KR19980049300A - Manufacturing method of polytrimethylene terephthalate false twisted yarn - Google Patents
Manufacturing method of polytrimethylene terephthalate false twisted yarn Download PDFInfo
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- KR19980049300A KR19980049300A KR1019960067992A KR19960067992A KR19980049300A KR 19980049300 A KR19980049300 A KR 19980049300A KR 1019960067992 A KR1019960067992 A KR 1019960067992A KR 19960067992 A KR19960067992 A KR 19960067992A KR 19980049300 A KR19980049300 A KR 19980049300A
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Abstract
본 발명은 폴리트리메틸렌테레프탈레이트(PTT) 가연사의 제조방법에 관한 것으로서, 1,3-프로판디올이 주쇄중에 85% 이상이며 고유점도가 0.75∼1.1인 폴리트리메틸렌테레프탈레이트를 2,500∼5,500m/min의 방사속도로 방사하여 POY사를 얻고 이를 연신 및 가연하는 것을 포함하며, 이러한 방법을 적용하면 폴리트리메틸렌테레프탈레이트로부터 고 권축성 가연사를 안정적으로 제조할 수 있게 된다.The present invention relates to a method for producing polytrimethylene terephthalate (PTT) false twisted yarn, wherein 1,3-propanediol has a polytrimethylene terephthalate of not less than 85% in the main chain and has an intrinsic viscosity of 0.75 to 1.1 at 2,500 to 5,500 m / It involves spinning at a spinning speed of min to obtain POY yarn, and stretching and combusting it, and by applying this method, it is possible to stably prepare highly crimpable twisted yarn from polytrimethylene terephthalate.
Description
본 발명은 폴리트리메틸렌테레프탈레이트(PTT) 가연사의 제조방법에 관한 것으로서, 보다 구체적으로는 폴리트리메틸렌테레프탈레이트로부터 고 권축성 가연사를 안정적으로 제조하는 방법에 관한 것이다.The present invention relates to a method for producing polytrimethylene terephthalate (PTT) false twisted yarn, and more particularly, to a method for stably producing high crimped false twisted yarn from polytrimethylene terephthalate.
최근 폴리에스터중에 폴리트리메틸렌테레프탈레이트라는 수지가 상업화가 되기 시작하고 있는데, 기존의 폴리에스터에 비해 신축성, 이염성이 우수하여 여러 섬유 용도로 전개가 모색되고 있다. 특히 가연사로 제조할 경우 PTT의 우수한 특성을 더욱 살릴 수 있어 기대할만하다.Recently, a resin called polytrimethylene terephthalate has begun to be commercialized in polyester, and it is being developed for various fiber applications because it has excellent elasticity and dyeing property compared to conventional polyester. In particular, it is expected that the excellent properties of PTT can be further enhanced when manufactured with false twisted yarn.
그러나 실제로 PTT를 가연할 경우 내열성이 부족하여 가연시 가연 온도를 100℃ 이상으로 올리지 못하므로 결과적으로 권축 특성이 나빠져 신축성을 제대로 발휘할 수 없다. 또한 가연 공정성도 좋지 못하여 사절이 자주 발생하며 모우 등의 외관이 불량하여 상업적으로 생산하기엔 많은 문제를 안고 있다.However, when PTT is actually burned, the heat resistance is insufficient, and thus the burnt temperature is not increased to 100 ° C. or more. In addition, because the flammability fairness is not good, the trimming occurs frequently, and the appearance of the cows is poor, so there are many problems for commercial production.
따라서 본 발명은 상기한 문제점이 없는 폴리트리메틸렌테레프탈레이트 가연사의 제조방법을 제공하는 것을 목적으로 한다.Accordingly, an object of the present invention is to provide a method for producing polytrimethylene terephthalate false twisted yarn without the above problems.
본 발명자들은 상기한 목적을 달성하기 위한 연구에서, PTT 섬유는 기존의 폴리에스터에 비해 강도와 내열성이 떨어지므로 이를 보완하기 위해 수지의 고유점도(IV)를 상당히 올리고, POY 원사 제조시 방속을 가능한 한 올리면 강도 및 내열성이 향상되고, 이러한 POY 원사는 100℃ 이상의 온도에서 가연이 안정적으로 이루어지고, 얻어진 가연사는 고 권축성을 나타낸다는 사실을 알게 되었다.In the research to achieve the above object, the inventors considerably increase the intrinsic viscosity (IV) of the resin in order to compensate for this, since PTT fibers are inferior in strength and heat resistance compared to conventional polyesters, and can be discharged when manufacturing POY yarns. It was found that raising the strength and heat resistance improved, such that the POY yarn was stably combusted at a temperature of 100 ° C. or higher, and that the obtained twisted yarn showed high crimpability.
