KR101047046B1 - A manufacturing method of polyester yarn - Google Patents

A manufacturing method of polyester yarn Download PDF

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Publication number
KR101047046B1
KR101047046B1 KR1020100127076A KR20100127076A KR101047046B1 KR 101047046 B1 KR101047046 B1 KR 101047046B1 KR 1020100127076 A KR1020100127076 A KR 1020100127076A KR 20100127076 A KR20100127076 A KR 20100127076A KR 101047046 B1 KR101047046 B1 KR 101047046B1
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South Korea
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polyester
tube
polyester fiber
yarn
undrawn yarn
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KR1020100127076A
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Korean (ko)
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최재호
장기혁
정상영
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주식회사 삼양사
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    • 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
    • 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
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters

Abstract

PURPOSE: A method of manufacturing polyester fiber is provided to offer polyester undrawn yarn having stretching uniformity with excellent properties of matter such as high elasticity and high intensity. CONSTITUTION: The method of manufacturing polyester fiber is as follows. In the method of manufacturing polyester fiber, a spinneret melt spins and cools a polyester resin of inherent viscosity of 0.8 - 1.5. The undrawn yarn has a tube having a path which is maintained at a temperature of 50-150°C, passes through the path of the tube, and is heated. The heated undrawn yarn is heat treated and stretched.

Description

폴리에스테르 섬유의 제조방법{A MANUFACTURING METHOD OF POLYESTER YARN}Manufacturing method of polyester fiber {A MANUFACTURING METHOD OF POLYESTER YARN}

본 발명은 폴리에스테르 섬유의 제조방법에 관한 것으로서, 더욱 상세하게는 공정성이 우수할 뿐만 아니라, 외부 충격 또는 변형에 대한 충분한 저항성을 나타내어 로프, 벨트, 토목용 구조체 등의 산업용 섬유로 매우 유용하게 사용될 수 있는 폴리에스테르 섬유의 제조방법에 관한 것이다.The present invention relates to a method for producing a polyester fiber, and more particularly, it is not only excellent in processability, but also exhibits sufficient resistance to external impact or deformation, which is very useful for industrial fibers such as ropes, belts, civil structures, etc. It relates to a method for producing a polyester fiber that can be.

폴리에스테르 수지는 테레프탈산 또는 디메틸테레프탈레이트와 에틸렌글리콜을 중합시켜 제조된다. Polyester resins are prepared by polymerizing terephthalic acid or dimethyl terephthalate with ethylene glycol.

폴리에스테르 수지로 된 섬유는 로프, 벨트, 타포린이나 트럭 커버지와 같은 코팅직물의 베이스 직물, 토목용 보강재 등 산업용 섬유로서 그 용도가 계속해서 확대되어 가고 있다. 이는 폴리에스테르 섬유가 갖는 우수한 기계적 물성 때문이다. Fibers made of polyester resins are increasingly being used as industrial fibers such as ropes, belts, base fabrics of coated fabrics such as tarpaulins or truck covers, and civil reinforcements. This is due to the excellent mechanical properties of polyester fibers.

최근에는 높은 탄성을 갖는 고강도의 폴리에스테르 섬유가 요구되고 있다. 이러한 요구조건에 부합되는 폴리에스테르 섬유를 얻기 위하여, 폴리에스테르 수지의 고유점도를 높이거나, 연신배율을 높이는 방법이 제안되었다. In recent years, high strength polyester fiber which has high elasticity is calculated | required. In order to obtain polyester fibers that meet these requirements, a method of increasing the intrinsic viscosity of the polyester resin or increasing the draw ratio has been proposed.

이 중, 폴리에스테르 수지의 고유점도를 높이는 방법은 수지의 고상중합 공정시 체류시간을 증가시켜야 하는데 이는 코스트 상승과 직결되며, 제조된 폴리에스테르 수지의 용융점도가 상승되므로 용융방사시 공정성을 제어하기가 어렵다는 문제가 있다.Of these, the method of increasing the intrinsic viscosity of the polyester resin should increase the residence time during the solid-state polymerization process of the resin, which is directly connected to the cost increase, and the melt viscosity of the produced polyester resin is increased to control the processability during melt spinning There is a problem that is difficult.

