KR20010057095A - Preparation of polytrimethyleneterephthalate fiber - Google Patents

Preparation of polytrimethyleneterephthalate fiber Download PDF

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KR20010057095A
KR20010057095A KR1019990058864A KR19990058864A KR20010057095A KR 20010057095 A KR20010057095 A KR 20010057095A KR 1019990058864 A KR1019990058864 A KR 1019990058864A KR 19990058864 A KR19990058864 A KR 19990058864A KR 20010057095 A KR20010057095 A KR 20010057095A
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spinning
polytrimethylene terephthalate
weight
intrinsic viscosity
fiber
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KR1019990058864A
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Korean (ko)
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KR100587120B1 (en
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김정철
박호진
손성균
김도균
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조민호
주식회사 휴비스
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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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • 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
    • D01D5/08—Melt 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
    • 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
    • D01F1/04—Pigments
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
    • D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch

Abstract

PURPOSE: A process for preparing polytrimethylene terephthalate staple fibers having improved operation stability by preventing the shrinkage of raw yarn during spinning is provided. Whereby, staple fibers having desired physical properties can be obtained. CONSTITUTION: The polytrimethylene terephthalate staple fibers are prepared by blending 70 to 95% by weight of polytrimethylene terephthalate having an intrinsic viscosity of 0.80 to 1.0 with 30 to 5% by weight of polyethylene terephthalate having an intrinsic viscosity of 0.60 to 0.65 and spinning under condition of a spinning temperature of 280 to 290deg.C, a retention time in a spinning machine of 10 to 20 min and a speed of 600 to 1,500m/min.

Description

폴리트리메틸렌테레프탈레이트 섬유의 제조방법{Preparation of polytrimethyleneterephthalate fiber}Manufacturing method of polytrimethylene terephthalate fiber {Preparation of polytrimethyleneterephthalate fiber}

본 발명은 폴리트리메틸렌테레프탈레이트 섬유의 제조방법에 관한 것으로서, 보다 구체적으로는 방사시 원사수축현상으로 방지하여 개선된 조업안정성으로 스테이플용 폴리트리메틸렌테레프탈레이트 섬유를 제조하는 방법에 관한 것이다.The present invention relates to a method for producing polytrimethylene terephthalate fiber, and more particularly, to a method for producing polytrimethylene terephthalate fiber for staples with improved operational stability by preventing yarn shrinkage during spinning.

폴리트리메틸렌테레프탈레이트(PTT)는 테레프탈산 또는 테레프탈산 디메틸로 대표되는 테레프탈산의 저급 알코올 에스테르와 트리메틸렌 글리콜(1,3-프로판디올)을 반응시켜 합성할 수 있는 고분자 물질로서, 최근에야 비로서 상업적인 생산이 가능하게 된 물질이다.Polytrimethylene terephthalate (PTT) is a polymeric material that can be synthesized by reacting a lower alcohol ester of terephthalic acid represented by terephthalic acid or dimethyl terephthalic acid with trimethylene glycol (1,3-propanediol). This is the substance that made it possible.

본 발명자는 PTT의 고유 물성이 스테이플 섬유에서 요구하는 물성을 만족하는 것임에 착안하여 스테이플용 PTT 섬유를 제조하기 위하여 방사한 결과 원사의 수축이 심하게 발생하여 (보통 20 내지 40%의 수축률이 발생), 연신성이 불량하고 섬도를 낮추는 것이 곤란한 등의 문제점이 있는 것을 알게 되었다.The inventors noticed that the intrinsic physical properties of PTT satisfy the physical properties required for staple fibers, and as a result of spinning to produce PTT fibers for staples, yarn shrinkage occurs severely (usually 20 to 40% shrinkage occurs). It has been found that there are problems such as poor elongation and difficulty in lowering the fineness.

따라서 본 발명은 상기한 문제점이 없이 스테이플용 PTT 섬유를 제조하는 방법을 제공하는 것을 기술적 과제로 한다.Therefore, the present invention is to provide a method for producing a staple PTT fiber without the above problems as a technical problem.

