KR960011608B1 - Polyester fiber and its preparation - Google Patents

Polyester fiber and its preparation Download PDF

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Publication number
KR960011608B1
KR960011608B1 KR1019940015615A KR19940015615A KR960011608B1 KR 960011608 B1 KR960011608 B1 KR 960011608B1 KR 1019940015615 A KR1019940015615 A KR 1019940015615A KR 19940015615 A KR19940015615 A KR 19940015615A KR 960011608 B1 KR960011608 B1 KR 960011608B1
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South Korea
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temperature
roller
polyester fiber
physical properties
heating
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KR1019940015615A
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Korean (ko)
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KR960001228A (en
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천재성
정기선
최덕용
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주식회사 코오롱
하기주
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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
    • D01F6/62Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • 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
    • D01D5/084Heating filaments, threads or the like, leaving the spinnerettes
    • 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
    • D01D5/088Cooling filaments, threads or the like, leaving the spinnerettes
    • 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
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02Yarns or threads characterised by the material or by the materials from which they are made
    • 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
    • D10B2331/04Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]

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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)
  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

The fiber is prepared by the high-speed spinning of more than 5,000mpm and thus has proper property of raw filament for the materials of clothes. Also the fiber prepared by the spinning of polyester polymer, more than 80mol % of repeating unit of the molecular chain of which comprising polyethylene terephthalate, particularly is made by: (A) performing heat treatment and then cooling using heating hood of 310 to 340 deg. C located in right below the spinneret; (B) passing the resultant through the heating bath of temperature of 140 to 160 deg. C located in below of the spinneret and consecutively imposing 1 to 1.03 times of orientation between the first godet roller of room temperature and the second godet roller of that of 130 to 160 deg. C; (C) winding the fiber 5 to 10 times between the second godet roller of high temperature and seperator roller, followed by winding the resultant fiber at a speed of more than 5,000mpm.

Description

폴리에스터 섬유 및 그 제조방법Polyester fiber and its manufacturing method

제1도는 종래의 제조방법의 일예를 나타낸 제조공정도.1 is a manufacturing process diagram showing an example of a conventional manufacturing method.

제2도는 종래의 제조방법의 또 다른 일예를 나타낸 제조공정도.2 is a manufacturing process diagram showing still another example of the conventional manufacturing method.

제3도는 종래의 제조방법의 일예를 나타낸 제조공정도.3 is a manufacturing process diagram showing an example of a conventional manufacturing method.

* 도면의 주요부분에 대한 부호의 설명* Explanation of symbols for main parts of the drawings

1 : 방사구금 2 : 방출사조1: spinneret 2: discharge thread

3 : 냉각장치 4 : 가열통3: cooling device 4: heating tube

5 : 급유장치 6 : 제1고뎃롤러5: Lubrication device 6: 1st high-pressure roller

7 : 제2고뎃롤러 8 : 인터레이스장치7: second go 뎃 roller 8: interlacing device

9 : 가열이완장치 10 : 세퍼레이터롤러9: heating and relaxation device 10: separator roller

11 : 권취기 12 : 가열후드11: winding machine 12: heating hood

본 발명은 폴리에스테르 섬유 및 그 제조방법에 관한 것으로, 특히 5,000mpm 이상의 고속방사시 의류용으로 적합한 원사물성을 갖는 폴리에스테르 섬유 및 그를 안정하게 제조하기 위한 제조방법에 관한 것이다.The present invention relates to a polyester fiber and a method for producing the same, and more particularly to a polyester fiber having a yarn property suitable for clothing at high speed spinning of 5,000mpm or more, and a manufacturing method for stably manufacturing the same.

일반적으로 폴리에스테르를 원료로 한 의류용 섬유의 제조방법으로는 폴리에스테르 중합체를 용융 방사하고, 일단 무배향, 비정상 구조의 미연신사를 권취한 후 연신공정에서 배향, 결정화 하고, 다시 최종 형태로 하기 위해 각종 가공처리를 하는 방법, 혹은 방사공정에 있어서 3,000∼4,000m/분의 고속으로 권취한 저배향, 저결정성 구조의 반연신사를 얻고 이것을 가공처리하는 방법 등이 이용되고 있다.In general, a method for producing a garment fiber using polyester as a raw material is melt-spun polyester polymer, once the unoriented non-oriented yarn is wound up, the orientation and crystallization in the stretching process, and the final form For this purpose, a method of performing various kinds of processing, or a method of obtaining a semi-oriented yarn having a low orientation and low crystal structure wound at a high speed of 3,000 to 4,000 m / min in a spinning process and processing the same is used.

