KR0160478B1 - Process for preparing polyester - Google Patents
Process for preparing polyester Download PDFInfo
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- KR0160478B1 KR0160478B1 KR1019900008868A KR900008868A KR0160478B1 KR 0160478 B1 KR0160478 B1 KR 0160478B1 KR 1019900008868 A KR1019900008868 A KR 1019900008868A KR 900008868 A KR900008868 A KR 900008868A KR 0160478 B1 KR0160478 B1 KR 0160478B1
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- polyester
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- speed
- ester
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/19—Hydroxy compounds containing aromatic rings
- C08G63/191—Hydroquinones
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Polyesters Or Polycarbonates (AREA)
- Artificial Filaments (AREA)
Abstract
내용없음.None.
Description
본 발명은 폴이에스터의 제조방법에 관한 것으로, 특히 폴리에스테의 분자 배향시 과도한 결정화를 억제시킬 수 있는 방법에 관한 것이다.The present invention relates to a method for producing polyester, and more particularly, to a method capable of suppressing excessive crystallization during molecular orientation of polyester.
폴리에틸렌테레프탈레이트로 대표되는 폴리에스터는 우수한 물리, 화학적 성질을 가지고 있기 때문에, 여러가지 용도, 특히 섬유로 널리 사용되고 있다. 폴리에스터 섬유는통상적으로 용융방사, 연신, 열세틸하는 방법으로 제조되고 있다. 근년에 들어서는제사 기술이 진보됨에 따라 용융방사시의 권취속도는 종래의 1000-1500m/분에서 2000m/분 이상으로 대폭 증가시키는 것이 가능하게 되었다. 특히 권취속도를 2500~4000m/분으로 하여 얻어진 부분배향 미연신사는 그대로 연신, 가연 공정에 제공되고 있으며, 이 용도는 계속 크게 증가하여 제사 기술의 주류를 이루고 있다.Polyesters typified by polyethylene terephthalate have excellent physical and chemical properties, and therefore are widely used for various applications, especially fibers. Polyester fibers are usually produced by melt spinning, stretching, and hot cetyl. In recent years, with the advance of the manufacturing technology, it is possible to greatly increase the winding speed during melt spinning from the conventional 1000-1500 m / min to 2000 m / min or more. Particularly oriented unstretched yarn obtained at a winding speed of 2500 to 4000 m / min is provided to the stretching and combusting process as it is, and its use continues to increase greatly to become the mainstream of the spinning technology.
한편, 권취속도를 4000m/분 이상으로 하는 초고속방사도 시험되고 있는데, 이러한 초고속 방사에서는 방사시의 사절이 다발하게 되고 최종 제품사의 강도가 현저하게 저하된다고 하는 결점이 있다. 이와 같은 결점을 해소하기 위해서, 방사조건(예를 들면, 방사온도, 냉각풍량, 냉각풍 온도 등)의 적정화 및 방사통과 방사 노즐의 구조개량들을 시험하고 있지만, 이러한 방법으로는 한계가 있고 대폭적인 개선은 기대할 수 없다.On the other hand, ultra-fast spinning with a winding speed of 4000 m / min or more has also been tested, but such high-speed spinning has a drawback in that the thread during spinning is more frequent and the strength of the final product yarn is significantly lowered. In order to overcome this drawback, we are testing the optimization of spinning conditions (e.g., spinning temperature, cooling air volume, cooling wind temperature, etc.) and structural improvements of spinning barrels and spinning nozzles, but these methods are limited and extensive. No improvement can be expected.
본 발명자들이 상기와 같은 문제점의 원인에 대하여 검토를 반복한 결과, 폴리에스터가 폴리에틸렌이나 폴리아미드 등에 비하여 결정화되기 어려운 성질을 가지고 있기는 하지만, 용융방사시의 권취속도가 2000m/분 이상으로 되면 방사장력에 의하여 분자배향이 일어나고, 이것과 함께 결정화가 일어나게 되므로, 방출사의배향이 충분하지 않음에도 불구하고 결정화가 크게 진행되어 앞서 말한 문제점이 발생하게 되는데, 이와 같은 경향은 권취속도가 4000m/분 이상으로 되면 더욱 현저하게 된다는 것을 알아냈다.As a result of repeating the investigation by the present inventors about the cause of the above problem, although polyester has a property which is hard to crystallize compared with polyethylene, a polyamide, etc., when the winding speed at the time of melt spinning becomes 2000 m / min or more, it radiates Molecular orientation occurs due to tension, and crystallization occurs with this, and although crystallization of the emitter is not sufficient, the crystallization proceeds greatly, and the above-mentioned problem occurs, and the winding speed is more than 4000 m / min. It turned out that it became more remarkable.
