KR20140089157A - Process for preparing polyester multifilament having excellent strength and chemical resistance for tire cord - Google Patents
Process for preparing polyester multifilament having excellent strength and chemical resistance for tire cord Download PDFInfo
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- KR20140089157A KR20140089157A KR1020130001041A KR20130001041A KR20140089157A KR 20140089157 A KR20140089157 A KR 20140089157A KR 1020130001041 A KR1020130001041 A KR 1020130001041A KR 20130001041 A KR20130001041 A KR 20130001041A KR 20140089157 A KR20140089157 A KR 20140089157A
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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
- 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
- D01D5/084—Heating filaments, threads or the like, leaving the spinnerettes
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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
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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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
- D02G3/48—Tyre cords
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
- D02J1/228—Stretching in two or more steps, with or without intermediate steps
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- D—TEXTILES; PAPER
- D07—ROPES; CABLES OTHER THAN ELECTRIC
- D07B—ROPES OR CABLES IN GENERAL
- D07B2501/00—Application field
- D07B2501/20—Application field related to ropes or cables
- D07B2501/2046—Tire cords
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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
- D10B2401/00—Physical properties
- D10B2401/06—Load-responsive characteristics
- D10B2401/062—Load-responsive characteristics stiff, shape retention
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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
- D10B2401/00—Physical properties
- D10B2401/06—Load-responsive characteristics
- D10B2401/063—Load-responsive characteristics high strength
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S57/00—Textiles: spinning, twisting, and twining
- Y10S57/902—Reinforcing or tire cords
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
Abstract
Description
본 발명은 타이어코드용 폴리에스테르 멀티필라멘트사의 제조방법에 관한 것으로, 더욱 상세하게는 폴리에스테르 멀티필라멘트사의 내열강력 및 내화학성을 향상시키기 위해 냉각공기의 온도구배를 주어 필라멘트 내/외부의 배향도를 조절하여 타이어코드용 소재로 사용할 수 있는 우수한 물성의 폴리에스테르 멀티필라멘트사의 제조방법에 관한 것이다.
The present invention relates to a process for producing a polyester multifilament yarn for a tire cord, and more particularly, to a process for producing polyester multifilament yarn for a tire cord by adjusting a temperature gradient of cooling air in order to improve heat resistant strength and chemical resistance of a polyester multifilament yarn, To a method of producing a polyester multifilament yarn having excellent physical properties which can be used as a material for a tire cord.
고강력 폴리에스테르 섬유는 고무보강용 타이어코드, 좌석벨트, 콘베이어벨트, V-벨트 및 호우스(hose)등을 포함하는 산업적인 용도에 다양하게 사용되고 있는바, 특히 타이어의 섬유 보강재로 적용하기 위하여 라텍스 처리 및 열 처리하여 처리코드로 전환시키는 경우 더욱 우수한 형태안정성 및 강도가 요구되고 있다.High strength polyester fibers are widely used in industrial applications including tire cord for rubber reinforcement, seat belts, conveyor belts, V-belts and hoses, and particularly for application as a fiber reinforcing material for tires In the case of converting into a treated cord by latex treatment and heat treatment, more excellent form stability and strength are required.
높은 고유점도(I.V.)에서, 좋기로는 고유점도(I.V.) 0.9 ~ 1.2에서 2,000 ~ 3,200m/분의 고속방사속도 범위 내에서는 중합물과 방사온도가 같고, 강력이 동일한 경우에 방사속도가 빠르면 빠를수록 처리코드의 형태안정성(dimensional stability) 및 원사의 강력이용율이 더욱 향상되는 경향을 보인다는 것은 산업용 폴리에스테르사의 제조분야에서는 일반적으로 잘알려진 사실이다.In the high intrinsic viscosity (IV), the spinning speed is fast if the spinning temperature of the polymerized material is the same and the strength is the same within the high spinning speed range of the intrinsic viscosity (IV) 0.9-1.2 to 2,000-3,200 m / min. It is well known in the art of industrial polyester manufacture that the dimensional stability of the treated cord and the tendency of the strength utilization of the yarn to further improve.