먼저 미연신사를 제조한 후 일단 권취한 다음 다시 연신하는 방법은 공정이 2단계로 나누어져 생산성이 낮은 문제점이 있었다. 그러므로 방사속도 3,000∼4,000mpm으로 고속권취하는 방법에 제안되기도 하였으나 이는 고속권취에 의한 원사의 물성이 안정화되지 않아 최종 가공상태의 조건변화에 따라 원사의 물성이 영향을 받는 문제가 있었다.First, after the undrawn yarn is manufactured, the method of winding once and then stretching again has a problem in that the productivity is low because the process is divided into two stages. Therefore, although a high speed winding method was proposed in the spinning speed of 3,000 to 4,000mpm, the physical properties of the yarn due to the high speed winding were not stabilized, and thus the properties of the yarn were affected by the change of the condition of the final processing state.

아울러 최근에는 생산성을 올리기 위하여 5,000mpm 이상의 고속방사 공정이 실시되고 있는 바, 고속에 따른 연신성 향상을 위해 제1도와 같은 공정인 일본 공개특허 소 62-162014호가 제안되고 있다.In addition, in recent years, a high-speed spinning process of 5,000mpm or more has been performed to increase productivity, and Japanese Patent Application Laid-Open No. 62-162014, which is the same process as in FIG. 1, is proposed to improve the stretchability at high speed.

상기 일본 공개특허 소 62-162014호는 고속방사에 따른 절사방지와 연신성 향상을 위해 가열처리를 하면서 연신을 실시하고 있는 방법이지만 이와 같이 열처리를 하면서 연신을 할 경우 고속권취에 따른 원사의 물성을 안정화할 시간이 없으므로 물성이 안정화되지 않아 후가공시 물성변화가 심하며, 또한 이들 공법에 의하여 고수축사 제조시 특정의 용도로 밖에 사용할 수 없는 제한이 있었다.The Japanese Laid-Open Patent Publication No. 62-162014 discloses a method of performing stretching while heating to prevent cutting off and improving elongation due to high-speed spinning. However, when extending during heat treatment, the physical properties of the yarn according to high-speed winding are obtained. Since there is no time to stabilize, the physical properties are not stabilized, so there is a serious change in physical properties during post-processing, and there is a limitation that these methods can be used only for specific purposes when manufacturing high shrinkage yarns.

따라서 물성안정화를 위해 제2도와 같이 고속으로 방사된 섬유를 제1고뎃롤러와 제2고뎃롤러 사이에서 이완 열처리하는 방법이 일본 공개특허 평 2-229212호 및 평 5-302210호에 제안되어 있다.Therefore, Japanese Patent Laid-Open Nos. 2-229212 and 5-302210 have proposed a method of relaxing heat treatment between fibers spun at high speed as shown in FIG. 2 to stabilize the physical properties between the first roller and the second roller.

그러나 이들 공법은 롤러와 롤러 사이에 별도의 열처리장치를 해야 하는 설비의 복잡함 및 제1고뎃롤러에서 인취된 원사를 바로 이완시킴으로써 충분한 배향 및 결정 등의 안정화를 부여할 수 없다는 문제점이 있어 후가공 공정조건에 따른 물성의 편차가 심해지는 문제가 있었다.However, these methods have the problems of the complexity of the equipment that requires a separate heat treatment device between the roller and the roller and the loosening of the yarn taken from the first gourd roller can not give sufficient orientation and crystallization stabilization, so that the post-processing conditions There was a problem that the deviation of the physical properties due to.

따라서 본 발명자는 상기 종래 기술의 문제를 해결하고 의류용에 적합한 폴리에스테르 원사를 안정한 공정으로 제조하기 위해 예의 연구한 결과 본 발명에 이르렀다.Therefore, the present inventors have come to the present invention as a result of earnestly researching to solve the problems of the prior art and to manufacture a polyester yarn suitable for clothing in a stable process.