한편, 폴리에스테르 섬유의 연신배율을 높이기 위한 방법으로서, 연신 구간에 연신점을 고정시키기 위하여 열풍이나 증기를 이용하거나, 방사노즐하단에 후두(hood) 히터를 설치하거나 보온 구간(Delayed zone)을 길게 설치하여 방사되는 수지의 연신특성을 조절하는 방법이 이용되고 있다. On the other hand, as a method for increasing the draw ratio of the polyester fiber, using hot air or steam to fix the stretching point in the stretching section, or to install a latitude (hood) heater at the bottom of the spinneret or lengthen the delayed zone (Delayed zone) The method of adjusting the extending | stretching characteristic of resin provided and spun is used.

연신점을 고정시키는 방법은 연신전 미연신사 자체의 연신특성이 불균일한 경우에는 크게 효과를 보기가 어렵다. The method of fixing the stretching point is hardly effective when the stretching characteristics of the unstretched yarn itself before stretching are uneven.

또한, 방사노즐하단에 히터 등의 설비를 이용하는 방법은 방사된 섬유에 존재하는 배향 불균일성을 해소하는데 유리하나, 이를 냉각공정을 통해 냉각시키는 과정에서 발생하는 미연신사의 배향 불균일성은 제어할 수는 없다. In addition, the method using a heater or the like at the bottom of the spinning nozzle is advantageous to solve the orientation nonuniformity existing in the spun fiber, but the orientation nonuniformity of the undrawn yarn generated during the cooling process through the cooling process cannot be controlled. .

한편, 일본국 특개소 46-6459호 등에는 방사 및 연신을 하나의 연속단계로 수행하는 직접방사연신법(Direct Spinning Drawing process)이 개시되어 있다. 이러한 직접방사연신법은 방사와 연신이 동시에 수행되어야 하므로, 열풍 역시 연신과정에서 이용되게 된다. On the other hand, Japanese Patent Laid-Open No. 46-6459 and the like disclose a direct spinning drawing process in which spinning and stretching are performed in one continuous step. In this direct radiation drawing method, the spinning and drawing must be performed at the same time, so hot air is also used in the drawing process.

본 발명이 해결하려는 과제는 상기한 문제점을 해결하기 위한 것으로서, 용융방사 및 냉각한 폴리에스테르 미연신사의 배향 불균일성을 효과적으로 해소하므로서, 이를 연신시 우수한 탄성과 강도를 갖는 폴리에스테르 섬유를 제조하는 방법을 제공하는데 있다.      The problem to be solved by the present invention is to solve the above problems, and to effectively solve the orientation non-uniformity of the melt-spun and cooled polyester non-drawn yarn, a method for producing a polyester fiber having excellent elasticity and strength during stretching To provide.

전술한 과제를 달성하기 위하여, 본 발명에 따른 폴리에스테르 섬유의 제조방법은,In order to achieve the above object, the manufacturing method of the polyester fiber according to the present invention,

(S1) 폴리에스테르 수지를 방사구금을 통해 용융방사하고 냉각시켜 미연신사를 제조하는 단계; (S1) melt spinning the polyester resin through a spinneret and cooling to prepare an unstretched yarn;

(S2) 길이방향으로 연장되며, 50 내지 150 ℃로 유지되는 통로를 갖는 튜브를 준비하고, 상기 미연신사를 튜브의 통로로 통과시켜 가열하는 단계; 및  (S2) preparing a tube having a passage extending in the longitudinal direction and maintained at 50 to 150 ° C., and heating the undrawn yarn by passing through the passage of the tube; And

(S3) 상기 가열된 미연신사를 열처리하며 연신하는 단계를 포함한다. (S3) heat treating and stretching the heated unstretched yarn.

본 발명에 따른 폴리에스테르 섬유의 제조방법에 있어서, 상기 폴리에스테르 수지의 고유점도(IV)는 0.8 내지 1.5인 것이 바람직하다. In the manufacturing method of the polyester fiber which concerns on this invention, it is preferable that the intrinsic viscosity (IV) of the said polyester resin is 0.8-1.5.

