KR960011606B1 - Process for producing polyester embroider yarn - Google Patents
Process for producing polyester embroider yarn Download PDFInfo
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- KR960011606B1 KR960011606B1 KR1019940013745A KR19940013745A KR960011606B1 KR 960011606 B1 KR960011606 B1 KR 960011606B1 KR 1019940013745 A KR1019940013745 A KR 1019940013745A KR 19940013745 A KR19940013745 A KR 19940013745A KR 960011606 B1 KR960011606 B1 KR 960011606B1
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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
- 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
- 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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- Textile Engineering (AREA)
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
Description
본 발명은 폴리에스테르 자수사의 제조방법에 관한 것으로서, 더욱 상세하게는 폴리에스테르 수지의 중합공정에 첨가제를 소량 투입함으로써 인장강도와 파단신도를 동시에 낮추고 4단 연신공정의 이완 연신배율과 열처리 온도를 조정함으로써 열수수축율을 낮추어 폴리에스테르 자수사를 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a polyester embroidery thread, and more particularly, by adding a small amount of an additive to a polymerization process of a polyester resin, simultaneously reducing tensile strength and elongation at break, and adjusting the relaxation elongation ratio and heat treatment temperature of a four-stage drawing process. The present invention relates to a method for producing a polyester embroidery thread by lowering a heat shrinkage rate.
일반적으로 자수사는 염색성이 좋고 기계자수나 컴퓨터자수 공정성이 뛰어난 레이온 섬유가 주로 사용되어져 왔다. 그러나 레이온 섬유는 연사 등 중간작업공정에서 피부병을 유발시키는 문제 등으로 인하여 직업병을 유발하지 않는 폴리에스테르 섬유 등으로의 대체가 요구되게 되었다.In general, embroidery yarns have been mainly used for rayon fibers that have good dyeability and excellent machine embroidery or computer embroidery processes. However, rayon fibers have been required to be replaced with polyester fibers, which do not cause occupational diseases, due to problems such as skin failure in intermediate work processes such as yarn.
폴리에스테르 섬유가 자수사로 사용되려면 인장강도가 2.5~3.5g/d이고, 파단신도가 15~25%, 열수수축율이 2% 이하가 되어야 한다.To be used as embroidery yarns, polyester fibers must have a tensile strength of 2.5 to 3.5 g / d, an elongation at break of 15 to 25%, and a heat shrinkage of 2% or less.
인장강도가 2.5g/d 미만이면 연사 등 중간공정에서 사절이 일어나기 쉽고 인장강도가 3.5g/d 보다 크면 자수 후 커팅공정이 불량하여 외관이 불량하여진다. 그리고 파단신도가 15% 미만이면 중간공정이 불량하여지고 파단신도가 25%를 초과하면 자수 후 퍼커링(Puckering) 현상에 의해 자수표면이 볼록하여진다. 또한 열수수축율이 2%를 초과하면 히트세트공정에서 수축이 일어나 원단의 외관이 불량하여진다.If the tensile strength is less than 2.5g / d, trimming is likely to occur in intermediate processes such as weaving, and if the tensile strength is greater than 3.5g / d, the cutting process after embroidery is poor and the appearance is poor. If the elongation at break is less than 15%, the intermediate process is poor. If the elongation at break is more than 25%, the embroidery surface is convex due to puckering after embroidery. In addition, if the heat shrinkage exceeds 2%, shrinkage occurs in the heat set process, resulting in poor appearance of the fabric.
그러나 기존 폴리에스테르 섬유는 인장강도가 5.0g/d이고, 파단신도 30%이며, 열수수축율이 8% 수준으로 자수사용으로 사용하기에는 적합하지 않으며 인장강도와 파단신도는 반비례 관계이기 때문에 제조공정 조건의 변경으로 인장강도와 파단신도를 동시에 낮추는데는 어려운 문제점이 있다.However, the existing polyester fiber has a tensile strength of 5.0g / d, an elongation at break of 30%, a heat shrinkage rate of 8%, and is not suitable for use as embroidery, and the tensile strength and elongation at break are inversely related. It is difficult to simultaneously lower the tensile strength and elongation at break due to the change.
따라서, 본 발명은 기존의 폴리에스테르의 무제점을 해결한 것으로 폴리에스테르 수지의 중합공정에 첨가제를 투입하여 인장강도와 파단신도를 동시에 낮추고 4단 연신공정의 이완연신 배율과 열처리 온도를 조정함으로써 열수수축율을 낮추어 폴리에스테르 자수사를 제조하는 방법을 제공하는데 있다.Therefore, the present invention solves the problem of the existing polyester, by adding an additive to the polymerization process of the polyester resin to lower the tensile strength and elongation at the same time and to adjust the relaxation stretch ratio and heat treatment temperature of the four-stage stretching process It is to provide a method for producing a polyester embroidery yarn by reducing the shrinkage.