즉, 본 발명은 5,000mpm 이상의 고속방사시 의류용으로 적합한 원사 물성을 갖는 폴리에스테르 섬유 및 그를 안정하게 제조하는 방법을 제공함을 목적으로 한다.That is, an object of the present invention is to provide a polyester fiber having a yarn physical property suitable for clothing during high-speed spinning more than 5,000mpm and a method for stably manufacturing the same.

이하, 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.

본 발명은 분자쇄의 반복단위 80몰% 이상이 폴리에틸렌 테레프탈레이트를 이루어진 폴리에스테르 폴리머를 방사하여 폴리에스테르 섬유를 제조함에 있어서, 구금직하에 위치한 온도 310∼340℃의 가열후드로 열처리하고 냉각한 후, 구금하 1.4∼1.9m에 위치한 온도 140∼160℃인 가열통에 통과시키고 연속하여 상온의 제1고뎃룰러와 130∼160℃인 제2고뎃롤러 사이에서 1∼1.03배의 연신을 부여하고 고온의 제2고뎃롤러와 세퍼레이터롤러 사이에서 5∼10회 권회시킨 후 권취속도 5,000mpm 이상으로 권취하는 폴리에스테르 섬유의 제조방법에 관한 것이다.The present invention is to produce a polyester fiber by spinning a polyester polymer consisting of polyethylene terephthalate of 80 mol% or more repeating units of the molecular chain, after heat treatment and cooling with a heating hood of 310 ~ 340 ℃ temperature After passing through a heating tube with a temperature of 140 ~ 160 ℃ located in 1.4 ~ 1.9m under detention, continuously give 1 ~ 1.03 times the elongation between the first high roller and the second high roller of 130 ~ 160 ℃. The present invention relates to a method for producing a polyester fiber obtained by winding five to ten times between a second gourd roller and a separator roller of a roller at a winding speed of 5,000 mpm or more.

본 발명의 제조공정을 제3도에 의거 더욱 상세히 설명하면 다음과 같다.Referring to the manufacturing process of the present invention in more detail based on Figure 3 as follows.

먼저 분자쇄의 80몰% 이상이 폴리에틸렌 테레프탈레이트로 이루어진 폴리에스테르 폴리머를 방사구금(1)을 통해 압출한다. 이때 방사구금직하에는 고온의 가열후드(12)가 있어 폴리에스테르 폴리머의 유동성을 향상시켜 양호한 연신성 및 물성의 안정화를 꾀하게 된다.First, at least 80 mol% of the molecular chain is extruded through the spinneret (1) of a polyester polymer made of polyethylene terephthalate. At this time, there is a high temperature heating hood 12 directly under the spinneret to improve the fluidity of the polyester polymer, thereby achieving good elongation and stabilization of physical properties.

이러한 가열후드의 온도는 310∼340℃, 좋기로는 320∼330℃가 적당하다. 만일 가열후드의 온도가 310℃ 미만일 경우에는 열처리 효과가 미약하여 유동성 향상 및 그에 따른 연신성 향상의 효과가 미약하며, 340℃가 넘을 경우는 폴리머의 열화로 인한 취화를 일으키는 문제가 발생된다.The temperature of such a heating hood is 310-340 degreeC, Preferably 320-330 degreeC is suitable. If the temperature of the heating hood is less than 310 ℃ the heat treatment effect is weak and the effect of improving the fluidity and thus the elongation is weak, if the temperature exceeds 340 ℃ causing a problem of embrittlement due to degradation of the polymer.

이와 같이 방사된 폴리에스테르 폴리머는 상온의 냉각풍으로 냉각하여 고화된 후 급유장치(5)에 의해 급유와 동시에 집속된다. 이러한 급유장치는 통상의 롤러타입 또는 오일제트타입이 모두 적용 가능하나 고속방사에 따른 급유효율의 향상을 위해서는 오일제트타입이 보다 바람직하다.The polyester polymer thus spun is cooled and solidified by cooling air at room temperature, and then concentrated by the oil supply device 5 at the same time. Such a fuel supply device is applicable to both a conventional roller type or an oil jet type, but in order to improve the oil supply efficiency according to the high-speed spinning, the oil jet type is more preferable.