본 발명에 따른 폴리에스테르 섬유의 제조방법에 있어서, 상기 튜브의 길이는 2 내지 4 m인 것이 바람직하다. In the method for producing a polyester fiber according to the present invention, the length of the tube is preferably 2 to 4 m.

본 발명에 따른 폴리에스테르 섬유의 제조방법에 있어서, 미연신사의 총 연신비는 6배 이상인 것이 바람직하고, 얻어진 폴리에스테르 섬유의 LASE 5% 값은 5.5 g/d 이상이고, 강도가 10.0 g/d 이상이고, 파단신도가 12% 이하인 것이 바람직하다.In the method for producing the polyester fiber according to the present invention, the total draw ratio of the undrawn yarn is preferably 6 times or more, the LASE 5% value of the obtained polyester fiber is 5.5 g / d or more, and the strength is 10.0 g / d or more. And elongation at break is preferably 12% or less.

본 발명은 용융방사한 폴리에스테르 미연신사를 소정 온도로 유지된 튜브 내부로 통과시켜 가열하므로서, 미연신사의 배향 불균일성을 해소한다. 가열 처리된 폴리에스테르 미연신사는 연신 균일성이 양호하므로, 이를 연신하면 고탄성, 고강도의 우수한 물성을 갖는 폴리에스테르 섬유를 용이하게 제조할 수 있다.The present invention solves the orientation nonuniformity of the undrawn yarn by passing the melt-spun polyester undrawn yarn into a tube maintained at a predetermined temperature to be heated. Heat-treated polyester unstretched yarn has a good stretching uniformity, it can be easily produced polyester fibers having excellent properties of high elasticity, high strength when drawn.

본 발명에 따라 제조된 폴리에스테르 섬유는 외부 충격 또는 변형에 대한 충분한 저항성을 나타내므로, 로프, 벨트, 토목용 구조체 등의 산업용 섬유로 매우 유용하게 사용될 수 있다. Polyester fibers produced according to the present invention exhibits sufficient resistance to external impact or deformation, and thus can be very usefully used as industrial fibers such as ropes, belts, civil structures and the like.

이하, 본 발명에 대하여 상세히 설명하기로 한다. 이에 앞서, 본 명세서 및 청구범위에 사용된 용어나 단어는 통상적이거나 사전적인 의미로 한정해서 해석되어서는 아니되며, 발명자는 그 자신의 발명을 가장 최선의 방법으로 설명하기 위해 용어의 개념을 적절하게 정의할 수 있다는 원칙에 입각하여 본 발명의 기술적 사상에 부합하는 의미와 개념으로 해석되어야만 한다.      Hereinafter, the present invention will be described in detail. Prior to this, terms or words used in the specification and claims should not be construed as having a conventional or dictionary meaning, and the inventors should properly explain the concept of terms in order to best explain their own invention. Based on the principle that can be defined, it should be interpreted as meaning and concept corresponding to the technical idea of the present invention.

본 발명에 따른 폴리에스테르 섬유의 제조방법은 다음과 같다.The manufacturing method of the polyester fiber which concerns on this invention is as follows.

먼저, 폴리에스테르 수지를 방사구금을 통해 용융방사하고 냉각시켜 미연신사를 제조한다(S1 단계).First, the polyester resin is melt-spun through a spinneret and cooled to prepare an unstretched yarn (S1 step).

사용되는 폴리에스테르 수지의 고유점도는 방사 작업성과 얻어지는 섬유의 물성을 고려할 때 0.8 내지 1.5인 것이 바람직하다. 이러한 고유점도를 갖는 폴리에스테르 수지를 용융방사 및 연신하여 얻어지는 최종적인 폴리에스테르 섬유의 고유점도는 통상 0.7 내지 1.2 정도가 된다. 폴리에스테르 수지의 고유점도가 0.8 이상일 때 얻어지는 섬유의 물성이 더욱 양호해지며, 1.5를 초과하면 가공성이 저하되어 충분한 연신성이 부여되기 어려울 수 있다.The intrinsic viscosity of the polyester resin to be used is preferably 0.8 to 1.5 in consideration of spinning workability and the physical properties of the fiber obtained. The intrinsic viscosity of the final polyester fiber obtained by melt spinning and stretching the polyester resin which has such an intrinsic viscosity becomes about 0.7-1.2 normally. When the intrinsic viscosity of the polyester resin is 0.8 or more, the physical properties of the fiber obtained are better, and when it exceeds 1.5, the workability is lowered, so that sufficient elongation may be difficult.

