KR970010721B1 - Process for preparing antistatic electricity polyester fiber - Google Patents

Process for preparing antistatic electricity polyester fiber Download PDF

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KR970010721B1
KR970010721B1 KR1019920015268A KR920015268A KR970010721B1 KR 970010721 B1 KR970010721 B1 KR 970010721B1 KR 1019920015268 A KR1019920015268 A KR 1019920015268A KR 920015268 A KR920015268 A KR 920015268A KR 970010721 B1 KR970010721 B1 KR 970010721B1
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polyester
lithium
reactive
nli
alkyl group
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KR940004092A (en
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김우섭
김문찬
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구창남
동양나이론주식회사
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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
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/09Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • 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
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00Physical properties
    • D10B2401/16Physical properties antistatic; conductive

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

Abstract

The polymer vessel that contains a polyethylene terephthalate oligomer 10[kg is kept to the temperature, 260 degree C, while the slurry produced by terephthalic acid and ethyleneglycol properly compounded, is fed to the vessel for 6 hours to produce 20[kg of an oligomer. And after being transferred 10[kg to another polymer, this oligomer is mixed with antimony trioxide, C12H2509(C2H40)40H, C12H25SO3Li and non reactive lithium amide, and the temperature is kept to 280 degree C.

Description

폴리에스터 제전사의 제조방법Manufacturing method of polyester maker

본 발명은 제전성능이 우수하면서도 일반 폴리에스터 섬유의 장점을 잃지않는 폴리에스터 제전사의 개량된 제조방법에 관한 것이다.The present invention relates to an improved method for producing polyester yarns that have excellent antistatic performance but do not lose the advantages of ordinary polyester fibers.

폴리에스터 섬유는 내열성, 내약품성, 강신도, 결정성, 굴곡강도 등의 물성이 우수하여 의류용으로 크게 각광을 받고 있지만 저온이며 저습도인 지역이나, 겨울철에는 안감이나, 란제리, 화운데이션, 기타 무진복이나 운동복 등 특수 기능복으로 사용하기에는 마찰에 의한 정전기의 발생으로 먼지들이 흡착, 오염이 쉽게 되고 착용자에게 쇼크가 불쾌감을 주게되는 문제점이 있다. 이러한 정전기적인 장애를 해결하기 위하여 많은 방법들이 제안되었다. 폴리옥시알킬렌글리콜에 메타크릴레이트나 비스페놀을 사용하고 폴라즈마방법으로 후가공처리하여 대전방지기능을 부여하는 방법이 있으나, 이 방법은 세탁후 제전성이 급격히 떨어지는 단점이 있었다. 이러한 내세탁성 문제를 해결하고 영구적인 제전성을 부여하기 위하여 일본 공개특허공보 소 52-47071호 및 동 52-47072호에서 소개된 폴리알킬렌글리콜과 알킬술폰산나트륨을 사용하여 폴리머를 개질하는 방법이 최근 많이 사용되고 있다. 알킬술폰산 나트륨은 폴리머에 이온성기를 도입시켜 전하의 이동을 활발하게 하고 또한 폴리알킬렌글리콜의 공중합물과의 상승작용으로 우수한 제전성능을 발현시킬 수 있는 장점을 가지고 있다. 그러나, 알킬술폰산나트륨은 폴리머내부에서의 분산성이 나쁘고 방사시 팩압을 증가시키는 요인이 된다. 또한 방사노즐 내부에 나트륨금속염이 잔존하는 경우가 생겨 방사불량이 생기고 팩교환주기가 짧아져 방사작업성이 떨어지고 폴리머내부에서의 분산성이 나빠, 염색불량의 원인이 되기도 한다.Polyester fiber is attracting much attention for clothing because it has excellent properties such as heat resistance, chemical resistance, elongation, crystallinity, and flexural strength, but in low temperature and low humidity areas, it is lining, lingerie, foundation, and other dust-free clothing in winter. In order to use it as a special functional clothing such as sportswear, there is a problem in that dust is easily adsorbed and contaminated by the generation of static electricity due to friction, and shock is uncomfortable to the wearer. Many methods have been proposed to solve this electrostatic disturbance. There is a method of imparting antistatic function by using methacrylate or bisphenol in polyoxyalkylene glycol and post-processing by the plasma method, but this method has a disadvantage in that the antistatic property is sharply reduced after washing. In order to solve the problem of washing resistance and to impart permanent antistatic properties, a method of modifying a polymer using polyalkylene glycol and sodium alkyl sulfonate introduced in Japanese Patent Laid-Open Nos. 52-47071 and 52-47072 This has been used a lot lately. Sodium alkyl sulfonate has an advantage of introducing an ionic group into the polymer to promote charge transfer and to express excellent antistatic performance by synergistic action with the copolymer of polyalkylene glycol. However, sodium alkyl sulfonate is poor in dispersibility inside the polymer and causes a pack pressure increase during spinning. In addition, sodium metal salts may remain inside the spinning nozzles, resulting in poor spinning and shorter pack replacement cycles, resulting in poor spinning workability, poor dispersibility within the polymer, and inferior dyeing.

