KR100587903B1 - A polyurethane elastic fiber, and a process of preparing the same - Google Patents

A polyurethane elastic fiber, and a process of preparing the same Download PDF

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KR100587903B1
KR100587903B1 KR1019990031903A KR19990031903A KR100587903B1 KR 100587903 B1 KR100587903 B1 KR 100587903B1 KR 1019990031903 A KR1019990031903 A KR 1019990031903A KR 19990031903 A KR19990031903 A KR 19990031903A KR 100587903 B1 KR100587903 B1 KR 100587903B1
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polyurethane elastic
elastic fiber
heat treatment
heat
shrinkage
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KR1019990031903A
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Korean (ko)
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KR20010016788A (en
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정길영
김시민
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주식회사 코오롱
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/70Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyurethanes
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/10Filtering or de-aerating the spinning solution or melt
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/04Dry spinning methods
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G1/00Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
    • D02G1/02Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist
    • D02G1/0206Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist by false-twisting
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02JFINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J13/00Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass
    • D02J13/001Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass in a tube or vessel

Abstract

본 발명은 열수축율이 낮은 폴리우레탄 탄성섬유 및 그의 제조방법에 관한 것이다.The present invention relates to a polyurethane elastic fiber having a low heat shrinkage and a process for producing the same.

본 발명은 방사, 가연(False Twisting) 및 권취공정순으로 폴리우레탄 탄성섬유를 제조함에 있어서, 상기 방사공정 아래에 열처리장치(14)를 설치하여 방사된 탄성섬유를 열처리하여 비등수수축율이 7% 이하이며, 100℃의 열풍오븐에서 1시간 처리후의 열수축율이 5% 이하인 폴리우레탄 탄성섬유를 제조한다.The present invention relates to a process for producing a polyurethane elastic fiber in the order of spinning, false twisting and winding process, wherein a heat treatment device (14) is provided under the spinning process to heat the spun elastic fiber to obtain a boiling water shrinkage ratio of 7% , And a polyurethane elastic fiber having a heat shrinkage of 5% or less after being treated in a hot air oven at 100 캜 for 1 hour is produced.

본 발명의 폴리우레탄 탄성섬유는 고품질의 스포츠용 의류 제조 등에 사용된다.The polyurethane elastic fiber of the present invention is used for manufacturing high quality sports clothing.

열수축율, 폴리우레탄, 탄성섬유, 열처리, 히팅튜브, 비등수수축율Heat shrinkage, polyurethane, elastic fiber, heat treatment, heating tube, boiling water shrinkage

Description

폴리우레탄 탄성섬유 및 그의 제조방법 {A polyurethane elastic fiber, and a process of preparing the same} TECHNICAL FIELD [0001] The present invention relates to a polyurethane elastic fiber and a process for preparing the same,             

도 1은 폴리우레탄 탄성섬유를 제조하는 종래의 공정 개략도 이다.BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic view of a conventional process for producing polyurethane elastic fibers. Fig.

도 2는 폴리우레탄 탄성섬유를 제조하는 본 발명의 공정 개략도 이다.2 is a schematic view of the process of the present invention for producing polyurethane elastic fibers.

* 도면중 주요부분에 대한 부호설명[0001] Description of the Related Art [0002]

1 : 방사원액 2 : 기어펌프 3 : 고온가스 유입구1: spinning stock solution 2: gear pump 3: hot gas inlet

4 : 방사구금 5 : 방사튜브 6 : 합착점4: spinneret 5: radiation tube 6: cemented point

7 : 가스배출구 8 : 가스유입구 9 : 가연기(False Twisting Unit)7: gas outlet 8: gas inlet 9: false twisting unit

10, 12 : 고뎃로울러 11 : 유제처리 로울러10, 12: Godet roller 11: Emulsion treatment roller

13 : 권취기 14 : 열처리장치 15 : 온도공급 및 제어기13: Winder 14: Heat treatment device 15: Temperature supply and controller

본 발명은 열수축율이 낮은 폴리우레탄 탄성섬유 및 그의 제조방법에 관한 것이다.The present invention relates to a polyurethane elastic fiber having a low heat shrinkage and a process for producing the same.

폴리우레탄 탄성섬유는 폴리우레탄 중합체를 주로 건식방사하여 제조된다.Polyurethane elastomeric fibers are produced by predominantly dry spinning of polyurethane polymers.

