KR0164449B1 - Manufacturing method of polyester fiber with antistatic property - Google Patents

Manufacturing method of polyester fiber with antistatic property Download PDF

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Publication number
KR0164449B1
KR0164449B1 KR1019950021793A KR19950021793A KR0164449B1 KR 0164449 B1 KR0164449 B1 KR 0164449B1 KR 1019950021793 A KR1019950021793 A KR 1019950021793A KR 19950021793 A KR19950021793 A KR 19950021793A KR 0164449 B1 KR0164449 B1 KR 0164449B1
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South Korea
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compound
polyester
polyester fiber
general formula
metal salt
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KR1019950021793A
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Korean (ko)
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KR970006567A (en
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장동호
김정현
이세영
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이명환
동양폴리에스터주식회사
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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
    • 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
    • D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • 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
    • 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
    • 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
    • D02G3/44—Yarns or threads characterised by the purpose for which they are designed
    • D02G3/441—Yarns or threads with antistatic, conductive or radiation-shielding properties
    • 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]
    • 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
    • D10B2401/00—Physical properties
    • D10B2401/16—Physical properties antistatic; conductive

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)
  • Polyesters Or Polycarbonates (AREA)

Abstract

본 발명은 폴리에스테르 섬유의 제조방법에 관한 것으로 보다 상세하게는 일반 폴리에스테르 섬유 장점을 그대로 보유하면서도 제전성 및 내열 안정성이 우수한 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 excellent in antistatic properties and heat resistance while retaining the advantages of the general polyester fiber as it is.

본 발명은 섬유용 폴리에스테르 중합 조성물에 폴리옥시알킬렌글리콜 및 비반응성 알칼술폰산 금속염과 함께 하기 일반식(Ⅰ)의 마그네슘 화합물을 첨가하여 공중합한 폴리에스테르 폴리머를 방사하는 것을 특징으로 한다.The present invention is characterized by spinning a polyester polymer copolymerized by adding a magnesium compound of the following general formula (I) together with a polyoxyalkylene glycol and a non-reactive alkalsulfonic acid metal salt to a polyester polymerization composition for fibers.

상기 식에서 X는 Cl, Br, I, O, S 중 어느 하나이며, Cl, Br, I 등과 같이 I가 화합물일 때는 n=2이며, O, S 등과 같이 2가 화합물일 때는 n=1이다.In the formula, X is any one of Cl, Br, I, O, S, n = 2 when I is a compound such as Cl, Br, I, and n = 1 when a divalent compound such as O, S and the like.

본 발명에 의해 수득되는 폴리에스테르 섬유는 본래의 우수한 제반물성을 그대로 보유하면서 제전성 및 내열성이 탁월하여 고급양복 안감지, 여성용 내의, 블라우스, 란제리, 스포츠 웨어 및 무진복 등의 기능복에 다양하게 사용될 수 있다.The polyester fiber obtained by the present invention is excellent in antistatic properties and heat resistance while retaining its original excellent general properties, and is variously used in functional clothes such as high-quality garment lining paper, women's underwear, blouse, lingerie, sportswear and dust-free clothing. Can be used.

Description

[발명의 명칭][Name of invention]

제전성이 우수한 폴리에스테르 섬유의 제조방법Manufacturing method of polyester fiber excellent in antistatic property

[발명의 상세한 설명]Detailed description of the invention

본 발명은 폴리에스테르 섬유의 제조방법에 관한 것으로 보다 상세하게는 일반 폴리에스테르 섬유의 장점을 그대로 보유하면서도 제전성 및 내열 안정성이 우수한 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 having excellent antistatic properties and heat resistance stability while retaining the advantages of the general polyester fiber as it is.

폴리에스테르 섬유는 내약품성, 강신도, 결정성, 굴곡강도 등 그 물성이 우수하여 의료용(醫療用)으로 널리 사용되고 있다. 그러나 저온 저습도인 지역이나 동절기에 안감지, 란제리, 파운데이션, 기타 무진복이나 운동복 등 특수 기능복으로 사용하기에는 마찰에 의한 정전기의 발생으로 먼지 등이 흡착되어 쉽게 오염되고 또한 땀이나 습기를 흡수하는 성질이 약해 착용자에게 쇼크나 불쾌감을 주는 문제점이 있다.Polyester fibers are widely used for medical purposes because of their excellent physical properties such as chemical resistance, elongation, crystallinity and flexural strength. However, to be used as special function clothes such as lining paper, lingerie, foundation, other dust-free or sportswear in low temperature and low humidity areas or winter, dust is adsorbed due to the generation of static electricity caused by friction, and it absorbs sweat and moisture. Due to its weak nature, there is a problem of shock or discomfort to the wearer.

