KR930007829B1 - Producing process of polyester monofilament for drafting paper - Google Patents

Producing process of polyester monofilament for drafting paper Download PDF

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KR930007829B1
KR930007829B1 KR1019910011459A KR910011459A KR930007829B1 KR 930007829 B1 KR930007829 B1 KR 930007829B1 KR 1019910011459 A KR1019910011459 A KR 1019910011459A KR 910011459 A KR910011459 A KR 910011459A KR 930007829 B1 KR930007829 B1 KR 930007829B1
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monofilament
ethylene
polyester
paper
weight
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KR1019910011459A
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KR930002609A (en
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신상일
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주식회사 삼양사
김상응
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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
    • D01F6/62Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • 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
    • D01D5/08Melt spinning methods
    • 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
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2331/00Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/04Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Paper (AREA)
  • Artificial Filaments (AREA)
  • Woven Fabrics (AREA)

Abstract

blending 50-99.9 wt.% of polyester polymer and 0.1-50 wt.% of ethylene-tetrafluoroethylene copolymer; or blending 40-99.8 wt.% of polyester polymer, 0.1-50 wt.% of ethylene-tetrafluoroethylene copolymer and 0.1-10 wt.% of polycarbodiimide; and melt-spinning the mixture. The purpose of this method is to impart durable anti-soiling property to the convas during the paper-making process, as well as to prevent hydrolysis of the monofilament by reducing the end-released carboxylic group.

Description

초지건조용 폴리에스테르 모노필라멘트의 제조방법Manufacturing method of polyester monofilament for papermaking

본 발명은 초지건조용 폴리에스테르 모노필라멘트의 제조방법에 관한 것으로서, 더욱 상세하게는 폴리에스테르 중합체와 열가소성 중합체인 에틸렌-테트라플루오르에틸렌 중합체를 함께 용융방사하거나, 여기에 플리카보디이미드를 추가로 혼합하여 응융방사하므로써 내오염성 및 내가수분해성을 갖도록 하는 모노필라멘트를 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a polyester monofilament for papermaking, and more particularly, melt-spun a polyester polymer and an ethylene-tetrafluoroethylene polymer, which is a thermoplastic polymer, or further mixes a plicabodiimide. The present invention relates to a method for producing a monofilament having a fouling resistance and hydrolysis resistance by fusion spinning.

일반적으로 초지용구는 포밍훼브릭(Forming Fabrics), 프래스펠트(Press Felts), 드라이 캔바스(Dry Canvas)로 구분할 수 있다.In general, papermaking equipment can be classified into Forming Fabrics, Press Felts, and Dry Canvas.

이중에서 드라이 캔바스는 초지를 포의 형태로 만들어주면서 회전하는 건조실린더에 설치되는 것으로서, 건조되지 않는 상태의 습지를 운반하는 역할을 수행하는 것인 바, 보통 제지기의 건조부는 상하로 건조실린더가 복잡하게 병설되어 대개 3개의 군으로 이루어져 있으며, 각 군은 드라이 캔바스가 벨트의 역할로서 상하가 연결되어 주행하면서 습지를 건조하게 된다.Among them, dry canvas is installed in a rotating drying cylinder while making paper in the form of a cloth, and serves to transport the wetland in an undried state. The complex is usually composed of three groups, and each group has a dry canvas as a belt, and the upper and lower parts are connected to each other to dry the wetlands.

이때 발생하는 문제점으로서는 캔바스의 오염에 의한 초지의 오염 및 통기성 저하로 인한 생산성의 저하, 그리고 초지건조를 위한 고온열풍으로 인한 모노필라멘트의 가수분해와 이로인한 기계적 물성의 저하등이 있다.Problems that may occur include a decrease in productivity due to contamination of the grass paper due to contamination of the canvas and a decrease in air permeability, and hydrolysis of the monofilament due to high temperature hot air for drying the paper, and thus a decrease in mechanical properties.

한편, 제지공장에서 초지의 형성작업 진행과정에서 발생되는 오염물질로는 초지의 원료인 펄프가 갖고 있는 단섬유와 송진등의 물질, 작업환경에 의해 발생되는 먼지, 폐지를 사용함에 따라 인쇄용 잉크가 초지의 표면에 부착된 것, 그리고 제지기가 회전하면서 발생되는 윤활물질의 낙하에 의한 것 등이 있는데, 이러한 오염물질이 초지 건조 과정중에 초지표면에 오염시켜 불량한 종이제품을 생산하게 되며, 또한 통기성을 저하시켜 초지건조 효과를 저하시킨다.On the other hand, as the pollutants generated during the papermaking process at the paper mill, the printing inks are produced by using the short fibers and rosin of the pulp, the raw material of the paper, dust generated by the working environment, and waste paper. Attached to the surface of the paper, and the fall of lubrication material generated by the paper machine's rotation. These pollutants contaminate the paper surface during the paper drying process, producing poor paper products. To lower the papermaking drying effect.

