KR100259494B1 - Process for preparing polyester fiber - Google Patents
Process for preparing polyester fiber Download PDFInfo
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- KR100259494B1 KR100259494B1 KR1019970067525A KR19970067525A KR100259494B1 KR 100259494 B1 KR100259494 B1 KR 100259494B1 KR 1019970067525 A KR1019970067525 A KR 1019970067525A KR 19970067525 A KR19970067525 A KR 19970067525A KR 100259494 B1 KR100259494 B1 KR 100259494B1
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- South Korea
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- polyester
- added
- pentaerythritol
- isophthalic acid
- polyester fiber
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Classifications
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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
- 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
- D01D5/08—Melt spinning methods
Abstract
Description
본 발명은 우수한 강도와 염색성 및 열수축 특성을 가지는 폴리에스터 섬유의 제조방법에 관한 것이다.The present invention relates to a method for producing a polyester fiber having excellent strength, dyeability and heat shrinkage properties.
폴리에스터는 여러가지 우수한 성질 때문에 광범위한 용도로 이용되고 있다.Polyesters are used for a wide range of applications because of their excellent properties.
폴리에스터는 통상 테레프탈산 또는 디메틸 테레프탈레이트와 에틸렌 글리콜을 에스터화 반응시켜 테레프탈산의 글리콜 유도체와 같은 저중합체를 만들고 이를 고온, 감압하에서 가열하여 필요한 중합도까지 중합시켜 제조한다. 이렇게 얻어진 폴리에스터는 용융상태에서 방사노즐로부터 섬유상으로 압출되고 연신된다.Polyesters are usually prepared by esterifying a terephthalic acid or dimethyl terephthalate with ethylene glycol to produce oligomers, such as glycol derivatives of terephthalic acid, and heating them under high temperature and reduced pressure to polymerize to the required degree of polymerization. The polyester thus obtained is extruded and stretched fibrous from the spinning nozzle in the molten state.
폴리에스터의 생산성을 높이고 염색성을 향상시키기 위해 폴리에스터 중합시에 측쇄제를 첨가하여 용융방사하는 방법이 알려져 있다. 대표적인 측쇄제인 펜타에리스리톨(pentaerythritol)을 테레프탈산 혹은 디메틸 테레프탈레이트에 대해 450ppm이 넌지 않도록 넣으면 모듈러스와 강도등을 향상시킨다는 것이 맥린(MacLean)등의 미국특허 4,113,704에 의해 알려져 있다. 맥린등은 펜타에리스리톨을 450ppm보다 많게 넣으면 강력과 염색성의 감소를 일으키며, 제한된 량만큼 사용하면 폴리에스터의 생산성을 높인다고 말하고 있다.In order to increase the productivity of the polyester and to improve the dyeability, a method of melt spinning by adding a side chain agent during polyester polymerization is known. It is known from U.S. Patent 4,113,704 to MacLean et al. That the addition of pentaerythritol, a typical branching agent, to improve modulus and strength when 450 ppm is not exceeded with respect to terephthalic acid or dimethyl terephthalate. McLean et al. Stated that adding more than 450ppm of pentaerythritol leads to a decrease in strength and dyeability, and a limited amount of polyester increases the productivity of polyester.
하지만 측쇄제를 첨가할 경우 방사성과 염색성이 떨어지게 되어 이에 대한 해결방법이 필요하다.However, when the side chain agent is added, the radioactivity and dyeability are reduced, and a solution for this is needed.
또한 이소프탈산(isophthalic acid)을 첨가하면 폴리에스터 섬유의 방사성과 염색성이 향상된다고 하는 사실은 잘 알려져 있다. 폴리에스터의 생산중 이소프탈산의 함량을 증가시키면 생산되는 섬유의 방사성이 증가한다. 그러나 방사성을 향상시키기 위해 첨가한 이소프탈산은 원사의 모듈러스와 강도, 열수축성을 저하시킨다.It is also well known that addition of isophthalic acid improves the spinning and dyeing properties of polyester fibers. Increasing the content of isophthalic acid in the production of polyester increases the spinning of the fibers produced. However, isophthalic acid added to improve the radioactivity decreases the modulus, strength, and heat shrinkability of the yarn.
따라서 폴리에스터 섬유의 염색성을 증진시키며 강도, 모듈러스, 방사성 등을 모두 증진시켜 줄 수 있는 적절한 첨가제가 절실하게 요구되고 있다.Therefore, there is an urgent need for suitable additives that can enhance the dyeing properties of polyester fibers and enhance both strength, modulus, and radioactivity.