그러므로 본 발명에 의하면 1,3-프로판디올이 주쇄중에 85% 이상이며 고유점도가 0.75∼1.1인 폴리트리메틸렌테레프탈레이트를 2,500∼5,500m/min의 방사속도로 방사하여 POY사를 얻고, 이를 연신 및 가연하는 것을 포함하는 폴리트리메틸렌테레프탈레이트 가연사의 제조방법이 제공된다.Therefore, according to the present invention, 1,3-propanediol is more than 85% in the main chain and spun polytrimethylene terephthalate having an intrinsic viscosity of 0.75 to 1.1 at a spinning speed of 2,500 to 5,500 m / min to obtain POY yarn, and drawing it. And it provides a method for producing a polytrimethylene terephthalate false twisted yarn comprising burning.
이하 본 발명을 보다 상세하게 설명하기로 한다.Hereinafter, the present invention will be described in more detail.
본 제조방법에서 사용되는 폴리트리메틸렌테레프탈레이트는 1,3-프로판디올이 주쇄중에 80% 이상이며 고유점도가 0.75∼1.1인 것이다. 고유점도가 0.75 미만의 경우에는 분자량이 작아 가연 공정이 좋지 않게 되며, 1.1을 초과하는 폴리트리메틸렌테레프탈레이트는 그 제조시간, 특히 중합반응시간이 오래 걸려 원가의 부담이 크므로 바람직스럽지 못하다.Polytrimethylene terephthalate used in the present production method is 1,3-propanediol is 80% or more in the main chain and has an intrinsic viscosity of 0.75 to 1.1. If the intrinsic viscosity is less than 0.75, the molecular weight is small, so the combustion process is not good, and polytrimethylene terephthalate of more than 1.1 is not preferable because the production time, especially the polymerization reaction time is long, the burden of the cost is high.
POY 원사의 제조에서, 방속은 2,500∼5,500m/min로 하는 것이 바람직한데, 이는 상기한 방속범위에서 원사 강도를 2.2g/d 이상으로 할 수 있고, 또한 열응력 최대온도를 45℃ 이상으로 할 수 있어 내열성 향상에 효과적이기 때문이다. 만일 방속이 2,500m/min 미만이면 원사 강도가 부적합하고 내열성이 부족하여 가연시 사절, 모우가 많이 발생하는 단점이 있다. 또한 방속이 5,500m/min을 초과하는 경우에는 원사 강도의 증가가 더 이상 이루어지지 않고 오히려 방사 공정의 불량만을 초래하게 된다.In the production of POY yarns, it is preferable to set the flux to be 2,500 to 5,500 m / min, which can make the yarn strength be 2.2 g / d or more and the maximum thermal stress temperature of 45 DEG C or more in the above discharge range. It is because it is effective in improving heat resistance. If the discharge speed is less than 2,500m / min, the strength of the yarn is inadequate and the heat resistance is insufficient, there is a disadvantage that a lot of trimming, moor occurs when burning. In addition, when the discharge rate exceeds 5,500m / min, the increase in yarn strength is no longer achieved, but rather only the failure of the spinning process.
이렇게 제조된 POY 원사는 가연시 100℃ 이상의 온도에서도 사절이나 모우가 없는 양호한 상태로 가연되며, 얻어진 가연사는 권축률 30% 이상의 우수한 권축성을 갖는다. 가연온도는 가급적 200℃ 이하로 조정하는 것이 바람직한데, 이는 200℃를 초과하는 가연온도에서 가연하게 되면 원사의 용융이 일어날 우려가 있기 때문이다.The POY yarn thus prepared is combusted in a good state without trimming or shaving even at a temperature of 100 ° C. or more during combustion, and the obtained twisted yarn has excellent crimpability of 30% or more of crimping rate. It is preferable to adjust the flammable temperature to 200 degrees C or less as possible, because when it burns at the combustion temperature exceeding 200 degreeC, there exists a possibility that the melting of a yarn may occur.
