KR100221567B1 - The polyester fiber manufacture method - Google Patents

The polyester fiber manufacture method Download PDF

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KR100221567B1
KR100221567B1 KR1019950021794A KR19950021794A KR100221567B1 KR 100221567 B1 KR100221567 B1 KR 100221567B1 KR 1019950021794 A KR1019950021794 A KR 1019950021794A KR 19950021794 A KR19950021794 A KR 19950021794A KR 100221567 B1 KR100221567 B1 KR 100221567B1
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polyester fiber
mol
polyester
present
young
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KR1019950021794A
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KR970006568A (en
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장동호
손양국
박재용
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조정래
주식회사효성생활산업
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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
    • D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
    • D01F6/84—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyesters
    • 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
    • D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
    • 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
    • D01D5/096—Humidity control, or oiling, of filaments, threads or the like, leaving the spinnerettes
    • 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
    • D01D5/098—Melt spinning methods with simultaneous stretching
    • 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
    • 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
    • D10B2331/04—Fibres 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)

Abstract

본 발명은 폴리에스테르 섬유의 제조방법에 관한 것이다.The present invention relates to a method for producing polyester fibers.

본 발명의 무감량 상압가염 폴리에스테르 섬유는 폴리에스테르 섬유 반복단위의 93 ∼ 95몰%가 폴리에틸렌텔레프탈레이트이고 나머지 5 ∼ 7몰%가 2관능성 알콜계로 구성되어 있는 공중합 개질폴리에스테르 폴리머를 6,000 미터/분의 방사속도로 용융방사함에 의해 제조되며 하기의 식을 만족시키는 것을 특징으로 한다.6,000 meters of copolymer-modified polyester polymer wherein 93 to 95 mol% of the polyester fiber repeating units are polyethylene terephthalate and the remaining 5 to 7 mol% are composed of difunctional alcohols. It is produced by melt spinning at a spinning speed of / min and is characterized by satisfying the following equation.

1) One)

단 Xc는 결정화도(%), Fa는 비결정 배향 팩터Where Xc is the degree of crystallinity (%) and Fa is the amorphous orientation factor

2) 영율(Young's Mod.) ≤ 60 g/d.2) Young's Mod. ≤ 60 g / d.

3) 파단강도 ≥ 3.5 g/d., 파단신도 ≤ 50%3) Breaking strength ≥ 3.5 g / d., Elongation at break ≤ 50%

본 발명에 따르면 별도의 감량 가공이 필요없이 유연성을 가지며, 상온 상압에서 염색이 가능한 무감량 상압 가염 폴리에스테르 섬유가 제공되는 효과가 있다.According to the present invention has a flexibility without the need for a separate weight reduction process, there is an effect that is provided a lossless atmospheric pressure salt polyester fiber that can be dyed at room temperature and normal pressure.

Description

무감량 상압가염 폴리에스테르 섬유의 제조방법Process for producing weightless atmospheric salt polyester fiber

본 발명은 폴리에스테르 섬유의 제조방법에 관한 것으로서, 보다 상세하게는 후가공에서 알칼리 감량공정을 생략할 수 있고 상온·상압에서 염색이 가능한 폴리에스테르 섬유의 제조방법에 관한 것이다.The present invention relates to a method for producing a polyester fiber, and more particularly, to a method for producing a polyester fiber which can be omitted at room temperature and atmospheric pressure can be omitted alkali reduction step in post-processing.

합성섬유중 의복재료용 소재로서 가장 높은 비중을 차지하고 있는 폴리에스테르 섬유는 강직한 분자쇄로 구성되어 있으며, 결정성이 높은 관계로 알칼리 감량을 하지 않으면 직물의 촉감이 뻣뻣하여 부드럽고 드레이프성이 있는 의복소재로서 부적절하며, 분산염료에 의해 고온 고압하에서만 염색이 가능하므로 후공정에서의 비용상승이 문제가 된다.Polyester fiber, which has the highest specific gravity as a material for garment material among synthetic fibers, is composed of rigid molecular chain, and because of high crystallinity, the fabric is stiff and soft and draped without any alkali reduction. Inappropriate as a material, it is possible to dye only under high temperature and high pressure by the disperse dye, so that the cost increase in the post process becomes a problem.

또한 이러한 후가공 공정상에서의 취약점으로 인해 비용의 증가 뿐만 아니라 다른 소재(면, 모, 기타의 합성섬유)와의 온용에 있어서 제한이 따르게 되는 문제점이 있다.In addition, due to the weakness in the post-processing process, there is a problem that not only increases the cost but also a restriction on the warming with other materials (cotton, wool, and other synthetic fibers).