상기한 과제를 해결하기 위하여 본 발명자는 다양한 실험을 거듭한 결과 PTT를 폴리에틸렌테레프탈레이트와 블랜드하여 특별히 제어된 방사조건에서 방사하면 안정된 조업성으로 스테이플 섬유로 적합한 PTT 섬유를 제조할 수 있게 된다는 사실을 알게 되어 본 발명을 완성하게 된 것이다.In order to solve the above problems, the present inventors have repeatedly conducted various experiments, and blended PTT with polyethylene terephthalate to produce PTT fibers suitable as staple fibers with stable operability when spun under specially controlled spinning conditions. The present invention is completed.

그러므로 본 발명에 의하면 고유점도 0.80∼1.0의 폴리트리메틸렌테레프탈레이트(PTT) 70∼95중량%를 고유점도 0.60∼0.65의 폴리에틸렌테레프탈레이트(PET) 30∼5중량%와 블랜드하여 방사온도 280∼290℃, 방사기내 체류시간 10∼20분 및 방사속도 600∼1,500m/분(mpm)의 조건으로 방사하는 것을 포함하는 스테이플용 폴리트리메틸렌테레프탈레이트 섬유의 제조방법이 제공된다.Therefore, according to the present invention, 70 to 95% by weight of polytrimethylene terephthalate (PTT) having an intrinsic viscosity of 0.80 to 1.0 is blended with 30 to 5% by weight of polyethylene terephthalate (PET) having an intrinsic viscosity of 0.60 to 0.65, and thus the spinning temperature is 280 to 290. Provided is a method for producing a polytrimethylene terephthalate fiber for staples, comprising spinning on conditions of 10 ° C., spin time 10-20 minutes and spinning speed 600-1,500 m / min (mpm).

이하, 본 발명을 보다 상세하게 설명하기로 한다.Hereinafter, the present invention will be described in more detail.

본 발명은 안정된 조업성으로 스테이플용 PTT 섬유를 제조하기 위하여, 고유점도 0.80∼1.0의 폴리트리메틸렌테레프탈레이트 70∼95중량%를 고유점도 0.60∼0.65의 폴리에틸렌테레프탈레이트 30∼5중량%와 블랜드하여 사용한다. 만일 블랜드중 폴리에틸렌테레프탈레이트의 비율이 5중량% 보다 적은 양으로 함유되는 경우에는 방사시 원사수축현상 방지효과가 미흡하여 안정된 조업성으로 섬유를 제조하는 것이 곤란하게 되고, 30중량%를 초과하는 경우에는 스테이플섬유로서 유용한 폴리트리메틸렌테레프탈레이트의 고유특성이 상실되므로 부적합하게 된다. 그러나 본 발명에 따라 압출방사되는 블랜드중 폴리에틸렌테레프탈레이트의 비율이 5∼30중량%이면 스테이플 용도로 적합한 폴리트리메틸렌테레프탈레이트의 우수한 특성을 유지하면서도 방사시 원사수축률을 10% 이하로 유지할 수 있어 양호한 연신성 및 적정수준의 섬도로 스테이플용 PTT 섬유를 용이하게 제조할 수 있게 된다.The present invention blends 70 to 95% by weight of polytrimethylene terephthalate having an intrinsic viscosity of 0.80 to 1.0 with 30 to 5% by weight of polyethylene terephthalate having an intrinsic viscosity of 0.60 to 0.65 in order to produce PTT fibers for staple with stable operability. use. If the ratio of polyethylene terephthalate in the blend is less than 5% by weight, the effect of preventing the shrinkage of yarn during spinning is insufficient, making it difficult to manufacture the fiber with stable operability, and exceeding 30% by weight. Is not suitable because the intrinsic properties of polytrimethylene terephthalate useful as staple fibers are lost. However, if the ratio of polyethylene terephthalate in the blend that is extruded and spun according to the present invention is 5 to 30% by weight, it is possible to maintain the yarn shrinkage during spinning while maintaining the excellent properties of polytrimethylene terephthalate suitable for staple use. It is possible to easily prepare a PTT fiber for staples with stretchability and an appropriate level of fineness.

또한 사용되는 폴리트리메틸렌테레프탈레이트의 고유점도는 0.80∼1.0이고 폴리에틸렌테레프탈레이트의 고유점도는 0.60∼0.65이어야 한다. 만일 각각의 고유점도가 상기한 범위를 벗어나면 동일온도에서 점도의 차이가 커져서 방사성이 불량하게 되므로 원하는 물성의 섬유를 제조하는 것이 곤란하게 된다.In addition, the intrinsic viscosity of the polytrimethylene terephthalate used should be 0.80 to 1.0 and the intrinsic viscosity of the polyethylene terephthalate should be 0.60 to 0.65. If each intrinsic viscosity is out of the above range, the difference in viscosity becomes large at the same temperature, so that the spinning is poor, it is difficult to manufacture the fiber of the desired physical properties.