이것을 이론적으로 고찰해보면 산업용 폴리에스테르사를 제조할 때 방사장력을 증가시켜 미연신사의 배향 및 결정과 결정을 연결해주는 타이체인(tie chain)의 형성을 증가시켜야만 최종 처리코드의 형태안정성(dimensional stability) 및 원사의 강력이용율을 높일 수 있으며, 보다 더 고강도의 처리코드를 얻기 위해서는 이러한 고배향의 미연신사를 가지고 고배율의 연신이 가능하도록 미연신사 필라멘트간의 섬도, 배향도에 대한 균일성을 더욱 향상시켜야한다.Theoretically, theoretically, when manufacturing industrial polyester yarns, it is necessary to increase the radiation tension to increase the formation of the tie chain which connects the orientation of the undrawn yarn and the crystal to the crystal, And the uniformity of the degree of fineness and the degree of orientation between the filaments of the non-drawn filaments should be further improved so as to enable high-magnification drawing with such high-orientation non-drawn filament yarns in order to obtain higher-
미국 특허 제 4,101,525 호 및 미국 특허 제 4,491,657 호에서는 높은 초기 모듈러스 및 낮은 수축율을 갖는 산업용 폴리에스테르 멀티필라멘트사를 개시하고 있다. 그러나 상기 특허들에 개시된 원사는 처리 코드로 전환되는 경우 강도가 감소하여 타이어 코드의 필요한 특성을 가지지 못한다는 단점을 가진다.U.S. Patent No. 4,101,525 and U.S. Patent No. 4,491,657 disclose industrial polyester multifilament yarns having high initial modulus and low shrinkage. However, the yarns disclosed in the above patents have a disadvantage in that when they are converted into processed codes, their strength decreases and they do not have the necessary characteristics of the tire cord.
이러한 문제점을 해결하기 위하여 멀티필라멘트 폴리에스테르 섬유의 강도를 높이는 방법으로 미국 특허 제4,690,866 호에서는 1.2 이상의 높은 고유점도(I.V.)를 갖는 폴리에스테르 칩을 사용하여 방사하는 방법이 제안되었다. 이와 같이 칩의 점도를 높이면 방사장력을 증가시켜 미연신사의 배향 및 결정과 결정을 연결해 주는 타이 체인(tie chain)의 형성을 증가시켜서 처리 코드로 전환하는 경우 우수한 강도를 나타낼 수 있도록 한다.In order to solve such a problem, US Pat. No. 4,690,866 discloses a method of increasing the strength of a multifilament polyester fiber by using a polyester chip having a high intrinsic viscosity (I.V.) of 1.2 or more. When the viscosity of the chip is increased, the spinning strength is increased to increase the formation of the tie chain which connects the orientation of the undrawn yarn and the crystal to the crystal so as to exhibit excellent strength when converted to the treated cord.
그러나 상기 방법에서 사용한 높은 고유점도의 폴리에스테르는 고상중합 시 표면과 중심 부분의 고유점도 차이가 심해 용융-방사하는 경우 점도 불 균일에 의해 방사성이 저하되고 필라멘트 컷(cut)이 발생하여 공정성 및 외관이 불량해질 뿐만 아니라, 높은 온도로 용융-방사시켜야 하기 때문에 열분해 및 가수분해 등이 발생하여 실제로 방사된 섬유는 칩이 갖는 만큼 높은 점도를 갖지 않는다는 문제점이 있다.
However, the polyester having a high intrinsic viscosity used in the above method has a problem in that when the intrinsic viscosity difference between the surface and the center portion in the solid phase polymerization is deeply melt-radiated, the spinnability is lowered due to the unevenness in viscosity and the filament cut occurs, But also pyrolysis and hydrolysis are generated due to melt-spinning at a high temperature. Thus, there is a problem in that the actually spun fibers do not have a viscosity as high as that of a chip.
본 발명은 상기와 같은 문제점을 해결하기 위해, 냉각공기(Quenching Air)의 온도구배를 부여하여 필라멘트 내/외부의 배향도 차이를 감소시킴과 동시에 외부 표면층의 배향도를 증가시켜 최종 딥코드의 내열강력 및 내화학성의 향상시키는 타이어코드용 폴리에스테르 멀티필라멘트사의 제조방법을 제공하는 것을 목적으로 한다.
In order to solve the above-mentioned problems, it is an object of the present invention to provide a temperature gradient of cooling air (quenching air) to reduce the difference in the degree of orientation between the inside and the outside of the filament and increase the degree of orientation of the external surface layer, And to provide a method for producing a polyester multifilament yarn for a tire cord which improves chemical resistance.
