KR970010723B1 - Process for preparing polyester for high speed spinning - Google Patents
Process for preparing polyester for high speed spinning Download PDFInfo
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- KR970010723B1 KR970010723B1 KR1019920015271A KR920015271A KR970010723B1 KR 970010723 B1 KR970010723 B1 KR 970010723B1 KR 1019920015271 A KR1019920015271 A KR 1019920015271A KR 920015271 A KR920015271 A KR 920015271A KR 970010723 B1 KR970010723 B1 KR 970010723B1
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- polyester
- high speed
- speed spinning
- spinning
- compound
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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
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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)
- Polyesters Or Polycarbonates (AREA)
- Artificial Filaments (AREA)
Abstract
Description
본 발명은 고속방사가 가능한 폴리에스터 섬유의 제조방법, 좀 더 상세하게 말하면 폴리에스터의 분자배향시 과도한 결정화를 억제시켜 고속방사가 가능한 폴리에스터 섬유의 제조방법에 관한 것이다.The present invention relates to a method for producing a polyester fiber capable of high-speed spinning, more specifically, to a method for producing a polyester fiber capable of high-speed spinning by inhibiting excessive crystallization during molecular orientation of the polyester.
폴리에스터는 우수한 물리적, 화학적 성질을 가지고 있기 때문에 여러가지 용도로 사용되며 그 중에서도 섬유로 널리 사용되고 있다. 폴리에스터 섬유는 여러방법으로 제조되며 최근에는 제사기술이 진보됨에 따라서 용융방사시의 권취속도는 종래의 1,000∼1, 500m/분에서 2,000m/분 이상으로 대폭 증가시키는 것이 가능하게 되었다.Polyester is used for various purposes because of its excellent physical and chemical properties, and is widely used as a fiber. Polyester fibers are manufactured by various methods, and recently, as the weaving technique is advanced, the winding speed during melt spinning can be greatly increased from 1,000 to 1,500 m / min to 2,000 m / min or more.
특히 권취속도를 2,500∼4,000m/분으로 하여 얻어진 부분배향 미연신사는 그대로 연신가연공정에 제공되고 있으며 이 용도는 크게 증가하여 제사기술의 주류를 이루고 있다.In particular, partially oriented undrawn yarn obtained at a winding speed of 2,500 to 4,000 m / min is provided as it is to the drawing and twisting process, and its use has been greatly increased, making it the mainstream of weaving technology.
한편, 권취속도틀 4,000m/분 이상으로 하는 초고속방사도 시험되고 있는데, 이러한 초고속 방사에서는 방사시의 사절이 다발하게 되고 최종 제품사의 강도가 현저히 저하된다는 결점이 있다. 이와 같은 결점을 해결하기 위하여, 방사조건이 적정화 및 방사통과 방사노즐의 구조개량 등을 시험하고 있지만 이러한 방법으로는 한계가 있고 대폭적인 개시는 기대할 수 없다.On the other hand, ultra-fast spinning with a winding speed frame of more than 4,000 m / min is also being tested. In such high-speed spinning, there is a drawback that the number of threads during spinning is increased and the strength of the final product yarn is significantly reduced. In order to solve these drawbacks, the radiation conditions have been tested for adequacy and structural improvement of the spinneret and the spinneret, but this method is limited and cannot be widely initiated.
본 발명들은 상기와 같은 문제점에 대해 예의 검토를 반복한 결과, 폴리에스테르가 폴리에틸렌이나 폴리아미드 등에 비해 결정화되기 어려운 성질을 가지고 있지만, 용융방사시의 권취속도가 2,000m/분 이상으로되면 방사장력에 의하여 분자배향이 일어나고, 이것과 함께 결정화가 일어나게 되므로 방사시의 배향이 충분치 않음에도 불구하고 결정화가 크게 진행되어 앞서 말한 문제점이 발생하게 되는데, 이와 같은 경향은 권취속도가 4,000m/분 이상으로 되면 더욱 현저하게 된다는 것을 알아냈다.The present invention has repeatedly studied the above problems, as a result, polyester has a property that is difficult to crystallize compared to polyethylene, polyamide, etc., but when the winding speed during melt spinning is 2,000m / min or more, the radiation tension Molecular orientation is caused by this, and crystallization occurs along with this, but the crystallization proceeds greatly in spite of the insufficient orientation of the radiation. However, the above-mentioned problem occurs when the winding speed is more than 4,000 m / min. It was found to be more pronounced.