본 발명에 이용한 폴리트리메틸렌 테레프탈레이트나 폴리트리메틸렌테레프탈레이트에는 필요에 따라 본 발명의 효과를 손상시키지 않는 범위에서 산 성분으로서 이소프탈산，호박산，아디핀산，2,6-나프탈렌디카르본산등이나 ，글리콜 성분으로서 에틸렌 글리콜，1,4-부탄디올，1,6－헥산디올，폴리옥시 알킬렌 글리콜등의 글리콜 성분이 공중합되고 있어도 좋다．또，필요에 따라 각종의 첨가제，예를 들면 무광택제，열 안정제，난연제，대전 방지제，소포제 등을 함유해도 좋다．Polytrimethylene terephthalate and polytrimethylene terephthalate used in the present invention may be used as isophthalic acid, succinic acid, adipic acid, 2,6-naphthalenedicarboxylic acid or the like as an acid component within the range that does not impair the effects of the present invention if necessary. As the glycol component, glycol components such as ethylene glycol, 1,4-butanediol, 1,6-hexanediol, and polyoxyalkylene glycol may be copolymerized. Various additives, for example, matting agents, may be used as necessary. It may contain a heat stabilizer, a flame retardant, an antistatic agent, an antifoaming agent and the like.

폴리트리메틸렌테레프탈레이트와 폴리에틸렌테레프탈레이트의 블랜드는 예를 들어 로타리 건조기를 사용하여 준비하거나, 또는 별도의 칩 호퍼로부터 계량하여(예를 들어 로타리 밸브를 사용하여) 준비하거나, 또는 도우징 머신(dozing machine)을 사용하여 폴리에틸렌테레프탈레이트를 사이드 피딩하는 것으로 준비할수 있다.Blends of polytrimethylene terephthalate and polyethylene terephthalate may be prepared, for example, using a rotary dryer, or metered from a separate chip hopper (for example using a rotary valve), or a dozing machine. This can be done by side feeding the polyethylene terephthalate using a machine.

본 발명에서는 이러한 블랜드를 방사온도 280∼290℃의 통상적인 PET 조건으로 방사하되, 방사기내 체류시간 10∼20분 및 방사속도 600∼1,500m/분(mpm)의 조건하게 수행하는 것을 또한 특징으로 한다.In the present invention, the blend is spun under normal PET conditions with a spinning temperature of 280 to 290 ° C., but is also carried out under conditions of 10 to 20 minutes in spinning time and 600 to 1500 m / min (mpm) of spinning speed. do.

방사기내 체류시간이 10분 미만이면 블랜드 효과가 미흡하게 되고, 20분을 초과하는 경우에는 열분해가 발생되어 제조되는 섬유의 물성을 손상시키게 되므로 상기한 범위로 유지시키는 것이 필요하다. 또한 방사속도가 상기한 범위를 벗어나면 조업성이 불량하게 된다.If the residence time in the spinning machine is less than 10 minutes, the blend effect is insufficient, and if it exceeds 20 minutes it is necessary to maintain the above range because pyrolysis occurs to damage the physical properties of the fiber produced. In addition, when the spinning speed is out of the above range, the operability is poor.

이와 같은 본 발명에 의하면 스테이플용으로 바람직한 PTT의 고유물성에 손상을 주지 않으면서 안정된 조업성으로 스테이플용 PTT 섬유를 제조하는 것이 가능하게 된다.According to the present invention, it is possible to produce staple PTT fibers with stable operability without damaging the intrinsic physical properties of PTT which is preferable for staples.

상술한 바와 같은 본 발명의 특징 및 기타의 장점은 후술되는 실시예로부터 보다 명백하게 될 것이다. 단, 본 발명은 하기 실시예로 한정되는 것은 아니다.Features and other advantages of the present invention as described above will become more apparent from the embodiments described below. However, the present invention is not limited to the following examples.