본 발명은 이러한 문제점을 해결한 것으로 이를 보다 상세히 설명하면 다음과 같다. 본 발명은 폴리에스터에 공중합성분을 투입 중합하여 제전사를 제조함에 있어서 공중합 성분으로 폴리옥시알킬렌글리콜화합물 및 미반응성 알킬술폰산리튬염과 함께 비반응성 리튬아미드를 사용하는 것을 특징으로 하는 폴리에스터 제전사의 제조방법에 관한 것이다.The present invention solves this problem and will be described in more detail as follows. The present invention is a polyester agent, characterized in that non-reactive lithium amide is used together with a polyoxyalkylene glycol compound and an unreacted alkylsulfonate lithium salt as a copolymerization component in preparing polymerization by adding a copolymerization component to a polyester. It relates to a method for producing a transfer.

본 발명에서 폴리옥시알킬렌글리콜 화합물은 수평균분자량이 2,000 이상 30,000 이하인 하기 일반식(I)의 화합물이 특히 적합하며, 폴리에스터 전량 대비 0.01∼3.5중량%를 축중합시기에 투입하여 폴리에스터 주쇄의 말단에 공중합시킨다. 투입량이 0.01중량% 이하일 경우 제전성이 극히 떨어지고 3.5중량% 이상일 경우에는 사의 기본물성이 저하된다.In the present invention, the polyoxyalkylene glycol compound is particularly suited to the compound of formula (I) having a number average molecular weight of 2,000 or more and 30,000 or less. It copolymerizes in the terminal of. If the input amount is 0.01% by weight or less, the antistatic property is extremely low, when the 3.5% by weight or more, the basic physical properties of the yarn is lowered.

(상기에서, Rl: C1∼C13인 알킬기 또는 H, R2: C2∼C16인 알킬렌기, n : 20∼150의 정수)(Wherein, R l: C 1 ~C 13 alkyl group or H, R 2: C 2 ~C 16 alkyl group, n: an integer of 20-150)

본 발명에서 사용하는 비반응성 알킬술폰산리튬염은 종래의 폴리알킬술폰산나트륨과는 다른것으로 특히 하기 일반식(II)의 비반응성 폴리알킬술폰산리튬을 사용하는 것이 바람직하다.The non-reactive lithium sulfonate salt used in the present invention is different from conventional sodium polyalkyl sulfonate, and it is particularly preferable to use non-reactive polyalkyl sulfonate lithium of the following general formula (II).

(상기에서, R3: C3∼C25인 알킬기 또는 C7∼C30인 아릴기)(Wherein, R 3: C 3 ~C 25 alkyl group or C 7 ~C 30 aryl group)

이때, 폴리알킬술폰산 리튬의 사용함량이 많으면 DEG의 함량이 많아 동일 용융점도에서 중합물을 배출할경우 고유점도가 높아져 사물성에서 신도가 너무 낮아지는 단점이 발생하고 적은 경우에는 점도가 낮아져서 곤란하다. 따라서 바람직한 첨가량은 0.01∼2중량%이다.At this time, when the amount of lithium polyalkylsulfonate used is large, the content of DEG is high, so that when the polymer is discharged at the same melt viscosity, the intrinsic viscosity becomes high, so that the elongation is too low in the physical property, and in the case of less, the viscosity is difficult to decrease. Therefore, preferable addition amount is 0.01 to 2 weight%.