본 발명의 적절한 실시 형태에 따르면, 치수안정성, 내열강력 및 내화학성이 우수한 타이어코드용 폴리에스테르 멀티필라멘트사를 제조함에 있어서, 에틸렌테레프탈레이트 단위를 함유하는 고상중합 폴리에스테르 칩을 290 내지 300℃의 온도로 압출용융하여 방출사를 제조하는 단계; 상기 방출사를 핫에어(Hot Air) 온도를 60 내지 100℃로 지연냉각 시키는 단계; 핫에서 직후 쿨에어(Coll Air) 온도를 20 내지 25℃로 급냉각 고화시키는 단계; 미연신사의 복굴절율과 밀도를 조절하는 방사속도로 사를 권취하는 단계; 상기 권취된 원사를 다단연신 시키는 단계를 포함하는 타이어코드용 폴리에스테르 멀티필라멘트사의 제조방법을 제공한다.
According to a preferred embodiment of the present invention, in producing a polyester multifilament yarn for tire cord excellent in dimensional stability, heat resistance, and chemical resistance, a solid phase-polymerized polyester chip containing ethylene terephthalate units is melt- Extruding and melting at a temperature to produce a discharged yarn; Retarding the discharged yarn by delaying the hot air temperature to 60 to 100 ° C; Rapid cooling and solidifying the Coll Air temperature immediately after hot from 20 to 25 ° C; Winding the yarn at a spinning speed to adjust the birefringence and density of the undrawn yarn; And a step of stretching the wound yarn in a multi-stage fashion. The present invention also provides a method for producing a polyester multifilament yarn for a tire cord.
본 발명의 다른 적절한 실시 형태에 따르면, 핫에어부와 쿨에어부의 길이가 1:1 내지 7:3의 비율을 가지는 것이 특징이다.
According to another preferred embodiment of the present invention, it is characterized in that the length of the hot air portion and the cool air portion is in the range of 1: 1 to 7: 3.
본 발명의 또 다른 적절한 실시 형태에 따르면, 냉각공기(Quenching Air)의 배출부 길이는 30 내지 60cm이고, 냉각공기는 0.3 내지 0.8m/s의 속도로 주입되는 것을 특징으로 한다.
According to another preferred embodiment of the present invention, the outlet length of the quenching air is 30 to 60 cm, and the cooling air is injected at a rate of 0.3 to 0.8 m / s.
상기와 같은 구성을 갖는 본 발명은, 필라멘트 내/외부의 배향도 차이를 감소시킴과 동시에 외부 표면층의 배향도를 증가시킴으로써 고강도, 저수축의 폴리에스테르 멀티필라멘트사를 얻을 수 있게 할 뿐 아니라 특히 표면 배향도 증가로 인한 내화학안정성 및 내열성이 향상되어 타이어코드용으로의 적용이 가능하다.
The present invention having such a constitution as described above can reduce the difference in the degree of orientation between the inside and the outside of the filament and increase the degree of orientation of the outer surface layer to thereby obtain a polyester multifilament yarn of high strength and low shrinkage, The chemical resistance and heat resistance of the tire can be improved and the tire can be applied to a tire cord.
도 1은 본 발명에 따른 타이어코드용 폴리에스테르 멀티필라멘트사의 제조공정에서 사용되는 방사장치를 도시한 것이다.
도 2은 본 발명에 따른 타이어코드용 폴리에스테르 멀티필라멘트사의 제조공정에서 사용되는 방사장치 중 일부를 도시한 것이다.
도 3은 본 발명에 따른 타이어코드용 폴리에스테르 멀티필라멘트사의 제조공정에서 온도 구배에 따른 멀티필라멘트사의 내/외부간의 배향도 차이를 도시한 것이다.BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 shows a spinning device used in a process for producing a polyester multifilament yarn for a tire cord according to the present invention.
Fig. 2 shows a part of a spinning device used in a process for producing a polyester multifilament yarn for a tire cord according to the present invention.
FIG. 3 shows the difference in orientation between the inside and the outside of the multifilament yarn according to the temperature gradient in the production process of the polyester multifilament yarn for a tire cord according to the present invention.
이하, 본 발명에 의한 바람직한 실시예를 첨부된 도면을 참조하면서 상세하게 설명한다. 또한, 본 실시예에서는 본 발명의 권리범위를 한정하는 것은 아니고, 단지 예시로 제시한 것이며, 그 기술적인 요지를 이탈하지 않는 범위 내에서 다양한 변경이 가능하다.
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. The present invention is not limited to the scope of the present invention, but is merely an example, and various modifications can be made without departing from the technical spirit of the present invention.