상기 폴리우레탄 중합체는 일반적으로 고분자량의 폴리올(디올화합물)과 과량의 디이소시아네이트화합물을 먼저 예비중합하여 1단계로 예비중합체를 제조한 다음, 여기에 디올 또는 디아민화합물인 쇄연장제를 투입하여 2단계로 쇄연장 및 쇄정지 반응 시키는 2단계 중합법으로 제조한다.The polyurethane polymer is prepared by first preliminarily polymerizing a high molecular weight polyol (diol compound) and an excess amount of a diisocyanate compound to prepare a prepolymer in one step, and then adding a chain extender such as a diol or a diamine compound thereto to prepare 2 Stage chain extension and chain termination reaction.

보다 구체적으로 상기 1단계 예비중합은 고분자량의 디올화합물인 폴리올(Polyol)과 과량의 디이소시아네이트의 반응에 의해 우레탄결합을 형성하며, 폴리올의 양말단에 이소시아네이트기를 가지는 예비중합체를 만드는 단계이다. More specifically, the one-step prepolymerization is a step of forming a urethane bond by reacting a high molecular weight diol compound, a polyol, with an excess of a diisocyanate, and forming a prepolymer having isocyanate groups at both ends of the polyol.

예비중합체는 15~30%의 하드세그멘트(Hard segment)함량을 갖는다. 일반적으로 폴리올의 분자량은 2,000g/몰 정도이며, NCO/OH비는 2에 가까운 값으로 중합이 진행된다. 상기 예비중합은 보통 용제가 없는 벌키상태로 약 60~90℃에서 1~2시간에 반응이 완료된다. The prepolymer has a hard segment content of 15-30%. Generally, the molecular weight of the polyol is about 2,000 g / mole, and the polymerization proceeds at a value close to 2 in the NCO / OH ratio. The prepolymerization is usually carried out in a solvent-free, bulky state at about 60 to 90 DEG C for 1 to 2 hours.

반응온도가 높을수록 반응속도는 빨라지며 디메틸아세트아미드(이하 "DMAc"라고 한다)나 디메틸포름아미드(이하 "DMF"라고 한다)와 같은 용매를 사용하면 용매의 촉매작용에 의해 반응속도가 상승하여 30~60℃에서 10~20분내에 반응이 완료된다.The higher the reaction temperature, the faster the reaction rate. When a solvent such as dimethylacetamide (hereinafter referred to as "DMAc") or dimethylformamide (hereinafter referred to as "DMF") is used, the reaction rate is increased by the catalytic action of the solvent The reaction is completed at 30 to 60 ° C within 10 to 20 minutes.

상기 2단계 쇄연장반응은 쇄연장제인 에틸렌디아민, 프로필렌디아민, 1,4-부탄디올 등과 같은 저분자량의 활성수소를 갖는 화합물과 예비중합체의 반응에 의해 중합도를 높이는 반응이다.The two-step chain extension reaction is a reaction for increasing the degree of polymerization by reacting a prepolymer with a compound having a low molecular weight active hydrogen such as ethylenediamine, propylenediamine, 1,4-butanediol, etc. as a chain extender.

디아민(Diamine)과 반응시킬 경우 우레아(uera)결합이 형성되며, 디올(Diol) 과 반응시키면 우레탄(Urethane)결합이 형성된다. 쇄연장반응은 예비중합과 달리 반응속도가 빠르며 발열반응이기 때문에 균일한 반응을 위해서 DMAc나 DMF와 같은 극성용매를 사용하여 용액중합을 한다. When reacted with a diamine, a urea bond is formed, and when it is reacted with a diol, a urea bond is formed. Since the chain extension reaction is an exothermic reaction which is different from the prepolymerization, the solution polymerization is carried out using a polar solvent such as DMAc or DMF for a uniform reaction.

특히 디아민(Diamine)이 쇄연장제로 사용될 경우 반응속도가 극히 빠르기 때문에 균일한 반응조건을 유지하기 위해서는 0~15℃의 저온에서 반응을 진행시키며 쇄연장제를 반응전기간에 걸처 서서히 투입한다. 또한 반응속도 및 반응도를 조절하기 위해 소량의 모노아민이 쇄연장 반응시 사용된다.In particular, when the diamine is used as a chain extender, the reaction rate is extremely high. Therefore, to maintain uniform reaction conditions, the reaction is carried out at a low temperature of 0 to 15 ° C. and the chain extender is slowly added throughout the reaction. A small amount of monoamine is used in the chain extension reaction to control the reaction rate and reactivity.

