KR100323611B1 - Manufacturing method of high shrinkage polyester bland - Google Patents
Manufacturing method of high shrinkage polyester bland Download PDFInfo
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- KR100323611B1 KR100323611B1 KR1019990033762A KR19990033762A KR100323611B1 KR 100323611 B1 KR100323611 B1 KR 100323611B1 KR 1019990033762 A KR1019990033762 A KR 1019990033762A KR 19990033762 A KR19990033762 A KR 19990033762A KR 100323611 B1 KR100323611 B1 KR 100323611B1
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- Prior art keywords
- pet
- polyester blend
- pei
- kneading
- shrinkage
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- 229920000728 polyester Polymers 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 22
- 229920000642 polymer Polymers 0.000 claims abstract description 22
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 8
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 4
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 abstract description 16
- 238000004898 kneading Methods 0.000 abstract description 14
- 238000009987 spinning Methods 0.000 abstract description 2
- 238000002074 melt spinning Methods 0.000 abstract 1
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 239000000835 fiber Substances 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 4
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 230000009477 glass transition Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- QPFMBZIOSGYJDE-UHFFFAOYSA-N 1,1,2,2-tetrachloroethane Chemical compound ClC(Cl)C(Cl)Cl QPFMBZIOSGYJDE-UHFFFAOYSA-N 0.000 description 2
- 238000005160 1H NMR spectroscopy Methods 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- 235000011037 adipic acid Nutrition 0.000 description 2
- 239000001361 adipic acid Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 150000002334 glycols Chemical class 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- TVTJEZFLHFYLOM-UHFFFAOYSA-N C(CO)O.[P] Chemical compound C(CO)O.[P] TVTJEZFLHFYLOM-UHFFFAOYSA-N 0.000 description 1
- 229920001634 Copolyester Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- JLVWYWVLMFVCDI-UHFFFAOYSA-N diethyl benzene-1,3-dicarboxylate Chemical compound CCOC(=O)C1=CC=CC(C(=O)OCC)=C1 JLVWYWVLMFVCDI-UHFFFAOYSA-N 0.000 description 1
- VNGOYPQMJFJDLV-UHFFFAOYSA-N dimethyl benzene-1,3-dicarboxylate Chemical compound COC(=O)C1=CC=CC(C(=O)OC)=C1 VNGOYPQMJFJDLV-UHFFFAOYSA-N 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- XRVCFZPJAHWYTB-UHFFFAOYSA-N prenderol Chemical compound CCC(CC)(CO)CO XRVCFZPJAHWYTB-UHFFFAOYSA-N 0.000 description 1
- 229950006800 prenderol Drugs 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000007573 shrinkage measurement Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C08G63/80—Solid-state polycondensation
-
- 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
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- 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
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyesters Or Polycarbonates (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
본 발명은 수축성이 높은 폴리에스테르 블랜드의 제조방법에 관한 것으로서 용융 방사 시에 방사성과 작업성을 향상시킬 수 있는 폴리에스테르 블랜드의 제조방법임.The present invention relates to a method for producing a high shrinkage polyester blend, a method for producing a polyester blend that can improve the spinning and workability during melt spinning.
본 발명은 폴리에틸렌테레프탈레이트(PET) 초기중합체와 폴리에틸렌이소프탈레이트(PEI) 초기 중합체를 각각 제조한 후 이들을 265∼300℃에서 5∼30분간 용융상태로 혼련시켜서 제조하는 방법임.The present invention is a method of preparing a polyethylene terephthalate (PET) prepolymer and a polyethylene isophthalate (PEI) initial polymer, respectively, and kneading them in a molten state at 265 to 300 ° C. for 5 to 30 minutes.
Description
본 발명은 폴리에틸렌테레프탈레이트(PET)와 폴리에틸렌이소프탈레이트(PEI)를 각각 따로 제조하여 고온에서 용융, 혼련(blending)하는 방법으로 낮은 제조 코스트와 높은 생산성의 고수축성 폴리에스테르 블랜드를 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a high shrinkable polyester blend of low production cost and high productivity by melting polyethylene and terephthalate (PET) and polyethylene isophthalate (PEI) separately and melting and kneading at a high temperature. will be.