본 발명에서 상기 두 화합물과 함께 특징적으로 사용하는 비반응성 리튬아미드는 예를들면 LiNH2, [(CH3)3Si]2NLi, (C6Hl1)2NLi, [(CH3)2CH2]NLi 등이 바람직하며, 이때 사용함량은 폴리에스터 대비0.001∼1중량%가 바람직하다. 0.001중량% 이하일 경우에는 제전성이 저하되고 1중량% 이상일 경우에는 점도상승과 방사불량의 원인이 된다. 또한 일반적으로 알려진 바와 같이 축중합시 촉매로서 Sb2O3를 200∼400ppm 첨가하고 아래와 같이 인화합물을 10∼200ppm 첨가한후 2시간동안 반응을 시킴으로써 열안정성을 높일 수 있다.Non-reactive lithium amides characteristically used with the two compounds in the present invention are for example LiNH 2 , [(CH 3 ) 3 Si] 2 NLi, (C 6 H 1 ) 2 NLi, [(CH 3 ) 2 CH 2 ] NLi and the like, and the content is preferably 0.001 to 1% by weight compared to the polyester. If it is 0.001 weight% or less, antistatic property will fall, and if it is 1 weight% or more, it will cause a viscosity increase and a radiation failure. In addition, as generally known, thermal stability can be improved by adding 200-400 ppm of Sb 2 O 3 as a catalyst during condensation polymerization, adding 10-200 ppm of phosphorus compound as described below, and reacting for 2 hours.

(여기에서, R4-6: H 또는 알킬기) Wherein R 4-6 : H or an alkyl group

본 발명은 통상의 중합공정 및 방사 연신공정을 통하여 수행될 수 있는 것으로 상세한 기재는 생략하며 본 발명에 따라 수득하는 폴리에스터 제전사는 폴리에스터 섬유 고유의 물성을 저해하지 않으면서도 제전성능이 우수하여 의류용 및 기능복에 널리 사용이 가능하다.The present invention can be carried out through a conventional polymerization process and spin drawing process, the detailed description is omitted, and the polyester antistatic yarn obtained according to the present invention has excellent antistatic performance without compromising the intrinsic properties of the polyester fiber clothing It can be widely used for dragon and functional clothes.

이하에 실시예를 들어 설명한다.An example is given and described below.

(실시예)(Example)

(측정방법)(How to measure)

(1) 디에틸렌글리콜(DEG)량 : 히드라진 수화물로 폴리에스터를 열분해하고 이것을 가스크로마토그래피로 측정한다.(1) Diethylene glycol (DEG) amount: Pyrolyse the polyester with hydrazine hydrate and measure this by gas chromatography.

(2) 비저항 : 항온항습실에서 일본 TOA사의 전기저항측정기를 사용하여 측정한다.(2) Resistivity: Measured by using an electric resistance measuring instrument of TOA of Japan in a constant temperature and humidity room.

(3) 마찰대전압, 반감기 : 가네보식 마찰대전압 측정기를 사용하여 측정한다.(3) Friction band voltage, half-life: Measured using a Kanebo friction belt voltage meter.

* 비저항, 마찰대전압, 반감기는 온도 20±2℃, 습도 40±2RH%에서 측정하였다.* The specific resistance, friction voltage, and half-life were measured at 20 ± 2 ℃ and 40 ± 2RH% humidity.

(실시예1)Example 1

폴리에틸렌테레프탈레이트 올리고머 10kg이 함유된 중합조를 260℃로 유지하면서 테레프탈산 8645kg과 에틸렌글리콜 3875g이 잘 혼합된 슬러리를 6시간에 결쳐시 투입하여 20kg의 올리고머를 제조한후 다른 중합조로 10kg을 옮긴다. 이 올리고머에 삼산화안티몬 5g과 일반식(I)의 화합물 C12H25O(C2H4O)40H 100g과 일반식(II)의 화합물 C12H25SO3Li 10g 및 미반응성 리튬 아미드 (C6H11)2NLi 5g을 투입한 후, 280℃에서 반응시켜 본발명의 폴리에스터를 제조하였다. 얻어진 중합체를 통상의 방법으로 건조한후, 구공 0.25mm 직경의 원형방사구공 36개를 가진 구금을 사용하여 295℃에서 1000m/min의 속도로 방사하였다. 얻어진 미연신사를 80℃로 유지된 가열로울러 및 120℃로 유지된 열판에 의해 1070m/min의 연신속도로 연신하여 75d/f의 연신사를 제조하고 물성을 평가하여 표-1에 정리하였다.While maintaining a polymerization tank containing 10 kg of polyethylene terephthalate oligomer at 260 ° C., a slurry mixed with 8645 kg of terephthalic acid and 3875 g of ethylene glycol was added in 6 hours to prepare a 20 kg oligomer, and then 10 kg was transferred to another polymerization tank. 5 g of antimony trioxide, compound C 12 H 25 O (C 2 H 4 O) 40 H 100 g and compound C 12 H 25 SO 3 Li 10 g of general formula (II) and unreactive lithium amide (C 6 H 11 ) 2 NLi 5g was added, and reacted at 280 ℃ to prepare a polyester of the present invention. The polymer obtained was dried in a conventional manner, and spun at a rate of 1000 m / min at 295 ° C. using a mold having 36 round spherical balls having a diameter of 0.25 mm. The obtained undrawn yarn was drawn at a drawing speed of 1070 m / min by a heating roller maintained at 80 ° C. and a hot plate kept at 120 ° C. to prepare a drawn yarn of 75 d / f, and the physical properties thereof were summarized in Table-1.