종래 폴리우레탄 탄성섬유는 이와 같이 중합된 폴리우레탄 중합체용액(이하 "방사원액"이라고 한다)을 도 1의 공정으로 건식방사하여 제조해 왔다.Conventionally, the polyurethane elastic fibers have been produced by dry-spinning the polymerized polyurethane polymer solution (hereinafter referred to as "spinning stock solution") in the process of Fig.

구체적으로 탈포, 여과를 거친 방사원액(1)을 기어펌프(2)를 이용하여 방사구금(4)을 통해 방사튜브(5)내로 토출한다. 이와 동시에 상기 방사튜브(5) 상부에 위치하는 고온가스유입구(3)을 통해 방사튜브(5) 내로 고온가스를 유입시킨다.Specifically, the spinning stock solution 1 subjected to defoaming and filtration is discharged into the spinning tube 5 through the spinneret 4 using the gear pump 2. At the same time, the hot gas is introduced into the radiation tube 5 through the hot gas inlet 3 located above the radiation tube 5.

그 결과, 토출된 필라멘트중의 용제는 고온가스에 의해 증발, 확산되고, 필라멘트의 고화 및 세화가 진행된다. 용제를 함유하는 고온가스는 방사튜브(5) 하단에 위치하는 가스배출구(7)를 통해 방사튜브(5) 밖으로 배출된다.As a result, the solvent in the discharged filament is evaporated and diffused by the hot gas, and the filament is solidified and refined. The hot gas containing the solvent is discharged to the outside of the radiation tube 5 through the gas outlet 7 located at the lower end of the radiation tube 5.

방사튜브(5)를 통과한 필라멘트는 계속해서 가연기[False Twisting Unit(9)]에서 가연처리된다. 그 결과 상기 필라멘트는 방사튜브(5)내의 일정지점(이하 "합착점(6)"이라고 한다)에서 서로 융착되어 모노필라멘트(Mono filament) 상으로 된다.The filament that has passed through the radiation tube 5 is then subjected to a false twist in the false twisting unit 9. As a result, the filaments are fused to each other at a certain point (hereinafter referred to as "cementing point 6") in the radiation tube 5 to be in the form of monofilaments.

이와 같은 가연처리에 의해 후공정시 사절을 예방 할수 있다. 가연기(9)를 통과한 필라멘트는 고뎃로울러(10, 12) 및 유제처리로울러(11)를 거처 권취기(13)에 권취된다.By such a burning treatment, it is possible to prevent embossing in a post-process. The filaments passing through the combustor 9 are wound around the godet rollers 10 and 12 and the emulsion treatment rollers 11 to the take-up machine 13.

상기와 같은 종래 건식방사 방법으로 제조된 폴리우레탄 탄성섬유는 염색 및 가공 등의 후공정에서 가해지는 비등수처리 및 열처리에 의해 너무 많이 수축되는 문제가 있었다. 비등수처리 및 열처리시 과도한 수축은 후공정성을 저하시킬 뿐만 아니라 최종 가공 직편물의 품질도 저하 시킨다.The polyurethane elastic fibers produced by the conventional dry spinning method as described above have a problem that they are shrunk too much by the boiling water treatment and the heat treatment which are applied in post-processes such as dyeing and processing. Excessive shrinkage during boiling water treatment and heat treatment not only lowers post-processability but also lowers the quality of the final processed knitted fabric.

이와 같은 문제점을 해결하기 위하여 종래 건식방사(도 1의 공정)중 방사튜브(5) 내부의 온도나 가연기(9)의 온도를 적절히 조절하거나, 고뎃로울러(10, 12)나 권취기(13)의 회전속도를 적절히 조절하는 방법이 시도되고 있으나, 근본적으로 비등수처리 및 열처리에 의해 폴리우레탄 탄성섬유가 너무많이 수축되는 문제를 해결할수 없었다.In order to solve such a problem, the temperature inside the spinning tube 5 and the temperature of the combustor 9 in the conventional dry spinning (the process of FIG. 1) are appropriately adjusted or the temperature of the godet rollers 10, 12 and the winder 13 ). However, the problem of too much shrinkage of the polyurethane elastic fibers due to boiling water treatment and heat treatment could not be solved.

