KR970010720B1 - Super high speed spinning process for polyester fiber - Google Patents
Super high speed spinning process for polyester fiber Download PDFInfo
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- KR970010720B1 KR970010720B1 KR1019900022702A KR900022702A KR970010720B1 KR 970010720 B1 KR970010720 B1 KR 970010720B1 KR 1019900022702 A KR1019900022702 A KR 1019900022702A KR 900022702 A KR900022702 A KR 900022702A KR 970010720 B1 KR970010720 B1 KR 970010720B1
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- polyester fiber
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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
- 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
Abstract
Description
본 발명은, 폴리에스터의 초고속 방사방법에 관한 것으로서, 더욱 상세하게는 폴리에스터를 5,000m/분 이상의 권취속도로 초고속방사할 때, 개질된 폴리에스터를 사용하여 사절발생을 극소화 시킬 수 있는 방법에 관한 것이다.The present invention relates to an ultrafast spinning method of polyester, and more particularly, to a method capable of minimizing trimming by using a modified polyester when ultrafast spinning of polyester at a winding speed of 5,000 m / min or more. It is about.
폴리에틸렌 테레프탈레이트로 대표되는 폴리에스터는 우수한 물리, 화학적 성질을 가지고 있기 때문에 여러가지 용도, 특히 섬유로 널리 사용되고 있다. 폴리에스터 섬유는 통상, 용융방사, 연신 열세팅하는 방법으로 제조되고 있다.Polyesters, represented by polyethylene terephthalate, have excellent physical and chemical properties and are widely used for various applications, especially fibers. Polyester fiber is normally manufactured by the method of melt spinning and extending | stretching heat setting.
근년에 들어서는 제사기술이 진보됨에 따라 용융방사시의 권취속도는 종래의 1,000∼1, 500m/분에서 2,500∼4,000m/분 정도로 대폭 증가시킬 수 있게 되었다.In recent years, as the spinning technology has been advanced, the winding speed during melt spinning can be greatly increased from 1,000 to 1,500 m / min to 2,500 to 4,000 m / min.
특히 권취속도를 2,500∼4,000m/분으로 하여 제조한 부분배향미 연신사는 그대로 연신, 가연 공정에 제공되고 있으며, 그 용도는 계속 크게 증가하여 제사기술의 주류를 이루고 있다.Particularly oriented rice drawn yarn manufactured at a winding speed of 2,500 to 4,000 m / min is provided to the drawing and burning process as it is, and its use continues to increase greatly to become the mainstream of the spinning technology.
한편, 최근에는 권취속도를 5,000m/분 이상으로 하는 초고속방사가 시험되고 있는데, 이러한 초고속 방사에서는, 방사시의 사절이 많이 발생하고, 최종제품사의 강도가 현저하게 저하된다고 하는 결점이 있다. 이와 같은 결점을 해소하기 위하여, 방사조건(예를 들면, 방사온도, 냉각풍량, 냉각풍 온도 등)의 적정화 및 방사통과 방사노즐의 구조개량 등을 시험하고 있지만 이러한 방법으로는 한계가 있고, 대폭적인 개선은 기대할 수없다.On the other hand, in recent years, ultra-fast spinning with a winding speed of 5,000 m / min or more has been tested, but in such high-speed spinning, there is a drawback that a large number of trimmings occur during spinning, and the strength of the final product yarn is significantly reduced. In order to solve the above-mentioned drawbacks, we have tested the optimization of spinning conditions (e.g., spinning temperature, cooling air volume, cooling wind temperature, etc.) and structural improvement of spinning barrels and spinning nozzles. No improvement can be expected.
본 발명자들이 상기와 같은 문제점의 원인에 대하여 검토 실험한 결과, 폴리에스터가 폴리에틸렌이나 폴리아마이드 등에비하여 결정화되기 어려운 성질을 가지고 있기는 하지만, 용융방사시의 권취속도가 3, 500m/분 이상이 되면 방사장력에 의하여 분자배향이 일어나고, 이것과 함께 결정화가 일어나기 때문에 그 결과 방출사의 배향이 충분치 않음에도 불구하고 결정화가 크게 진행되어 앞서 말한 문제점이 발생하게 되는 것이고, 이와 같은 경향은 권취속도가 5,000m/분 이상으로 되면 더욱 현저하게 된다는 것을 알아냈다.As a result of examining and examining the causes of the problems described above, the inventors of the present invention show that polyester has a property that is difficult to crystallize compared to polyethylene, polyamide, and the like. Molecular orientation is caused by the radial tension, and crystallization occurs with this, and as a result, the crystallization proceeds largely despite the insufficient orientation of the emitter, and the above-mentioned problem occurs, and the winding speed is 5,000 m. It was found out that more than / min becomes more remarkable.