그 동안 이러한 정전기적인 장애를 해결하기 위해 제전사의 제조방법들이 많이 제안되어 왔다. 그러나 이러한 종래의 방법에 의해 제조된 제전자에 있어서, 내열성이 취약하여 중합시 제전제의 비산에 의한 진공라인 막힘 등의 중합공정의 불안을 야기하였고 또한 비산에 의한 함량 불균일 및 방사시 폴리에스테르의 점도 강하에 의하여 최종 제품의 염색반 발생의 원인이 되었으며 건조 및 방사공정 및 여러 공정을 지니면서 사물성도 불균일하게 되는 문제점이 있었다.In order to solve such electrostatic disturbances, many methods have been proposed for the manufacture of static eliminators. However, in the former manufactured by such a conventional method, the heat resistance is weak, causing anxiety in the polymerization process such as clogging of the vacuum line due to scattering of the antistatic agent during the polymerization, and also causing uneven content of the polyester during scattering and spinning. The lowering of the viscosity caused the staining of the final product, and there was a problem in that the objectivity was also uneven while having drying and spinning processes and various processes.

본 발명의 목적은 상술한 바와 같은 문제점을 해결하기 위한 것으로 본래의 우수한 물성을 그대로 유지하면서 제전성 및 내열성이 향상된 폴리에스테르 섬유의 제조방법을 제공하는 것이다.An object of the present invention is to solve the problems as described above, and to provide a method for producing a polyester fiber with improved antistatic and heat resistance while maintaining the original excellent properties.

본 발명은 섬유용 폴리에스테르 중합 조성물에 폴리옥시알킬렌글리콜 및 비반응성 알킬술폰산 금속염과 함께 하기 일반식(Ⅰ)의 마그네슘 화합물을 첨가하여 공중합한 폴리에스테르 폴리머를 방사하는 것을 특징으로 한다.The present invention is characterized by spinning a polyester polymer copolymerized by adding a magnesium compound of the following general formula (I) together with a polyoxyalkylene glycol and a non-reactive alkylsulfonic acid metal salt to a polyester polymerization composition for fibers.

상기 식에서 X는 Cl, Br, I, O, S 중 어느 하나이며, Cl, Br, I 등과 같이 I가 화합물일 때는 n=2이며, O, S 등과 같이 2가 화합물일 때는 n=1이다.In the formula, X is any one of Cl, Br, I, O, S, n = 2 when I is a compound such as Cl, Br, I, and n = 1 when a divalent compound such as O, S and the like.

본 발명에서는, 상기 일반식(Ⅰ)의 마그네슘 화합물이 폴리에스테르의 말단기와 반응하여 방사공정 등의 폴리에스테르 중합물의 가열 용융시 수분의 존재로 인한 분해와 열화의 문제점을 해결할 수 있으며, 따라서 사의 강도가 개선되고 내가수분해성이 우수하게 된다.In the present invention, the magnesium compound of the general formula (I) reacts with the end group of the polyester to solve the problems of decomposition and deterioration due to the presence of water during the heating and melting of the polyester polymer, such as spinning process, The strength is improved and the hydrolysis resistance is excellent.

본 발명에서 상기 일반식(Ⅰ)의 화합물은 폴리에스테르에 대해서 50 ∼ 500ppm의 양으로 첨가된다. 상기 일반식(Ⅰ)의 화합물이 첨가량이 상기 범위보다 적으면 방사공정시 발생하는 점도 강하의 개선효과 및 기타 물성의 개선효과가 미흡하고, 상기 범위를 초과하면 폴리에스테르의 용융점도가 높아지고 사물성이 저하되므로 상기 일반식(Ⅰ)의 화합물의 첨가량은 상기 범위내로 유지하는 것이 바람직하다.In the present invention, the compound of the general formula (I) is added in an amount of 50 to 500 ppm relative to the polyester. When the amount of the compound of the general formula (I) is less than the above range, the effect of improving the viscosity drop and other physical properties generated during the spinning process is insufficient. When the compound exceeds the above range, the melt viscosity of the polyester increases and Since it falls, it is preferable to keep the addition amount of the compound of the said general formula (I) within the said range.