본 발명의 타이어코드의 주재료로 사용되는 폴리에스테르는 에틸렌글리콜 및 테레프탈렌 디카르복실산 또는 이들의 유도체 그리고 하나 또는 그 이상의 에스테르-형성 성분으로부터 유도된 소량의 유니트를 공중합체 유니트로 포함할수 있다.
The polyester used as the main material of the tire cord of the present invention may contain a small amount of units derived from ethylene glycol and terephthalenedicarboxylic acid or derivatives thereof and one or more ester-forming components as a copolymer unit.
폴리에틸렌 테레프탈레이트 유니트와 공중합가능한 다른 에스테르 형성 성분의 예는1,3-프로판디올, 1,4-부탄디올, 1,6-헥산디올등과 같은 글리콜과, 테레프탈산, 이소프탈산, 헥사하이드로테레프탈산, 스틸벤 디카르복실산, 비벤조산, 아디프산, 세바스산, 아젤라산과 같은 디카르복실산을 포함한다.
Examples of other ester forming components that can be copolymerized with the polyethylene terephthalate unit include glycols such as 1,3-propanediol, 1,4-butanediol, 1,6-hexanediol and the like, and glycols such as terephthalic acid, isophthalic acid, hexahydroterephthalic acid, And dicarboxylic acids such as dicarboxylic acid, bibenzoic acid, adipic acid, sebacic acid, and azelaic acid.
본 발명에 따른 폴리에스테르 멀티필라멘트사의 제조방법은 고유점도가 1.0 내지 1.2이상인 폴리에스테르 칩을 290 내지 300℃의 온도로 압출 용융한 후, 80℃에서 지연냉각시킨 다음 20℃의 조건에서 급냉각 고화시키는 단계를 거쳐 3000m/min의 방사조건에서 제조하는 제조방법을 포함한다.
A method for producing a polyester multifilament yarn according to the present invention comprises the steps of extruding and melting a polyester chip having an intrinsic viscosity of 1.0 to 1.2 or more at a temperature of 290 to 300 占 폚 and then lagging and cooling at 80 占 폚, Followed by an evolving step at a spinning speed of 3000 m / min.
이와 같이 제조된 폴리에스테르 멀티필라멘트사의 강도는 8.6g/d 이상이며, 섬도는 1500d이상을 가지며, 형태안정성 지수도 6.0이하로 물성과 공정성이 우수하다. 이때, 형태 안정성 지수가 6.0을 초과하면 타이어코드용으로 부적절하다.
The polyester multifilament yarn thus produced has a strength of 8.6 g / d or more, a fineness of 1500 d or more, and a morphological stability index of 6.0 or less, which are excellent in physical properties and processability. At this time, if the shape stability index exceeds 6.0, it is inappropriate for tire cord.
도 1을 참조하면, PET 칩은 익스트루드(1), 기어펌프, 노즐(2) 및 가열장치(3)를 통해 290 내지 310℃의 방사온도로 저온 용융 방사되어 열분해 및 가수분해에 의한 중합체의 점도의 저하가 방지된다.
1, a PET chip is melt-spun at a low temperature of 290 to 310 占 폚 through an extruder 1, a gear pump, a nozzle 2 and a heating device 3 to produce a polymer by pyrolysis and hydrolysis Is prevented from being lowered.
제조된 용융 방출사는 핫에어(Hot Air)(4)로 지연냉각 구역과 쿨에어(Cool Air)(5)를 통과하여 급냉 고화되고, 그리고 필요에 따라 노즐(2)의 바로 아래쪽 냉각구역(4,5) 시작점까지의 거리, 즉 후드의 길이(L) 구간에 짧은 가열장치(3)가 설치될 수 있다.
The produced melt release yarn is quenched and solidified through a delayed cooling zone and a Cool Air 5 with a hot air 4 and is cooled and cooled as needed in the cooling zone 4 immediately below the nozzle 2 , 5) a short heating device 3 can be installed in the section of the distance L to the starting point, that is, the length L of the hood.
후드의 길이(L) 구간은 지연 냉각구역 또는 가열구역이 되고 그리고 50 내지 250mm의 길이 및 250 내지 400℃의 온도(공기접촉 표면온도)를 갖는다.
The length (L) section of the hood becomes a delayed cooling zone or heating zone and has a length of 50 to 250 mm and a temperature of 250 to 400 ° C (air contact surface temperature).
냉각구역(4,5)에서 냉각공기를 불어주는 방법은 방사형 인플로우 냉각(radial inflow quenching)법이 적용된다.