(실시예 2∼3, 및 비교예 l∼3)(Examples 2-3 and Comparative Examples l-3)

공중합성분의 조성을 표 1과 같이 한 것외에는 실시예 1과 동일한 방법으로 실시하고 그 물성을 평가하였다.Except having made the composition of the copolymer component as Table 1, it carried out by the same method as Example 1, and evaluated the physical property.

[표1]Table 1

Claims (4)

폴리에스터에 공중합 성분을 첨가 중합하여 제전성을 부여함에 있어서, 공중합 성분으로 폴리옥시알킬렌글리콜 화합물 및 비반응성 알킬술폰산리튬염과 함께 비반응성 리튬아미드를 사용하는 것을 특징으로 하는 폴리에스터 제전사의 제조방법.In adding and copolymerizing a copolymerization component to polyester to impart antistaticity, a non-reactive lithium amide is used as a copolymerization component together with a polyoxyalkylene glycol compound and a non-reactive alkyl sulfonate lithium salt. Manufacturing method. 제1항에 있어서, 상기 비반응성 리튬아미드가 LiNH2, [(CH3)3Si2NLi, (C6Hl1)2NLi, [(CH3)2CH]2NLi 중에서 선택된 적어도 일종이고 함량이 폴리에스터 대비 0.001∼1중량%임을 특징으로 하는 폴리에스터의 제전사의 제조방법.The method of claim 1, wherein the non-reactive lithium amide is at least one selected from LiNH 2 , [(CH 3 ) 3 Si 2 NLi, (C 6 H 1 ) 2 NLi, [(CH 3 ) 2 CH] 2 NLi A method for producing a positive woven yarn of polyester, characterized in that 0.001 to 1% by weight relative to the polyester. 제1항에 있어서, 상기 폴리옥시알킬렌글리콜 화합물이 수평균분자량이 2,000 이상 30,000 이하인 하기 일반식(I)의 화합물이고 폴리에스터 전량 대비 0.01∼35중량%로 첨가하는 것을 특징으로 하는 폴리에스터제전사의 제조방법.The polyester agent according to claim 1, wherein the polyoxyalkylene glycol compound is a compound of formula (I) having a number average molecular weight of 2,000 or more and 30,000 or less and added at 0.01 to 35% by weight relative to the total amount of polyester. Method of Making a Transcription. (상기에서, Rl: C1∼C13인 알킬기 또는 H, R2: C2∼C|16인 알킬렌기, n : 20∼150의 정수)(Wherein, R l: C 1 ~C 13 alkyl group or H, R 2: C 2 ~C | 16 alkyl group, n: an integer of 20-150) 제1항에 있어서, 상기 비반응성 알킬술폰산리튬염이 하기 일반식(II)의 비반응성 폴리알킬술폰산리튬이고 폴리에스터 정량 대비 0.0l∼2중량%로 첨가함을 특징으로 하는 폴리에스터 제전사의 제조방법.The method of claim 1, wherein the non-reactive lithium lithium sulfonate salt is a non-reactive lithium polyalkyl sulfonate of the general formula (II) is added to the polyester quantitative agent of 0.01 to 2% by weight based on the amount of polyester Manufacturing method. (상기에서, R3: C3∼C25인 알킬기 또는 C7∼C30인 아릴기)(Wherein, R 3: C 3 ~C 25 alkyl group or C 7 ~C 30 aryl group)
KR1019920015268A 1992-08-25 1992-08-25 Process for preparing antistatic electricity polyester fiber KR970010721B1 (en)

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