본 발명의 목적은 후공정성 및 가공원단의 품질향상을 위해 열수축율이 낮은, 다시말해 열적성질이 안정화된 폴리우레탄 탄성섬유를 제공하기 위한 것이다.An object of the present invention is to provide a polyurethane elastic fiber having a low heat shrinkage, that is, a thermally stabilized thermal property, in order to improve the post-processability and the quality of the processed fabric.

본 발명은 열적성질이 안정되어 비등수처리나 열처리시 수축율이 낮은 폴리우레탄 탄성섬유 및 그의 제조방법을 제공하고자 한다.
Disclosed is a polyurethane elastic fiber having a stable thermal property and a low shrinkage ratio during boiling water treatment or heat treatment, and a process for producing the same.

본 발명은 비등수처리나 열처리시 수축율이 낮은 폴리우레탄 탄성섬유 및 그의 제조방법에 관한 것이다.The present invention relates to a polyurethane elastic fiber having a low shrinkage ratio during boiling water treatment or heat treatment, and a process for producing the same.

더욱 구체적으로 본 발명은 비등수수축율이 7% 이하이며, 100℃의 열풍오븐에서 1시간 처리후의 열수축율이 5% 이하인 것을 특징으로 하는 폴리우레탄 탄성섬유에 관한 것이다.More specifically, the present invention relates to a polyurethane elastic fiber characterized by a boiling water shrinkage of 7% or less and a heat shrinkage of 5% or less after being treated in a hot air oven at 100 캜 for 1 hour.

또한 본 발명은 방사, 가연(False Twisting) 및 권취공정순으로 폴리우레탄 탄성섬유를 제조함에 있어서, 상기 방상공정 아래에 열처리장치(14)를 설치하여 방사된 탄성섬유를 열처리함을 특징으로 하는 폴리우레탄 탄성섬유의 제조방법에 관한 것이다.The present invention also provides a method for producing polyurethane elastic fibers in the order of spinning, false twisting and winding, wherein a heat treatment device (14) is provided under the above-mentioned emulsification step to heat- To a method for producing elastic fibers.

이하 본 발명을 상세하게 설명한다.Hereinafter, the present invention will be described in detail.

먼저 본 발명은 고분자량의 디올화합물(폴리올)과 과량의 디이소시아네이트 화합물을 반응시켜 폴리올의 양말단에 이소시아네이트기를 가지는 예비중합체를 제조한다.First, the present invention provides a prepolymer having an isocyanate group at both ends of a polyol by reacting a high molecular weight diol compound (polyol) with an excessive amount of a diisocyanate compound.

이때 고분자량의 디올화합물로는 폴리테트라메틸렌글리콜(PTMG)을 디이소시아네이트 화합물로는 4,4'-디페닐메탄디이소시아네이트를 사용하는 것이 바람직 하다.At this time, it is preferable to use polytetramethylene glycol (PTMG) as the high molecular weight diol compound and 4,4'-diphenylmethane diisocyanate as the diisocyanate compound.

다음으로 상기 예비중합체에 디메틸아세트아미드(DMAC) 또는 디메틸포름아미드(DMF) 등의 유기용매를 첨가하여 예비중합체 용액을 제조한다.Next, the addition of organic solvents such as dimethylacetamide (DM AC) or dimethylformamide (DMF) to the prepolymer to prepare a prepolymer solution.

계속해서 상기 예비중합체에 쇄연장제로서 에틸렌디아민과 같은 디아민 화합 물을 첨가하여 예비중합체의 중합도를 향상시킨다. 이때 균일한 반응조건을 유지하기 위해 온도를 0~15℃로 유지하면서, 상기 쇄연장제를 반응전기간에 걸쳐 서서히 투입하는 것이 바람직 하다.Subsequently, a diamine compound such as ethylenediamine is added to the prepolymer as a chain extender to improve the degree of polymerization of the prepolymer. At this time, in order to maintain uniform reaction conditions, it is preferable that the chain extender is gradually added over the entire reaction period while maintaining the temperature at 0 to 15 ° C.