아울러 방사된 원사는 가열통(4)에 의해 열처리되면서 연신이 일어나기 때문에 사조(2)는 가열통(4) 내부에서 충분히 열처리를 받아야 하므로 사조(2)의 집속을 가열통(4) 상단에서가 아닌 하단에서 해주는 것이 바람직하다.In addition, since the yarn is stretched while being heat treated by the heating tube 4, the yarn 2 should be sufficiently heat treated inside the heater 4 so that the focus of the yarn 2 is increased from the top of the heater 4 It is preferable to do it at the bottom.

또한 필요에 따라서 급유장치(5)는 2단으로 설치해도 좋다. 이처럼 원사는 방사구금(1)과 5,000mpm 이상으로 회전하는 제1고뎃롤러(6) 사이에서 가열통(4)에 의해 열처리를 받으며 연신이 일어나는데 가열통(4)은 양호한 연신성 및 물성의 안정화를 꾀하기 위해 사용한다.In addition, the oil supply apparatus 5 may be provided in two stages as needed. In this way, the yarn is subjected to heat treatment by the heating tube 4 between the spinneret 1 and the first gourd roller 6 rotating at more than 5,000 mpm, and stretching occurs. The heating tube 4 has good elongation and stabilization of physical properties. Use it to try.

즉, 가열통(4)의 가열조건에 의해 분자쇄의 배향, 결정화의 거동이 지배받으므로 가열통(4)의 온도분포는 가열통(4)내를 주행하는 사조(2)의 균일한 연신과 결정화에 매우 중요한 요소로 작용한다.That is, since the orientation of the molecular chain and the crystallization behavior are governed by the heating conditions of the heating tube 4, the temperature distribution of the heating tube 4 is uniformly stretched of the thread 2 traveling in the heating tube 4. It is a very important factor in the crystallization.

본 발명에서는 가열통(4)의 온도는 140∼160℃로 하는 바, 본 발명과 같이 빠른 방사속도에 따른 제조공정에서 가열통의 열처리 온도를 140℃ 미만으로 사용한 경우는 원사에 열처리가 충분히 되지 않음에 따른 사절이 발생하고 결정의 성장이 균일하게 이루어지지 않으므로 물성의 균일화가 이루어지기 어렵다.In the present invention, the temperature of the heating tube 4 is 140 to 160 ° C. When the heat treatment temperature of the heating tube is used below 140 ° C in the manufacturing process according to the fast spinning speed as in the present invention, the heat treatment is not sufficient for the yarn. It is difficult to achieve uniformity of physical properties because trimming occurs due to no growth and crystal growth is not uniform.

또한 열처리 온도를 160℃ 보다 높게 하여 열처리할 경우는 폴리머의 유동성 향상 및 그에 따른 분자쇄의 배향의 향상, 결정의 성장에 따라 저수축 특성을 갖게 되는 문제가 발생되어 일반의 의류용 원사의 용도로는 사용이 어렵고, 특정의 저수축 특성을 요구하는 용도로 밖에 사용할 수 없는 단점이 있다.In addition, when the heat treatment is performed at a heat treatment temperature higher than 160 ° C., the fluidity of the polymer is improved, the orientation of the molecular chain is improved, and a low shrinkage characteristic is caused by the crystal growth. Is difficult to use, and can be used only for the purpose of requiring a specific low shrinkage property.

이러한 가열통은 비접촉식 타입이 원사에 손상을 주지 않아 적당하며 가열통의 길이와 사조(2)가 통과하는 내경의 지름은 길이가 1∼3m, 내경이 10∼50mm이면 원하는 물성을 얻을 수 있으나 길이가 너무 짧으면 불균일한 열처리가 될 수 있고, 너무 길면 장치를 설치, 운전하기가 힘들므로 길이는 1.3∼1.8m 정도가 적당하고, 내경은 20∼40mm 정도가 적당하다.Such a heating tube is suitable because the non-contact type does not damage the yarn, and the length of the heating tube and the diameter of the inner diameter through which thread thread 2 passes is 1 to 3 m in length and 10 to 50 mm in inner diameter to obtain desired properties. If too short, it may be uneven heat treatment. If too long, it is difficult to install and operate the device, so the length is suitable about 1.3 to 1.8 m, and the inner diameter is about 20 to 40 mm.

