KR960011592B1 - Anti-static polyester fiber - Google Patents
Anti-static polyester fiber Download PDFInfo
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- KR960011592B1 KR960011592B1 KR1019940015244A KR19940015244A KR960011592B1 KR 960011592 B1 KR960011592 B1 KR 960011592B1 KR 1019940015244 A KR1019940015244 A KR 1019940015244A KR 19940015244 A KR19940015244 A KR 19940015244A KR 960011592 B1 KR960011592 B1 KR 960011592B1
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- 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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
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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
- D01F1/10—Other agents for modifying properties
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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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)
- Multicomponent Fibers (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
Description
첨부된 도면은 본 발명 시스-코아 복합섬유의 단면개략도.The accompanying drawings are schematic cross-sectional views of the present invention cis-core composite fiber.
* 도면의 주요부분에 대한 부호의 설명* Explanation of symbols for main parts of the drawings
S : 시스부분 C : 코아부분S: Sheath C: Core
본 발명은 제전성 폴리에스테르 섬유에 관한 것으로, 더욱 상세하게는 흡습성 물질인 폴리에틸렌글리콜을 공중합시킨 시스(sheath)용 폴리에스테르 중합체와, 이온성 물질인 인산에스테르염을 공중합시킨 코아(core)용 폴리에스테르 중합체로 이루어진 제전성 폴리에스테르 섬유에 관한 것이다.The present invention relates to an antistatic polyester fiber, more specifically, a sheath polyester copolymerized with polyethylene glycol, a hygroscopic material. The present invention relates to an antistatic polyester fiber composed of a polyester polymer for cores obtained by copolymerizing a polymer and a phosphate ester salt which is an ionic substance.
현재 널리 사용되고 있는 폴리에스테르 제전사의 제조원리는 다음과 같다.Principles of manufacture of polyester electrostatic yarn currently widely used are as follows.
첫째, 폴리에틸렌글리콜과 같은 흡습성 물질을 첨가하여 섬유의 평형 수분율을 올리는 방법, 둘째, 저분자량의 이온성 물질을 첨가하여 발생된 정전기를 누설시키는 방법.First, the method of raising the equilibrium moisture content of the fiber by adding a hygroscopic material such as polyethylene glycol, and second, the static electricity generated by adding the low molecular weight ionic material. How to leak.
예를 들면 상기 첫째 방법으로는 일본 특공소 39-5214호, 44-31828호 등이 있고, 첫째 및 둘째방법을 조합한 방법으로서 일본 특공소 47-11280, 47-10246호 등이 있다.For example, as the first method, there are Japanese special public offices 39-5214, 44-31828, etc., and the Japanese special public office as a method combining the first and second methods. 47-11280, 47-10246, etc.
그러나 이들 방법은 제전제의 함량이 높아야 충분한 제전성을 발휘하며 염가공에서 폴리에틸렌글리콜이 빠져 나오는 단점을 안고 있다.However, these methods have a high content of an antistatic agent to exhibit sufficient antistatic properties and have a disadvantage in that polyethylene glycol is released from salt processing.
또한, 제사공정이 불량한 단점을 안고 있다.In addition, the sacrificial process has a disadvantage.
이에 본 발명에서는 염가공공정이나 사용도중 제전제가 섬유로부터 빠져나오는 것을 방지하기 위하여 폴리에틸렌글리콜을 시스용 폴리에스테르 중합체 주쇄중에 공중합시키고, 이온성 물질을 코아용 폴리에스테르 중합체만 첨가하여 제전성 및 내구성이 우수한 폴리에스테르 섬유를 제조하였다.Accordingly, in the present invention, polyethylene glycol is added to the polyester polymer main chain for the sheath in order to prevent the antistatic agent from escaping from the fiber during the salt processing process or during use. The polyester fiber was copolymerized and only the polyester polymer for core was added to prepare polyester fiber having excellent antistatic property and durability.
이하, 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.
