KR0152762B1 - Method of manufacturing polyester fiber with fire retardant and anti-pilling properties - Google Patents
Method of manufacturing polyester fiber with fire retardant and anti-pilling properties Download PDFInfo
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- KR0152762B1 KR0152762B1 KR1019960005127A KR19960005127A KR0152762B1 KR 0152762 B1 KR0152762 B1 KR 0152762B1 KR 1019960005127 A KR1019960005127 A KR 1019960005127A KR 19960005127 A KR19960005127 A KR 19960005127A KR 0152762 B1 KR0152762 B1 KR 0152762B1
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- pilling
- polyester fiber
- general formula
- polyester
- flame retardant
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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
- 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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- 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
- D01D5/098—Melt spinning methods with simultaneous stretching
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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
- 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
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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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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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/443—Heat-resistant, fireproof or flame-retardant yarns or threads
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Polyesters Or Polycarbonates (AREA)
- Artificial Filaments (AREA)
Abstract
본 발명은 난연성과 항필링성을 겸비한 폴리에스테르섬유의 제조방법임.The present invention is a method for producing a polyester fiber having flame retardancy and anti-pilling properties.
본 발명은 디카르복실산 성분과 디올 성분으로 폴리에스테르중합체를 중합하고 상기 중합체를 용융방사, 연신하여 폴리에스테르섬유를 제조함에 있어서, 폴리에스테르중합시에 다음 일반식(Ⅰ)의 난연제와 일반식(Ⅱ)의 항필링성부여제를 첨가하여 중합시킴을 특징으로 하는 방법임.The present invention polymerizes a polyester polymer with a dicarboxylic acid component and a diol component, and melt-spun and stretches the polymer to produce polyester fibers.At the time of polyester polymerization, a flame retardant of the following general formula (I) and a general formula It is a method characterized by superposing | polymerizing by adding the antifilling agent of (II).
단, R은 에틸 또는 메틸기 n은 0 혹은 1Provided that R is ethyl or methyl is n or 0
Description
본 발명은 난연성과 항필링성(抗 pilling性)을 겸비한 폴리에스테르섬유의 제조방법에 관한 것이다.The present invention relates to a method for producing a polyester fiber having both flame retardancy and anti-pilling property.
잘 알려진 바와 같이 폴리에스테르는 우수한 기계적 성질, 내약품성, 내열성등을 보유하고 있어 파이버, 필름 등 여러분야에서 사용되고 있지만 본래부터 가연성물질이므로 착화하여 연소하기 쉬운 단점이 있다.As is well known, polyester has excellent mechanical properties, chemical resistance, heat resistance, etc., so it is used in fiberglass, film, etc., but it is inherently flammable material, so it is easy to ignite and burn.
특히 유럽이나 미국등지에서는 유아 및 노인용 의류, 커튼, 카펫트등에 난연기준을 법으로 규정하고 있는데, 이러한 분야로의 용도를 전개하려면 폴리에스테르의 난연화가 절실하게 요청된다.In particular, in Europe and the United States, flame retardant standards are prescribed by law for clothes for children and the elderly, curtains, carpets, and the like.