The method of blowing cooling air in the cooling zones (4, 5) is radial inflow quenching.
냉각구역(4,5)을 통과하여 고화된 방출사는 유제 공급장치(6)에 의해 0.5 내지 1.0%로 오일링이 되어 미연신사가 된다.
The solidified release yarn passing through the cooling zones (4,5) is oiled to 0.5-1.0% by the emulsion feeder (6) to become undrawn.
미연신사는 연신롤러(7-11)을 거쳐 스핀드로(spin draw) 공법으로 연신되어 권취 롤러에서 최종 연신사(12)로 얻어진다.
The unstretched yarn is drawn by a spin draw method via a stretching roller 7-11 and is obtained as a
연신롤러(7-11)에서 권취롤러(12)로 가는 과정에서 인터레이스 노즐에서 공기 교락과정이 수행된다.
In the process of going from the stretching roller 7-11 to the take-
도 2을 참조하면, 종래에는 에틸렌 테레프탈레이트 단위를 함유하는 폴리에스테르 칩을 압출용융된 방출사를 급냉각 고화단계를 거친 다음 방사하여 최종원사를 제조되는데 반해, 본 발명은 폴리에스테르 칩을 압출용융된 방출사를 핫에어로 지연냉각시키는 단계와 쿨에어로 급냉각 고화시키는 단계로 온도구배를 부여하는 방법으로 최종원사가 제조 되어진다.
Referring to FIG. 2, a polyester chip containing ethylene terephthalate units is extruded and melted, and the resulting yarn is subjected to a quenching and solidifying step, followed by spinning to produce a final yarn. The final yarn is manufactured by a method of retarding the discharged yarn by hot air and a step of cooling the yarn by cooling the yarn.
도 3을 참조하면, 온도구배를 부여하여 제조된 최종원사는 종래의 방법으로 제조된 폴리에스테르 필라멘트사에 비해 내/외부 배향도의 차이를 감소시킴과 동시에 외부 표면층의 배향도가 증가되어 내화학안정성 및 내열성이 향상되는 특징을 가진다.
Referring to FIG. 3, the final yarn produced by applying the temperature gradient reduces the difference in the degree of inner / outer orientation as compared with the polyester filament yarn prepared by the conventional method, and the degree of orientation of the outer surface layer is increased, .
실시예 및 비교예의 물성평가는 아래와 같이 측정 또는 평가하였다.
The physical properties of Examples and Comparative Examples were measured or evaluated as follows.
<물성 측정 방법>≪ Method for measuring physical properties &
1) 강신도1)
Instron 5565(Instron, USA)를 이용하여, ASTM D 885에 따라 표준 상태(20, 65% 상대습도)하에서 시료길이 250mm, 인장속도 300mm/분 및 80turns/m의 조건으로 측정하였다.
Under the conditions of a sample length of 250 mm, a tensile rate of 300 mm / min, and 80 turns / m under standard conditions (20, 65% relative humidity) according to ASTM D 885 using an Instron 5565 (Instron, USA).
2) 중간신도2)
강신도 S-S 커브 상에서 원사는 4.5g/d에 해당하는 하중에서의 신도를 측정하고, 처리 코드는 하중 2.25g/d 에서의 신도를 측정하였다.
The elongation at the load corresponding to 4.5 g / d was measured and the elongation at the load of 2.25 g / d was measured on the SS curve.
3) 수축율3) Shrinkage
시료를 20, 65% 상대습도의 표준 상태하에서 24시간 이상 방치한 후 0.05g/d에 상당하는 중량을 달아 길이(L0)를 측정하고, 무장력 상태하에서 드라이 오븐을 이용하여 150하에서 30분간 처리한 다음 꺼내어 4시간 이상 방치한 후, 0.05g/d에 상당하는 하중을 달아 길이(L)를 측정하여 하기 수학식 4에 의해 수축율을 계산하였다.The sample was allowed to stand for at least 24 hours under standard conditions of relative humidity of 20, 65%, and the length (L 0 ) was measured by weighing 0.05 g / d and treated for 30 minutes at 150 under a dry oven And then left for more than 4 hours. Then, a load corresponding to 0.05 g / d was applied to measure the length (L), and the shrinkage ratio was calculated by the following equation (4).