용융방사의 온도는 폴리에스테르 수지를 충분히 용융시켜 섬유상으로 방사할 수 있으면서도 폴리에스테르 수지의 열분해를 최소화할 수 있는 온도로서, 사용되는 폴리에스테르 수지의 고유점도에 따라 적절히 결정할 수 있다. 방사된 섬유상의 폴리에스테르 수지는 예를 들어 20 내지 25 ℃의 급랭 공기로 냉각시킴으로서 미연신사를 제조한다. 제조된 미연신사는 권취기에 권취하여 다음 공정에 투입될 수 있다.The melt spinning temperature is a temperature at which the polyester resin can be sufficiently melted and spun into a fibrous shape while minimizing thermal decomposition of the polyester resin, and can be appropriately determined according to the intrinsic viscosity of the polyester resin used. The spun fibrous polyester resin is produced unstretched yarn, for example, by cooling with quench air at 20 to 25 ° C. The prepared non-drawn yarn may be wound up in a winding machine and put into the next process.

S1 단계에 따라 냉각된 미연신사는 분자쇄들의 배향이 매우 불균일하다. 이에 따라 미연신사를 바로 연신하는 경우, 연신이 불균일해져서 얻어지는 섬유의 물성이 불량해진다.The undrawn yarn cooled according to the step S1 is very uneven in the orientation of the molecular chains. Thereby, when extending | stretching unstretched yarn immediately, extending | stretching becomes nonuniform and the physical property of the fiber obtained will become bad.

이러한 문제점을 해결하기 위하여, 본 발명은 길이방향으로 연장되며, 50 내지 150 ℃로 유지되는 통로를 갖는 튜브를 준비하고, 상기 미연신사를 튜브의 통로로 통과시켜 가열하였다(S2 단계). In order to solve this problem, the present invention extends in the longitudinal direction, and prepared a tube having a passage maintained at 50 to 150 ℃, and the undrawn yarn was passed through the passage of the tube and heated (step S2).

이와 같이, 폴리에스테르 미연신사를 소정 온도로 유지된 튜브의 통로로 통과시켜 가열하면, 미연신사의 배향 불균일성을 해소된다. 가열 처리된 폴리에스테르 미연신사는 연신 균일성이 양호해지며, 미연신사의 연신비를 높일 수 있게 된다. 즉, 가열 처리하여 배향 불균일성을 해서한 미연신사를 연신하면, 우수한 물성을 갖는 폴리에스테르 섬유를 제조할 수 있다. In this way, when the polyester non-drawn yarn is passed through a passage of a tube maintained at a predetermined temperature and heated, the orientation unevenness of the undrawn yarn is eliminated. The heat treated polyester unstretched yarn has a good stretching uniformity, and can increase the draw ratio of the unstretched yarn. That is, when extending | stretching the unstretched yarn which performed the heat processing and performed the orientation nonuniformity, the polyester fiber which has the outstanding physical property can be manufactured.

튜브의 길이는 미연신사가 통과하며 배향 불균일성이 해소될 수 있도록 충분히 가열처리될 수 있는 길이라면 제한되지 않는데, 2 m 이상이 바람직하고, 더욱 바람직하게는 2 내지 4 m이다. 튜브의 가운데에 형성된 통로의 단면 형상은 미연신사가 잘 주행할 수 있도록 원형 또는 타원형인 것이 바람직하나, 사각형, 삼각형 등 다른 단면 형상도 가능하다. 이러한 튜브를 이용하면, 적은 에너지로 미연신사를 안정적으로 열처리할 수 있다. The length of the tube is not limited as long as it can be sufficiently heat treated so that the undrawn yarn passes and the orientation nonuniformity is eliminated, preferably 2 m or more, more preferably 2 to 4 m. The cross-sectional shape of the passage formed in the center of the tube is preferably circular or elliptical so that the undrawn yarn can run well, but other cross-sectional shapes such as squares and triangles are possible. By using such a tube, unstretched yarn can be stably heat treated with little energy.