또한, 초지건조를 위한 고온열풍으로 인해 작업장 내부가 고온 다습해지기 쉽고 이로인해 모노필라멘트의 가수분해가 발생하여 캔바스의 기계적 물성저하가 촉진된다.In addition, due to the high temperature hot air for paper drying, the inside of the workplace is easily heated to high temperature and humidity, thereby causing hydrolysis of the monofilament, thereby facilitating the mechanical properties of the canvas.

종래의 일반적인 제지공정에서는 위와같은 이유로 캔바스를 자주 교체하여야 하기 때문에 공정의 중단으로 인해 종이의 생산성이 떨어지게 되는 요인으로 작용하고 있다.In the conventional general papermaking process, the canvas must be frequently replaced for the same reason as described above, which causes a decrease in the productivity of the paper due to the interruption of the process.

따라서, 위와같은 문제점을 해결하는 방안으로서 캔바스 교체시기를 연장시키기 위해 내오염성을 개선하는 공지된 기술로는 저분자 불소화합물을 이용하는 방법(미국특허 제4,388,372호), 모노에테르기가 포함된 폴리글리콜을 이용하는 방법(미국특허 제4,754,142호) 등이 있으나, 이와같은 방법들은 단순히 섬유나 직물의 표면에 내오염성의 부여기능을 갖는 저분자 화합물을 표면에 도포하는 방법으로서, 이 방법들에 의해서는 내오염성 효과는 일시적인 효과만을 얻을 수 있을 뿐, 실제 사용시에는 쉽게 마모되어 캔바스에 도포된 화합물의 도포효과가 없어지기 때문에 이렇게 내구성이 없는 것이 문제로 지적되고 있다.Therefore, as a solution to the above problems, a known technique for improving fouling resistance in order to extend the canvas replacement time is a method using a low molecular fluorine compound (US Pat. No. 4,388,372), using a polyglycol containing a monoether group. (US Pat. No. 4,754,142) and the like, but these methods are simply a method of applying a low-molecular compound having a fouling resistance imparting function to the surface of the fiber or fabric, the contamination resistance effect by these methods It is pointed out that such a lack of durability is obtained because only a temporary effect can be obtained and the wear effect of the compound applied to the canvas disappears easily in actual use.

또한, 내가수분해성을 부여하는 방법으로는 일본특허 공개공보 소50-59,525호(1975)에서 폴리에스테르와 페닐렌 비옥사조린 화합물을 첨가하여 모노필라멘트의 가수분해 억제를 위해 말단 유리카르복실기를 감소시키는 방법이 소개되어 있으나, 용융과정에서 폴리에스테르가 분해되어 분자량이 저하될 뿐만 아니라 말단 유리카르복실기도 충분히 감소시키지 못하는 단점이 있다.In addition, as a method of imparting hydrolysis resistance, Japanese Patent Laid-Open Publication No. 50-59,525 (1975) adds a polyester and a phenylene bioxazorine compound to reduce terminal free carboxyl groups to suppress hydrolysis of monofilaments. Although the method has been introduced, there is a disadvantage in that the polyester is decomposed in the melting process to lower the molecular weight as well as the terminal free carboxyl groups are not sufficiently reduced.

따라서, 본 발명의 목적은 제지과정에서 캔바스의 오염도를 저하시키기 위한 방법으로서, 초지용 모노필라멘트 제조시 열가소성 폴리에스테르 중합체와 에틸렌-테트라플로로에틸렌 공중합체, 그리고 폴리카보디이미드를 혼합하여 용융가공하므로써, 내오염성을 영구적으로 부여하여 내구성을 향상시키는 동시에 말단 유리카르복실기를 감소시켜 가수분해를 방지한 초지건조용 모로필라멘트를 제공하는데 있다.Accordingly, an object of the present invention is a method for reducing the contamination of the canvas during the papermaking process, the melt processing by mixing the thermoplastic polyester polymer, ethylene-tetrafluoroethylene copolymer, and polycarbodiimide during the manufacture of monofilament for papermaking Accordingly, to provide a paper-drying morofilament that prevents hydrolysis by permanently imparting pollution resistance to improve durability and at the same time reduce the terminal free carboxyl group.

이하, 본 발명을 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.

본 발명은 폴리에스테르 중합체를 이용하여 초지건조용 모노필라멘트를 제조함에 있어서, 폴리에스테르 중합체 50~99.9 중량%에 에틸렌-테트라플루오르에틸렌 공중합체 0.1~50 중량%를 혼합하여 용융방사하여 제조하는 것을 특징으로 한다.The present invention is to prepare a papermaking drying monofilament using a polyester polymer, it is characterized in that the melt polymer is prepared by mixing the ethylene-tetrafluoroethylene copolymer 0.1-50% by weight to 50 ~ 99.9% by weight of the polyester polymer It is done.