이와 같은 사실로부터 고속방사시에 있어, 고배향이고, 저결정화로 되는 폴리에스터에 관하여 그결정화 및 분자배향의 거동면에서 계속 검토하고, 분자 배향시의 결정화를 억제시킬수 있는 각종 첨가제에 관하여 조사한 결과, 폴리에스터의 제조 등에 하이트로퀴논을 첨가하는 것에 의해 현저한 효과가 있음을 알아냈고 다음과 같은 본 발명에 도달한 것이다.From these facts, polyesters with high orientation and low crystallization in high-speed spinning are continuously examined in terms of their crystallization and molecular orientation behavior, and various additives capable of suppressing crystallization during molecular orientation are found. It has been found that the addition of a hytroquinone has a remarkable effect in the production of polyester and the like, and the present invention has been reached as follows.
본 발명은 주된 반복구조단위가 에틸렌테레프탈레이트인 폴리에스터를 제조함에 있어서, 중합반응이 완결되기 이전의 임으의 단계에서 하이드로퀴논 또는 그 에스테르 형서성 유도체를 폴리에스터를구성하는 산 성분에 대하여 0.2~2.0몰%첨가, 반응시키는 것을 특징으로 한다.In the present invention, in the preparation of a polyester whose main repeating unit is ethylene terephthalate, the hydroquinone or its ester form derivative is 0.2 to the acid component constituting the polyester at any stage before the polymerization reaction is completed. 2.0 mol% is added and made to react.
본 발명에 있어서 사용되는 하이드로퀴논의 에스테르 형성성 유도체의 예로는 파라디아세톡시벤젠이 사용 가능하다. 이러한 하이드로퀴논 또는 그 에스테르 형성서 유도체의 첨가시기는 특별히 한정된 것은 아니지만, 에스테르화 혹은 에스테르 교환 반응이 실질적으로 개시되는 시점으로부터 중축합 반응이 시작되기 직전까지의 단계에서 첨가하는 것이공정상 편리하다.Paradiacetoxybenzene can be used as an example of the ester-forming derivative of hydroquinone used in this invention. Although the addition time of such hydroquinone or its ester formation derivative is not specifically limited, It is convenient for process to add in the stage from the time when esterification or transesterification reaction is actually started until just before the polycondensation reaction starts.
또한 이들의첨가량이 너무 적으면, 본 발명에서 말하는 분자배향시의 결정화억제 효과가 얻어지지 않고, 반대로 너무 많게 되면, 얻어지는 폴리에스터의 연화점이 낮아지고, 색상이 악화되기 때문에 폴리에스터의 제조시 사용되는 디카르복실산에 대하여 0.2~2.0몰%의 범위로 하는 것이 좋다.In addition, when the addition amount is too small, the crystallization inhibitory effect in the molecular orientation referred to in the present invention is not obtained. On the contrary, when the addition amount is too high, the softening point of the polyester obtained is lowered and the color is deteriorated. It is good to set it as the range of 0.2-2.0 mol% with respect to dicarboxylic acid used.