본 발명은 폴리에스테르 시스(sheath)-코아(core) 복합섬유에 있어서, 디올과 디카르본산 또는 이의 에스테르 화합물로부터 생성되는 폴리에스테르 중합공정의 에스테르화 교환반응 중에 평균분자량 400∼4,000의 폴리에틸렌글리콜을 3∼10중량%를 투입하여 공중합시켜 제조된 시스용 공중합체(S)와, 디올과 디카르본산 또는 이의 에스테르 화합물로부터 생성되는 폴리에스테르 중합공정의 중축합 반응 중에 다음 식(Ⅰ)로 표시되는 저분자량의 인산에스테르염을 0.5∼2중량% 투입하여 제조된 코아용 공중합체(C)로 이루어진 것을 특징으로 하는 제전성 폴리에스테르 섬유이다.The present invention is a polyester sheath-core (core) composite fiber, polyester produced from diol and dicarboxylic acid or ester compounds thereof Sheath copolymer (S) prepared by incorporating 3 to 10% by weight of polyethylene glycol having an average molecular weight of 400 to 4,000 in the esterification exchange reaction of the polymerization step, The low molecular weight phosphate ester salt represented by the following formula (I) during the polycondensation reaction of the polyester polymerization step produced from diol and dicarboxylic acid or ester compound thereof An antistatic polyester fiber comprising a copolymer for core (C) prepared by adding 0.5 to 2% by weight.
CmH2m+1-O-(CH2CH2O)n-PO3Na2(Ⅰ)C m H 2m + 1 -O- (CH 2 CH 2 O) n -PO 3 Na 2 (Ⅰ)
상기 식에서 m은 1∼9의 정수, n은 1∼10의 정수이다.In said formula, m is an integer of 1-9, n is an integer of 1-10.
이하, 본 발명을 더욱 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in more detail.
본 발명에서 시스용 중합체의 중합공정의 에스테르교환반응 중에 첨가되는 폴리에틸렌글리콜의 분자량이 400미만이면 반응도중 휘발되기 쉽고, 4,000을 초과하면 반응성이 불량해진다.In the present invention, when the molecular weight of the polyethylene glycol added during the transesterification reaction of the polymer for the sheath is less than 400, it is liable to volatilize during the reaction. If exceeded, the reactivity becomes poor.
또한, 그 첨가량은 3중량% 미만이면 제전성이 부족해지고, 10중량%를 초과하면 방사공정이 불량해진다.If the added amount is less than 3% by weight, the antistatic property is insufficient, and if it exceeds 10% by weight, the spinning process is poor.
코아용 중합체의 중합공정의 중축합 반응중에 첨가되는 인산에스테르염은 그 첨가량이 0.5중량% 미만이면 효과가 없고, 2중량%를 초과하면 염색성등이 불량해진다.Phosphate ester salt added during the polycondensation reaction in the polymerization process of the core polymer has no effect when the addition amount is less than 0.5% by weight, and when it exceeds 2% by weight, the dyeability, etc. It becomes bad.
본 발명에서 시스 및 코아용 중합체를 사용하여 시스-코아 복합방사를 할 때 시스중합체와 코아중합체의 용융점도를 비슷하게 맞추어야 제사성이 양호하며, 또한 그들의 면적비도 균형을 이루어야 제사성이 좋아진다.In the present invention, when the cis-core composite spinning using the cis and core polymers, the melt viscosity of the cis polymer and the core polymer should be similarly adjusted, and the sacrificial property is good. Their area ratio must also be balanced to improve sacrificiality.
대개 폴리에틸렌글리콜이 함유된 중합체가 그렇지 않은 것보다 동일한 고유점도에서 용융점도가 낮다. 본 발명에서는 시스와 코아의 고유점도 차이가 0.03∼0.05일 때와 면적비 40 : 60∼60 : 40일 때 제사공정성이 가장 좋았다.Usually, polymers containing polyethyleneglycol have lower melt viscosity at the same intrinsic viscosity than they do not. In the present invention, the difference in intrinsic viscosity of the sheath and core The sacrificial processability was the best when the ratio was 0.03 to 0.05 and the area ratio was 40:60 to 60:40.
이와 같이 하여 제조된 본 발명의 섬유는 일반 안감용이나 여성용 블라우스, 드레스 및 자동차용 시트 등에 사용 가능하다.The fiber of the present invention prepared in this way can be used for general lining, women's blouse, dress and car seat.