이와 같은 사실로부터 고속방사시에 있어서의 그 결정화 및 분자배향의 거동면에서 계속 검토를 하고, 분자배향시의 결정화를 억제시킬 수 있는 각종 첨가제에 관하여 연구를 수행한 결과 폴리에스터의 제조 중에하기 일반식(I)의 화합물을 첨가하는 것에 의해 현저한 효과가 있음을 알아내고 본 발명을 완성하게 되었다.From these facts, studies on the behavior of crystallization and molecular orientation during high-speed spinning, and researches on various additives that can suppress crystallization during molecular orientation resulted in general production of polyester. By adding the compound of formula (I), it was found that there was a remarkable effect and the present invention was completed.
(단, R은 H 또는 탄소수 1∼l0인 알킬기, 아릴기, 아릴알킬기, 나트륨, 칼슘)(Wherein R is H or an alkyl group having 1 to 10 carbon atoms, an aryl group, an arylalkyl group, sodium, calcium)
즉, 본 발명은 주된 반복구조 단위가 에틸렌테레프탈레이트인 폴리에스터를 제조함에 있어서, 중합반응 단계에서 일반식(I)의 화합물을 폴리에스터를 구성하는 산성분에 대하여 0.05∼5몰% 첨가하여 반응시키는 것을 특징으로 하는 고속방사용 폴리에스터 섬유의 제조방법을 제공하는 것이다.That is, in the present invention, in preparing a polyester in which the main repeating unit is ethylene terephthalate, the reaction is performed by adding 0.05 to 5 mol% of the compound of formula (I) with respect to the acid component constituting the polyester in the polymerization step. It is to provide a method for producing a high-speed spinning polyester fiber characterized in that.
본 발명에서 일반식(I)의 화합물의 첨가량은 상술한 바와 같이 하는 것이 가장 좋은데 이것이 너무 적으면 분자배향시의 결정화 억제효과가 얻어지지 않고 반대로 첨가량이 너무 많으면 폴리에스터의 물성이 나빠지기 때문에 바람직하지 못하다. 구체적으로 만일 일반식(I)의 화합물 첨가량이 5몰%를 초과하면 칩의 황변현상이 일어나는 결정적인 단점이 있으면 부생성물 과다생성 및 반응시간 연장 등으로 생산성이 저하된다.In the present invention, it is best to add the compound of general formula (I) as described above, but if it is too small, the effect of suppressing crystallization at the time of molecular orientation is not obtained. On the contrary, if the amount is too large, the physical properties of the polyester are deteriorated. I can't. Specifically, if the amount of the compound added in Formula (I) exceeds 5 mol%, there is a decisive disadvantage in that yellowing of the chip occurs, resulting in a decrease in productivity due to overproduct formation and prolongation of reaction time.
본 발명의 적용대상물은 폴리에틸렌 테레프탈레이트로 되어 있는 폴리에스터이지만 폴리에스터의 물성개량을 위하여 디카르복실산 성분 또는 글리콜성분의 일부를 다른 성분으로 치환시킨 폴리에스터도 유용하다. 이와 같이 본 발명에 따라 수득하는 폴리에스터는 중합 후 방사시에 3,000m/분 이상의 고속으로 방사하여도 방사 및 연신공정 중에 발생하는 사절이 종래에 비해 현저히 감소되었으며 물성이 안정화되고 생산성이 크게 향상되었다.The object of the present invention is a polyester made of polyethylene terephthalate, but a polyester in which a part of a dicarboxylic acid component or a glycol component is substituted with another component is also useful for improving physical properties of the polyester. As described above, the polyesters obtained according to the present invention have significantly reduced trimming during spinning and stretching processes compared to the prior art even when spinning after polymerization at a high speed of 3,000 m / min or more, and stabilized physical properties and greatly improved productivity. .
이하에 실시예를 들어 설명한다.An example is given and described below.