수학식 1Equation 1
S(%) = (L0 - L)/L0 × 100
S (%) = (L 0 - L) / L 0 100
4) E-S(치수안정성)4) E-S (dimensional stability)
처리 코드의 치수안정성은 타이어 측벽 결각화(Side Wall Indentation, SWI) 및 핸들링에 관계되는 물성으로서 주어진 수축율에서의 높은 모듈러스로 정의되고, E2.25(2.25g/d에서의 신장율)+FS(자유수축율)는 서로 다른 열처리과정을 거친 처리 코드에 대한 치수안정성의 척도로서 유용하며 낮을수록 더 우수한 치수안정성을 나타낸다.
The dimensional stability of the treated cords is defined by the high modulus at a given shrinkage as the properties related to tire side wall indentation (SWI) and handling and is defined as E2.25 (elongation at 2.25 g / d) + FS Shrinkage) is useful as a measure of dimensional stability for treated cords subjected to different heat treatments, and exhibits better dimensional stability at lower temperatures.
실시예 1Example 1
본 발명의 에틸렌테레프탈레이트 단위를 함유하는 고상중합 폴리에스테르 칩을 290 내지 300℃의 온도로 압출 용융한 후, 방출사를 핫에어부 배출길이가 30cm이고 60℃의 조건에서 지연냉각시킨 다음 쿨에어부 배출길이가 30cm이고 20℃의 조건에서 급냉각 고화시켜 제조하였다. 이 연신사는 2900m/분으로 권취하여 1538데니어의 최종 원사를 제조하였다.
The solid phase-polymerized polyester chips containing the ethylene terephthalate unit of the present invention were extruded and melted at a temperature of 290 to 300 DEG C, and the discharged yarn was delayed and cooled at a temperature of 60 DEG C with a hot- Cooled and solidified at a temperature of 20 캜 at a discharge length of 30 cm. This stretched yarn was wound at 2900 m / min to produce a final yarn of 1538 denier.
실시예 2Example 2
본 발명의 에틸렌테레프탈레이트 단위를 함유하는 고상중합 폴리에스테르 칩을 290 내지 300℃의 온도로 압출 용융한 후, 방출사를 핫에어부 배출길이가 30cm이고 60℃의 조건에서 지연냉각시킨 다음 쿨에어부 배출길이가 30cm이고 25℃의 조건에서 급냉각 고화시켜 제조하였다. 이 연신사는 2900m/분으로 권취하여 1539데니어의 최종 원사를 제조하였다.
The solid phase-polymerized polyester chips containing the ethylene terephthalate unit of the present invention were extruded and melted at a temperature of 290 to 300 DEG C, and the discharged yarn was delayed and cooled at a temperature of 60 DEG C with a hot- It was prepared by quenching and solidifying at a temperature of 25 캜 with a fisher discharge length of 30 cm. This stretched yarn was wound at 2900 m / min to produce an end yarn of 1539 denier.
실시예 3Example 3
본 발명의 에틸렌테레프탈레이트 단위를 함유하는 고상중합 폴리에스테르 칩을 290 내지 300℃의 온도로 압출 용융한 후, 방출사를 핫에어부 배출길이가 60cm이고 80℃의 조건에서 지연냉각시킨 다음 쿨에어부 배출길이가 40cm이고 20℃의 조건에서 급냉각 고화시켜 제조하였다. 이 연신사는 3000m/분으로 권취하여 1540데니어의 최종 원사를 제조하였다.
The solid phase-polymerized polyester chips containing the ethylene terephthalate unit of the present invention were extruded and melted at a temperature of 290 to 300 DEG C, and the discharged yarn was delayed and cooled at a temperature of 80 DEG C with a hot- It was prepared by quenching and solidifying under the condition of 20 cm. The drawn yarn was wound at 3000 m / min to produce an end yarn of 1540 denier.
실시예 4Example 4
본 발명의 에틸렌테레프탈레이트 단위를 함유하는 고상중합 폴리에스테르 칩을 290 내지 300℃의 온도로 압출 용융한 후, 방출사를 핫에어부 배출길이가 60cm이고 80℃의 조건에서 지연냉각시킨 다음 쿨에어부 배출길이가 40cm이고 25℃의 조건에서 급냉각 고화시켜 제조하였다. 이 연신사는 2980m/분으로 권취하여 1542데니어의 최종 원사를 제조하였다.
The solid phase-polymerized polyester chips containing the ethylene terephthalate unit of the present invention were extruded and melted at a temperature of 290 to 300 DEG C, and the discharged yarn was delayed and cooled at a temperature of 80 DEG C with a hot- It was prepared by quenching and solidifying at a temperature of 25 캜 at a discharge length of 40 cm. This stretched yarn was wound at 2980 m / min to produce an end yarn of 1542 denier.