이와 같이 중합된 폴리우레탄 중합체용액(방사원액)을 도 2의 공정으로 건식방사하여 본 발명의 폴리우레탄 탄성섬유를 제조한다. 도 2는 본 발명의 공정 개략도 이다.The polyurethane polymer solution (spinning solution) thus polymerized is dry-spun by the process of Fig. 2 to produce the polyurethane elastic fiber of the present invention. 2 is a schematic process drawing of the present invention.

구체적으로 탈포, 여과를 거친 방사원액(1)을 기어펌프(2)를 이용하여 방사구금(4)을 통해 방사튜브(5)내로 토출한다. 이와 동시에 상기 방사튜브(5) 상부에 위치하는 고온가스유입구(3)을 통해 방사튜브(5) 내로 고온가스를 유입시킨다.Specifically, the spinning stock solution 1 subjected to defoaming and filtration is discharged into the spinning tube 5 through the spinneret 4 using the gear pump 2. At the same time, the hot gas is introduced into the radiation tube 5 through the hot gas inlet 3 located above the radiation tube 5.

그 결과, 토출된 필라멘트중의 용제는 고온가스에 의해 증발, 확산되고, 필라멘트의 고화 및 세화가 진행된다. 용제를 함유하는 고온가스는 방사튜브(5) 하단에 위치하는 가스배출구(7)를 통해 방사튜브(5) 밖으로 배출된다.As a result, the solvent in the discharged filament is evaporated and diffused by the hot gas, and the filament is solidified and refined. The hot gas containing the solvent is discharged to the outside of the radiation tube 5 through the gas outlet 7 located at the lower end of the radiation tube 5.

방사튜브(5)를 통과한 필라멘트는 계속해서 가연기[False Twisting Unit(9)]에서 가연처리된다. 그 결과 상기 필라멘트는 방사튜브(5)내의 일정지점(이하 "합착점(6)"이라고 한다)에서 서로 융착되어 모노필라멘트(Mono filament) 상으로 된다. 이와 같은 가연처리에 의해 후공정시 사절을 예방 할수 있다.The filament that has passed through the radiation tube 5 is then subjected to a false twist in the false twisting unit 9. As a result, the filaments are fused to each other at a certain point (hereinafter referred to as "cementing point 6") in the radiation tube 5 to be in the form of monofilaments. By such a burning treatment, it is possible to prevent embossing in a post-process.

계속해서 가연기(9)를 통과한 필라멘트는 열처리장치(14)에서 100℃ 이상의 온도로 열처리된 후 고뎃로울러(10, 12) 및 유제처리로울러(11)를 거쳐 권취기(13)에 권취된다.The filament that has passed through the false twister 9 is heat-treated at a temperature of 100 ° C or higher in the heat treatment apparatus 14 and wound around the winding machine 13 via the godet rollers 10 and 12 and the emulsion treatment roller 11 .

이와 같은 본 발명은 방사된 필라멘트를 열처리장치(14)에서 열처리함을 특징으로 한다. 상기 열처리장치(14)는 방사공정 아래에 설치되며, 가연공정과 권취공정 사이에 설치하는 것이 보다 바람직 하다.The present invention is characterized in that the irradiated filament is heat-treated in a heat treatment apparatus (14). The heat treatment apparatus 14 is installed under the spinning process, and it is more preferable to install it between the flammable process and the winding process.

열처리장치(14)에서의 열처리온도는 100℃ 이상, 보다 바람직하기로는 100~150℃로 한다. 열처리온도가 상기범위 보다 낮으면 필라멘트의 열안정성이 저하되어 비등수처리 및 열처리에 의해 열수축이 많이 일어나게 되며, 상기 범위를 초과하는 경우에는 필라멘트의 물성이 저하한다.The heat treatment temperature in the heat treatment apparatus 14 is 100 DEG C or higher, more preferably 100 to 150 DEG C. If the heat treatment temperature is lower than the above range, the thermal stability of the filament deteriorates and heat shrinkage is caused by boiling water treatment and heat treatment. If the heat treatment temperature is higher than the above range, the properties of the filament deteriorate.