하기 실시예에서 제시되는 수축률은 방사한 원사를 즉시 샘플링하여 랩리일(wrap reel)에 3,000데니어가 되도록 감아 타래를 만들고 한쪽 끝을 고정시키고 상온에서 24시간 방치후 길이변화를 측정하여 하기 수학식 1로 계산하여 구한 값이다.Shrinkage is presented in the following examples are immediately sampled spinning yarn (wrap reel) to wrap to 3,000 deniers to make a skein, fixed one end and left for 24 hours at room temperature to measure the length change It is calculated by.

[실시예 및 비교예][Examples and Comparative Examples]

통상의 폴리에스테르 미연신사(UDY) 제조용 방사기에서 폴리에틸렌테레프탈레이트(PET)칩과 폴리트리메틸렌테레프탈레이트(PTT)칩을 진공식 회전 건조기에 투입하고 150℃에서 10시간동안 건조하면서 블랜딩하였다. 이때 상기 폴리에틸렌테레프탈레이트칩과 폴리트리메틸렌테레프탈레이트칩의 고유점도 및 블랜드 비은 하기 표 1과 같이 하였다.Polyethylene terephthalate (PET) chip and polytrimethylene terephthalate (PTT) chip in a conventional spinning machine for undrawn yarn (UDY) was introduced into a vacuum rotary dryer and blended while drying at 150 ° C. for 10 hours. In this case, the intrinsic viscosity and blend ratio of the polyethylene terephthalate chip and the polytrimethylene terephthalate chip were as shown in Table 1 below.

이와 같이 건조된 블랜딩칩을 직경이 0.27㎜이고, 길이가 0.5㎜인 36홀의 방사노즐을 통하여 방사온도 285℃에서 표 1과 같은 방사속도로 방사하여 300데니어/36필라멘트의 미연신사를 제조한후, 수축율을 측정하여 표 2에 나타내었다.The unblended yarn of 300 denier / 36 filament was manufactured by spinning the blended chip thus dried at a spinning speed as shown in Table 1 at a spinning temperature of 285 ° C. through a 36-hole spinning nozzle having a diameter of 0.27 mm and a length of 0.5 mm. , The shrinkage was measured and shown in Table 2.

방사기내 체류시간은 검정색의 원착칩을 방사중에 소량 투입하여 측정하였으며 그 결과는 표 1와 같다.The residence time in the spinning machine was measured by inserting a small amount of black chips into the spinning. The results are shown in Table 1.

제조된 미연신사를 24시간동안 상온에서 방치후 통상의 연신기를 사용하여 연신속도 300mpm, 연신비 4.0으로 연신하여 신도 35%의 폴리에스테르사를 제조하였다. 이때 핫롤러(hot roller)의 온도는 80℃이고, 비접촉식 핫플레이트(hot plate)의 온도는 180℃로 하였다.The prepared undrawn yarn was left at room temperature for 24 hours, and then stretched using a conventional drawing machine at a drawing speed of 300 mpm and a drawing ratio of 4.0 to prepare a polyester yarn having a elongation of 35%. At this time, the temperature of the hot roller (hot roller) is 80 ℃, the temperature of the non-contact hot plate (hot plate) was set to 180 ℃.

제조된 폴리에스테르사의 영율, 방사공정성 및 연신공정성을 측정 및 평가하여 표 2에 나타내었다.Table 2 shows the Young's modulus, spinning processability and stretching processability of the prepared polyester yarn.

구분division PET고유점도PET specific viscosity PTT고유점도PTT intrinsic viscosity PET 블랜드비(중량%)PET blend ratio (% by weight) PTT 블랜드비(중량%)PTT blend ratio (% by weight) 방사기내체류시간(분)Length of stay in the radiator (minutes) 방사속도(mpm)Spinning speed (mpm) 실시예 1Example 1 0.630.63 0.920.92 1010 9090 1010 600600 실시예 2Example 2 0.630.63 0.920.92 1010 9090 1010 1,0001,000 실시예 3Example 3 0.630.63 0.920.92 1010 9090 1010 1,5001,500 실시예 4Example 4 0.630.63 0.920.92 2020 8080 1010 1,0001,000 실시예 5Example 5 0.630.63 0.920.92 3030 7070 1010 1,0001,000 실시예 6Example 6 0.630.63 0.920.92 2020 8080 2020 1,0001,000 실시예 7Example 7 0.630.63 0.820.82 2020 8080 2020 1,0001,000 비교예 1Comparative Example 1 0.630.63 0.920.92 100100 00 1010 600600 비교예 2Comparative Example 2 0.630.63 0.920.92 100100 00 1010 1,0001,000 비교예 3Comparative Example 3 0.630.63 0.920.92 4040 6060 1010 1,0001,000 비교예 4Comparative Example 4 0.630.63 0.920.92 2020 8080 55 1,0001,000 비교예 5Comparative Example 5 0.630.63 0.920.92 2020 8080 2525 1,0001,000 비교예 6Comparative Example 6 0.630.63 0.720.72 2020 8080 1010 1,0001,000 비교예 7Comparative Example 7 0.630.63 1.141.14 2020 8080 1010 1,0001,000