본 발명에서 폴리에스테르 주쇄말단에 공중합되어 제전제로 사용되는 폴리옥시알킬렌글리콜은 수평균분자량이 2.000 ∼30,000인 하기 일반식(Ⅱ)의 화합물이 가장 바람직하며 그 첨가량은 전체 폴리에스테르 대비 0.01 ∼ 3.5 중량%인 것이 바람직하다. 이때 상기 폴리옥시알킬렌글리콜의 첨가량이 0.01 중량% 미만이면 제조되는 사의 제전성이 극히 불량해지고 3.5 중량% 이상일 경우에는 사의 기본물성이 저하된다.In the present invention, the polyoxyalkylene glycol copolymerized at the polyester main chain end and used as an antistatic agent is most preferably a compound represented by the following general formula (II) having a number average molecular weight of 2.000 to 30,000, and the amount thereof is 0.01 to 3.5 compared to the total polyester. It is preferable that it is weight%. At this time, when the amount of the polyoxyalkylene glycol added is less than 0.01% by weight, the antistatic property of the manufactured yarn is extremely poor, and when the amount of the polyoxyalkylene glycol is 3.5% by weight or more, the basic physical properties of the yarn decrease.

상기 식에서 R1: C1∼ C13알킬기 또는 수소Wherein R 1 : C 1 to C 13 alkyl group or hydrogen

R2: C2∼ C16인 알킬렌기,R 2 : alkylene group having 2 to 16 carbon atoms,

n : 20 ∼ 150 사이의 정수n: integer between 20 and 150

본 발명에서 사용하는 비반응성 알킬술폰산 금속염은 하기 일반식(Ⅲ)의 비반응성 폴리알킬술폰산 금속염이 특히 바람직하며 그 첨가량은 전체 폴리에스테르 대비 0.01 ∼ 2 중량%인 것이 바람직하다. 하기 일반식(Ⅲ)의 비반응성 폴리알킬술폰산 금속염의 첨가량이 2중량% 이상일 경우에는 디에틸렌글리콜의 함량이 많아져서 동일 용융점에서 중합물을 베출할 경우 고유점도가 높아져 사물성중 신도가 너무 낮아지는 단점이 있고 그 첨가량이 0.01중량% 미만일 경우에는 점도가 너무 낮아져 방사가 곤란하다.The non-reactive alkylsulfonic acid metal salt used in the present invention is particularly preferably a non-reactive polyalkylsulfonic acid metal salt of the following general formula (III), and the amount thereof is preferably 0.01 to 2% by weight based on the total polyester. When the amount of the non-reactive polyalkylsulfonic acid metal salt of the following general formula (III) is 2% by weight or more, the content of diethylene glycol is increased, and when the polymer is ejected at the same melting point, the intrinsic viscosity becomes high, and the elongation in object is too low. If there is a disadvantage and the addition amount is less than 0.01% by weight, the viscosity is too low to be difficult to spin.

상기 식에서 R3: C3∼ C25인 알킬기 또는 C7∼ C30인 아릴기,In the formula, R 3 : C 3 ~ C 25 Alkyl group or C 7 ~ C 30 An aryl group,

M : Na, K, Li 중의 하나이다.M is one of Na, K, and Li.

본 발명에서는 또한 일반적으로 알려진 바와 같이 축중합 반응시 촉매로서 삼산화 안티몬을 200 ∼ 500ppm 첨가하여 반응을 진행시킨다.In the present invention, as is generally known, 200 to 500 ppm of antimony trioxide is added as a catalyst during the polycondensation reaction to advance the reaction.

본 발명에 따라 폴리에스테르 섬유를 제조하는 구체적 단계를 예를 들어 기술하For example, specific steps for making polyester fibers according to the invention are described.