종래의 폴리에스테르, 특히 PET는 우수한 내약품성, 내열성, 내후성, 고강력, 고탄성률 등을 보유하여 산업용 섬유, 필름, 용기, 일반 성형품등에 대량으로 사용되지만, 폴리에스테르 본래의 우수한 성능을 손상시키지 않는 범위에서 제3성분을 공중합하여 고수축성등 새로운 성능을 지닌 공중합 폴리에스테르를 얻고자 하는 시도가 많이 제안되어 있다.Conventional polyesters, especially PET, have excellent chemical resistance, heat resistance, weather resistance, high strength, high elastic modulus, and are used in large quantities in industrial fibers, films, containers, and general molded articles, but do not impair the excellent performance of polyester. Many attempts have been made to copolymerize a third component in the range to obtain a copolyester having new performance such as high shrinkage.
고수축성 PET 섬유의 제조 방법에 관한 기술은 많이 알려져 있으나, 공업적으로 유용하고 현재 가장 많이 이용되고 있는 방법은 중합체의 중합 공정에서 산성분인 아디핀산, 세바스산 등의 카르본산을 사용하거나 알코올 성분인 에틸렌 글리콜 대신 디에틸렌 글리콜, 2,2-디메틸-1,3 프로판디올, 2,2-디에틸-1,3 프로판디올등의 고급 글리콜이나 치환된 글리콜을 이용하여 공중합하는 방법을 사용하고 있다.Although there are many known techniques for producing highly shrinkable PET fibers, industrially useful methods and the most widely used methods are carboxylic acids such as adipic acid and sebacic acid, which are used in the polymerization process of polymers, or alcohol components. Instead of phosphorus ethylene glycol, copolymerization is performed using higher glycols or substituted glycols such as diethylene glycol, 2,2-dimethyl-1,3 propanediol, and 2,2-diethyl-1,3 propanediol. .
이 방법은 섬유 구조 내에 비결정부를 많이 형성시키는 방법인데, 이 중 아디핀산, 세바스산 혹은 상기의 디올을 사용하는 경우에는 유리 전이 온도가 낮아져 저온에서 수축이 생기는 저온 수축 현상이 나타나는 단점이 있다.This method is a method of forming a large number of amorphous portions in the fiber structure, of which adipic acid, sebacic acid or the above-mentioned diol is used when the glass transition temperature is low, there is a disadvantage that the low temperature shrinkage phenomenon that occurs shrinkage at low temperatures.
또한, 이소프탈산이나 그의 유도체를 사용하는 경우에는 중합체 내의 분자쇄 꺽임이 부여되어 결정화 온도가 높아지고, 결정화 속도가 저하되어 비결정 영역이 많이 생성되어 고수축사를 만들 수 있게 된다.In addition, when isophthalic acid or its derivatives are used, molecular chain breakage in the polymer is imparted, the crystallization temperature is increased, the crystallization rate is lowered, and a large number of amorphous regions are generated, thereby making it possible to produce high shrinkage yarns.
그러나, 이 방법을 포함한 기존의 방법들은 모두 배치(batch)중합 방식으로 생산되고 있는바, 이와 같은 배치방식은 생산성이 낮고 제조 경비가 높아서 원가 면에서 불리한 점을 안고 있다.However, the existing methods including this method are all produced by batch polymerization method, which has disadvantages in terms of cost due to low productivity and high manufacturing cost.
본 발명은 고수축성 폴리에스테르 블랜드를 저 비용으로 생산성 높게 제조하는 방법을 제공하는 데 그 목적을 둔 것이다.The present invention aims to provide a method for producing a highly shrinkable polyester blend at low cost and with high productivity.