지금까지 소개된 폴리에스테르의 난연화 방법은 중합시 난연효과를 주는 물질을 첨가하는 방법과 섬유유제등에 난연성분을 섞어서 사용하는 후가공 처리법등으로 크게 나누어 볼 수 있다. 먼저 후가공처리법의 경우는 경제적인 잇점이 있는 반면 제품의 표면을 거칠게 하고 세탁등에 의해 난연성분이 탈락하여 난연내구성이 떨어지는 등의 단점을 갖고 있다. 또 중합시 난연물질을 첨가하는 방법에 사용되는 난연성 물질은 통상 무기물이나 할로겐계 및 인계유기물이 보편화되어 있다. 무기물계통의 난연성분으로는 안티모니 트리옥시드가 대표적인 예인데 이경우 유기물인 폴리에스테르와의 상용성이 없어 사용에 제한을 받고 있으며, 할로겐계 난연제의 경우는 고분자의 착색 및 열분해시 유독성 개스를 발생시켜 각국에서 사용에 규제를 가하고 있는 형편이다. 다음으로 인계의 난연제를 사용하는 경우가 있는데 그 예로는 미국특허 제3,941,752 및 일본특공소 55-41610 및 한국특허공고 83-59등이 있고 그외에도 일본특공소 38-1750, 소 45-9197, 소 52*17050, 미국특허 제3,076,010 및 4,157,436등 다수가 있으나 공정이 복잡하고 실질적으로 인 화합물의 잔존율이 낮아 과량의 인 화합물을 투여하는데 따른 촉매의 활성도를 떨어뜨리거나 폴리머의 융점을 저하시켜 가공시 작업성을 불량하게 하며 또한 기계적 물성을 나쁘게하는 등의 문제를 안고 있다.The flame retardant method of polyester introduced so far can be divided into the method of adding a material which has a flame retardant effect during polymerization, and the post-processing method using a flame retardant component mixed with a fiber emulsion. First, the post-processing method has economic advantages, while the surface of the product is rough and the flame retardant component is dropped due to washing off of the flame retardant component. In addition, the flame-retardant substance used for the method of adding a flame-retardant substance at the time of superposition | polymerization is the inorganic, halogen-type, and phosphorus organic substance in general. Antimony trioxide is a representative example of the inorganic flame retardant component. In this case, it is restricted to use because it is incompatible with polyester, which is organic. Countries are restricting their use. Next, there are cases of using a flame retardant of phosphorus. Examples include U.S. Patent No. 3,941,752, Japanese Patent Application No. 55-41610, and Korean Patent Publication 83-59, and others Japanese Patent Application No. 38-1750, Small 45-9197, Small 52 * 17050, U.S. Patent No. 3,076,010 and 4,157,436, etc., but the process is complicated and the residual rate of the phosphorus compound is substantially low, thus reducing the activity of the catalyst or the melting point of the polymer when the excess phosphorus compound is administered. There are problems such as poor workability and bad mechanical properties.
아울러 폴리에스테르섬유를 의류에 사용하였을때 직물표면의 섬유 일부분이 사용중에 마찰에 의해 절단되면서 모우가 형성되고 이러한 모우가 서로 엉켜 옥상(玉狀)으로 직물표면에 붙어있게 되는데, 이러한 현상을 방적사로 된 직물에서 발생한 것을 필(fill)이라 하며 필라멘트로 된 직물에 나타난 것은 스낵(snag)이라고 칭한다[본 발명에서는 통털어 필링(pilling)현상으로 칭한다].In addition, when the polyester fiber is used in clothing, a portion of the fiber surface of the fabric is cut by friction during use, and a wool is formed, and these wools are entangled with each other and are attached to the fabric surface with a roof. What happens in the fabric is called a fill and what appears in the fabric of the filament is called a snack (in the present invention, it is called a pilling phenomenon).
이러한 필링현상은 천연섬유에 비해 폴리에스테르섬유와 같은 합성섬유를 주재료로 하는 의복에서 현저히 증각되며, 상기 현상은 의복의 외관 및 촉감을 크게 저하시키기 때문에 합성제품의 소재설계 및 상품설계에 큰 제약을 주고 있다.This peeling phenomenon is remarkably increased in garments composed mainly of synthetic fibers, such as polyester fibers, compared to natural fibers, and this phenomenon greatly reduces the appearance and feel of the garments. Giving.
일반적으로 필링현상을 억제하기 위한 수단으로는, 첫째, 모우의 발생을 적게하는 방법, 둘째, 모우가 엉키거나 휘말리는 것을 최소화하는 방법, 셋째, 발생된 모우 및 형성된 필(pill)을 쉽게 탈락시키는 방법등이 있다.Generally, as a means for suppressing peeling phenomenon, first, a method of reducing the occurrence of cows, second, a method of minimizing the entanglement or entangling of the cows, third, a method of easily dropping the generated cows and the formed pill (pill) Etc.