이하, 본 발명은 상세하게 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.
본 발명은 이관능성 카르복실산과 이관능성 글리콜을 축합반응시켜 폴리에스테르 자수사를 제조함에 있어서, 이관능성 카르복실산으로는 디메틸테레프탈레이트 100몰%에 디메틸설포네이트를 0.5~5.0몰%, 디메틸아디페이트 1~10몰%를 첨가하고 이관능성 글리콜로는 에틸렌글리콜을 사용하여 축중합한 다음 용융, 방사, 연신하여 인장강도가 2.5~3.5g/d, 파단신도가 15~25%, 열수수축율이 2% 미만임을 특징으로 하는 폴리에스테르 자수사의 제조방법에 관한 것이다.The present invention condensation reaction of bi-functional carboxylic acid and di-functional glycol to prepare polyester embroidery yarn, the bi-functional carboxylic acid in the dimethyl terephthalate 100 mol% 0.5 to 5.0 mol% dimethyl sulfonate, dimethyladi 1-10 mol% of pate was added and ethylene glycol was condensation-polymerized using difunctional glycol, followed by melting, spinning and stretching to obtain tensile strength of 2.5 to 3.5 g / d, elongation at break of 15 to 25%, and thermal shrinkage. It relates to a method for producing a polyester embroidery yarn characterized in that less than 2%.
이하, 본 발명을 더욱 상세하게 설명하면 다음과 같다.Hereinafter, the present invention will be described in more detail.
본 발명은 디메틸테레프탈레이트에 디메틸설포네이트와 디메틸아디페이트를 첨가한 다음 에틸렌글리콜을 축합반응시켜 폴리에스테르 중합체를 제조하고 이를 용융, 방사, 연신하여 폴리에스테르 자수사를 제조하는 방법에 관한 것으로, 일반적으로 디메틸설포네이트를 소량 첨가하면 폴리에스테르 섬유의 염색성이 향상되나 축합반응시 용융점도가 증가하여 일정한 수준의 분자량을 얻기가 어렵다고 알려져 있다.The present invention relates to a method for preparing a polyester embroidery yarn by adding dimethyl sulfonate and dimethyl adipate to dimethyl terephthalate and then condensing ethylene glycol to prepare a polyester polymer and melting, spinning and stretching it. The addition of a small amount of dimethylsulfonate improves the dyeability of the polyester fiber, but it is known that it is difficult to obtain a certain level of molecular weight due to an increase in the melt viscosity during the condensation reaction.
따라서, 디메틸설포네이트를 첨가함으로써 인장강도와 파단신도가 낮은 폴리에스테르 섬유를 얻을 수 있는데, 디메틸설포네이트의 첨가량이 0.5몰% 미만이면 강·신도 저하 효과가 거의 없고 5.0몰%를 초과하면 용융점도가 급격히 증가하여 중합공정이 불량하여진다.Therefore, polyester fiber having low tensile strength and elongation at break can be obtained by adding dimethyl sulfonate. When the amount of dimethyl sulfonate added is less than 0.5 mol%, there is almost no effect of lowering strength and elongation. Increases rapidly, resulting in poor polymerization process.
디메틸아디페이트를 첨가하면 용융점도가 낮아져서 중합공정을 향상시킬 수 있는데, 디메틸아디페이트의 첨가량이 1몰% 미만이면 용융점도 개선효과가 거의 없으며, 10몰%를 초과하면 비결정 부분이 많아져서 방사, 연신공정이 불량하여진다.When dimethyl adipate is added, the melt viscosity is lowered, thereby improving the polymerization process. If the amount of dimethyl adipate is less than 1 mol%, there is little effect of improving the melt viscosity. The stretching process is poor.
이때 얻어진 폴리에스테르 중합체의 고유점도가 0.5~0.6인 것이 공정성 및 물성측면에서 바람직하였는데, 고유점도가 0.5 미만이면 분자량이 낮아 섬유형성 능력이 떨어지며, 0.6 보다 크면 강·신도가 증가하여 자수사용으로는 적합하지 않다.At this time, the intrinsic viscosity of the obtained polyester polymer is preferably 0.5 to 0.6 in terms of processability and physical properties. If the intrinsic viscosity is less than 0.5, the molecular weight is low to lower the fiber forming ability. Inappropriate.