튜브 통로의 온도가 50 ℃ 미만이면, 미연신사의 분자쇄들이 잘 유동될 수 없어 배향 균일화의 효과가 작다. 튜브 통로의 온도가 150 ℃를 초과하면, 급격한 결정화가 진행되어 많은 미세결정들이 생성 및 성장한다. 이들 미세결정들은 연신시 취약점으로 작용하게 된다. 그 결과, 강도가 저하되고 품질 면에서 모우 등의 문제가 현저해지며, 심한 경우 실의 절단을 초래할 수 있어 공정 안정성을 확보하기 어려워진다. If the temperature of the tube passage is less than 50 ° C., the molecular chains of the undrawn yarn cannot flow well, so that the effect of orientation uniformity is small. When the temperature of the tube passage exceeds 150 ° C., rapid crystallization proceeds to produce and grow many microcrystals. These microcrystals act as vulnerabilities in stretching. As a result, the strength is lowered, and problems such as cattle in terms of quality become remarkable, and in severe cases, it can cause cutting of the yarn, making it difficult to secure process stability.

튜브 통로를 전술한 온도로 유지시키는 방법으로는 열풍을 튜브 통로로 불어넣으면서 유지시키는 방법이 효과적이며, 이 외에 히터를 이용하여 적정 온도를 유지시키는 방법 등이 사용될 수 있다.As a method of maintaining the tube passage at the above-mentioned temperature, a method of maintaining hot air while blowing it into the tube passage is effective. In addition, a method of maintaining a proper temperature using a heater may be used.

그런 다음, 튜브 통로에서 가열된 미연신사를 열처리하며 연신한다(S3 단계). Then, the unstretched yarn heated in the tube passage is stretched by heat treatment (step S3).

튜브 통로에서 가열된 미연신사는 연속적으로 폴리에스테르 섬유의 통상적인 연신방법에 따라 수행된다. 즉, 연신이 가능하도록 온도가 설정되어 있으며, 속도가 다르게 회전하는 롤러 사이로 미연신사를 통과시켜 연신을 수행하는데, 미연신사의 연신은 통상적인 연신방법에 따라 2단계로 진행하는 것이 바람직하나, 이에 한정되는 것은 아니다. 미연신사의 총 연신비는 고강력 폴리에스테르 섬유를 얻을 수 있도록 6배 이상인 것이 바람직하다. 연신된 폴리에스테르 섬유는 필요에 따라 통상적인 열셋팅 처리를 할 수 있다. The undrawn yarn heated in the tube passage is continuously carried out according to the conventional drawing method of polyester fiber. That is, the temperature is set to allow the stretching, the stretching is carried out by passing the undrawn yarn between the rollers rotate at different speeds, the stretching of the undrawn yarn is preferably carried out in two steps in accordance with a conventional drawing method, It is not limited. The total draw ratio of the undrawn yarn is preferably 6 times or more so as to obtain a high strength polyester fiber. The stretched polyester fiber can be subjected to conventional heat setting treatments as necessary.

전술한 제조방법에 따라 미연신사를 튜브의 통로로 주행시켜 가열처리 및 연신 공정을 거쳐 얻은 폴리에스테르 섬유는 고탄성과 고강도를 나타내는데, 폴리에스테르 섬유의 LASE 5% 값이 5.5 g/d 이상, 강도가 10.0 g/d 이상, 파단신도가 12% 이하로 제조하는 것이 바람직하다.According to the above-mentioned manufacturing method, polyester fiber obtained by running unstretched yarn through a passage of a tube and undergoing a heat treatment and stretching process has high elasticity and high strength. The LASE 5% value of the polyester fiber is 5.5 g / d or more and the strength is high. It is preferable to manufacture 10.0 g / d or more and breaking elongation 12% or less.

이러한 폴리에스테르 섬유는 모노필라멘트 또는 멀티필라멘트로 이용되어 산업용, 특히 토목용 보강재나 안전벨트용으로서 유용하다. These polyester fibers are used as monofilaments or multifilaments and are useful for industrial, in particular civil reinforcement or safety belts.