또한 이러한 가열통 입구의 위치는 구금하 1.4∼1.9m가 적당한 바, 만일 1.4m 보다 가깝게 설치한 경우 또는 1.9m 보다 멀게 설치한 경우에는 가열통과 제1고뎃롤러간의 거리가 멀거나 또는 냉각장치와 가열통간의 거리가 멀어서 불균일한 연신 및 방사장력이 상승되는 문제가 발생한다.In addition, the position of the inlet of the heating tube is appropriately in the range of 1.4-1.9m. If it is installed closer than 1.4m or farther than 1.9m, the distance between the heating tube and the first roller is too long, or The distance between the heating barrels is so long that there is a problem that the uneven stretching and the radial tension is increased.

이처럼 가열통(4)에 의해 열처리되면서 연신된 사조는 상온의 제1고뎃롤러와 130∼160℃인 제2고뎃롤러(7)에서 1∼1.03배 연신한 후 제2고뎃롤러(7)와 세퍼레이터롤러(10) 사이에서 5∼10회 권회시킨다.The yarns drawn while being heat treated by the heating tube 4 are stretched 1 to 1.03 times in the first gourd roller at room temperature and the second gourd roller 7 at 130 to 160 ° C, and then the second gourd roller 7 and the separator. It is wound 5-10 times between the rollers 10.

본 발명에서는 제2고뎃롤러를 고온으로 하여 제조하는데 그 이유는 가열통(4)에서 고속주행하면서 열처리되는 사조는 열처리와 빠른 방사속도에 의해 결정이 발생하여 성장하게 되는데 가열통(4)만으로는 충분히 균일하게 이루어지지 않으므로 제2고뎃롤러(7)에서 2차로 열처리를 실시하여 폴리에스테르 섬유의 내부 구조가 균일하게 성장하도록 처리하기 위함이다.In the present invention, the second gourd roller is manufactured at a high temperature. The reason for this is that yarns that are heat-treated while driving at high speed in the heating tube 4 are grown by crystallization by heat treatment and fast spinning speed, but the heating tube 4 alone is sufficient. Since it is not made uniformly, the second gourd roller 7 is subjected to a second heat treatment to treat the internal structure of the polyester fiber to grow uniformly.

이때 연신배율, 제2고뎃롤러의 온도범위, 제2고뎃롤러와 세퍼레이터롤러의 권회수가 상기 조건을 벗어날 경우는 균일한 열처리가 이루어지지 않아 폴리에스테르 섬유의 내부 구조가 균일하게 성장하지 못해 물성편차가 생기며 본 발명에서 요구하는 물성에 이르지 못하는 문제점이 발생한다.At this time, if the draw ratio, the temperature range of the second high roller and the number of turns of the second high roller and the separator roller are out of the above conditions, there is no uniform heat treatment, so the internal structure of the polyester fiber is not grown uniformly and the property deviation There arises a problem that does not reach the physical properties required by the present invention.

이렇게 제조된 폴리에스테르 섬유는 인터레이스장치(8)에 의해 교락처리된 후 권취기(11)에서 권취된다.The polyester fiber thus produced is entangled by the interlacing device 8 and then wound up in the winder 11.

상기 방법으로 제조된 원사는 다음과 같은 Ⅰ군의 물성을 동시에 만족하거나 Ⅱ군의 물성을 동시에 만족하는 물성을 갖게 된다.Yarn produced by the above method will have the physical properties of satisfying the properties of the group I at the same time or at the same time as the group II.

[Ⅰ군][Group I]

·결정완전성 파라메타(Cn) : 0.44∼0.53Crystal perfection parameter (Cn): 0.44 to 0.53

·융해피크온도 : 252∼258℃Melting peak temperature: 252 ~ 258 ℃

·Tmax(역학적 손실정접(tanδ의 최대온도))=132∼140℃Tmax (mechanical loss tangent (maximum temperature of tanδ)) = 132-140 ° C

(tanδ)max(tanδ의 피크값)=0.12∼0.18(tanδ) max (peak value of tanδ) = 0.12 to 0.18

[Ⅱ군][Group II]

·비정부 복굴절율(△na)=0.13∼0.14Irregular birefringence (Δn a ) = 0.13 to 0.14

·건열수축율(△Sd)=11.5∼14.0%Dry heat shrinkage (ΔSd) = 11.5-14.0%

·결정배향도=84.0∼93.0%Crystal orientation = 84.0-93.0%

·100℃에서의 수축응력=140∼190mg/dShrinkage stress at 100 ° C. = 140 to 190 mg / d

상기 물성은 다음과 같은 방법에 의하여 측정하였다.The physical properties were measured by the following method.