본 발명은 극한점도(IV)가 0.4∼0.9dl/g인 폴리에틸렌테레프탈레이트 초기 중합체 80∼95몰%와 극한점도가 0.4∼0.9dl/g인 폴리에틸렌이소프탈레이트 초기 중합체 5∼20몰%를 265∼300℃의 온도에서 5∼30분간 용융, 혼련시키는 것을 특징으로 하는 고수축성 폴리에스테르 블랜드의 제조방법에 관한 것이다.The present invention is 80 to 95 mol% of polyethylene terephthalate initial polymer having an intrinsic viscosity (IV) of 0.4 to 0.9 dl / g and 5 to 20 mol% of polyethylene isophthalate initial polymer having an intrinsic viscosity of 0.4 to 0.9 dl / g. It relates to a method for producing a highly shrinkable polyester blend, which is melted and kneaded at a temperature of 300 ° C. for 5 to 30 minutes.
이하, 본 발명을 보다 상세하게 설명하기로 한다.Hereinafter, the present invention will be described in more detail.
본 발명에서는 PET와 PEI를 연속중합방식에 의하여 각각 따로 제조하여 용융, 혼련시키는 방법을 사용함으로써 이소프탈산을 공중합시키는 배치 중합 방식보다 생산성이 높게 고수축성 폴리에스테르 블랜드를 제조할 수 있으며, 또 낮은 비용으로 제조할 수 있다.In the present invention, by using a method of separately producing the PET and PEI by the continuous polymerization method, melting and kneading, it is possible to produce a highly shrinkable polyester blend with higher productivity than the batch polymerization method of isophthalic acid copolymerization, and low cost It can be prepared by.
특히, 본 발명은 PET 초기 중합체 약 80 내지 95몰%와 PEI 초기 중합체 5몰 내지 20몰%의 혼합물을 단축 또는 이축 혼련기에서 용융, 블렌딩시켜서 극한점도(IV) 0.60dl/g 이상, 수축률 20∼25% 이상의 고수축성 폴리에스테르 블랜드를 제조할 수 있다.In particular, the present invention melts and blends a mixture of about 80 to 95 mol% of PET initial polymer and 5 to 20 mol% of PEI initial polymer in a single or twin screw kneader to yield an ultimate viscosity (IV) of at least 0.60 dl / g, shrinkage of 20 High shrinkage polyester blends of at least -25% can be prepared.
예를 들면 PEI는 이소프탈산 또는 디에스테르(디메틸 이소프탈산레이트 또는 디에틸이소프탈레이트)를 통상적인 방법인 에틸렌 글리콜(EG)과 반응시킴으로써 제조할 수 있으며, 보통 모든 반응물은 축중합 단계가 이어지는 에스테르화 또는 트랜스 에스테르화 단계에 첨가하여 PEI 초기 중합체를 제조한다.For example, PEI can be prepared by reacting isophthalic acid or diesters (dimethyl isophthalate or diethylisophthalate) with conventional ethylene glycol (EG), usually all reactants are esterified followed by a condensation polymerization step. Or in addition to the trans esterification step to prepare the PEI initial polymer.
PET 초기 중합체 역시 유사한 방법으로 제조할 수 있다.PET initial polymers can also be prepared in a similar manner.
본 발명의 방법에 사용된 PET 및 PEI 초기 중합체는 극한점도(IV) 0.4dl/g 이상이며, 바람직하게는 각각의 초기 중합체는 0.4에서 0.9dl/g의 극한점도(IV)를 가지며, 더욱 좋기로는 보통 0.55 내지 0.70dl/g의 극한점도를 갖는다.The PET and PEI initial polymers used in the process of the present invention have an ultimate viscosity (IV) of at least 0.4 dl / g, preferably each initial polymer has an ultimate viscosity (IV) of 0.4 to 0.9 dl / g, and even better. The furnace usually has an intrinsic viscosity of 0.55 to 0.70 dl / g.
고온에서 용융 블렌딩하는 PET와 PEI 초기 중합체의 혼합물을 제조하기 위해서 단축 또는 이축 압출기내에서 시키는 방법을 사용하였다.The process was carried out in a single screw or twin screw extruder to produce a mixture of PET and PEI initial polymer melt blended at high temperature.
이 경우 각각 따로 제조한 PEI와 PET의 칩을 함께 혼합한다.In this case, the chips of PEI and PET prepared separately are mixed together.
