KR930007880B1 - Process for preparation of polyester - Google Patents
Process for preparation of polyester Download PDFInfo
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- KR930007880B1 KR930007880B1 KR1019900019384A KR900019384A KR930007880B1 KR 930007880 B1 KR930007880 B1 KR 930007880B1 KR 1019900019384 A KR1019900019384 A KR 1019900019384A KR 900019384 A KR900019384 A KR 900019384A KR 930007880 B1 KR930007880 B1 KR 930007880B1
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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
- C08G63/78—Preparation processes
-
- 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
- C08G63/60—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from the reaction of a mixture of hydroxy carboxylic acids, polycarboxylic acids and polyhydroxy compounds
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Artificial Filaments (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
Description
본 발명은 폴리에스터의 분자배향시 과도한 결정화를 억제시킬 수 있는 폴리에스터의 제조방법에 관한 것이다.The present invention relates to a method for producing a polyester that can suppress excessive crystallization during molecular orientation of the polyester.
폴리에스터는 우수한 물리적, 화학적 성질을 가지고 있기 때문에 여러가지 용도로 사용되며 그중에서도 섬유로 널리 사용되고 있다. 폴리에스터 섬유는 여러방법으로 제조되며 최근에는 제사기술이 진보됨에 따라서 용융방사시의 권취속도는 종래의 1,000~1,500m/분에서 2,000m/분 이상으로 크게 높일 수 있게 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 in various ways, and recently, as the weaving technique is advanced, the winding speed during melt spinning can be greatly increased from 1,000 to 1500 m / min to 2,000 m / min or more.
특히 권취속도를 2,500~4,000m/분으로 하여 제조한 부분배향 미연신사는 그대로 연신, 가공공정에 제공되고 있으며, 그 용도는 계속 확대되고 있다.In particular, the partially oriented undrawn yarn manufactured at a winding speed of 2,500 to 4,000 m / min is provided as it is to the stretching and processing process, and its use is continuously expanding.
한편, 권취속도를 4,000m/분으로 하는 초고속 방사도 시도되고 있는데, 이러한 초고속 방사에서는 방사시 사절이 자주 발생하고 최종 제품의 강도가 현저하게 저하되는 문제점이 있다.On the other hand, ultra-fast spinning with a winding speed of 4,000 m / min has also been attempted. In such high-speed spinning, there is a problem in that trimming occurs frequently during spinning and the strength of the final product is significantly reduced.
이와 같은 결점을 해결하기 위하여 방사조건의 적정화 및 방사노즐의 구조개량 등을 시도하고 있지만 이러한 방법으로는 만족할 만한 효과를 기대하기 어려웠다.In order to solve these drawbacks, the optimization of the radiation conditions and the structural improvement of the spinning nozzle have been attempted, but it was difficult to expect a satisfactory effect with this method.
본 발명자들은 상기와 같은 문제점의 원인에 대하여 검토한 결과, 폴리에스터를 용융방사할 때 권취속도가 2,000m/분 이상으로 되면 방사장력에 의해 분자배향이 일어나고 동시에 결정화가 일어나게 되는바, 이때 배향이 충분하게 이루어지지 않은 상태에서 결정화가 크게 진행되기 때문에 앞서 언급한 문제점이 발생되며 이와 같은 현상은 권취속도가 빠를수록 더욱 현저하게 된다는 것을 알게 되었다.The present inventors have investigated the causes of the problems described above, when melt spinning the polyester, when the winding speed is 2,000m / min or more, the molecular orientation is caused by the radial tension and crystallization occurs at the same time, the orientation is Since the crystallization proceeds greatly in a state in which it is not sufficiently made, the above-mentioned problem occurs, and it is found that such a phenomenon becomes more remarkable as the winding speed is increased.
이와 같은 사실을 기초로 하여서 고속방사시 고배향이고, 저결정화가 되는 폴리에스터에 관하여 그 결정화 및 분자배향의 거동면에서 계속 검토를 하고 분자배향시 결정화를 억제시킬 수 있는 각종 첨가제에 관하여 조사한 결과, 폴리에스터 제조중에 다음 일반식(Ⅰ)로 표시되는 화합물을 첨가하는 것이 효과가 있음을 알아내고 본 발명을 완성하게 되었다.Based on the above facts, polyesters with high orientation and low crystallization during high-speed spinning are continuously examined in terms of their crystallization and molecular orientation behavior, and various additives that can suppress crystallization during molecular orientation are found. In the preparation of polyester, it was found that adding a compound represented by the following general formula (I) was effective and completed the present invention.
단, R은 H 또는 탄소수 1~15인 알킬기, 아릴기, 아릴알킬기 중 하나임.Provided that R is one of H or an alkyl group having 1 to 15 carbon atoms, an aryl group, or an arylalkyl group.
본 발명을 상세히 설명하면 아래와 같다. 본 발명은 주된 반복 구조단위가 에틸렌 테레프탈레이트인 폴리 에스터를 제조함에 있어서, 중합반응 단계에서 일반식(Ⅰ)의 화합물을 폴리에스터를 구성하는 산성분에 대하여 0.05~4.0몰% 첨가하여 반응시키는 것을 특징으로 한다.Hereinafter, the present invention will be described in detail. In the present invention, in the production of a polyester in which the main repeating structural unit is ethylene terephthalate, the reaction of adding the compound of the general formula (I) to the acid component constituting the polyester in the polymerization step by adding 0.05 to 4.0 mol% It features.