이렇게 얻어진 폴리에스테르 중합체를 방사, 연신하여 섬유를 제조하게 되는데 열수수축율을 낮추기 위하여 4단 연신의 이완 연신배율을 0.90~0.98로 하고, 열처리 온도를 200~240℃로 하는 것이 바람직하였는데, 이완 연신배율이 0.90 미만이면 과다한 이완에 의해 연신사도가 불량하여지고, 0.98을 초과하면 열수수축율의 개선효과가 적었으며, 또한 열처리 온도가 200℃ 미만이면 열처리 효과가 적으며, 240℃ 보다 높으면 사융착이 발생하였다.The polyester polymer thus obtained was spun and stretched to produce fibers. In order to lower the heat shrinkage rate, it was preferable to set the relaxation stretching ratio of the four-stage stretching to 0.90 to 0.98 and the heat treatment temperature to 200 to 240 ° C. If less than 0.90, the elongation is poor due to excessive relaxation, and if it exceeds 0.98, the effect of improving heat shrinkage is less. Also, if the heat treatment temperature is less than 200 ° C., the heat treatment effect is less. It was.
이와 같이 제조된 본 발명의 폴리에스테르 자수사는 인장강도가 2.5~3.5g/d이고, 파단신도가 15~25%이고, 열수수축율이 2% 미만으로 기존의 레이온 자수사를 대체할 수 있는 우수한 물성을 나타내었다.The polyester embroidery yarn of the present invention prepared as described above has excellent tensile strength of 2.5-3.5g / d, elongation at break of 15-25%, thermal shrinkage of less than 2%, and can replace existing rayon embroidery yarn. Indicated.
본 발명에서의 열수수축율은 JIS L 1073의 방법에 따라 평가하였는데 리일수축율 방법을 사용하여 측정하였다.The heat shrinkage rate in the present invention was evaluated according to the method of JIS L 1073, but was measured using the real shrinkage rate method.
이하, 본 발명을 실시예를 통하여 구체적으로 설명하겠는 바, 본 발명이 실시예에 의해 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail with reference to Examples, but the present invention is not limited by Examples.
[실시예 1]Example 1
교반기, 증류기, 질소 도입관을 갖춘 반응기에 디메틸테레프탈레이트 100몰%, 디메틸설포네이트 2.0몰%, 디메틸아디페이트 3.0몰%, 에틸렌글리콜 210몰%, 코발트아세테이트 0.021몰%, 소디움아세테이트 0.65몰%를 넣고 내온 160℃에서 에스테르 교환반응을 시키면서 2시간에 걸쳐 200℃로 승온한 후 이론 메탄올량의 85%이상의 메탄올을 유출시킨 후 트리메틸포스페이트 0.319몰%, 안티모니트리옥사이드 0.064몰%를 첨가하고 내온을 240℃로 승온한 후 저진공하에서 40분, 0.1mmHg이하의 고진공하에서 70분 반응을 시킨 후 칩 형상으로 제조하였으며, 이 수지의 오르소클로로페놀 용액의 고유점도는 0.55dl/g이었다.100 mol% of dimethyl terephthalate, 2.0 mol% of dimethylsulfonate, 3.0 mol% of dimethyl adipate, 210 mol% of ethylene glycol, 0.021 mol% of cobalt acetate, and 0.65 mol% of sodium acetate in a reactor equipped with a stirrer, a distillator, and a nitrogen inlet tube. After the temperature was raised to 200 ° C. over 2 hours while undergoing a transesterification reaction at 160 ° C., 0.385 mol% of trimethyl phosphate and 0.064 mol% of antimonitrioxide were added. After heating up to 240 ° C., 40 minutes of reaction under low vacuum and 70 minutes of reaction under high vacuum of 0.1 mmHg or less were made in the form of chips. The intrinsic viscosity of the orthochlorophenol solution was 0.55 dl / g.
이렇게 얻어진 수지를 130℃에서 3시간, 160℃에서 10시간 진공건조한 후 스크류압출식 방사기에서 직경 0.1mm, 36홀의 와이형 노즐을 통해 방사온도 300℃, 권취속도 1000m/분으로 해서 375데니어의 미연신사를 얻었다. 이 미연신사를 4단 연신기에서 연신속도 1000m/분, 1차 연신배율 1.006, 2차 연신배율 2.73, 3차 연신배율 1.199, 이완 연신배율 0.95, 열처리 온도 220℃의 조건으로 연신하여 120데니어의 연신사를 얻었다.The resin thus obtained was vacuum dried at 130 ° C. for 3 hours and at 160 ° C. for 10 hours, and then, at a screw extrusion type spinner, with a diameter of 0.1 mm and a 36-hole-type nozzle, the spinning temperature was 300 ° C. and the winding speed was 1000 m / min. Got a gentleman. The unstretched yarn is drawn in a four-stage drawing machine under the conditions of drawing speed of 1000m / min, first draw ratio 1.006, second draw ratio 2.73, third draw ratio 1.199, relaxation draw ratio 0.95, and heat treatment temperature 220 ℃. A drawing company was obtained.