1. 융해피크온도(℃)1. Melting peak temperature (℃)

퍼킨엘머(Perkin-Elmer)사제 DSC-Ⅱ형 시차주사 열량계를 사용, 20℃/분의 가열속도로 승온하여 DSC 곡선의 융점 곡선의 피크온도를 구하여 융점 피크온도로 한다.Using a DSC-II differential scanning calorimeter manufactured by Perkin-Elmer, the temperature was raised at a heating rate of 20 ° C./min, and the peak temperature of the melting point curve of the DSC curve was determined to be the melting point peak temperature.

2. (tanδ)max(역학적 손실정접(tanδ)의 피크값) 및 최대온도 Tmax2. (tanδ) max (peak value of mechanical loss tangent (tanδ)) and maximum temperature Tmax

역학적 손실정접은 일본 동약 반드윈사제(Toyo Baldwin), 레오-바이브론(Rheo-Vibron) DDV-Ⅱc형 동적점 탄성측정장치를 사용하여 측정주파수 110Hz, 승온온도 10℃/분으로 건조한 공기중에서 측정한다. tanδ-온도곡선에서 tanδ의 피크온도(Tmax)(℃)와 피크값(tanδ)max가 구해진다.Mechanical loss tangent is measured in dry air at a measuring frequency of 110Hz and an elevated temperature of 10 ° C / min using the Toyo Baldwin, Rheo-Vibron DDV-IIc dynamic viscometer. do. In the tanδ-temperature curve, the peak temperature Tmax (° C.) and the peak value tanδ max of tanδ are obtained.

3. 비정부 복굴절율(△na)3. Non-governmental birefringence (△ na)

이학전기사(理學電氣社)제 광각 X선 회절장치를 이용, 2θ26°의 피크와 같은 방위각방향의 회절곡도곡선에서 통상의 방법에 따라 결정배항 함수 fc를 구한다.2θ using a wide-angle X-ray diffractometer manufactured by Science and Engineering From the diffraction curve in the azimuth direction such as the peak at 26 °, the crystal doubling function f c is obtained according to a conventional method.

비정부 복굴절율 △na는 다음 식으로 구한다.The non-governmental birefringence Δn a is obtained from the following equation.

단, △n은 간섭현미경에서 구한 평균복굴절율Where Δn is the average birefringence obtained from the interference microscope

X는 밀도법에 따라 다음 식에서 구한 결정화도X is the crystallinity obtained from the following equation according to the density method

PET의 경우 비정밀도 Pa=1.334(g/cm2)Non-Precise Pa = 1.334 (g / cm 2 ) for PET

결정밀도 Pc=1.445(g/cm2)Crystal density Pc = 1.445 (g / cm 2 )

△nc는 결정부 복굴절율Δn c is the crystal birefringence

△ncm은 PET의 극한복굴절율 0.212임.Δn cm is 0.212 of the extreme birefringence of PET.

4. 건열수축율(%)(△Sd)4. Dry Heat Shrinkage (%) (△ Sd)

둘레길이 1m의 실감는 기계에 10회 감고 0.18g/d의 하중을 걸면서 원래의 길이(l0)를 측정한 후 200℃의 가열기중에서 5분간 처리한다. 이렇게 처리후 0.1g/d의 하중하에서 시료길이(l1)를 측정하여 아래 식에 의하여 산출한다.The 1m circumference is wound on the machine 10 times and the original length (l 0 ) is measured while applying a load of 0.18g / d and processed in a 200 ℃ heater for 5 minutes. After the treatment, the sample length (l 1 ) was measured under the load of 0.1g / d and calculated by the following equation.