첫번째 방법은 섬유 상호간의 구속력을 크게 해 줌으로써 섬유의 이동을 억제하는 방법으로 이는 섬유의 굵기, 길이, 꼬임수 및 직물의 조직, 밀도, 가공공정등에 대하여 충분한 고려를 필요로 한다.The first method is to suppress the movement of fibers by increasing the binding force between the fibers, which requires sufficient consideration of the thickness, length, number of twists and the fabric, density, and processing of the fabric.
두번째 방법은 섬유의 벤딩레질리언스(bending resilience)를 크게 해 줌으로써 필의 생성을 억제하는 방법으로서 열처리에 의한 기계권축의 소실 방법 및 섬유선단부분의 권축을 직선화시킨 특수 권축섬유를 제조하는 방법등이 있다.The second method is to increase the bending resilience of the fiber and to suppress the formation of the peel. The method of eliminating the mechanical crimp by heat treatment and manufacturing the special crimped fiber straightening the crimp of the fiber tip part, etc. There is this.
세번째 방법은 항필링화 수단의 적극적인 방법으로서 섬유의 강신도를 저하시킴으로써 마찰에 의한 필의 탈락을 촉진시키는 방법이다. 예를 들면 일본특공소 35-8562에 제안되어 있는 저중합도법은 중합도를 낮추어서 섬유의 강도를 낮추는 방법이나 용융점도가 낮아져서 방사성이 나쁠뿐 아니라 후가공시에 많은 문제를 야기시키게 되며, 일본특허공소 50-22617호에는 미연신토우를 연신한 후 10∼30℃로 냉각하여 권축처리하므로서 섬유 내부구조가 파괴되도록 하여 강신도를 저하시키는 방법이 기술되어 있는바, 이 방법에 의하면 섬유의 내부구조가 균일하게 파괴되지 않아 방적공정에서 단섬유발생이 많아지게 되고 냉각공정 때문에 작업성과 생산성이 저하된다.The third method is an aggressive method of anti-pilling means, which promotes peeling of the peel due to friction by lowering the strength of the fiber. For example, the low-polymerization method proposed in Japanese Patent Application No. 35-8562 is a method of lowering the strength of fibers by lowering the degree of polymerization or lowering the viscosity of the melt, resulting in poor radioactivity and many problems in post-processing. -22617 describes a method of lowering the elongation by breaking the inner structure of the fiber by stretching the unstretched toe after cooling it to 10 to 30 ° C., and according to this method, the inner structure of the fiber is uniform. Since it is not destroyed, short fibers are generated in the spinning process, and workability and productivity are reduced due to the cooling process.
또 종래에도 폴리에스테르 난연사에 항필링성을 부여하는 기술들이 미국특허 제5,180,793호, 제5,145,941호 및 제5,151,494호에 소개된바 있으나, 상기 방법들은 다량의 난연제를 투입하는 방법이므로 폴리에스테르섬유의 물성을 저하시켰으며 항필링성이 탁월한 폴리에스테르섬유를 제조할 수 없었던 문제점이 있었다.In addition, in the past, techniques for imparting anti-pilling property to polyester flame retardant yarn have been introduced in US Pat. Nos. 5,180,793, 5,145,941 and 5,151,494. However, since the methods are a method of adding a large amount of flame retardant, Deteriorated physical properties and there was a problem that could not be produced polyester fibers with excellent anti-pilling properties.
본 발명은 상술한 바와 같은 종래기술들의 문제점을 해결한 것으로써 소량첨가하더라도 충분한 난연효과를 얻을 수 있으며 동시에 작용기가 3개인 화합물을 사용하여 항필링성을 크게 향상시킬 수 있는 방법인바, 이하 상세히 설명하면 다음과 같다.The present invention solves the problems of the prior art as described above, even if the addition of a small amount can be obtained a sufficient flame retardant effect and at the same time a method that can greatly improve the anti-pilling properties using a compound having three functional groups, will be described in detail below Is as follows.