면 폴리에틸렌텔레프탈레이트 올리고머가 저장된 중합조를 약 260℃로 유지하면서 텔레프탈산과 에틸렌글리콜을 반응이론양으로 취하여 잘 혼합한 슬러리를 약 4시간에 걸쳐서 투입하여 올리고머를 제조한 후 중축합 중합조로 소정량을 옮긴다. 이어서 중축합 반응단계에서 본 발명의 일반식(Ⅰ) 및 (Ⅱ)의 화합물을 80 ∼100℃에서 반응시킨 것을 투입한 다음 일반식(Ⅲ)의 화합물을 첨가하여 약 280℃에서 상의 방법에 따라 건조하고 방사, 연신을 행하여 폴리에스테르 섬유를 제조한다.While maintaining the polymerization tank in which the cotton polyethylene terephthalate oligomer was stored at about 260 ° C., the reaction mixture was prepared by taking the telephthalic acid and ethylene glycol as the amount of reaction theory. Move it. Subsequently, the compound of general formula (I) and (II) of the present invention was reacted at 80 to 100 ° C. in the polycondensation reaction step, and then the compound of general formula (III) was added thereto at about 280 ° C. according to the phase method. It is dried, spun and stretched to produce polyester fibers.

이하에서 본 발명의 바람직한 실시형태에 따라서 실시예들이 기술되어지고, 이 실시예들과 비교하기 위하여 비교예들이 개시되어질 것이다. 그러나 이 실시예들은 본 발명을 단지 예시적으로 보여주기 위한 것으로 본 발명의 범위를 국한시키는 것으로 이해되어져서는 안될 것이다.In the following, examples are described according to preferred embodiments of the present invention, and comparative examples will be disclosed for comparison with these examples. However, these examples are only intended to illustrate the invention and should not be understood as limiting the scope of the invention.

[실시예 Ⅰ]Example I

텔레프탈산 8.65㎏, 에틸렌글리콜 3.65㎏, 삼산화안티몬 3g을 잘혼합하여 슬러리를 제조한후 환류탑이 장치된 에스테르화 반응기에 서서히 투입하고 260℃에서 에스테르화 반응을 진행시켜서 비스-(2-히드록시에틸) 텔레프탈레이트 및 그 저중합체를 수득한다. 수득된 저중합체를 중축합 반응장치에 옮긴 다음 일반식(Ⅱ)의 화합물 C12H25O(C2H4O)40H 50g과 일반식(Ⅲ)의 화합물 C12H25SO3Na 100g 및 일반식(Ⅰ)의 화합물 MgO 2g을 투입하고 280℃에서 반응시켜 폴리에스테르 중합물을 제조하였다.8.65 kg of telephthalic acid, 3.65 kg of ethylene glycol, and 3 g of antimony trioxide were mixed well to prepare a slurry, and then slowly added to an esterification reactor equipped with a reflux tower, followed by an esterification reaction at 260 ° C. to give bis- (2-hydroxy Ethyl) telephthalate and its oligomer. The obtained oligomer was transferred to a polycondensation reactor, and then 40 g 50 H of compound C1 2 H 25 O (C 2 H 4 O) of general formula (II) and 100 g of compound C 12 H 25 SO 3 Na of general formula (III) And 2g of compound MgO of Formula (I) was added and reacted at 280 ℃ to prepare a polyester polymer.

수득된 종합물을 통상의 방법으로 건조한 후 방사하여 얻어진 미연신사를 80℃로 유지된 가열로울러 및 120℃로 유지된 열판에 의해 1500m/min의 연신속도로 연신하여 75d/36f의 연신사를 제조하고 그 물성을 평가하여 하기 표 1에 나타내었다.The resultant composite was dried by spinning in a conventional manner, and the undrawn yarn obtained by stretching was drawn at a drawing speed of 1500 m / min by a heating roller maintained at 80 ° C. and a hot plate kept at 120 ° C. to produce a drawn yarn of 75 d / 36f. And the physical properties were evaluated and shown in Table 1 below.

[실시예 2∼7 및 비교예 1∼6][Examples 2 to 7 and Comparative Examples 1 to 6]

하기 표 1과 같이 각 화합물이 첨가량을 변경시키는 것 이외에는 실시예 1과 동일한 방법으로 폴리에스테르 제전사를 제조하고 그 물성을 평가하여 하기 표 1에 나타내었다.Except for changing the amount of each compound as shown in Table 1 below to prepare a polyester electrostatic yarn in the same manner as in Example 1 and to evaluate the physical properties are shown in Table 1 below.