상술한 바와 같은 본 발명의 특징 및 기타의 장점은 후술되는 실시예로부터 보다 명백하게 될 것이다. 물론 하기 실시예는 본 발명의 이해를 돕기 위해서 예시되는 것일 뿐 제한하기 위한 것은 아니다. 하기 실시예 및 비교예에서 제시되는 물성은 다음과 같은 방법으로 측정된 것이다.Features and other advantages of the present invention as described above will become more apparent from the embodiments described below. Of course, the following examples are only intended to aid understanding of the present invention and are not intended to be limiting. Physical properties shown in the following Examples and Comparative Examples are measured by the following method.
◎ 권축률:가연사 시료를 워프리일(warp reel)로 권취한 후 한 쪽 끝을 스케일(scale) 판에 걸고 초하중(2/1,000g), 중하중(1/10g)을 걸고, 1분 경과후 길이(L0)를 잰다. 중하중을 제거한 후, 이 시료를 끓는 물중에서 20분간 처리한 후 꺼내어 초하중을 제거하고 실온에서 24시간 건조한다. 그 후 이 시료에 초하중, 중하중을 다시 걸고 1분 경과후 길이(L1)를 읽는다. 그 후 즉시 중하중을 제거하여 1분후 길이(L2)를 읽는다. 상기와 같이 측정한 길이들로부터 하기 식에 의거 권축률을 구한다.◎ Crimping rate: After winding the false twisted sample with warp reel, hang one end on the scale plate and apply super load (2 / 1,000g), heavy load (1 / 10g), 1 After the minute, the length (L 0 ) is measured. After removing the heavy load, the sample is treated in boiling water for 20 minutes and then taken out to remove the superload and dried at room temperature for 24 hours. After this, the sample is reloaded with super and heavy loads, and the length (L 1 ) is read after 1 minute. Then immediately remove the heavy load and read the length (L 2 ) after 1 minute. The crimp rate is calculated | required based on the following formula from the length measured as mentioned above.
◎ 고유점도(IV):120℃ 오르토-클로로페놀에 1% 농도로 용해후 30℃ 항온조에서 우벨로드형 점도계를 사용하여 측정.◎ Intrinsic viscosity (IV): Measured using a Ubelrod viscometer in a 30 ° C thermostat after dissolving at 120% ortho-chlorophenol at 1% concentration.
◎ 열응력:가네보사 열응력 시험기를 사용하여 초하중 10g, 승온속도 300/분으로 하여 열응력을 측정.◎ Thermal Stress: The thermal stress is measured by using Kanebo's thermal stress tester at a super load of 10g and a heating rate of 300 / min.
[실시예 1]Example 1
고유점도가 0.76인 PTT 수지를 사용하여 진공 건조기에서 150℃로 6시간 건조한 후 통상의 방사기를 사용하여 방사하였다. 방사온도는 265℃, 방사속도는 3000m/min으로 하여 0.3mm 노즐을 사용하여 115데니어 36필라멘트의 POY 원사를 제조하였다. 이렇게 제조한 POY 원사를 디스크 타입의 가연기를 사용하여 사속 400m/min, 가연온도 150℃에서 가연하였다. 본 실시예의 물성 및 공정변수를 하기 표 1에 정리하여 나타내었다.After drying for 6 hours at 150 ℃ in a vacuum dryer using a PTT resin having an intrinsic viscosity of 0.76 was spun using a conventional spinning machine. The spinning temperature was 265 ° C. and the spinning speed was 3000 m / min. POY yarn of 115 denier 36 filaments was manufactured using a 0.3 mm nozzle. The POY yarn thus prepared was combusted at a yarn speed of 400 m / min and a combustion temperature of 150 ° C. using a disc type combustor. Physical properties and process parameters of this example are summarized in Table 1 below.
[실시예 2]Example 2
고유점도가 1.0인 PTT 수지를 사용하고, 방사온도를 270℃, 가연온도를 160℃로 변경한 것을 제외하고는 실시예 1과 동일한 절차를 반복하였다.The same procedure as in Example 1 was repeated except that PTT resin having an intrinsic viscosity of 1.0 was used and the spinning temperature was changed to 270 ° C and the flammable temperature was changed to 160 ° C.