본 발명은 디카르복실산 성분과 디올 성분을 사용하여 폴리에스테르를 중합시킬때 난연성 부여성분으로 인(P)과 질소(N)원자를 함께 보유하고 있는 일반식(Ⅰ)의 화합물과 함께, 항필링성 부여성분으로 작용기가 3개인 일반식(Ⅱ)의 화합물을 첨가하여 중합시킨 다음에 상기 중합체를 통상의 방법으로 방사, 연신하여 제조하는 방법이다.The present invention relates to a compound of formula (I) having phosphorus (P) and nitrogen (N) atoms together as a flame retardant imparting component when polymerizing a polyester using a dicarboxylic acid component and a diol component. It is a method of preparing by polymerizing by adding a compound of formula (II) having three functional groups as a peeling imparting component and then spinning and stretching the polymer by a conventional method.
단, R은 에틸 혹은 에틸기 n은 0 혹은 1R is ethyl or ethyl n is 0 or 1
[트리메리틱 안하이드라이드(Trimellitic Anhidride)][Trimellitic Anhidride]
본 발명에 사용한 일반식(Ⅰ)의 화합물은 구조가 비교적 단순하고 고유의 고리 스티레인(Ring Strain) 때문에 반응성이 좋으며 또 인성분과 질소성분을 함께 가지고 있기 때문에 소량으로도 폴리에스테르섬유의 물성저하를 거의 일으키지 않으면서 충분한 난연효과를 줄 수 있다.The compound of formula (I) used in the present invention is relatively simple in structure, has good reactivity due to its inherent ring strain, and has both phosphorus and nitrogen components, thereby reducing the physical properties of the polyester fiber in a small amount. It can give a sufficient flame retardant effect with little generation.
상기 일반식(Ⅰ)의 화합물은 통상 포스포러스 헥사알킬트리아미드에 에틸렌 혹은 프로필렌 글리콜을 염기촉매하에 저온(0∼10℃)에서 벤젠 혹은 디에틸에테르를 용매로 사용하여 반응시켜 얻거나, 싸이클릭 클로로안하이드라이드에 에틸렌 혹은 프로필렌 글리콜을 염기촉매하에 저온(0∼10℃)에서 벤젠 혹은 디에틸에테르를 용매로 사용하여 반응시켜 얻는다.The compound of the general formula (I) is usually obtained by reacting ethylene or propylene glycol with phosphorus hexaalkyltriamide at low temperature (0 to 10 ° C) using a benzene or diethyl ether as a solvent, or a cyclic It is obtained by reacting chloro anhydride with ethylene or propylene glycol at low temperature (0 to 10 DEG C) under a base catalyst using benzene or diethyl ether as a solvent.