본 발명은 테레프탈산이나 디메틸 테레프탈레이트, 에틸렌 클리콜로 중합하는 폴리에스터 체인내에 펜타에리스리톨과 이소프탈산을 함께 첨가시켜서 폴리에스터 공중합물을 합성함으로서 방사성과 생산성이 좋으며 강도, 모듈러스 및 염색성이 우수한 폴리에스터 섬유의 제조방법을 제공하는데 목적이 있는 것이다.The present invention synthesizes a polyester copolymer by adding pentaerythritol and isophthalic acid to a polyester chain polymerized with terephthalic acid, dimethyl terephthalate, and ethylene glycol, thereby synthesizing a polyester copolymer. The purpose is to provide a manufacturing method.
이하 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.
본 발명은 테레프탈산 혹은 디메틸테레프탈레이트와 에틸렌글리콜 그리고 측쇄제를 사용하여 폴리에스터를 공중합시킬 때 테레프탈산 또는 디메틸 테레프탈레이트에 대해 이소프탈산을 1∼5몰% 첨가시키고, 펜타에리스리톨을 중량비로 100∼450ppm 첨가시켜서 공중합시킴을 특징으로 하는 것이다. 위와같이 공중합시킨 공중합물은 용융방사한 후 충분한 연신비와 온도로 연신하고, 이어서 연신사를 충분히 높은 온도로 가열 고정하여 폴리에스터 섬유를 제조한다.In the present invention, when copolymerizing polyester using terephthalic acid or dimethyl terephthalate with ethylene glycol and a side chain agent, 1 to 5 mol% of isophthalic acid is added to terephthalic acid or dimethyl terephthalate, and 100 to 450 ppm of pentaerythritol is added by weight. It is characterized in that the copolymerization. The copolymer copolymerized as described above is melt-spun and then stretched to a sufficient draw ratio and temperature, and then the stretched yarn is heat-fixed to a sufficiently high temperature to prepare polyester fibers.
펜타에리스리톨은 측쇄제로 작용하여 생산성을 향상시키지만 함량의 증가에 따라 원사의 균일성이 저하되어 방사성이 떨어지고 염색성이 저하되는 결점이 있다. 따라서 방사성과 염색성을 향상시켜주는 이소프탈산을 첨가하면 방사성과 생산성이 높으며 염색성과 강도, 모듈러가 우수한 섬유를 만들 수 있다.Pentaerythritol improves productivity by acting as a side chaining agent, but as the content is increased, the uniformity of the yarn decreases, so that the radioactivity and the dyeability decrease. Therefore, the addition of isophthalic acid, which improves the spinning and dyeing properties, can produce fibers with high spinning and productivity and excellent dyeing, strength and modularity.
그러나, 펜타에리스리톨을 1OOppm미만 첨가할 경우는 생산성과 염색성을 향상시킬 수 없으며, 450ppm을 초과하면 방사성이 급격하게 저하하고 원사의 강도, 모듈러스, 열수축성등이 급격히 감소하므로 바람직하지 않다. 또한 이소프탈산을 1 몰%미만 첨가할 경우는 방사성을 향상시킬 수 없고, 5몰%를 초과하여 첨가할 경우는 강도의 급격한 저하가 나타나서 바람직하지 않다.However, the addition of less than 100 ppm of pentaerythritol cannot improve the productivity and dyeability, and if it exceeds 450 ppm, the radioactivity is drastically lowered, and the strength, modulus, heat shrinkability, etc. of the yarn are decreased. In addition, when less than 1 mol% of isophthalic acid is added, the radioactivity cannot be improved, and when it is added in excess of 5 mol%, a sharp drop in strength appears, which is not preferable.
[실시예 1∼2, 비교예 1∼3]EXAMPLES 1-2, COMPARATIVE EXAMPLES 1-3
폴리에스터 중합체 체인내에 펜타에리스리톨과 이소프탈산을 표 1과 같이 변화시키면서 첨가하여 공중합체로 만든 다음 방사온도를 290℃로 하여 방사구금직경 0.2mm(구멍수 36)으로 하고, 최종연신사의 섬도가 75데니어가 되도록 토출량을 조절하여 3600m/분으로 방사한뒤, 연신하여 비교하였다.Pentaerythritol and isophthalic acid were added to the polyester polymer chain while changing it as shown in Table 1 to make a copolymer, and the spinneret diameter was 0.2mm (36 holes) with spinning temperature of 290 ° C. The discharge amount was adjusted to be denier and spun at 3600 m / min, followed by stretching.
〈측정방법〉<How to measure>
실시예중 폴리에스터사의 염색성은 원사를 환편기로 10∼30cm의 길이가 되도록 핀직한 후 아래와 같은 방법으로 염색을 하여 평가하였다.In Example, the dyeability of polyester yarn was pinned to a length of 10 to 30cm with a circular knitting machine and then dyed by the following method.