용융 혼련기에 공급된 PET와 PEI 초기 중합체는 265∼300℃의 온도에서 5∼30분간 용융, 혼련되어 폴리에스테르 블랜드가 제조된다.The PET and PEI initial polymer supplied to the melt kneader are melted and kneaded at a temperature of 265 to 300 ° C. for 5 to 30 minutes to prepare a polyester blend.
혼련 온도가 265℃ 미만이며 중합체와의 융점 차이가 적어서 혼련 및 반응이 불충분하게 이루어지므로 균일한 폴리에스테르 블랜드가 얻어지기 힘들며, 300℃를 넘게 되면 열분해를 일으켜서 바람직하지 않게 된다.Since the kneading temperature is less than 265 ° C. and the melting point with the polymer is small, the kneading and the reaction are insufficient, so that a uniform polyester blend is hardly obtained, and when it exceeds 300 ° C., thermal decomposition occurs, which is undesirable.
또한 혼련시간이 5분 미만이면 반응을 동반한 충분한 혼련이 이루어지지 않고, 균일한 폴리에스테르 블랜드가 얻어지기 힘들며, 30분을 초과하면 열분해를 일으켜서 바람직하지 않게 된다.In addition, when the kneading time is less than 5 minutes, sufficient kneading with the reaction is not performed, and a uniform polyester blend is hardly obtained, and when the kneading time is more than 30 minutes, thermal decomposition occurs, which is undesirable.
용융, 혼련되는 두 중합체의 비율은 PET 80 내지 95 몰%와 PEI 5 내지 20몰%를 사용한다.The ratio of the two polymers to be melted and kneaded uses 80 to 95 mol% of PET and 5 to 20 mol% of PEI.
바람직하게는 PET 85 내지 90몰%와 PEI 10 내지 15몰%를 사용한다.Preferably, 85 to 90 mol% PET and 10 to 15 mol% PEI are used.
용융 혼련 후 얻어지는 혼합물 상태의 폴리에스테르 블랜드는 응고 후 칩(chip) 또는 펠렛(pellet) 상태로 제조하여 통상의 PET 섬유 제조 장치를 사용하여 방사, 연신 및 권축할 수 있다.The blended polyester blend obtained after melt kneading may be prepared in a chip or pellet state after solidification and spun, stretched and crimped using a conventional PET fiber manufacturing apparatus.
실시 예에 나타난 평가 항목의 측정은 다음과 같다.The measurement of the evaluation item shown in the Example is as follows.
시험방법Test Methods
1. 이소프탈산의 몰% 측정1. Measurement of mole% of isophthalic acid
폴리에스테르 블랜드의 이소프탈산 몰%는 폴리에스테르 브랜드를 트리플로로 아세트산에 용해하여 부루커(Bruker)사의 DRX-300 프로톤 핵 자기공명장치(1H NMR)를 이용하여 측정하였다.The molar% of isophthalic acid of the polyester blend was measured using a DRX-300 proton nuclear magnetic resonance apparatus (1H NMR) from Bruker by dissolving the polyester brand in trichloroacetic acid.
2. 유리전이온도 및 융점 측정2. Glass transition temperature and melting point measurement
열시차주사열량계(Perkin Elmer DSC-7)를 이용하여 유리전이온도와 융점을 측정하였다.The glass transition temperature and melting point were measured using a differential differential scanning calorimeter (Perkin Elmer DSC-7).
3. 극한점도(Intrinsic Viscosity : IV)3. Intrinsic Viscosity (IV)
칩을 페놀/테트라클로로에탄(중량비 50/50)에 녹여 0.5wt% 용액을 만든 후 우베드로 점도계로 25℃에서 측정하였다.The chip was dissolved in phenol / tetrachloroethane (50/50 by weight) to make a 0.5 wt% solution, and then measured at 25 ° C. with an Ubedro viscometer.
4. 수축률 측정4. Shrinkage Measurement
100℃의 물에서 무장력 하에서 초기 길이에 대한 수축한 길이의 비로 수축률을 측정하였다.Shrinkage was measured as the ratio of the retracted length to the initial length under tension in water at 100 ° C.