5. 결정완전성 파라메타(Cn)5. Crystal Integrity Parameters (Cn)

X선 회절장치를 이용하여 시료두께를 약 0.5mm로 하여, 30kV, 80mA, 스케닝 속도 1°/분, 챠트속도 10mm/분의 조건에서 회절각 2θ7°에서 35°까지의 회절강도곡선을 얻었다.Using an X-ray diffractometer, a sample thickness of about 0.5 mm was used to obtain a diffraction intensity curve from diffraction angles 2θ7 ° to 35 ° under conditions of 30 kV, 80 mA, scanning speed of 1 ° / minute, and chart speed of 10 mm / minute.

2θ=17∼26°의 범위에서 나타낸 3개의 주요반사를 저각도측으로부터 (100), (010),으로 한다. 2θ=7°와 35°사이에 있는 회절강도곡선을 직선으로 이어 기선으로 한다.The three main reflections shown in the range of 2θ = 17 to 26 ° are obtained from (100), (010), It is done. The diffraction intensity curve between 2θ = 7 ° and 35 ° is a straight line followed by a baseline.

각 피크에서 기선에 수직선을 그어 그 수직선을 회절강도로 한다.At each peak, draw a perpendicular line to the baseline and use that as the diffraction intensity.

(010)면과면 사이에 어깨와 만나는 점에서의 회절강도를 I0으로 하고,면의 피크의 회절강도를 I라고 하면 결정완전성 파라메타 Cn은 다음 식으로 나타낼 수 있다.(010) cotton The diffraction intensity at the point where the shoulder meets between the faces is I 0 , If the diffraction intensity of the surface peak is I, the crystal perfection parameter Cn can be expressed by the following equation.

본 발명의 방법에 의해 제조된 폴리에스테르 섬유는 상기의 Ⅰ군 또는 Ⅱ군 물성을 모두 만족하므로서 일반 연신사와 동일, 유사한 물성을 갖게 되어 일반 연신사보다 높은 생산성(고속방사)으로 폴리에스테르 섬유를 제조할 수 있음과 동시에 제조된 원사의 물성이 정규 연신사와 거의 같고 물성이 안정화되어 매우 우수한 품질의 원사를 얻을 수 있는 장점이 있다.The polyester fiber produced by the method of the present invention satisfies all of the above-described group I or group II properties and has the same physical properties as those of general drawn yarns to produce polyester fibers with higher productivity (higher-speed spinning) than general drawn yarns. At the same time, the physical properties of the yarns produced are almost the same as those of regular stretched yarns, and the physical properties are stabilized.

이하, 본 발명을 실시예에 의거 설명하겠는 바, 본 발명이 실시예로 한정되는 것은 아니다.Hereinafter, the present invention will be described based on Examples, but the present invention is not limited to Examples.

[실시예 1]Example 1

고유점도 0.65인 폴리에틸렌 테레프탈레이트를 주성분으로 하는 폴리에스테르 폴리머를 방사블럭 온도 294℃인 36홀의 구금을 사용, 토출량 43.51g/분으로 하여 5,350mpm으로 방사하였다. 이때 구금직하는 온도 330℃인 가열후드를 설치하였다.A polyester polymer containing polyethylene terephthalate having an intrinsic viscosity of 0.65 as its main component was spun at 5,350 mpm with a discharge rate of 43.51 g / min using a 36-hole detention cap having a spinning block temperature of 294 ° C. At this time, a heating hood having a temperature of 330 ° C. was installed.

이렇게 토출된 폴리에틸렌 테레프탈레이트 폴리머를 온도 19℃, 풍속 0.45m/초의 공기로 냉각한 후 구금하 1.7m에 있는 길이 1.6m, 내경 30mm의 150℃인 가열통에 통과시키고 급유한 후 5,350mpm으로 회전하는 제1고뎃롤러 및 5,400mpm으로 회전하는 140℃의 제2고뎃롤러와 세퍼레이터롤러 7.5회 권회시키면서 통과시킨 후 교락처리하여 5,250mpm의 속도로 권취하여 75D/36F의 원사를 제조하였다.The polyethylene terephthalate polymer thus discharged is cooled with air at a temperature of 19 ° C and a wind speed of 0.45m / sec, passed through a heating tube of 1.6m in length of 1.7m and 150 ° C of internal diameter 30mm, and lubricated, and then rotated at 5,350mpm. The first gourd roller and the second gourd roller at 140 ° C. rotating at 5,400mpm and the separator roller were wound while passing 7.5 times, followed by entanglement treatment and winding at a speed of 5,250mpm to produce 75D / 36F yarn.