이하, 본 발명을 실시예를 통하여 더욱 구체적으로 설명하겠는바, 본 발명이 실시예에 의해 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited by Examples.
실시예 및 비교예에서 부는 중량부를 의미한다.In Examples and Comparative Examples, parts means parts by weight.
[실시예 1]Example 1
(A) 시스부 중합체 제조 :(A) Cisbu Polymer Preparation:
디메틸테레프탈산 100부, 에틸렌글리콜 60부, 평균분자량 1,000의 폴리에틸렌글리콜 4부 및 초산아세테이트 0.03부를 응축기가 부착된 반응기에 넣고 2시간에 걸쳐 250℃까지 승온시키면서 메탄올을 완전히 유출시켜 에스테르 교환반응을 시킨다. 에스테르 교환반응이 종료되면 인산 0.01부, 이산화티탄 0.4부, 삼산화안티몬 0.035부를 넣고 10분간 더 교반한 후, 저진공 반응 20분 후 285℃에서 1mmHg이하의 고진공 반응을 1시간 30분 시킨 후 고유점도 0.67의 칩을 제조하였다.100 parts of dimethyl terephthalic acid, 60 parts of ethylene glycol, 4 parts of polyethylene glycol having an average molecular weight of 1,000 and 0.03 parts of acetate acetate were placed in a reactor equipped with a condenser. Methanol was completely distilled off while heating up to 250 degreeC over 2 hours, and it transesterified. 0.01 parts of phosphoric acid and titanium dioxide after transesterification 0.4 parts and 0.035 parts of antimony trioxide were added and stirred for 10 minutes. After 20 minutes of low vacuum reaction, a high vacuum reaction of 1 mmHg or less was performed at 285 ° C. for 1 hour and 30 minutes. After making a chip having an intrinsic viscosity of 0.67.
(B) 코아부 중합체 제조 :(B) Coabu polymer preparation:
디메틸테레프탈산 100부, 에틸렌글리콜 60부, 초산아세테이트 0.03부를 응축기가 부착된 반응기에 넣고 2시간에 걸쳐 250℃까지 승온시키면서 메탄올을 완전히 유출시켜 에스테르 교환반응을 시킨다. 에스테르 교환반응이 종료되면 인산 0.01부, 이산화티탄 0.4부, 삼산화안티몬 0.035부를 넣고 10분간 더 교반한 후, 저진공반응을 20분 시키고 285℃에서 1mmHg이하의 고진공 반응을 1시간 30분 시킨 다음, 진공을 파기한 후 상기 식(Ⅰ)중 m=8, n=4인 인산에스테르염 2부를 넣고 다시 진공을 걸어 1시간 더 반응을 시켜 고유점도 0.63의 칩을 제조하였다.100 parts of dimethyl terephthalic acid, 60 parts of ethylene glycol, and 0.03 parts of acetate acetate were placed in a reactor equipped with a condenser, and methanol was heated to 250 ° C. over 2 hours. Completely distillate to undergo transesterification. When the transesterification reaction is completed, add 0.01 part phosphoric acid, 0.4 part titanium dioxide, and 0.035 part antimony trioxide. After further stirring for 10 minutes, the low vacuum reaction was performed for 20 minutes, and the high vacuum reaction of 1 mmHg or less was performed for 1 hour and 30 minutes at 285 ° C. In the formula (I), 2 parts of phosphate ester salts having m = 8 and n = 4 were added and subjected to vacuum again for further 1 hour to prepare chips having an intrinsic viscosity of 0.63.
이렇게 하여 얻어진 중합체를 각각 진공 건조한 후 시스-코아 복합방사기를 사용하여 시스와 코아의 면적비가 동일하도록 토출량을 조절하여 방사온도 285℃, 권취속도 1,100m/분, 24홀 노즐을 사용하여 방사한 후, 연산속도 900m/분으로 3.1배 연신하여 75데니어 24홀의 연신사를 얻었다.The polymer thus obtained was vacuum dried, and then the discharge amount was adjusted such that the area ratio of the sheath and the core was the same by using a cis-core composite spinning machine, so that the spinning temperature was 285 ° C., After spinning with a winding speed of 1,100 m / min and a 24-hole nozzle, the film was stretched 3.1 times at a calculation speed of 900 m / min to obtain a 75 denier 24-hole stretch yarn.