이렇게 얻어진 연신사의 물성을 측정하여 표 1에 나타내었다.The physical properties of the drawn yarn thus obtained were measured and shown in Table 1.
[실시예 2]Example 2
실시예 1에서 디메틸설포네이트를 1.5몰%, 디메틸아디페이트를 5.0몰% 투입하고 실시예 1과 동일한 조건으로 반응을 시켰다. 이렇게 얻어진 수지의 고유점도는 0.58dl/g이었다.In Example 1, 1.5 mol% of dimethyl sulfonate and 5.0 mol% of dimethyl adipate were added thereto, and the reaction was carried out under the same conditions as in Example 1. The intrinsic viscosity of the resin thus obtained was 0.58 dl / g.
또한 실시예 1과 동일한 조건으로 방사하였고 4단 연신공정에서 이완 연신배율을 0.975, 열처리 온도 210℃의 조건으로 연신하여 연신사를 얻었으며, 연신사의 물성을 측정하여 표 1에 나타내었다.In addition, the yarns were spun under the same conditions as in Example 1, and stretched yarns were stretched under the conditions of 0.975 and a heat treatment temperature of 210 ° C. in the four-stage stretching process to obtain a stretched yarn.
[실시예 3]Example 3
실시예 1과 동일한 조건으로 중합반응을 시키면서 고진공하에서 60분 반응을 시킨 후 칩 형상으로 제조하였는데, 이렇게 얻어진 수지의 고유점도는 0.53dl/g이었다.After the polymerization reaction was carried out under the same conditions as in Example 1 for 60 minutes under high vacuum to prepare a chip shape, the intrinsic viscosity of the resin thus obtained was 0.53dl / g.
또한 실시예 1과 동일한 조건으로 방사하였고 4단 연신공정에서 이완 연신배율을 0.93으로 연신하여 연신사를 얻었다.In addition, the yarn was spun under the same conditions as in Example 1, and the stretched stretch ratio was stretched to 0.93 in the four-stage stretching process to obtain a stretched yarn.
[비교예 1]Comparative Example 1
실시예 1에서 디메틸설포네이트와 디메틸아디페이트를 첨가하지 않고 동일한 조건으로 중합반응을 실시하여 고유점도 0.53dl/g의 수지를 제조하였다.In Example 1, a polymerization reaction was performed under the same conditions without addition of dimethylsulfonate and dimethyl adipate, thereby preparing a resin having an intrinsic viscosity of 0.53 dl / g.
또한 실시예 1과 동일한 조건으로 방사, 연신하여 연신사를 얻었다.In addition, spinning and stretching were carried out under the same conditions as in Example 1 to obtain a stretched yarn.
[비교예 2]Comparative Example 2
실시예 2와 동일한 조건으로 중합반응을 시켜서 고진공하에서 90분 반응을 시킨 후 칩 형상으로 제조하였는데, 이렇게 얻어진 수지의 고유점도는 0.63dl/g이었다.After the polymerization reaction was carried out under the same conditions as in Example 2, the reaction was carried out under high vacuum for 90 minutes to prepare a chip shape. The inherent viscosity of the resin thus obtained was 0.63 dl / g.
또한 실시예 1과 동일한 조건으로 방사, 연신하여 연신사를 얻었다.In addition, spinning and stretching were carried out under the same conditions as in Example 1 to obtain a stretched yarn.
[비교예 3]Comparative Example 3
실시예 1과 동일한 조건으로 중합, 방사를 행한 후, 4단 연신공정에서 이완 연신배율 0.99, 열처리 온도 230℃의 조건으로 연신하여 연신사를 얻었다.After superposing | polymerizing and spinning on the conditions similar to Example 1, it extended | stretched on the conditions of relaxation stretch ratio 0.99 and heat processing temperature 230 degreeC in the 4-step drawing process, and obtained the stretched yarn.
Claims (3)
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KR1019940013745A KR960011606B1 (en) | 1994-06-17 | 1994-06-17 | Process for producing polyester embroider yarn |
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KR960011606B1 true KR960011606B1 (en) | 1996-08-24 |
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