비교예 1Comparative Example 1
본 발명의 에틸렌테레프탈레이트 단위를 함유하는 고상중합 폴리에스테르 칩을 290 내지 300℃의 온도로 압출 용융한 후, 방출사를 쿨에어부 배출길이가 60cm이고, 20℃의 조건에서 급냉각 고화시켜 제조하였다. 이 연신사는 2800m/분으로 권취하여 1541데니어의 최종 원사를 제조하였다.
The solid phase-polymerized polyester chip containing the ethylene terephthalate unit of the present invention is extruded and melted at a temperature of 290 to 300 ° C, and the discharged yarn is rapidly cooled and solidified at a temperature of 20 ° C, Respectively. This stretched yarn was wound at 2800 m / min to produce a final yarn of 1541 denier.
비교예 2Comparative Example 2
본 발명의 에틸렌테레프탈레이트 단위를 함유하는 고상중합 폴리에스테르 칩을 290 내지 300℃의 온도로 압출 용융한 후, 방출사를 쿨에어부 배출길이가 60cm이고, 25℃의 조건에서 급냉각 고화시켜 제조하였다. 이 연신사는 2850m/분으로 권취하여 1540데니어의 최종 원사를 제조하였다.
The solid phase-polymerized polyester chip containing the ethylene terephthalate unit of the present invention is extruded and melted at a temperature of 290 to 300 ° C, and the discharged yarn is rapidly cooled and solidified at a temperature of 25 ° C, Respectively. This stretched yarn was wound at 2850 m / min to produce an end yarn of 1540 denier.
표 1에 나타낸 바와 같은 방사조건에서 상기 실시예 1 내지 4와 비교예 1 내지 2를 수행하여 최종원사를 제조하였다.
Examples 1 to 4 and Comparative Examples 1 and 2 were conducted under the spinning conditions as shown in Table 1 to prepare final yarns.
-
-
-
-
(cm)Discharge length
(cm)
(cm)Discharge length
(cm)
이와 같이 제조된 폴리에스테르 멀티필라멘트사의 물성을 평가하여 하기 표 2에 나타내었다.
The properties of the polyester multifilament yarn thus produced were evaluated and are shown in Table 2 below.
(cm)Discharge length
(cm)
(cm)Discharge length
(cm)
온도 구배를 부여하지 않는 조건에서 제조한 비교예 1과 온도 구배를 부여하여 제조한 실시예3의 물성을 비교하여 하기 표 3에 나타내었다.
The physical properties of Comparative Example 1 prepared under the condition of no temperature gradient and Example 3 prepared by applying the temperature gradient are shown in Table 3 below.
Yarn
Yarn
D/C 물성
D / C Properties
Strong Utilization
D / C heat resistance
Endothelium
상기 방법으로 제조된 폴리에스테르 멀티필라멘트사의 물성은 강력이용율(YarnD/C)이 89.4%이고, 가류후 강력보존율 및 내피로도가 각각 79.1%, 89.8%로 비교예 1에 비하여 향상되었다. 또한, 실시예 3의 최종딥코드(D/C)의 수축율은 1.5%로, 비교예 1의 최종딥코드(D/C)의 수축율은 2.2%보다 더 향상된 수치를 나타났다. 이것으로, 핫에어로 지연냉각시키는 단계와 쿨에어로 급냉각 고화시키는 온도구배를 부여하여 제조된 최종원사가 저수축의 효과를 보이는 것으로 나타났다.
The physical properties of the polyester multifilament yarn produced by the above method were 89.4% in terms of strength utilization (YarnD / C), 79.1% in strength retention and 89.8% in fatigue strength after vulcanization, respectively, as compared with Comparative Example 1. In addition, the shrinkage ratio of the final dipped cord (D / C) of Example 3 was 1.5%, and the shrinkage ratio of the final dipped cord (D / C) of Comparative Example 1 was more improved than 2.2%. As a result, it was shown that the final product manufactured by applying a delayed cooling process to the hot air and a temperature gradient to cool and cool the product to aero-grade level had a low shrinkage effect.
위에서 본 발명은 실시예를 이용하여 상세하게 설명되었지만, 제시된 실시예는 예시적인 것으로서 본 발명의 범위는 위와 같은 실시예에 대한 변형 및 수정 발명에 의하여 제한되지 않는다는 것은 당업자에게 자명할 것이다. 본 발명의 범위는 아래의 청구범위에 의해서만 제한된다.