◇ 염색시험 : 염료인 코우-네이비(S Type)를 염료농도 2% o.w.p로 만든 후 분산제(VGT) 1g/ℓ, pH 4.5∼5.5(초산), 액비 1 대 25로 조제하여 염색온도를 30℃에서 95℃까지 분당 1℃씩 균일하게 승온시킨 후 95℃에서 30분간 염색하였다.◇ Dyeing test: Kou-navy (S Type) dye is made with 2% owp of dye concentration, dispersant (VGT) 1g / ℓ, pH 4.5 ~ 5.5 (acetic acid), liquid ratio of 1: 25 and dyeing temperature is 30 ℃ The temperature was uniformly increased by 1 ° C. per minute to 95 ° C. and then dyed at 95 ° C. for 30 minutes.
◇ 염색성 : 염색이 끝난 시료를 충분히 건조시킨 후 백색판을 넣어 육안으로 염색 등급을 판정하였는데 일반적인 원사의 등급을 보통으로 할 때, 상대적으로 비교하여 우수한 경우, 매우 우수한 경우, 불량한 경우로 나누어 단계적으로 평가하였다.◇ Dyeing: After dyeing the sample after drying enough, white plate was added to determine the dyeing grade visually. When the grade of general yarn is normal, it is divided relatively into excellent cases, very good cases, and poor cases. Evaluated.
[표 1]TABLE 1
표 1에 나타난 바와같이 실시예 1, 실시예 2에서는 펜타에리스리톨과 이소프탈산을 함께 첨가한 공중합체를 사용하였으므로 원사의 물성이 저하되지 않으면서 방사성과 염색성 및 물성이 매우 우수하였다.As shown in Table 1, in Example 1 and Example 2, a copolymer in which pentaerythritol and isophthalic acid were added together was used, and thus the yarn properties and the dyeing properties and the physical properties of the yarn were excellent.
실시예 1과 비교예 1을 비교해보면 펜타에리스리톨과 이소프탈산을 동시에 첨가하는 경우 첨가하지 않은 경우에 비하여 방사성과 염색성이 매우 우수해지며,강도, 모듈러스, 건열수축율등은 저하되지 않음을 알 수 있다.Comparing Example 1 and Comparative Example 1, when pentaerythritol and isophthalic acid are added at the same time, the radioactivity and dyeability are excellent compared to those without addition, and the strength, modulus, dry heat shrinkage ratio, etc. are not reduced. .
실시예 2와 비교예 2를 비교해보면 펜타에리스리톨만을 첨가하였을 경우 방사성이 떨어지나, 이소프탈산을 함께 첨가하면 방사성이 매우 우수해지며, 염색성도 향상됨을 알 수 있다.Comparing Example 2 and Comparative Example 2, the addition of pentaerythritol alone is poor in radioactivity, but when isophthalic acid is added together, it can be seen that the radioactivity is very excellent and the dyeability is also improved.
실시예 2와 비교예 3을 비교해보면 이소프탈산만 첨가하였올 경우, 방사성과 염색성은 향상되는 반면 강도, 모듈러스, 건열수축율 등의 특성이 저하됨을 알 수 있고, 펜타에리스리톨과 동시에 첨가하면 방사성과 염색성이 우수할 뿐만 아니라 상기 물성도 저하되지 않음을 알 수 있다.Comparing Example 2 and Comparative Example 3, it can be seen that when only isophthalic acid is added, the radioactivity and dyeability are improved while the properties such as strength, modulus and dry heat shrinkage are deteriorated. Not only is this excellent but it can be seen that the physical properties are not reduced.
본 발명은 측쇄제인 펜타에리스리톨과 이소프탈산을 적량함께 사용함으로써 각각을 단독으로 첨가하였을 경우에 발생되는 단점들을 상호 보완시켜 주기 때문에 방사성과 생산성이 좋으며 물성(강도, 모듈러스 및 염색성)이 개선된 폴리에스터 섬유를 제조할 수 있다.In the present invention, the pentaerythritol and isophthalic acid, which are side chains, are used in an appropriate amount together to compensate for the disadvantages of each addition alone, so that the polyester has improved radioactivity and productivity and improved physical properties (strength, modulus, and dyeability). Fibers can be produced.
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| KR1019970067525A KR100259494B1 (en) | 1997-12-10 | 1997-12-10 | Process for preparing polyester fiber |
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| KR1019970067525A KR100259494B1 (en) | 1997-12-10 | 1997-12-10 | Process for preparing polyester fiber |
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| KR100305840B1 (en) * | 1999-08-11 | 2001-09-13 | 조 정 래 | Process for Preparing Polyester Filament Yarn Having High Strength, Modulus, and Good Dyeing Property |
| EP3693507A1 (en) * | 2015-03-17 | 2020-08-12 | Kuraray Co., Ltd. | Napped artificial leather dyed with cationic dye |
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