이와 같은 사실을 기초로 하여 고속방사시에 있어서, 고배향이고 저결정화로 되는 폴리에스터에 관하여 그 결정화 및 분자배향의 거동면에서 계속 검토를 하고, 분자배향시의 결정화를 억제시킬 수 있는 방법에 관하여 연구한 결과, 폴리에스터의 제조중에 특정의 화합물을 첨가, 공중합시키면 현저한 효과가 있다는 사실을 알게 되어 본 발명에 도달한 것이다.Based on these facts, polyesters that are highly oriented and low crystallized in high-speed spinning are continuously examined in terms of their crystallization and molecular orientation behavior, and a method for suppressing crystallization during molecular orientation is proposed. As a result of research, it has been found that the addition and copolymerization of a specific compound during the preparation of the polyester has a remarkable effect and the present invention has been reached.
즉, 본 발명은 주된 반복구조단위가 에틸렌 테레프탈레이트인 폴리에스터를 적어도 5,000m/분 이상의 권취속도로 용융방사하여 폴리에스터 필라멘트사를 제조함에 있어서, 폴리에스터 폴리머의 중합반응이 완결되기 이전의 임의의 단계에서 아래의 일반식(I)으로 표시되는 화합물을 폴리에스터를 구성하는 산 성분에 대하여 0.5∼2.9몰% 첨가, 반응시켜 제조한 폴리에스터를 사용하는 것을 특징으로 하는 폴리에스터의 초고속 방사 방법에 관한 것이다.That is, in the present invention, the polyester filament yarn is melt spun at a winding speed of at least 5,000 m / min or more of polyester whose main repeating unit is ethylene terephthalate, and thus, before the polymerization reaction of the polyester polymer is completed. Ultrafast spinning method of polyester, characterized by using a polyester prepared by adding and reacting the compound represented by the general formula (I) below 0.5 to 2.9 mol% with respect to the acid component constituting the polyester in the step of It is about.
아래bottom
(단, R1은 탄소수가 2∼4인 2가의 지방족기)(Wherein R 1 is a divalent aliphatic group having 2 to 4 carbon atoms)
본 발명에 있어서 상기 일반식으로 표시되는 화합물의 첨가시기는 특별히 한정되는 것은 아니지만, 에스테르화 혹은 에스테르 교환 반응이 실질적으로 개시되는 시점으로부터 중축합 반응이 시작되기 직전까지의 단계에서 첨가하는 것이 공정상 편리하다.Although the addition time of the compound represented by the said general formula in this invention is not specifically limited, It is process process to add in the stage from the time from which a esterification or transesterification reaction is actually started just before starting a polycondensation reaction. It is convenient.
또한 이들의 첨가량이 너무 적으면, 본 발명에서 말하는 분자배향시의 결정화 억제효과가 얻어지지 않고, 반대로 너무 많게 되면, 얻어지는 폴리에스터의 연화점이 낮아지고, 색상이 악화되기 때문에 폴리에스터의 제조시에 사용되는 디카르복실산에 대하여 0.5∼2.9몰%의 범위로 하는 것이 좋다.If the addition amount is too small, the crystallization inhibiting effect at the time of molecular orientation according to the present invention is not obtained. On the contrary, if the amount is too high, the softening point of the obtained polyester is lowered and the color is deteriorated. It is good to set it as the range of 0.5-2.9 mol% with respect to the dicarboxylic acid used.
그리고 이러한 폴리에스터의 제조방법으로는 통상 테레프탈산을 에틸렌글리콜로 에스테르화 시키거나, 디메틸 테레프탈레이트를 에틸렌글리콜로 에스테르 교환시키거나, 혹은 테레프탈산과 에틸렌옥사이드를 반응시켜, 테레프탈산의 글리콜 에스테르 및/또는 그 저중합체를 얻고, 이것을 감압하에서 교반 및 가열하여 중축합 반응시키는 공지의 방법을 사용하면 된다.In the polyester production method, terephthalic acid is usually esterified with ethylene glycol, dimethyl terephthalate is transesterified with ethylene glycol, or terephthalic acid and ethylene oxide are reacted to form a glycol ester of terephthalic acid and / or its low. What is necessary is just to use a well-known method of obtaining a polymer, stirring and heating this under reduced pressure and carrying out polycondensation reaction.