본 발명에 의한 난연성과 항필링성이 우수한 폴리에스테르는 디카르복실산 성분과 디올 성분 및 상기의 일반식(Ⅰ)의 화합물과 식(Ⅱ)의 화합물로 제조되는데, 이때 반응조건, 즉 에스테르 교환반응과 에스테르화 반응 및 증축합반응시의 조건은 공지의 방법과 같으며, 이 중에서 특히 디카르복실산 성분으로 테레프탈산을 사용하고, 디올 성분으로는 에틸렌글리콜을 사용하여 폴리에스테르를 제조하는 경우에 있어서는 공지의 알카리 금속이나 알카리토금속 또는 아연이나 망간, 티탄 또는 코발트등의 금속화합물들을 촉매로 하여 140℃ 내지 240℃의 온도에서 에스테르 교환반응을 행하며 에스테르 교환반응에서 사용되었던 것과 같은 금속화합물을 촉매로 하여 상압내지는 5kg/cm2의 압력과 200℃ 내지는 280℃의 온도조건하에서 에스테르화 반응을 진행하고, 이때 얻어진 소정의 반응 생성물을 안티몬이나 게르마늄 혹은 티탄등의 금속화합물 존재하에서 1토르(torr)이하의 진공속에서 250℃ 내지는 320℃의 온도조건하에 중축합시켜서 원하는 폴리에스테르를 제조하였다.Polyesters having excellent flame retardancy and anti-pilling properties according to the present invention are prepared from the dicarboxylic acid component, the diol component, the compound of the general formula (I) and the compound of the formula (II), wherein the reaction conditions, that is, transesterification The reaction, esterification, and condensation reaction conditions are the same as those in the known method. Among them, in the case of producing polyester using terephthalic acid as the dicarboxylic acid component and ethylene glycol as the diol component, By using a known alkali metal or alkaline earth metal or a metal compound such as zinc, manganese, titanium or cobalt as a catalyst to perform a transesterification reaction at a temperature of 140 ℃ to 240 ℃ by using a metal compound as the catalyst used in the transesterification reaction naejineun naejineun atmospheric pressure and 200 ℃ of 5kg / cm 2 Jin the esterification reaction under a temperature condition of 280 ℃ , At which time under the presence of metal compounds such as certain of the reaction product of antimony or germanium or titanium obtained 1 Torr (torr) naejineun 250 ℃ in vacuum by the following polycondensation under a temperature condition of 320 ℃ to prepare the desired polyester.
본 발명에서 일반식(Ⅰ)의 투입량은 인기준으로 0.25% 이상이면 충분한 난연효과를 갖게되고 0.6중량%를 초과하면 과량투입으로 인하여 색상 및 반응시간에 영향을 주게 된다. 또한 항필링성을 제공하는 일반식(Ⅱ)의 화합물의 양은 전체 산성분에 대해 0.03몰% 이상 3몰% 이하의 범위가 적당하며 0.03몰% 미만인 경우에서는 항필링성이 부족하고 3몰% 초과할 경우에는 중합시 용융점도의 상승이 급격하게 높아져 반응 및 섬유물성의 제어가 어렵다.In the present invention, the input amount of the general formula (I) has a sufficient flame retardant effect when 0.25% or more on the basis of phosphorus, and when it exceeds 0.6% by weight, the color and reaction time are affected due to the excessive injection. In addition, the amount of the compound of formula (II) which provides anti-pilling property is suitably in the range of 0.03 mol% or more and 3 mol% or less with respect to the total acid component, and in the case of less than 0.03 mol%, the anti-pilling property is insufficient and more than 3 mol%. In this case, it is difficult to control the reaction and the fiber properties because the increase of the melt viscosity during polymerization is sharply increased.
위와같이 제조된 섬유는 일본 나아가 유럽과 미국지역의 의류 및 비의류분야에서 난연사 평가기준에 적합한 충분한 난연성을 보유할 뿐만 아니라 항필링성이 탁월하다는 특징을 갖는다.The fiber produced as described above has not only a sufficient flame retardancy suitable for the flame retardant yarn evaluation criteria in the field of clothing and non-clothing in Japan and Europe and the United States, but also has an excellent anti-pilling property.
중합체의 분석에 사용된 방법으로는 극한점도(Ⅳ)로서 중합도를, 디에틸렌글리콜(DEG)의 함량으로 물성저하를 나타냈으며, 착색여부는 색가(b)를 측정하여 비교하였다.As the method used for the analysis of the polymer, the degree of polymerization was shown as the ultimate viscosity (IV), and the physical property was decreased by the content of diethylene glycol (DEG), and the coloring was compared by measuring the color value (b).
극한점도(Ⅳ)는 오르소 클로로페놀 용액을 사용하여 25℃에서 측정하였으며, DEC의 함량은 폴리에스테르 중합체를 가수분해시킨 후, 가스크로마토그래프법에 따라 에틸렌글리콜(EG)과 디에틸렌글리콜 DEG을 정량한 뒤 전체 글리콜에 대한 DEG의 양을 몰%로 표시하였다.Intrinsic viscosity (IV) was measured at 25 ° C. using an ortho chlorophenol solution. The content of DEC was determined by hydrolyzing the polyester polymer, followed by ethylene glycol (EG) and diethylene glycol DEG according to the gas chromatograph method. After quantification, the amount of DEG relative to the total glycol was expressed in mol%.