따라서 폴리에스테르 섬유의 감량공정을 생략하거나 용이하게 하기 위한 노력이나, 상압에서 염색이 가능하도록 하는 시도가 있어 왔는데, 일본국 특허공개공보 소 53-147814 호 및 55-128013 호에서는 폴리에스테르 중합시 텔레프탈릭산과 에틸렌글리콜의 2성분이외에 제3성분의 공중합 물질을 첨가함으로써 염색성을 개선하고 알칼리 감량이 용이하도록 하고 있으며, 국내 특허공고공보 제 95-732 호 및 95-734 호 등에서도 무감량 폴리에스테르섬유의 제조방법 및 이염성(異染性) 폴리에스테르섬유의 제조방법에 대한 기술이 제안되어 있으나 본 발명과 같이 무감량 및 상압염색을 동시에 만족시키는 폴리에스테르 섬유는 아직 개발되고 있지 않다.Therefore, efforts have been made to omit or facilitate the weight loss process of polyester fibers or to allow dyeing at normal pressure. In Japanese Patent Laid-Open Publication Nos. 53-147814 and 55-128013, telepolymers are not used. In addition to the two components of phthalic acid and ethylene glycol, addition of a copolymer of a third component improves dyeability and facilitates the reduction of alkalis, and is also a weight loss polyester in Korean Patent Publication Nos. 95-732 and 95-734. A technique for producing a fiber and a method for producing a dye-soluble polyester fiber have been proposed, but polyester fibers satisfying both weight loss and atmospheric dyeing as in the present invention have not been developed yet.

종래에 알려진 무감량 폴리에스테르 섬유의 제조방법은 제3성분의 공중합을 통해 섬유의 배향도 및 결정화도를 조절하여 초기 탄성율(영율 : YOUNG'S MODULUS)을 떨어뜨림으로써 감량공정을 거치지 않고도 충분히 유연한 감촉을 부여하는 것이나, 그것만으로는 상압염색 문제가 해결되지 않으며, 상압염색을 가능케 하기 위한 방법으로 초고속방사에 의한 방법이나 3성분 공중합개질에 의한 결정화 억제방법, 양이온 친화 개질제의 공중합 방법 등이 있으나, 초고속방사 방법에 의한 것은 본 발명자의 실험에 의하면 설비의 특별한 개조없이는 현재 공업화된 최고속도 영역인 방사속도 7,000 미터/분에서 담색에서만 상압염색이 가능하며 농색의 경우 염료흡진율이 130℃의 고온 고압에서 염색한 것에 미치지 못함을 확인하였으며, 공중합 개질에 의한 방법은 개질제의 함량이 10몰% 이상이어야 하므로 고가의 개질제 투입으로 인한 원가상승의 부담이 크고 열적, 기계적 물성의 취화, 염색견뢰도의 저하 현상과 같은 단점을 갖게 되며, 또한 감량공정을 생략하기에는 부족하다.Conventionally known method for producing a weightless polyester fiber is to adjust the orientation and crystallinity of the fiber through the copolymerization of the third component to drop the initial elastic modulus (Young's modulus) to give a sufficiently flexible feel without a weight loss process However, this alone does not solve the problem of atmospheric staining, and methods for enabling atmospheric staining include a method of ultrafast spinning, a method of inhibiting crystallization by three-component copolymerization modification, and a method of copolymerizing a cationic affinity modifier, but an ultrafast spinning method. According to the experiment of the present inventors, it is possible to dye at atmospheric pressure only at light color at the emission speed of 7,000 meters / minute, which is the highest industrialized speed range, without special modification of the equipment. It was confirmed that it does not reach, and the method by copolymerization modification The content of jilje must be at least 10 mol%, so will have the disadvantages such as brittleness, degradation of the color fastness of the large thermal and mechanical properties, the burden of rising costs due to expensive modifiers commitment, it is also not enough to omit the reduction process.

따라서 본 발명자는 무감량 및 상압염색의 두가지 목적을 동시에 만족시키기 위해 예의 연구한 결과 다음과 같은 조건을 만족하는 무감량 상압가염 폴리에스테르 섬유를 제조할 수 있게 되었다.Therefore, the present inventors have earnestly researched to satisfy two purposes of weight loss and atmospheric dyeing at the same time, and thus, can produce a weightless atmospheric salt polyester fiber satisfying the following conditions.

1) One)

이때, Xc는 결정화도(%), Fa는 비결정 배향 팩터Xc is the crystallinity (%), Fa is the amorphous orientation factor

2) 영율 (Young's Mod.) ≤ 60 g/d.2) Young's Mod. ≤ 60 g / d.