이하, 본 발명을 구체적으로 설명하기 위해 실시예를 들어 상세하게 설명하기로 한다. 그러나, 본 발명에 따른 실시예들은 여러 가지 다른 형태로 변형될 수 있으며, 본 발명의 범위가 아래에서 상술하는 실시예들에 한정되는 것으로 해석되어져서는 안된다. 본 발명의 실시예들은 당업계에서 평균적인 지식을 가진 자에게 본 발명을 보다 완전하게 설명하기 위해서 제공되어지는 것이다.
Hereinafter, the present invention will be described in detail with reference to Examples. However, embodiments according to the present invention can be modified in many different forms, the scope of the present invention should not be construed as limited to the embodiments described below. Embodiments of the present invention are provided to more completely explain the present invention to those skilled in the art.

고유점도(IV)Intrinsic Viscosity (IV)

페놀과1,1,2,2-테트라클로로에탄올을 6:4(무게비)로 혼합한 시약(90℃)에 폴리에스테르 수지 0.1g을 90분 동안 용해시킨 후, 우베로데(Ubbelohde) 점도계에 옮겨 담아 30℃의 항온조에서 10분 동안 유지시키고, 점도계와 애스피레이터(Aspirator)를 이용하여 용액의 낙하초수를 구하였다. 용제의 낙하초수 역시 동일한 방법으로 구한 다음, 고유점도 계산법에 따라 고유점도(I.V.) 값을 계산하였다.After dissolving 0.1 g of a polyester resin for 90 minutes in a reagent (90 ° C.) in which phenol and 1,1,2,2-tetrachloroethanol were mixed at 6: 4 (weight ratio), a Ubbelohde viscometer was used. Transfer was carried out, it was maintained for 10 minutes in a 30 degreeC thermostat, and the fall second of the solution was calculated | required using a viscometer and an aspirator. The number of falling seconds of the solvent was also calculated in the same manner, and then the intrinsic viscosity (I.V.) value was calculated according to the intrinsic viscosity calculation method.

섬유의 모듈러스와 강신도 측정방법How to measure modulus and elongation of fiber

섬유를 표준상태인 조건, 즉 온도 25℃ 와 상대습도 65%인 상태의 항온항습실에서 24시간 동안 방치한 후, ASTM D-885의 방법에 따라 인장시험기를 통해 섬유의 모듈러스와 강신도를 측정하였다.After the fibers were left in a constant temperature and humidity room at a standard condition, that is, a temperature of 25 ° C. and a relative humidity of 65% for 24 hours, the modulus and elongation of the fibers were measured by a tensile tester according to the method of ASTM D-885.

건열 수축률 측정방법How to measure dry heat shrinkage

섬유를 표준상태, 즉 온도25℃와 상대습도 65%의 항온항습실에서 24시간 동안 방치한 다음, 190℃의 오븐에서 5분 동안 열처리하였다. 오븐에서 열처리한 섬유를 꺼낸 다음, 표준상태에서 24시간 동안 방치하고, 섬유의 줄어든 수축률을 아래 식에 따라 측정하였다.The fibers were allowed to stand for 24 hours in a constant temperature and humidity chamber of standard conditions, i.e., a temperature of 25 ° C and a relative humidity of 65%, followed by heat treatment for 5 minutes in an oven at 190 ° C. After removing the heat-treated fiber in the oven, it was left for 24 hours in a standard state, and the reduced shrinkage of the fiber was measured according to the following equation.

수축률(%) =(L0 ―L1) / L0 × 100 Shrinkage (%) = (L0-L1) / L0 × 100

위 식에서, L0은 섬유를 전술한 표준상태에서 24시간 동안 방치한 후 초하중(0.01g/d)하에서 측정한 길이이고, L1은 오븐에서 열처리한 섬유를 표준상태에서 다시 방치한 다음 초하중(0.01g/d)하에서 줄어든 시료의 길이이다.
In the above formula, L0 is the length measured under superload (0.01 g / d) after leaving the fiber for 24 hours in the above standard condition, and L1 is the superload ( Length of sample reduced under 0.01 g / d).