(실시예 1, 3, 5)(Examples 1, 3, 5)
폴리에스터의 중합단계에서 1, 3-아다만탄디카르복실산{일반식(I)에서 R이 H인 경우}을 표-1의 함량으로 첨가하여 제조한 극한점도 0.65인 폴리에스터를 방사온도 285℃, 토출량 44.5g/분으로 방사노즐을 통해 방사하고 15℃의 공기를 0.5m/분의 풍속으로 불어주어 냉각시켜 접속 및 유제를 부여한 후 4,000m/분의 속도로 권취하여 부분연신사를 얻고 이것을 연신미1.332로 연신하여 75D/36fi1의 원사를 얻었다. 이때 방사 및 연신의 작업성을 사절율로 나타낸 결과는 표-1과 같다.In the polymerization step of the polyester, a polyester having an intrinsic viscosity of 0.65, prepared by adding 1,3-adamantanedicarboxylic acid (where R in Formula (I) is H) to the content of Table-1, was radiated at a spinning temperature. It spins through a spinning nozzle at 285 ℃ and discharge rate 44.5g / min, blows air at 15 ℃ at a wind speed of 0.5m / min, cools it, connects it with emulsion, and winds it up at a speed of 4,000m / min. This was stretched to 1.332, which was obtained as yarn 75D / 36fi1. In this case, the results showing the workability of spinning and drawing as the trimming rate are shown in Table-1.
(실시예 2, 4)(Examples 2 and 4)
메틸 1, 3-아다만탄디카르복실레이트 {일반식(I)에서 R이 탄소수l의 알킬기인 경우}를 첨가하여 제조한 폴리에스터를 사용한 것 외에는 실시예 1과 동일한 방법으로 실시하였으며 그 결과를 표-1과 같다.The procedure was carried out in the same manner as in Example 1 except for using a polyester prepared by adding methyl 1,3-adamantanedicarboxylate (when R is an alkyl group having 1 carbon atom in general formula (I)). Is shown in Table-1.
(비교예 1, 2)(Comparative Examples 1 and 2)
비교예 1은 첨가제 없이, 비교예 2는 실시예 1의 첨가제를 10몰% 함유한 폴리에스터를 사용하여 실시예1과 동일한 방법으로 실시하였으며, 그 결과는 표-1과 같다.Comparative Example 1 was performed without additives, Comparative Example 2 was carried out in the same manner as in Example 1 using a polyester containing 10 mol% of the additive of Example 1, the results are shown in Table-1.
[표- 1]Table-1
* 방사작업성은 1,000 시간을 기준으로 하여 사절수와 총 도핑수(333번)에 대한 사절발생 도핑수의 백분율(=사절율)로 나타내었다.* Radio workability is expressed as the percentage of trimming occurrence doping number (= trimming rate) with respect to the number of trimmings and the total number of dopings (number 333) based on 1,000 hours.
* 연신작업성은 3,000추 연신시 사절방생추의 백분율(=사절율)로 나타내었다.* Stretch workability is expressed as the percentage of trimming spine at 3,000 strokes.
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Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019920015271A KR970010723B1 (en) | 1992-08-25 | 1992-08-25 | Process for preparing polyester for high speed spinning |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019920015271A KR970010723B1 (en) | 1992-08-25 | 1992-08-25 | Process for preparing polyester for high speed spinning |
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| Publication Number | Publication Date |
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| KR940004094A KR940004094A (en) | 1994-03-14 |
| KR970010723B1 true KR970010723B1 (en) | 1997-06-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| KR1019920015271A KR970010723B1 (en) | 1992-08-25 | 1992-08-25 | Process for preparing polyester for high speed spinning |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2020222536A1 (en) * | 2019-05-02 | 2020-11-05 | 주식회사 엘지화학 | Cyclohexane triester plasticizer composition and resin composition comprising same |
| TWI816045B (en) * | 2019-07-30 | 2023-09-21 | 南韓商Ｌｇ化學股份有限公司 | Citrate-based plasticizer composition and resin composition comprising the same |
| KR102361973B1 (en) * | 2020-04-29 | 2022-02-11 | 애경케미칼주식회사 | Composite plasticizer and polyvinyl chloride resin composition containing the same |
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