Although the present invention has been described in detail with reference to the embodiments thereof, it is to be understood by those skilled in the art that the disclosed embodiments are illustrative and that the scope of the present invention is not limited by the modification and the modification of the embodiments. The scope of the present invention is limited only by the following claims.
1 : 익스트루더 2 : 노즐
3 : 가열장치 4 : 지연냉각구역
5 : 급냉각구역 6 : 유제공급장치
7, 8, 9, 10, 11 : 연신롤러 12 : 권취롤러1: Extruder 2: Nozzle
3: Heating device 4: Delayed cooling zone
5: Rapid cooling zone 6: Emulsion feeder
7, 8, 9, 10, 11: stretching roller 12:
Claims (3)
에틸렌테레프탈레이트 단위를 함유하는 고상중합 폴리에스테르 칩을 290 내지 300℃의 온도로 압출용융하여 방출사를 제조하는 단계;
상기 방출사를 핫에어(Hot Air) 온도를 60 내지 100℃로 지연냉각 시키는 단계;
핫에어 직후 쿨에어(Coll Air) 온도를 20 내지 25℃로 급냉각 고화시키는 단계;
미연신사의 복굴절율과 밀도를 조절하는 방사속도로 사를 권취하는 단계;
상기 권취된 원사를 다단연신 시키는 단계를 포함하는 타이어코드용 폴리에스테르 멀티필라멘트사의 제조방법.
In producing a polyester multifilament yarn for tire cord excellent in dimensional stability, heat resistance strength and chemical resistance,
Extruding and melting a solid-phase-polymerized polyester chip containing ethylene terephthalate units at a temperature of 290 to 300 캜 to prepare a discharged yarn;
Retarding the discharged yarn by delaying the hot air temperature to 60 to 100 ° C;
Rapidly cooling and solidifying the Coll Air temperature to 20 to 25 ° C immediately after hot air;
Winding the yarn at a spinning speed to adjust the birefringence and density of the undrawn yarn;
And stretching the wound yarn in a multi-stage manner.
핫에어부와 쿨에어부의 길이가 1:1 내지 7:3의 비율을 가지는 것을 특징으로 하는 타이어코드용 폴리에스테르 멀티필라멘트사의 제조방법.
The method according to claim 1,
Characterized in that the length of the hot air portion and the cool air portion is in the range of 1: 1 to 7: 3.
냉각공기(Quenching Air)의 배출부 길이는 30 내지 60cm이고, 냉각공기는 0.3 내지 0.8m/s의 속도로 주입되는 것을 특징으로 하는 타이어코드용 폴리에스테르 멀티필라멘트사의 제조방법.The method according to claim 1,
Wherein the outlet length of the quenching air is 30 to 60 cm and the cooling air is injected at a rate of 0.3 to 0.8 m / s.
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WO2017113955A1 (en) * | 2015-12-29 | 2017-07-06 | 江苏恒力化纤股份有限公司 | Ultra-low shrinkage polyester industrial yarn and preparation method thereof |
CN109722718A (en) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | A kind of manufacturing method of high strength industrial silk |
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KR100627960B1 (en) * | 2004-02-19 | 2006-09-25 | 주식회사 효성 | Polyester Multifilament Yarn for Rubber Reinforcement and Process for Producing the Same |
KR20070071189A (en) * | 2005-12-29 | 2007-07-04 | 주식회사 효성 | A method for producing polyester multi filament for tire cord |
KR101007331B1 (en) * | 2007-12-21 | 2011-01-13 | 코오롱인더스트리 주식회사 | Method for preparing polyether filament yarn, and polyester filament yarn prepared therefrom, and polyester tire cord the comprising the same |
KR101047046B1 (en) | 2010-12-13 | 2011-07-06 | 주식회사 삼양사 | A manufacturing method of polyester yarn |
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WO2017113955A1 (en) * | 2015-12-29 | 2017-07-06 | 江苏恒力化纤股份有限公司 | Ultra-low shrinkage polyester industrial yarn and preparation method thereof |
US10041192B1 (en) | 2015-12-29 | 2018-08-07 | Jiangsu Hengli Chemical Fibre Co., Ltd. | Ultra-low shrinkage polyester industrial yarn and its preparation method |
CN109722718A (en) * | 2017-10-27 | 2019-05-07 | 中国石油化工股份有限公司 | A kind of manufacturing method of high strength industrial silk |
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