[실시예 3]Example 3
고유점도가 0.76인 PTT 수지를 사용하고, 방사속도를 5,500m/min, 가연온도를 150℃로 변경한 것을 제외하고는 실시예 1과 동일한 절차를 반복하였다.The same procedure as in Example 1 was repeated except that PTT resin having an intrinsic viscosity of 0.76 was used, and the spinning speed was changed to 5,500 m / min and the combustion temperature was changed to 150 ° C.
[실시예 4]Example 4
고유점도가 1.0인 PTT 수지를 사용하고, 방사속도를 5,500m/min, 가연온도를 150℃로 변경한 것을 제외하고는 실시예 1과 동일한 절차를 반복하였다.The same procedure as in Example 1 was repeated except that PTT resin having an intrinsic viscosity of 1.0 was used, and the spinning speed was changed to 5,500 m / min and the combustion temperature was changed to 150 ° C.
[비교예 1]Comparative Example 1
고유점도 0.65인 PTT 수지를 사용한 것을 제외하고는 실시예 1과 동일한 절차를 반복하였다.The same procedure as in Example 1 was repeated except that PTT resin having an intrinsic viscosity of 0.65 was used.
[비교예 2]Comparative Example 2
고유점도 0.65인 PTT 수지를 사용하고, 가연온도를 120℃로 변경한 것을 제외하고는 실시예 1과 동일한 절차를 반복하였다.The same procedure as in Example 1 was repeated except that PTT resin having an intrinsic viscosity of 0.65 was used and the combustion temperature was changed to 120 ° C.
[비교예 3]Comparative Example 3
고유점도 0.76인 PTT 수지를 사용하고, 방사속도를 2,000m/min로 변경한 것을 제외하고는 실시예 1과 동일한 절차를 반복하였다.The same procedure as in Example 1 was repeated except that PTT resin having an intrinsic viscosity of 0.76 was used and the spinning speed was changed to 2,000 m / min.
[비교예 4][Comparative Example 4]
가연온도를 120℃로 변경한 것을 제외하고는 비교예 3과 동일한 절차를 반복하였다.The same procedure as in Comparative Example 3 was repeated except that the combustion temperature was changed to 120 ° C.
[표 1]TABLE 1
○ … 모우가 거의 또는 전혀 발생하지 않음○…. Little or no moor
× … 모우의 발생정도가 심함×… High incidence of cattle
상기 표 1로부터 알 수 있는 바와 같이, 고유점도가 0.75∼1.1인 폴리트리메틸렌테레프탈레이트를 2,500∼5,500m/min의 방사속도로 방사하는 실시예 1 내지 4의 경우에는 상기한 범위에서 벗어나는 비교예 1 내지 4의 경우에 비하여 가연시 100℃ 이상의 온도에서도 사절이나 모우가 없는 양호한 상태로 가연되며, 얻어진 가연사는 권축률 30% 이상의 우수한 권축성을 갖는다.As can be seen from Table 1, in the case of Examples 1 to 4 spinning the polytrimethylene terephthalate having an intrinsic viscosity of 0.75 to 1.1 at a spinning speed of 2,500 to 5,500 m / min, the comparative example deviated from the above range. Compared to the case of 1 to 4, even at a temperature of 100 ° C. or more at the time of combustion, the product is combusted in a good state without trimming or shaving.
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US6685859B2 (en) | 2000-03-03 | 2004-02-03 | E. I. Du Pont De Nemours And Company | Processes for making poly(trimethylene terephthalate) yarn |
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KR100522791B1 (en) * | 1998-11-28 | 2005-12-21 | 주식회사 휴비스 | Manufacturing method of polytrimethylene terephthalate fine thread |
KR20000037734A (en) * | 1998-12-02 | 2000-07-05 | 조민호 | Process for producing polytrimethyleneterephthalate partially oriented yarn(poy) |
US6685859B2 (en) | 2000-03-03 | 2004-02-03 | E. I. Du Pont De Nemours And Company | Processes for making poly(trimethylene terephthalate) yarn |
US6998079B2 (en) | 2000-03-03 | 2006-02-14 | E. I. Du Pont De Nemours And Company | Process of making partially oriented poly(trimethylene terephthalate) yarn |
KR20010111187A (en) * | 2000-06-08 | 2001-12-17 | 조 정 래 | Manufacture of polytrimethylenetelephtalate fiber |
KR100441422B1 (en) * | 2002-05-20 | 2004-07-23 | 한국섬유개발연구원 | Preparation of torqueless draw textured Poly Trimethylene Terephthalate yarn |
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