본 발명에서 말하는 폴리에스터로는 테레프탈산 성분과에틸렌글리콜 성분을 사용하는 폴리에틸렌테레프탈레이트를 주된 대상으로 하지만, 폴리에스터의 물성개량을 위하여, 디카르복실산 성분 또는 클리콜 성분의 일부(통산 15몰% 이하)를 다른 성분으로 치환시킨 폴리에스터라도 좋다. 그리고 각종 첨가제, 예를 들면 산화티탄과 같은 소여제, 이염제, 난연제, 제전제, 친수제, 착색제, 안정제 등을 소량 함유하고 있는 폴리에스터이어도 좋다. 본 발명에 의하면, 방사속도가 3000m/분 이상인 고속 방사 및 연신 공정중에 다발하는 사절이 현저하게 감소되어 공정이 안정화되고, 생산성이 크게 향상된다.The polyester used in the present invention is mainly a polyethylene terephthalate using a terephthalic acid component and an ethylene glycol component, but a part of a dicarboxylic acid component or a glycol component (15 mol% in total) for improving physical properties of the polyester. The polyester which substituted the following) with another component may be sufficient. The polyester may contain various additives such as a scavenger such as titanium oxide, a dyeing agent, a flame retardant, an antistatic agent, a hydrophilic agent, a colorant and a stabilizer. According to the present invention, the thread trimming during the high-speed spinning and stretching process with a spinning speed of 3000 m / min or more is significantly reduced, so that the process is stabilized and productivity is greatly improved.
이하 실시예를 들어 본 발명을 더욱 상세히 설명하고자 한다.Hereinafter, the present invention will be described in more detail with reference to the following examples.
그러나 실시예에 의하여 본 발명이 한정되는 것은 아니며, 부는 중량부를 나타낸다.However, the present invention is not limited by the examples, and parts represent parts by weight.
[실시예 1-4, 비교예 1,2][Example 1-4, Comparative Examples 1,2]
표-1과 같이 하이드로퀴논 단위를 함유하는 폴리에스터(극한점도 0.64-0.66)를 방사온도 285℃, 토출량44.5g/분으로 방사노즐을 통하여 방출하고, 15℃의 공기를 0.5m/분의 풍소그로 불어주어 냉각시킨 후 집속 및 유제부여를 한 다음 4000m/분의 속도로 권취하여 미연신사를 얻고, 이것을 연신비 1.332로 연신하였다. 이때의 사절 발생률을 표-1에 나타냈다.As shown in Table-1, the polyester containing the hydroquinone unit (intrinsic viscosity 0.64-0.66) was discharged through the spinning nozzle at a spinning temperature of 285 ° C and discharged at 44.5 g / min, and air at 15 ° C was discharged at 0.5 m / min. After cooling by blowing, focusing and emulsification were carried out, and then wound at a speed of 4000 m / min to obtain an undrawn yarn, which was stretched to a draw ratio of 1.332. The incidence of trimming at this time is shown in Table-1.
[실시예 5-6, 비교예 3][Example 5-6, Comparative Example 3]
표-2와 같이 하이드로퀴논 단위를 함유하는 폴리에스터(극한점도 0.64-0.66)를 방사온도 285℃, 토출량 42.5g/분으로 방사노즐을 통하여 방출하고, 15℃의 공기를 0.5m/분의 풍속으로 불어주어 냉각시킨 후 집속 및 유제부여를 한 다음 6500m/분의 속도로 권취하였다. 이때의 사절 발생률을 표-2에 나타냈다.As shown in Table 2, the polyester containing the hydroquinone unit (intrinsic viscosity 0.64-0.66) was discharged through the spinning nozzle at a spinning temperature of 285 ° C and discharged at 42.5 g / minute, and air at 15 ° C was flowed at a speed of 0.5 m / min. After blowing to cool, focused and emulsified, then wound at a speed of 6500m / min. The incidence of trimming at this time is shown in Table-2.
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Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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KR1019900008868A KR0160478B1 (en) | 1990-06-16 | 1990-06-16 | Process for preparing polyester |
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Application Number | Priority Date | Filing Date | Title |
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KR1019900008868A KR0160478B1 (en) | 1990-06-16 | 1990-06-16 | Process for preparing polyester |
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KR920000826A KR920000826A (en) | 1992-01-29 |
KR0160478B1 true KR0160478B1 (en) | 1999-01-15 |
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KR1019900008868A KR0160478B1 (en) | 1990-06-16 | 1990-06-16 | Process for preparing polyester |
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KR19990068638A (en) * | 1999-06-07 | 1999-09-06 | 김찬모 | Equipment for bean sprouts cultivation |
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