필라멘트가 열처리장치(14)를 통과하는 시간(열처리시간)은 0.01~0.05초가 바람직 하다. 상기 열처리시간은 고뎃로울러(10, 12)의 회전선속도로 조절할수 있다. 열처리장치(14)로는 히팅튜브 또는 히팅롤(Heating Roll)을 사용한다.The time (heat treatment time) during which the filament passes through the heat treatment apparatus 14 is preferably 0.01 to 0.05 seconds. The heat treatment time can be adjusted by the rotation speed of the godet rollers 10 and 12. As the heat treatment apparatus 14, a heating tube or a heating roll is used.

상기 히팅튜브에는 온도공급 및 제어기(15)가 부착되어 있고, 필라멘트가 통과하는 히팅튜브 내벽은 필라멘트 융착을 방지하기 위해 테프론코팅 되어 있다. 히팅튜브의 길이는 20~30cm가 바람직 하다.The heating tube is provided with a temperature controller and a controller 15. The inner wall of the heating tube through which the filament passes is Teflon coated to prevent filament fusion. The length of the heating tube is preferably 20 to 30 cm.

이와 같은 열처리공정은 고온의 방사튜브(5)를 통과한 필라멘트가 바로 상온으로 냉각될때 일어나는 구조의 불안정 현상을 방지하기 위한 것이다. 다시말해 상기 열처리 공정에 의해 필라멘트의 구조가 안정되어 열처리시 필라멘트의 수축율이 낮아진다.This heat treatment process is intended to prevent the instability of the structure that occurs when the filament passing through the high-temperature radiation tube 5 is cooled to room temperature. In other words, the structure of the filament is stabilized by the heat treatment process, and the shrinkage ratio of the filament during heat treatment is lowered.

본 발명의 방법으로 제조한 폴리우레탄 탄성섬유는 비등수수축율이 7% 이하이고, 100℃의 열풍오븐에서 처리후의 열수축율이 5% 이하 이다. 통상적으로 본 발명의 방법으로 제조한 폴리우레탄 탄성섬유는 비등수수축율이 5~7% 이고, 100 ℃의 열풍오븐에서 처리후의 열수축율이 3~5% 이다. 그 결과 본 발명의 폴리우레탄 탄성섬유는 염색, 가공 등의 후공정성이 향상되고 최종 가공지의 품질도 향상된다.The polyurethane elastic fiber produced by the method of the present invention has a boiling water shrinkage of 7% or less and a heat shrinkage of 5% or less after treatment in a hot air oven at 100 캜. Generally, the polyurethane elastic fibers produced by the method of the present invention have a boiling water shrinkage of 5 to 7% and a heat shrinkage after treatment in a hot air oven at 100 캜 of 3 to 5%. As a result, the polyurethane elastic fiber of the present invention improves the post-processability such as dyeing, processing and the like, and also improves the quality of the final processed paper.

본 발명에 있어서 비등수수축율 및 열처리수축율은 다음과 같이 평가한다.In the present invention, boiling water shrinkage ratio and heat treatment shrinkage ratio are evaluated as follows.

·비등수수축율(%)· Boiling water shrinkage (%)

비등수에 폴리우레탄 탄성섬유를 15분간 침지처리한 후 상온에서 1시간 방치하고, 처리전과 처리후의 섬유길이를 아래식에 대입하여 비등수수축율을 구한다.The polyurethane elastic fibers are immersed in boiling water for 15 minutes, then left at room temperature for 1 hour, and the fiber length before and after treatment is substituted into the following equation to determine boiling water shrinkage.

비등수수축율(%) =

Figure 111999009033814-pat00001
× 100Boiling water shrinkage (%) =
Figure 111999009033814-pat00001
× 100

·열수축율(%)Heat shrinkage (%)

100℃의 열풍오븐에서 폴리우레탄 탄성섬유를 1시간동안 열처리한후 상온에서 1시간 방치하고, 처리전과 처리후의 섬유길이를 아래식에 대입하여 열수축율을 구한다.Heat the polyurethane elastic fibers in a hot air oven at 100 ° C for 1 hour, then stand at room temperature for 1 hour, and calculate the heat shrinkage ratio by substituting the fiber length before and after treatment into the following formula.

열수축율(%) =

Figure 111999009033814-pat00002
× 100Heat shrinkage (%) =
Figure 111999009033814-pat00002
× 100

이하 실시예 및 비교실시예를 통하여 본 발명을 보다 구체적으로 살펴본다. 그러나 본 발명이 아래 실시예에만 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples and Comparative Examples. However, the present invention is not limited to the following examples.