*) 방사성 평가 : 방사작업성이 90% 이상이면 양호, 80% 이상이면 보통, 80% 미만이면 불량으로 판정*) Radioactivity evaluation: Good if the workability is over 90%, normal if over 80%, bad if less than 80%

상술한 바와 같이 하여 본 발명에 의해 수득되는 폴리에스테르 섬유는 본래의 우수한 제반물성을 그대로 보유하면서 제전성 및 내열성이 탁월하여 고급양복 안감지, 여성용 내의, 블라우스, 란제리, 스포츠 웨어 및 무진복 등의 기능복에 다양하게 사용될 수 있다.The polyester fiber obtained by the present invention as described above is excellent in antistatic properties and heat resistance while retaining the original excellent general properties, such as high-end clothing lining paper, women's underwear, blouse, lingerie, sportswear and dust-free clothing It can be used for various functions.

Claims (3)

폴리옥시알킬렌글리콜 화합물 및 비반응성 알킬술폰산 금속염과 함께 하기 일반식(Ⅰ)의 마그네슘 화합물을 폴리에스테르에 대하여 50 ∼500ppm 첨가하여 공중합한 것을 방사하여 제조되는 것을 특징으로 하는 제전성이 우수한 폴리에스테르 섬유의 제조방법.A polyester having excellent antistatic properties, which is prepared by spinning 50 to 500 ppm of a copolymer of magnesium compound of the following general formula (I) with a polyoxyalkylene glycol compound and a non-reactive alkylsulfonic acid metal salt. Method of making fibers. 상기 식에서 X는 Cl, Br, I, O, S 중 어느 하나이며, Cl, Br, I 등과 같이 I가 화합물일 때는 n=2이며, O, S 등과 같이 2가 화합물일 때는 n=1이다.In the formula, X is any one of Cl, Br, I, O, S, n = 2 when I is a compound such as Cl, Br, I, and n = 1 when a divalent compound such as O, S and the like. 제1항에 있어서, 상기 폴리옥시알킬렌글리콜은 수평균 분자량이 2,000 ∼ 30,000인 하기 일반식(Ⅱ)의 화합물이고, 그 첨가량은 전체 폴리에스테르 대비 0.01 ∼ 3.5 중량%인 것을 특징으로 하는 상기 제전성이 우수한 폴리에스테르 섬유의 제조방법.The compound according to claim 1, wherein the polyoxyalkylene glycol is a compound of the following general formula (II) having a number average molecular weight of 2,000 to 30,000, and the amount of the polyoxyalkylene glycol is 0.01 to 3.5% by weight based on the total polyester. Method for producing polyester fibers with excellent malleability. 상기 식에서 R1: C1∼ C13알킬기 또는 수소, R2: C2∼ C16인 알킬렌기, n : 20 ∼ 150 사이의 정수이다.In the above formula, R 1 : C 1 to C 13 alkyl group or hydrogen, R 2 : C 2 to C 16 alkylene group, n: It is an integer between 20 to 150. 제1항에 있어서, 상기 비반응성 알킬술폰산 금속염이 하기 일반식(Ⅲ)의 비반응성 폴리알킬술폰산금속염이고 그 첨가량은 전체 폴리에스테르 대비 0.01 ∼ 2 중량%인 것을 특징으로 하는 상기 제전성이 우수한 폴리에스테르 섬유의 제조방법.According to claim 1, wherein the non-reactive alkyl sulfonic acid metal salt is a non-reactive polyalkyl sulfonic acid metal salt of the general formula (III) and the addition amount is 0.01 to 2% by weight based on the total polyester, the excellent antistatic Process for producing ester fiber. 상기 식에서 R3: C3∼ C25인 알킬기 또는 C7∼ C30인 아릴기, M : Na, K, Li 중의 하나이다.In the above formula, R 3 : C 3 ~ C 25 Alkyl group or C 7 ~ C 30 An aryl group, M: Na, K, Li is one of.
KR1019950021793A 1995-07-22 1995-07-22 Manufacturing method of polyester fiber with antistatic property KR0164449B1 (en)

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