한편, 난연성은 한국소방법규에 표시되어 있는 방법에 의거하여 45°Coil법에서의 접염횟수를 5회 반복측정하여 그 평균값으로 나타내었다.On the other hand, flame retardancy was expressed as the average value of five times the number of times of contact in the 45 ° Coil method according to the method indicated in the Korean Fire Code.
또 항필링성은 JIS L1076에서 규정한 ICI시험기를 이용하여 회전시간을 5시간으로 하였으며 필의 발생 및 생성된 필의 탈락상황을 1-5등급으로 분류하여 5회 측정하여 그 평균값을 나타내었다.In addition, anti-pilling property was the rotation time was 5 hours using the ICI tester specified in JIS L1076, and the occurrence of peel and dropping condition of the generated peel were classified into 1-5 grades, and the average value was shown.
[실시예 1]Example 1
환류가 가능하도록 설계된 응축기와 교반장치가 설치된 스테인레스 스틸 반응기에 디메틸테레프탈레이트와 에틸렌글리콜을 1:1.5의 몰비가 되도록 하고 이어 일반식(Ⅰ)의 화합물을 중합체에 대해 인기준으로 0.25wt%, 식(Ⅱ)의 화합물을 디메틸테레프탈레이트에 대해 0.03mole% 첨가하고난 후, 통상적으로 사용되는 에스테르 교환반응 촉매를 첨가하고 가열교반하여 온도를 220℃에서 230℃ 범위로 상승시키면서 에스테르 교환반응을 시킨다.In a stainless steel reactor equipped with a condenser and agitator designed to reflux, dimethyl terephthalate and ethylene glycol were molar ratio of 1: 1.5, and then the compound of formula (I) was 0.25 wt% based on phosphorus based on polymer. After adding 0.03 mole% of the compound of (II) to the dimethyl terephthalate, a transesterification catalyst is added and the mixture is heated and stirred to carry out the transesterification while raising the temperature from 220 ° C to 230 ° C.
에스테르 교환반응이 완료되면 통상적으로 사용되는 중축합 촉매를 가하고 온도를 서서히 올려서 최종온도가 265℃∼285℃가 되게 하며, 서서히 감압하여 최종 감압도가 0.2torr 이하가 되도록 하여 100분간 반응을 진행시켜 극한점도 0.61의 폴리머를 얻었다.When the transesterification reaction is completed, a commonly used polycondensation catalyst is added and the temperature is gradually raised to a final temperature of 265 ° C. to 285 ° C., and the pressure is gradually reduced to a final pressure of 0.2torr or less to proceed with the reaction for 100 minutes. A polymer having an intrinsic viscosity of 0.61 was obtained.
이 중합체를 통상의 방법대로 방사 및 연신하고 절단하여 스테이플파이비를 만들고 방적 및 제적하여 난연성 및 항필링성을 측정하였다. 측정결과는 표 1에 나타냈다.The polymer was spun, stretched and cut in the usual manner to form a staple fiby and spun and dipped to measure flame retardancy and anti-pilling. The measurement results are shown in Table 1.
[실시예 2∼6 및 비교예 1∼4][Examples 2 to 6 and Comparative Examples 1 to 4]
일반식(Ⅰ) 및 (Ⅱ)의 화합물을 표 1에 기재된 양만큼 첨가한 것을 제외하고는 실시예 1과 동일한 방법으로 직물을 얻고, 물성을 측정 및 평가하여 그 결과를 표 1에 기재하였다.Except for the addition of the compounds of the general formula (I) and (II) in the amount shown in Table 1 to obtain a fabric in the same manner as in Example 1, measured and evaluated the physical properties and the results are shown in Table 1.
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