실시예 1Example 1

분자량 2,200의 폴리테트라메틸렌글리콜 1몰에 4,4'-디페닐메탄디이소시아네이트 2몰을 혼합하여 90℃에서 90분간 반응시켜 양말단에 이소시아네이트를 갖는 예비중합체를 합성하였다.1 mole of polytetramethylene glycol having a molecular weight of 2,200 and 2 moles of 4,4'-diphenylmethane diisocyanate were mixed and reacted at 90 DEG C for 90 minutes to synthesize a prepolymer having isocyanate groups at both ends.

이 예비중합체를 40℃로 냉각시킨 후 N,N'-디메틸아세트아마이드를 첨가하여 약 45%의 예비중합체를 포함하는 용액을 제조한다. 이 예비중합체용액을 5℃까지 낮춘후 격렬히 교반하면서 예비중합체에 대하여 에틸렌디아민을 96당량%, 디에틸아민을 6당량%를 함유한 N,N'-디메틸아세트아마이드용액을 천천히 가하면서 예비중합체를 쇄연장 시켜 방사원액을 제조한다.This prepolymer is cooled to 40 占 폚 and N, N'-dimethylacetamide is added to prepare a solution containing about 45% of the prepolymer. While the prepolymer solution was lowered to 5 캜 and vigorously stirred, N, N'-dimethylacetamide solution containing 96 equivalent% of ethylenediamine and 6 equivalent% of diethylamine was slowly added to the prepolymer while the prepolymer was stirred Chain extension to prepare a spinning stock solution.

상기 방사원액(1)을 탈포, 여과한 후 기어펌프(2)를 이용하여 방사구금(4)을 통해 방사튜브(5)내로 토출한다. 이와 동시에 고온가스유입구(3)를 통해 방사튜브(5)내로 고온가스를 유입시킨다. 유입된 고온가스는 필라멘트 내의 유기용제를 증발시켜 함유한 상태로 가스배출구(7)를 통해 방사튜브(5) 밖으로 배출된다.The spinning stock solution 1 is defoamed and filtered, and is discharged into the spinning tube 5 through the spinneret 4 using the gear pump 2. At the same time, the hot gas is introduced into the radiation tube 5 through the hot gas inlet 3. The introduced high temperature gas evaporates the organic solvent in the filament and discharges it out of the radiation tube 5 through the gas outlet 7 in a state containing it.

계속해서 방사튜브(5)를 통과한 필라멘트를 가연기(9)로 가연처리한 후 100℃의 히팅튜브에서 0.05초동안 열처리한다. 상기 히팅튜브의 길이는 25cm 이다.Then, the filament passing through the radiation tube 5 is subjected to a burning treatment with a combustor 9, followed by heat treatment in a heating tube at 100 ° C for 0.05 second. The length of the heating tube is 25 cm.

열처리된 필라멘트를 고뎃로울러(10, 12) 및 유제처리 로울러(11)를 통과시킨 다음 권취기(13)에 권취하여 폴리우레탄 탄성섬유를 제조한다. 제조한 탄성섬유의 비등수수축율 및 열처리수축율을 평가한 결과는 표 2와 같다.The heat-treated filaments are passed through the godet rollers (10, 12) and the emulsion treatment rollers (11), and then wound on a winder (13) to produce polyurethane elastic fibers. Table 2 shows the results of evaluating boiling water shrinkage ratio and heat treatment shrinkage ratio of the produced elastic fibers.

실시예 2~실시예 7 및 비교실시예 1Examples 2 to 7 and Comparative Example 1

열처리장치(14)의 종류, 열처리온도 및 열처리시간을 표 1과 같이 변경한 것을 제외하고는 실시예 1과 동일한 공정 및 조건으로 폴리우레탄 탄성섬유를 제조한다. 제조한 탄성섬유의 비등수수축율 및 열처리수축율을 평가한 결과는 표 2와 같다.Polyurethane elastic fibers were produced under the same process and conditions as in Example 1 except that the kind of heat treatment apparatus 14, the heat treatment temperature and the heat treatment time were changed as shown in Table 1. Table 2 shows the results of evaluating boiling water shrinkage ratio and heat treatment shrinkage ratio of the produced elastic fibers.