3) 파단강도 ≥ 3.5 g/d., 파단신도 ≤ 50%3) Breaking strength ≥ 3.5 g / d., Elongation at break ≤ 50%

본 발명은 폴리에스테르 섬유 반복단위의 93 ∼ 95 몰%가 폴리에틸렌텔레프탈레이트이고, 나머지 5 내지 7 몰%는 제3성분으로서 2관능성 알콜계로 구성되어 있는 공중합 개질폴리머를 권취속도 5000 내지 7000 m/분으로 초고속방사함으로써 무감량 상압가염이 가능한 폴리에스테르 섬유를 제조하였다.In the present invention, 93 to 95 mol% of the polyester fiber repeating unit is polyethylene terephthalate, and the remaining 5 to 7 mol% is a copolymerization modified polymer composed of a bifunctional alcohol system as the third component. The winding speed is 5000 to 7000 m / By super fast spinning in minutes to prepare a polyester fiber capable of weight loss atmospheric pressure salting.

본 발명을 좀더 상세히 설명하면 다음과 같다.The present invention will be described in more detail as follows.

본 발명자가 정의하는 이염지수 즉, 섬유의 비결정 영역의 비율(100 - 결정화도(%))을 비결정 영역의 배향으로 나눈 값이 4 이상일 경우 상압염색이 가능함을 알 수 있으며, 동시에 섬유의 초기탄성계수(영율)가 60 g/d. 미만이며 파단 강신도가 의복재료로서 문제가 없는 조건을 만족한다.The dichroism index defined by the present inventors, that is, the ratio (100-degree of crystallization (%)) of the amorphous region of the fiber divided by the orientation of the amorphous region can be seen that the atmospheric pressure dyeing is possible at the same time, the initial elastic modulus of the fiber Young's modulus is 60 g / d. It is less than one, and the elongation at break is satisfied as a garment material.

상기식에서 영율의 기준은 일반적인 폴리에스테르 섬유의 감량조건하에서 감량한 원사의 영율(10% 감량시 63 g/d.)을 기준으로 한 것이며, 상압가염의 기준은 98℃ 상압하에서의 평균염착량이 85% 이상인 것으로 하였다.In the above formula, the Young's modulus is based on the Young's modulus (63 g / d at 10% reduction) of the yarns reduced under ordinary polyester fiber reduction conditions. It was set as above.

상기의 식들을 만족시키기 위해서는 필연적으로 초고속방사공법을 적용해야 하는데, 기존의 방사-연신 2단계공법을 이용하는 경우 비정 영역의 체적은 다소 커지지만 비결정 영역의 배향이 급격히 증가하므로 결과적으로 염색성이 저하되며, 영율 또한 증가하여 무감량사로서는 적절치 못하게 된다.In order to satisfy the above equations, it is necessary to apply the ultra-fast spinning method. In the case of using the conventional two-step method of spinning, the volume of the amorphous region is rather large, but the orientation of the amorphous region is rapidly increased, and as a result, the dyeability is degraded. In addition, the Young's modulus also increases, making it unsuitable for weightless yarn.

또, 제3성분 개질제의 함량이 7 몰%를 초과하는 경우 물성의 취화가 심해져서 의료용사(衣料用絲)로는 부적합하게 된다.In addition, when the content of the third component modifier exceeds 7 mol%, the embrittlement of the physical properties becomes severe, making it unsuitable for medical spraying.

이하에서 본 발명의 바람직한 실시예 및 비교예를 통하여 본 발명이 보다 구체적으로 기술되어질 것이나, 이하의 실시예들이 본 발명의 범위를 국한시키는 것은 아니다.Hereinafter, the present invention will be described in more detail through preferred examples and comparative examples of the present invention, but the following examples do not limit the scope of the present invention.

[실시예 1]Example 1

고유점도가 0.64이고 2관능성 알콜계의 제3성분이 5몰%로 공중합 개질된 폴리에틸렌텔레프탈레이트 폴리머를 방사온도 290℃에서 직경이 0.20mm이고 구멍의 수가 36개인 방사구금을 통해 방사시키고 냉각 공기에 의해 고화시킨후 구금직하 130cm에서 급유장치를 통해 급유, 집속하여 70℃의 제1 고뎃 로울러, 125℃의 제2 고뎃 로울러를 통과하여 권취속도 6,000 미터/분으로 권취하여 75d/36f의 폴리에스테르 섬유를 얻었으며 그 물성을 표 1에 나타내었다.Polyethylene terephthalate polymer copolymerized and modified with the intrinsic viscosity of 0.64 and the third component of the difunctional alcohol system at 5 mol% was spun through a spinneret having a diameter of 0.20 mm and 36 holes at a spinning temperature of 290 ° C. and cooling air After solidifying by lubrication, refueling and concentrating at 130cm under the oil supply device, passing through the first high roller at 70 ° C, the second high roller at 125 ° C, and winding at a winding speed of 6,000 meters / min, and 75d / 36f polyester. Fibers were obtained and their physical properties are shown in Table 1.