[비교예 1∼2][Comparative Examples 1 and 2]
시스, 코아부분의 중합체는 실시예 1과 동일하거나 면적비만 달리하여 제사하였고 그 조건 및 결과를 다음 표 1에 나타내었다.The polymer of cis and core part was prepared by the same or different area ratios as in Example 1, and the conditions and results are shown in Table 1 below.
[비교예 3∼4]Comparative Examples 3 to 4
코아부분의 중합체는 실시예 1과 동일하되 고유점도를 달리하여 중합하였다. 제사는 실시예 1과 동일한 조건으로 하였고, 그 조건 및 결과를 다음 표 1에 나타내었다.The polymer of the core portion was the same as in Example 1, but was polymerized with different intrinsic viscosity. The ritual was made under the same conditions as in Example 1, and the conditions and results are shown in Table 1 below. Indicated.
[비교예 5][Comparative Example 5]
실시예 1에서 시스와 코아의 중합체를 서로 바꿔 발사하였고, 그 결과를 다음 표 2에 나타내었다.In Example 1, the polymer of cis and core was fired interchangeably, and the results are shown in Table 2 below.
[비교예 6]Comparative Example 6
디메틸테레프탈산 100부, 에틸렌글리콜 60부, 평균분자량 1,000의 폴리에틸렌글리콜 4부 및 초산아세테이트 0.03부를 응축기가 부착된 반응기에 넣고 2시간에 걸쳐 250℃까지 승온시키면서 메탄올을 완전히 유출시켜 에스테르 교환반응을 시켰다.100 parts of dimethyl terephthalic acid, 60 parts of ethylene glycol, 4 parts of polyethylene glycol having an average molecular weight of 1,000 and 0.03 parts of acetate acetate were placed in a reactor equipped with a condenser. Methanol was completely distilled off while heating up to 250 degreeC over 2 hours, and it transesterified.
에스테르 교환반응이 종료되면 인산 0.01부, 이산화티탄 0.4부, 삼산화안티몬 0.035부를 넣고 10분간 더 교반한 후, 저진공 반응을 20분 시키고 285℃에서 1mmHg이하의 고진공 반응을 1시간 30분 시킨후, 진공을 파기하고 인산에스테르염 2부를 넣고 다음 다시 진공을 걸어 1시간 더 반응을 시켜 고유점도 0.63대의 칩을 제조하였다.When the transesterification reaction was completed, 0.01 parts of phosphoric acid, 0.4 parts of titanium dioxide, 0.035 parts of antimony trioxide were added thereto, and the mixture was stirred for 10 minutes. After a high vacuum reaction of 1 mmHg or less at 285 ° C. for 1 hour and 30 minutes, the vacuum was broken and 2 parts of phosphate ester salts were added, followed by vacuum again for 1 hour. To make 0.63 inherent viscosity chips.
제사는 복합방사가 아닌 일반 방사법을 사용하였고 그 결과를 다음 표 2에 나타내었다.The ritual used the general spinning method, not the complex spinning, and the results are shown in Table 2 below.
상기 표 1 및 표 2에서 마찰대전압의 측정은 다음의 방법으로 하였다.In Table 1 and Table 2, the measurement of the friction band voltage was made by the following method.
[마찰대전압 측정][Frictional belt voltage measurement]
연신사를 2합하여 제편기에서 제편한 후, 회전식 마찰대전압 측정기를 사용하여 20℃, 43% RH에서 마찰대전압을 측정하였다.After combining two stretched yarns and knitting them in a knitting machine, the frictional zone voltage was measured at 20 ° C. and 43% RH using a rotary frictional zone voltage meter.
제전성 내구성 평가는 50회 세탁후 마찰대전압을 비교하였다.Antistatic durability evaluation was compared with the friction voltage after 50 washes.
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KR1019940015244A KR960011592B1 (en) | 1994-06-29 | 1994-06-29 | Anti-static polyester fiber |
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KR1019940015244A KR960011592B1 (en) | 1994-06-29 | 1994-06-29 | Anti-static polyester fiber |
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KR960011592B1 true KR960011592B1 (en) | 1996-08-24 |
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1994
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