시킨다. 이렇게 하여 얻은 공중합물의 상대점도는 3.2정도이다. 중합 및 모노필라멘트제조방법은 실시예1과 동일하게 행하고 그 결과를 표.1에 나타내었다.2100 g of epsilon caprolactam, 980 g of hexamethylenediamine aqueous solution, and 752 g of adipic acid and 980 g of distilled water were added to a reactor and reacted at 260 ° C. The relative viscosity of the copolymer thus obtained is about 3.2. The polymerization and monofilament production methods were carried out in the same manner as in Example 1, and the results are shown in Table 1.
[ 물성 평가 방법][Property evaluation method]
(1) 결절강도 및 직선강도는 JlSL 1070에 준하여 측정한 값을 나타낸다.(1) Nodule strength and linear strength indicate values measured according to JlSL 1070.
(2) 유연성은 길이 5cm의 모노필라멘트사를 유연 측정기로 측정한 값을 나타내며 이 값은 크기가 작을수록 더욱 유연함을 나타낸다.(2) Flexibility refers to the measurement of 5cm length of monofilament yarn with a flexible measuring instrument. The smaller the size, the more flexible.
(3) 투명성의 평가는 각 폴리아미드를 상기의 방법으로 압출하여 모노필라멘트로 만들었을때 직경에 따라 복측으로 평가 하였다.(3) Evaluation of transparency evaluated each polyamide extruded by the above-mentioned method into a monofilament, and evaluated it by the abdomen according to the diameter.
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JPS6485315A (en) * | 1987-09-24 | 1989-03-30 | Momoi Fishing Net Mfg Co Ltd | Polyamide monofilament and production thereof |
AU664163B2 (en) * | 1990-11-20 | 1995-11-09 | Invista Technologies S.A.R.L. | Terpolyamides and multipolyamides containing amide units of 2-methylpentamethylenediamine and products prepared therefrom |
KR0178053B1 (en) * | 1992-12-29 | 1999-05-15 | 구창남 | Polyamide composition having excellent thermal shrinkage stability |
KR950002615A (en) * | 1993-07-02 | 1995-02-16 | 김광수 | Manufacturing method of mugwort bamboo salt |
KR960022685A (en) * | 1994-12-28 | 1996-07-18 | 백영배 | Polyamide resin composition excellent in transparency |
KR100186902B1 (en) * | 1995-12-11 | 1999-05-15 | 백영배 | The composition of polyamide monofilament having high transparency |
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