<실시예 1 내지 7><Example 1 to 7>

고유점도가 1.0인 폴리에스테르 칩을, 방사온도는 300도로하고, 폴리머 기어펌프를 이용하여 분당 333g의 토출량으로 hole 구경이 0.4mm이고, 구멍이 192개인 노즐을 통해 용융중합체를 압출시키고, 20~25℃의 급랭공기로 냉각시켜 미연신사를 제조하였다. 이어서, 가열된 공기가 충진된 길이 4m의 튜브 통로로 미연신사를 통과시킨 다음, 계속해서 온도가 90 ℃ 및 130 ℃로 유지되는 고데트 롤러와, 230 ℃로 유지되는 가열 롤러들을 통과시켜 연신 및 열처리를 행하였다. 고데트 롤러의 GR 4의 속도를 3,000m/min로 하여 1,000데니어의 섬도로 권취하였다. Intrinsic viscosity 1.0 The polyester chip, the spinning temperature is 300 degrees, using a polymer gear pump with a discharge amount of 333g per minute to extrude the molten polymer through a nozzle with a hole diameter of 0.4mm and a hole of 192, the quenching air of 20 ~ 25 ℃ Undrawn yarn was prepared by cooling with. Subsequently, the undrawn yarn was passed through a tube passage of 4 m length filled with heated air, followed by drawing through a high-det roller maintained at temperatures of 90 ° C. and 130 ° C., and heating rollers maintained at 230 ° C. Heat treatment was performed. The speed | rate of GR4 of a high-det roller was 3,000 m / min, and it wound up at 1,000 denier fineness.

튜브 통로의 온도와 총 연신배율을 하기 표 1에 기재하였으며, 얻어진 폴리에스테르 섬유에 대하여 측정한 물성값을 표 1에 기재하였다.The temperature and the total draw ratio of the tube passages are shown in Table 1 below, and the physical property values measured for the obtained polyester fibers are shown in Table 1.

<비교예 1 내지 3><Comparative Example 1 to 3>

하기 표 2에 기재된 조건으로 변화시킨 것을 제외하고는, 실시예와 동일하게 실시하였다. 얻어진 폴리에스테르 섬유에 대하여 측정한 물성값을 표 2에 기재하였다.It carried out similarly to the Example except having changed to the conditions of following Table 2. The physical property values measured about the obtained polyester fiber are shown in Table 2.

  실시예 1Example 1 실시예 2Example 2 실시예 3Example 3 실시예 4Example 4 실시예 5Example 5 실시예 6Example 6 실시예 7Example 7 Spin tube
Hot air 온도(℃)
Spin tube
Hot air temperature (℃)
5050 7070 9090 100100 110110 130130 150150
총연신배율Total draw ratio 6.00 6.00 6.10 6.10 6.00 6.00 6.10 6.10 6.206.20 6.006.00 6.10 6.10 강도burglar 10.5110.51 10.3010.30 10.5110.51 10.6810.68 10.5310.53 10.5910.59 10.6210.62 신도Shinto 10.1010.10 9.349.34 10.2910.29 9.309.30 9.489.48 9.129.12 8.818.81 LASE5%LASE5% 5.455.45 5.475.47 5.775.77 6.286.28 5.225.22 6.416.41 6.476.47 열수축율Heat shrinkage 15.215.2 15.815.8 15.315.3 16.116.1 15.315.3 16.416.4 16.316.3 외관Exterior 양호Good 양호Good 양호Good 양호Good 양호Good 양호Good 양호Good

  비교예 1Comparative Example 1 비교예 2Comparative Example 2 비교예 3Comparative Example 3 튜브 통로의 온도Temperature of tube passage 사용안함not used 4040 170170 총연신배율Total draw ratio 5.80 5.80 5.90 5.90 6.00 6.00 강도burglar 9.899.89 9.959.95 10.1010.10 신도Shinto 11.1411.14 11.211.2 11.4211.42 LASE5%LASE5% 4.744.74 4.954.95 5.505.50 열수축율Heat shrinkage 15.615.6 16.316.3 15.715.7 외관Exterior 불량(모우)Poor (Mow) 불량(모우)Poor (Mow) 불량(모우)Poor (Mow)

표의 결과를 참조하면, 실시예의 섬유는 모두 6배 이상의 연신배율로 연신이 가능하였고, 섬유의 파단강도, LASE5% 탄성율 등의 물성이 모두 우수하였다.Referring to the results of the table, the fibers of the examples were all stretched at a draw ratio of 6 times or more, and the physical properties such as breaking strength of the fiber, LASE 5% elastic modulus were all excellent.