구분division 미연신사수축율(%)Unstretched Shrinkage (%) 방사공정성Radiation fairness 연신공정성Stretch process 영율(㎏/㎟)Young's modulus (㎏ / ㎠) 비고Remarks 실시예 1Example 1 1One 양호Good 양호Good 620620 -- 실시예 2Example 2 22 양호Good 양호Good 570570 -- 실시예 3Example 3 44 양호Good 양호Good 510510 -- 실시예 4Example 4 33 양호Good 양호Good 550550 -- 실시예 5Example 5 66 양호Good 양호Good 530530 -- 실시예 6Example 6 33 양호Good 양호Good 520520 -- 실시예 7Example 7 33 양호Good 양호Good 570570 -- 비교예 1Comparative Example 1 3737 양호Good 불량Bad 420420 -- 비교예 2Comparative Example 2 4545 양호Good 불량Bad 450450 -- 비교예 3Comparative Example 3 2828 양호Good 불량Bad 450450 물성불량Physical defects 비교예 4Comparative Example 4 66 보통usually 보통usually 560560 -- 비교예 5Comparative Example 5 44 불량Bad 불량Bad 550550 -- 비교예 6Comparative Example 6 44 불량Bad 불량Bad 550550 -- 비교예 7Comparative Example 7 44 불량Bad 불량Bad 570570 --

상기한 실시예 및 비교예의 결과로부터 명백하게 되는 바와 같이, 본 발명에 의하면 방사시 원사 수축현상을 방지되어 안정된 조업성으로 스테이플용도로 우수한 폴리트레메틸렌테레프탈레이트 섬유를 제조하는 것이 가능하게 된다.As will be apparent from the results of the above-described examples and comparative examples, the present invention prevents yarn shrinkage during spinning so that it is possible to produce polytremethylene terephthalate fibers excellent in staple use with stable operability.

Claims (1)

폴리에스테르 섬유의 제조에 있어서, 고유점도 0.80∼1.0의 폴리트리메틸렌테레프탈레이트 70∼95중량%를 고유점도 0.60∼0.65의 폴리에틸렌테레프탈레이트 30∼5중량%와 블랜드하여 방사온도 280∼290℃, 방사기내 체류시간 10∼20분 및 방사속도 600∼1,500m/분(mpm)의 조건으로 방사하는 것을 포함하는 스테이플용 폴리트리메틸렌테레프탈레이트 섬유의 제조방법.In the production of polyester fibers, 70 to 95% by weight of polytrimethylene terephthalate having an intrinsic viscosity of 0.80 to 1.0 is blended with 30 to 5% by weight of polyethylene terephthalate having an intrinsic viscosity of 0.60 to 0.65 and a spinning temperature of 280 to 290 ° C. A method for producing a polytrimethylene terephthalate fiber for staples, which comprises spinning under conditions of a residence time of 10 to 20 minutes and a spinning speed of 600 to 1500 m / min (mpm).
KR1019990058864A 1999-12-18 1999-12-18 Preparation of polytrimethyleneterephthalate fiber KR100587120B1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100622204B1 (en) * 2000-01-10 2006-09-07 주식회사 휴비스 Polytrimethyleneterephthalate fiber and preparation thereof
US9809907B2 (en) 2007-01-02 2017-11-07 Mohawk Carpet, Llc Carpet fiber polymeric blend

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US5972505A (en) * 1989-04-04 1999-10-26 Eastman Chemical Company Fibers capable of spontaneously transporting fluids

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100622204B1 (en) * 2000-01-10 2006-09-07 주식회사 휴비스 Polytrimethyleneterephthalate fiber and preparation thereof
US9809907B2 (en) 2007-01-02 2017-11-07 Mohawk Carpet, Llc Carpet fiber polymeric blend

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