[실시예 2]Example 2

고유점도가 0.64이고 2관능성 알콜계의 제3성분이 7몰%로 공중합 개질된 폴리에틸렌텔레프탈레이트 폴리머를 실시예 1과 갈은 조건으로 방사, 권취하여 그 물성을 표 1에 나타내었다.The polyethylene terephthalate polymer in which the intrinsic viscosity was 0.64 and the third component of the bifunctional alcohol system was copolymerized and modified at 7 mol% was spun and wound under the same conditions as in Example 1, and the physical properties thereof are shown in Table 1.

[비교예 1]Comparative Example 1

고유점도가 0.64이고 2관능성 알콜계의 제3성분이 3몰%로 공중합 개질된 폴리에틸렌텔레프탈레이트 폴리머를 실시예 1과 같은 조건으로 방사, 권취하여 그 물성을 표 1에 나타내었다.The polyethylene terephthalate polymer in which the intrinsic viscosity was 0.64 and the third component of the difunctional alcohol system was copolymerized to 3 mol% was spun and wound under the same conditions as in Example 1, and the physical properties thereof are shown in Table 1.

[비교예 2]Comparative Example 2

고유점도가 0.64이고 2관능성 알콜계의 제3성분이 9몰%로 공중합 개질된 폴리에틸렌 텔레프탈레이트 폴리머를 실시예 1과 같은 조건으로 방사, 권취하여 그 물성을 표 1에 나타내었다.The polyethylene terephthalate polymer having an intrinsic viscosity of 0.64 and the third component of the bifunctional alcohol system copolymerized and modified at 9 mol% was spun and wound under the same conditions as in Example 1, and the physical properties thereof are shown in Table 1.

[비교예 3]Comparative Example 3

고유점도가 0.64이고 2관능성 알콜계의 제3성분이 5몰%로 공중합 개질된 폴리에틸렌텔레프탈레이트 폴리머를 방사온도 285℃에서 직경이 0.25mm이고 구멍의 수가 36개인 방사구금을 통해 방사시키고 냉각 공기에 의해 고화시킨후 권취속도 1,500 미터/분으로 권취하여 250 d/36f의 폴리에스테르 미연신사를 얻었으며, 연신공정에서 연신비 3.1, 연신 로울러 온도 75℃, 열고정온도 140℃로 열연신하여 75d/36f의 폴리에스테르 섬유를 얻었으며 그 물성을 <표 1>에 나타내었다.Polyethylene terephthalate polymer copolymerized and modified with the intrinsic viscosity of 0.64 and the third component of the difunctional alcohol system by 5 mol% was spun through a spinneret having a diameter of 0.25 mm and 36 holes at a spinning temperature of 285 ° C., and cooling air After the solidification by the winding rate of winding at 1,500 meters / min to obtain a polyester unstretched yarn of 250 d / 36f, in the stretching process, the stretching ratio 3.1, the stretching roller temperature 75 ℃, heat-extended at 140 ℃ heat stretching 75d / 36 f of polyester fiber was obtained, and the physical properties thereof are shown in Table 1.

상술한 바와 같이 본 발명에 따르면 별도의 감량 가공이 필요없이 유연성을 가지며 상온 (98℃) 상압에서 염색이 가능한 무감량 상압가염 폴리에스테르 섬유가 제공되는 효과가 있다.As described above, according to the present invention, there is an effect of providing a weight-free atmospheric salt polyester fiber which can be dyed at room temperature (98 ° C.) and normal pressure without the need for additional weight processing.

Claims (1)

폴리에스테르 섬유 반복단위의 93 ∼ 95몰%가 폴리에틸렌텔레프탈레이트이고 나머지 5 ∼ 7몰%가 2관능성 알콜계로 구성되어 있는 공중합 개질폴리에스테르 폴리머를 6,000 미터/분의 방사속도로 용융방사함에 의해 제조되며 하기의 식을 만족시키는 것을 특징으로 하는 폴리에스테르 섬유의 제조방법.93-95 mol% of polyester fiber repeating units are produced by melt spinning a copolymer-modified polyester polymer composed of polyethylene terephthalate and the remaining 5-7 mol% of a bifunctional alcohol system at a spinning speed of 6,000 meters / minute. And a method of producing a polyester fiber, characterized by satisfying the following formula. 1) One) 단, Xc는 결정화도(%), Fa는 비결정 배향 팩터Xc is the crystallinity (%) and Fa is the amorphous orientation factor 2) 영율 (Young's Mod.) ≤ 60 g/d.2) Young's Mod. ≤ 60 g / d. 3) 파단강도 ≥ 3.5 g/d., 파단신도 ≤ 50%3) Breaking strength ≥ 3.5 g / d., Elongation at break ≤ 50%
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