실시예 1∼5Examples 1-5
PET 초기 중합체와 PEI 초기 중합체를 몰%와 혼련 조건을 변화시키면서 이축 혼련기로 혼련하였다.PET initial polymer and PEI initial polymer were kneaded with a biaxial kneader with varying molar% and kneading conditions.
이 두 초기 중합체의 용융 혼합물은 조건에 따라 특성치가 다르게 나타났다.The molten mixture of these two initial polymers showed different properties depending on the conditions.
두 초기 중합체가 균일한 폴리에스테르 블랜드를 형성시킨다는 사실은 핵 자기공명장치(1H NMR)를 이용하여 확인하였다.The fact that the two initial polymers form a uniform polyester blend was confirmed using nuclear magnetic resonance devices (1H NMR).
제조된 폴리에스테르 블랜드를 280℃에서 1,000m/분의 속도로 용융 방사한 후 연신 온도 75∼85℃, 연신 배율 3.4∼3.7배, 열고정 온도 190∼230℃의 조건으로 연신하여 80데니어/24필라멘트인 고수축성 폴리에스테르 블랜드로 섬유를 제조하였다.The polyester blend was melt spun at 280 ° C. at a rate of 1,000 m / min, and then stretched under the conditions of a stretching temperature of 75 to 85 ° C., a stretching ratio of 3.4 to 3.7 times, and a heat setting temperature of 190 to 230 ° C. to 80 denier / 24. The fibers were made from a filament high shrink polyester blend.
* 방사성 및 작업성 ◎ : 매우 좋음, ○: 좋음, △ : 보통, ×: 나쁨* Radioactive and workability ◎: Very good, ○: Good, △: Normal, ×: Poor
비교예 1∼2Comparative Examples 1 and 2
초기 중합체의 점도를 낮게 하거나 혼련 조건을 변화시키는 것 이외에는 실시예 1∼5의 조건과 동일하게 제조하였다.It manufactured like the conditions of Examples 1-5 except having made the viscosity of an initial polymer low or changing kneading conditions.
혼련 시간이 짧았을 경우 균일한 폴리에스테르 블랜드를 얻을 수 없었으며 그로 인하여 수축률도 낮은 결과를 나타내었고, 혼련 시간이 너무 길게 되면 열분해 효과가 나타나 극한점도가 낮아지고 방사성 및 작업성도 좋지 않았다.When the kneading time was short, it was not possible to obtain a uniform polyester blend, and as a result, the shrinkage ratio was also low. When the kneading time was too long, the pyrolysis effect was lowered, the intrinsic viscosity was lowered, and radioactivity and workability were not good.
비교예 3Comparative Example 3
PET/PEI 몰%와 혼련 조건을 변화시키는 것 이외에는 실시예 1∼5의 조건과 동일하게 하였다.It carried out similarly to the conditions of Examples 1-5 except changing PET / PEI mol% and kneading conditions.
PEI의 몰%가 높게 되면 수축성이 현저하게 저하되는 결과를 나타내었다.When the mole% of PEI was high, shrinkage was remarkably reduced.
비교예 4Comparative Example 4
이소프탈산을 이용하여 기존의 배치(batch) 중합 공정대로 공중합 폴리에스테르를 제조하였으며 방사 및 연신 등의 조건은 실시예 1∼5와 동일하게 하였다.Co-polyester was prepared according to a conventional batch polymerization process using isophthalic acid, and the conditions such as spinning and stretching were the same as in Examples 1 to 5.
기존의 배치 방식의 경우 수축률이 본 발명보다도 낮게 측정되었다.In the case of the conventional batch method, the shrinkage was lower than that of the present invention.
본 발명으로 제조한 폴리에스테르 블랜드는 종래의 배치식 방법으로 제조한 것에 비하여 높은 수축률을 나타냈으며 방사성과 작업성도 향상시킬 수 있다.The polyester blends produced by the present invention exhibited higher shrinkage and improved radioactivity and workability compared to those produced by conventional batch methods.
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