한편, 비교예 1의 섬유는 최대 연신배율이 낮아서 고강도와 고탄성을 구현하는 것이 어려웠으며, 제품외관 상태에서 불량결점인 모우(FLUFFY YARN)가 많이 발생함을 관찰할 수 있었다. 비교예 2의 섬유는 튜브 통로의 hot air 온도가 낮아서 균일 배향에 충분한 열전달이 이루어지지 않음을 알 수 있었다. 비교예 3의 섬유는 튜브 통로의 hot air 온도가 너무 높아서 통로를 통과하는 중에 미연신사들이 융착되는 등의 문제가 발생하고, 공정성이 불량하였다On the other hand, the fiber of Comparative Example 1 has a low maximum draw ratio, it was difficult to implement high strength and high elasticity, it can be observed that a lot of defects (FLUFFY YARN) occurs in the product appearance state. It was found that the fiber of Comparative Example 2 did not have sufficient heat transfer for uniform orientation due to the low hot air temperature in the tube passage. The fiber of Comparative Example 3 had a problem such that the undrawn yarn was fused while passing through the passage because the hot air temperature of the tube passage was too high, resulting in poor processability.

Claims (5)

(S1) 고유점도(IV)가 0.8 내지 1.5인 폴리에스테르 수지를 방사구금을 통해 용융방사하고 냉각시켜 미연신사를 제조하는 단계;
(S2) 길이방향으로 연장되며, 50 내지 150 ℃로 유지되는 통로를 갖는 튜브를 준비하고, 상기 미연신사를 튜브의 통로로 통과시켜 가열하는 단계; 및
(S3) 상기 가열된 미연신사를 열처리하며 연신하는 단계를 포함하는 폴리에스테르 섬유의 제조방법.
(S1) melt spinning and cooling a polyester resin having an intrinsic viscosity (IV) of 0.8 to 1.5 through a spinneret and cooling to prepare an unstretched yarn;
(S2) preparing a tube having a passage extending in the longitudinal direction and maintained at 50 to 150 ° C., and heating the undrawn yarn by passing through the passage of the tube; And
(S3) A method for producing a polyester fiber comprising the step of stretching the heated undrawn yarn.
삭제delete 제1항에 있어서,
상기 튜브의 길이는 2 내지 4 m인 것을 특징으로 하는 폴리에스테르 섬유의 제조방법.
The method of claim 1,
Method for producing a polyester fiber, characterized in that the length of the tube is 2 to 4 m.
제1항에 있어서,
상기 미연신사의 총 연신비는 6배 이상인 것을 특징으로 하는 폴리에스테르 섬유의 제조방법.
The method of claim 1,
The total draw ratio of the non-drawn yarn is a method for producing a polyester fiber, characterized in that more than six times.
제1항에 있어서,
상기 폴리에스테르 섬유의 LASE 5% 값이 5.5 g/d 이상이고, 강도가 10.0 g/d 이상이고, 파단신도가 12% 이하인 것을 특징으로 하는 폴리에스테르 섬유의 제조방법.
The method of claim 1,
The LASE 5% value of the polyester fiber is 5.5 g / d or more, the strength is 10.0 g / d or more, the elongation at break is 12% or less.
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KR101427834B1 (en) 2013-01-04 2014-08-08 주식회사 효성 Process for preparing polyester multifilament having excellent strength and chemical resistance for tire cord
CN104195653A (en) * 2014-07-29 2014-12-10 中国石油化工股份有限公司 PBT fiber manufacturing method based on high speed one-step method

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KR101427834B1 (en) 2013-01-04 2014-08-08 주식회사 효성 Process for preparing polyester multifilament having excellent strength and chemical resistance for tire cord
CN104195653A (en) * 2014-07-29 2014-12-10 中国石油化工股份有限公司 PBT fiber manufacturing method based on high speed one-step method

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