<표 1> 제조조건<Table 1> Manufacturing conditions

구 분division 열처리장치 종류Type of heat treatment equipment 열처리온도(℃)Heat treatment temperature (캜) 열처리시간(초)Heat treatment time (sec) 실시예 1Example 1 히팅튜브Heating tube 100100 0.050.05 실시예 2Example 2 히팅튜브Heating tube 110110 0.040.04 실시예 3Example 3 히팅튜브Heating tube 120120 0.030.03 실시예 4Example 4 히팅튜브Heating tube 130130 0.020.02 실시예 5Example 5 히팅튜브Heating tube 140140 0.010.01 실시예 6Example 6 히팅튜브Heating tube 150150 0.010.01 실시예 7Example 7 히팅롤Heating roll 120120 0.030.03 비교실시예 1Comparative Example 1 열처리장치 사용하지 않음No heat treatment device used 00 00

<표 2> 섬유물성평가 결과<Table 2> Fiber Property Evaluation Results

구 분division 비등수수축율(%)Boiling water shrinkage (%) 열풍오븐처리후 수축율(%) (열수축율)Shrinkage after hot air oven treatment (%) (heat shrinkage) 실시예 1Example 1 6.76.7 4.44.4 실시예 2Example 2 6.46.4 4.44.4 실시예 3Example 3 6.26.2 4.34.3 실시예 4Example 4 5.95.9 4.04.0 실시예 5Example 5 5.55.5 4.04.0 실시예 6Example 6 5.35.3 3.83.8 실시예 7Example 7 6.36.3 4.44.4 비교실시예 1Comparative Example 1 15.015.0 16.016.0

본 발명의 폴리우레탄 탄성섬유는 열적안정성이 우수하여 비등수처리나 열처리시 수축율이 낮다. 그 결과 염색, 가공 등의 후공정성이 향상되며, 최종 가공지의 품질도 향상된다.The polyurethane elastic fiber of the present invention is excellent in thermal stability and has a low shrinkage ratio during boiling water treatment or heat treatment. As a result, post-processability such as dyeing and processing is improved, and the quality of the final processed paper is also improved.

Claims (9)

방사, 가연(False Twisting), 열처리 및 권취공정순으로 폴리우레탄 탄성섬유를 제조함에 있어서, 가연된 폴리우레탄 탄성섬유를 길이가 20∼30㎝이며, 형태가 히팅튜브 및 히팅롤(Heating Roll) 중에서 선택된 하나이며, 온도가 100℃∼150℃인 열처리 장치(14)내에서 0.01∼0.05초 동안 열처리하는 것을 특징으로 하는 폴리우레탄 탄성섬유의 제조방법.In producing polyurethane elastic fibers in the order of spinning, false twisting, heat treatment and winding, the twisted polyurethane elastic fibers are 20 to 30 cm in length, and the shape is selected from heating tubes and heating rolls Wherein the heat treatment is carried out for 0.01 to 0.05 seconds in a heat treatment apparatus (14) having a temperature of 100 占 폚 to 150 占 폚. 삭제delete 삭제delete 삭제delete 삭제delete 삭제delete 비등수수축율이 7% 이하이며, 100℃의 열풍오븐에서 1시간 처리후의 열수축율이 5% 이하인 것을 특징으로 하는 폴리우레탄 탄성섬유.Wherein the boiling water shrinkage is 7% or less, and the heat shrinkage after treatment in a hot air oven at 100 캜 for 1 hour is 5% or less. 7항에 있어서, 비등수수축율이 5~7%인 것을 특징으로 하는 폴리우레탄 탄성섬유.7. The polyurethane elastic fiber according to claim 7, wherein boiling water shrinkage ratio is 5 to 7%. 7항에 있어서, 100℃의 열풍오븐에서 1시간 처리후의 열수축율이 3~5%인 것을 특징으로 하는 폴리우레탄 탄성섬유.7. The polyurethane elastic fiber according to claim 7, wherein the heat shrinkage after treatment in a hot air oven at 100 DEG C for 1 hour is 3 to 5%.
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Publication number Priority date Publication date Assignee Title
WO2020169417A1 (en) 2019-02-19 2020-08-27 Basf Se A process for producing a thermoplastic polyurethane fiber with low shrinkage, and the use of the fiber

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