이렇게 하여 제조된 원사의 물성을 측정하여 [표 2]에 나타내었다.The physical properties of the yarn thus prepared were measured and shown in [Table 2].

[실시예 2∼7, 비교예 1∼5]EXAMPLES 2-7, COMPARATIVE EXAMPLES 1-5

실시예 1과 동일한 방법으로 행하되 가열후드온도(℃), 가열통온도(℃), 구금에서 가열통간의 거리(m), 제1고뎃롤러 및 제2고뎃롤러의 속도(mpm), 제2고뎃롤러의 온도(℃)를 [표 1]과 같이 변경하여 제조하여 그 물성을 측정, [표 2], [표 3], [표 4]에 나타내었다.Perform the same method as in Example 1 except that the heating hood temperature (° C.), heating barrel temperature (° C.), the distance between the heating cylinders in the detention (m), the speed of the first high roller and the second high roller (mpm), and the second high beam The temperature (° C.) of the roller was changed and manufactured as shown in [Table 1], and the physical properties thereof were measured and shown in [Table 2], [Table 3], and [Table 4].

* A : 결정완전성 파라메타(Cn) B : 융해피크온도(℃)* A: Crystal perfection parameter (Cn) B: Melt peak temperature (℃)

C : Tmax(℃) D : (tanδ)maxC: Tmax (° C.) D: (tanδ) max

E : 비정부 복굴절율(△n) F : 검열수축율(%)E: Non-governmental birefringence rate (△ n) F: Censorship shrinkage rate (%)

G : 결정배향도(%) H : 100℃에서의 수축응력(mg/d)G: Crystal orientation (%) H: Shrinkage stress at 100 ° C (mg / d)

Claims (4)

분자쇄 반복단위의 80몰% 이상의 폴리에틸렌 테레프탈레이트로 이루어진 폴리에스터 폴리머를 방사하여 폴리에스터 섬유를 제조함에 있어서, 구금직하에 위치한 온도 310∼340℃의 가열후드로 열처리하고 냉각한 후, 구금하 1.4∼1.9m에 위치한 온도 140∼160℃인 가열통에 통과시키고 연속하여 상온의 제1고뎃롤러와 130∼160℃인 제2고뎃롤러 사이에서 1∼1.03배 연신을 부여하고, 제2고뎃롤러와 세퍼레이터롤러에 5∼10회 권회시킨 후 권취함을 특징으로 하는 폴리에스터 섬유의 제조방법.In producing polyester fiber by spinning polyester polymer composed of polyethylene terephthalate of 80 mol% or more of the molecular chain repeating unit, it is heat-treated and cooled with a heating hood having a temperature of 310 to 340 ° C. located directly under detention, and then detained in 1.4. Passed through a heating tube at a temperature of 140 to 160 ° C. located at ˜1.9 m, successively giving 1 to 1.03 times the stretching between the first high speed roller at room temperature and the second high speed roller at 130 to 160 ° C., A method for producing a polyester fiber, wherein the separator is wound up 5 to 10 times after winding. 제1항에 있어서, 상기 가열통의 길이가 1.3∼1.8m, 내경이 20∼40mm임을 특징으로 하는 폴리에스터 섬유의 제조방법.The method of producing a polyester fiber according to claim 1, wherein the heating tube has a length of 1.3 to 1.8 m and an inner diameter of 20 to 40 mm. 다음의 물성을 만족함을 특징으로 하는 제1항의 제조방법에 의해 제조된 폴리에스터 섬유.Polyester fiber produced by the manufacturing method of claim 1, characterized by satisfying the following physical properties. 다음의 물성을 만족함을 특징으로 하는 제1항의 제조방법에 의해 제조된 폴리에스터 섬유.Polyester fiber produced by the manufacturing method of claim 1, characterized by satisfying the following physical properties.
KR1019940015615A 1994-06-30 1994-06-30 Polyester fiber and its preparation KR960011608B1 (en)

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