본 발명에서의 폴리에스터로는 테레프탈산 성분과 에틸렌글리콜 성분을 사용하는 폴리에틸렌 테레프탈레이트를 주된 대상으로 하지만, 폴리에스터의 물성개량을 위하여, 각종의 첨가제, 예를 들면 산화티탄과 같은 소염제, 이염제, 난연제, 제전제, 친수제, 착색제, 안정제 등을 소량 함유하고 있는 폴리에스터이어도 좋다.The polyester in the present invention is mainly a polyethylene terephthalate using a terephthalic acid component and an ethylene glycol component, but for improving physical properties of the polyester, various additives, for example, an anti-inflammatory agent such as titanium oxide, a dyeing agent, The polyester may contain a small amount of a flame retardant, an antistatic agent, a hydrophilic agent, a colorant, a stabilizer and the like.
본 발명에 의하면, 방사속도가 5,000m/분 이상인 초고속방사시의 방사공정중에 다발하는 사절이 현저하게 감소되어 공정이 안정화되고, 생산성이 크게 향상된다.According to the present invention, the trimming bundles during the spinning process during the ultra-fast spinning having a spinning speed of 5,000 m / min or more is remarkably reduced, so that the process is stabilized and productivity is greatly improved.
(실시예 1∼3 및 비교예 1∼2)(Examples 1-3 and Comparative Examples 1-2)
일반식(I)의 R1이 에틸렌기인 화합물(A)을 표 1과 같은 비율로 함유하는 폴리에스터(극한점도 0.61∼0.63)을 방사온도 285℃, 토출량 42.5g/분으로 방사노즐을 통하여 토출하고, 15℃의 공기를 0.5m/분의 풍속으로 불어주어 냉각시킨 후 집속 및 유제부여를 한 다음 6,000m/분의 속도로 권취하였으며, 이때의 사절 발생율을 표 1에 나타냈다.A polyester (intrinsic viscosity of 0.61 to 0.63) containing a compound (A) in which R 1 in formula (I) is an ethylene group at the same ratio as in Table 1 was discharged through a spinning nozzle at a spinning temperature of 285 ° C. and a discharge amount of 42.5 g / min. Then, the air at 15 ° C. was blown at a wind speed of 0.5 m / min, cooled, concentrated and emulsified, and then wound up at a rate of 6,000 m / min, and the incidence rate of trimming was shown in Table 1.
[표1]Table 1
*) 사절율 계산은 1,000시간을 기준으로 하여 총 도핑수(333번)에 대한 사절발생 도핑수의 백분율임.*) The trimming rate calculation is a percentage of the number of trimming dopings to the total number of dopings (333) based on 1,000 hours.
*) FB%는 단위시간에 생산되는 무사절 도핑수의 백분율임.*) FB% is the percentage of free doping produced in unit time.
*) 비교예 2의 경우 폴리에스터의 색상이 악화되고(b치 증가) 융점의 저하가 커서 실용화 할수 없음.*) In the case of Comparative Example 2, the color of polyester deteriorated (b value increased) and the melting point decreased so that it could not be put to practical use.
(실시예 4, 5 및 비교예 3)(Examples 4 and 5 and Comparative Example 3)
화합물 A 대신에 일반식(I)의 R1이 테트라메틸렌기인 화합물(B)를 함유하는 폴리에스터(극한점도 0.56~0.60)를 사용한 것 외에는 실시예 1과 모두 같은 조건으로 방사 및 연신을 하였으며, 그 결과는 표 2와 같다.Instead of compound A, spinning and stretching were carried out under the same conditions as in Example 1, except that polyester (intrinsic viscosity of 0.56 to 0.60) containing compound (B) in which R 1 of formula (I) was tetramethylene group was used. The results are shown in Table 2.
[표2][Table 2]
(실시예 6, 7 및 비교예 4)(Examples 6 and 7 and Comparative Example 4)
표 3와 같이 화합물 A를 함유하는 폴리에스터(극한점도 0.62∼0.64)를 방사온도 285℃, 토출량 42.5g/분으로 방사노즐을 통하여 토출하고, 15℃의 공기를 0.5m/분의 풍속으로 불어주어 냉각시킨 후 집속 및 유제부여를 한 다음 7,000m/분의 속도로 권취하였다. 이때의 사질 발생율을 표 3에 나타냈다.As shown in Table 3, the polyester containing the compound A (intrinsic viscosity 0.62 to 0.64) was discharged through the spinning nozzle at a spinning temperature of 285 ° C. and discharged at 42.5 g / min, and the air at 15 ° C. was blown at a wind speed of 0.5 m / min. After cooling, the solution was concentrated and emulsified, and then wound up at a speed of 7,000 m / min. The incidence of sand quality at this time is shown in Table 3.
[표3]Table 3
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