본 발명에서 일반식(Ⅰ)의 화합물의 첨가량이 너무 작으면 분자배향시의 결정화 억제효과가 얻어지지 않고 반대로 첨가량이 너무 많으면 폴리에스터의 물성이 나빠지기 때문에 폴리에스터의 제조시에 사용되는 디카르복실산에 대하여 0.05~5.0몰%만큼 첨가하는 것이 좋다.In the present invention, when the addition amount of the compound of the general formula (I) is too small, the effect of suppressing crystallization at the time of molecular orientation is not obtained. On the contrary, when the addition amount is too large, the physical properties of the polyester deteriorate. It is good to add 0.05-5.0 mol% with respect to an acid.
만일 5몰%를 초과하면 칩의 황변현상이 일어나는 결정적인 단점이 있으며, 부생성물 과다 생성 및 반응시간 연장 등으로 생산성이 저하된다.If it exceeds 5 mol%, there is a decisive disadvantage in that yellowing of the chip occurs, and productivity is reduced due to excessive production of by-products and extension of reaction time.
본 발명의 대상물은 폴리에틸렌 테레프탈레이트로 되어 있는 폴리에스터이지만 폴리에스터의 물성개량을 위하여 디카르복실산 성분 또는 글리콜성분의 일부를 다른 성분으로 치환시킨 폴리에스터에게도 유용하다. 본 발명에 의하면 3,000m/분 이상의 방사속도로 고속방사할 때 방사 및 연신공정중에 발생하는 사절이 현저하게 감소되었으며 공정이 안정화되고 생산성이 크게 향상되었다.The object of the present invention is a polyester made of polyethylene terephthalate, but is also useful for a polyester in which a part of a dicarboxylic acid component or a glycol component is substituted with another component for improving physical properties of the polyester. According to the present invention, when high-speed spinning at a spinning speed of 3,000 m / min or more, the trimming occurring during the spinning and stretching process is significantly reduced, the process is stabilized and productivity is greatly improved.
[실시예 1, 3, 5][Examples 1, 3, 5]
살리실 살리실릭산{일반식(Ⅰ)의 R이 H인 경우}을 첨가하여 제조한 극한점도 0.65인 폴리에스터를 방사온도 285℃, 토출량 44.5g/분으로 방사노즐을 통해 방사하고 15℃의 공기를 0.5m/분의 풍속으로 불어 주어 냉각시킨 후, 집속 및 유제부여한 후, 4,000m/분의 속도로 권취하여 미연신사를 얻고 이것을 연신비 1.332로 연신하였다. 이때 방사 및 연신의 작업성을 사절율로 나타낸 결과는 표 1과 같다.Salicylic salicylic acid (When R in Formula (I) is added to H) A polyester having an intrinsic viscosity of 0.65 was spun through a spinning nozzle at a spinning temperature of 285 ° C. and discharged at 44.5 g / min. The air was blown at a wind speed of 0.5 m / min to cool, concentrated and emulsified, then wound at a rate of 4,000 m / min to obtain undrawn yarn, which was stretched to a draw ratio of 1.332. At this time, the results showing the workability of the spinning and stretching as the trimming rate is shown in Table 1.
[실시예 2,4][Examples 2 and 4]
메틸 살리실 살리실레이트{일반식(Ⅰ)의 R이 탄소수 1인 경우}를 첨가하여 제조한 폴리에스터를 사용한 것외에는 실시예 1과 동일한 방법으로 실시하였으며, 그 결과는 표 1과 같다.The same procedure as in Example 1 was conducted except that the polyester prepared by adding methyl salicylic salicylate (when R in Formula (I) has 1 carbon atom) was used. The results are shown in Table 1 below.
[비교예 1, 2][Comparative Examples 1 and 2]
비교예 1은 첨가제 없이 비교예 2는 실시예 1의 첨가제를 8몰% 함유한 폴리에스터를 사용하여 실시예 1과 동일한 방법으로 실시하였으며, 그 결과는 표 1과 같다.Comparative Example 1 was carried out in the same manner as in Example 1 using a polyester containing 8 mol% of the additive of Example 1 without the additive, the results are shown in Table 1.
[표 1]TABLE 1
※ 방사작업성은 1,000시간을 기준으로 하여 사절수와 총 도핑수(333번)에 대한 사절 발생 도핑수의 백분율(=사절율)로 나타내었다.※ The radio workability is expressed as the percentage of the number of trimming occurrences (= trimming rate) to the number of trimmings and the total number of dopings (number 333) based on 1,000 hours.
※ 연신작업성은 3,000추 연신시 사절발생 추의 백분율(=사절율)로 나타내었다.※ Stretch workability is expressed as the percentage of trimming incidence (= trimming rate) at 3,000 strokes.
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KR1019900019384A KR930007880B1 (en) | 1990-11-28 | 1990-11-28 | Process for preparation of polyester |
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KR1019900019384A KR930007880B1 (en) | 1990-11-28 | 1990-11-28 | Process for preparation of polyester |
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KR930007880B1 true KR930007880B1 (en) | 1993-08-21 |
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