또한, 본 발명은 폴리에스테르 중합체 40~99.8 중량%와 에틸렌-테트라플루오르에틸렌 공중합체 0.1~50 중량%, 그리고 폴리카보디이미드 0.1~10 중량%를 혼합하여 용융방사하여 제조하는 것을 특징으로 한다.In another aspect, the present invention is characterized in that the polyester polymer 40 to 99.9% by weight, ethylene-tetrafluoroethylene copolymer 0.1 to 50% by weight, and polycarbodiimide by mixing 0.1 to 10% by weight of the melt spinning prepared.

이와같은, 본 발명을 더욱 상세히 설명하면 다음과 같다.As described above, the present invention will be described in more detail.

본 발명은 폴리에스테르 중합체로서 고유점도 0.6~1.2dl/g의 폴리에틸렌 테레프탈레이트 또는 고유점도 0.9~1.2dl/g의 폴리부틸렌 테레프탈레이트 50~99.9 중량%에 에틸렌-테트라플루오르에틸렌 공중합체 0.1~50 중량%를 혼합하고 용융방사하므로써 초지건조시 내오염성을 갖는 모노필라멘트를 제조하는 것이다.The present invention is a polyester polymer 0.1 to 50 ethylene-tetrafluoroethylene copolymer to polyethylene terephthalate having an intrinsic viscosity of 0.6 to 1.2 dl / g or 50 to 99.9 wt% of polybutylene terephthalate having an intrinsic viscosity of 0.9 to 1.2 dl / g. By mixing the weight percent and melt spinning to produce monofilament having stain resistance during paper drying.

이때 상기 에틸렌-테트라플루오르에틸렌 공중합체의 사용량이 0.1 중량% 미만이면 첨가효과를 나타내지 못하므로 내오염성을 향상시킬 수 없고, 50 중량%를 초과하면 모노필라멘트의 강력이 저하되는 현상이 발생한다.At this time, if the amount of the ethylene-tetrafluoroethylene copolymer used is less than 0.1% by weight, the effect of addition may not be improved, and thus, the stain resistance may not be improved. If the amount of the ethylene-tetrafluoroethylene copolymer is more than 50% by weight, the strength of the monofilament decreases.

또한, 본 발명은 폴리에스테르 중합체로서 폴리에틸렌 테레프탈레이트 또는 폴리부틸렌 테레프탈레이트 40~99.8 중량%와 에틸렌-테트라플루오르에틸렌 공중합체 0.1~50 중량%, 그리고 위 성분외에 추가로 폴리카보디이미드 0.1~10 중량%를 혼합하여 동일방법으로 용융방사하는 것을 포함한다.In addition, the present invention is a polyester polymer 40 to 99.9% by weight of polyethylene terephthalate or polybutylene terephthalate and 0.1 to 50% by weight of ethylene-tetrafluoroethylene copolymer, and in addition to the above components 0.1 to 10 polycarbodiimide It includes mixing the melt by weight in the same manner.

이때 상기 에틸렌-테트라플루오르에틸렌 공중합체는 그 접촉각 측정시 표면장력이 큰 값을 가지므로 오염물질이 용이하게 탈락되는 장점을 이용한 것인데, 그 사용량이 0.1 중량% 미만이면 첨가효과를 나타내지 못하므로 내오염성의 향상을 기대하기 어렵고 50 중량%를 초과하면 모노필라멘트의 강력이 저하되는 현상이 발생한다.At this time, the ethylene-tetrafluoroethylene copolymer has the advantage that the pollutant is easily removed because the surface tension is large when the contact angle is measured. It is difficult to expect the improvement of and exceeds 50% by weight, a phenomenon that the strength of the monofilament is lowered.

또한, 폴리카보디이미드의 사용량이 0.01 중량% 미만이면 폴리에스테르 말단 유리카르복실기를 붕쇄 또는 연결하는 효과가 없으며, 10 중량%를 초과하면 폴리카보이미드의 열분해로 모노필라멘트의 색상이 변화하고 오히려 말단 유리카르복실기의 함량이 증가되는 문제점이 있다.In addition, when the amount of polycarbodiimide is less than 0.01% by weight, there is no effect of disintegrating or linking the polyester terminal free carboxyl group, and when the amount of the polycarbodiimide exceeds 10% by weight, the color of the monofilament is changed by thermal decomposition of the polycarbodiimide, but rather the terminal glass There is a problem that the content of the carboxyl group is increased.

이와같이 본 발명은 첨가제로서 폴리카보디이미드를 첨가하여서 폴리에스테르의 분해에 촉매작용을 하는 말단 유리카르복실기를 붕쇄하거나 소멸시키므로써 유리 카르복실기의 함량을 10meq/kg 이하로 조정하여서 폴리에스테르의 가수분해에 의한 수명 단축을 방지하는 것이다. 즉, 폴리에스테르를 고온 다습한 조건에서 사용하더라도 가수분해를 지연시키는 효과를 나타내어 안정화시키는 역할을 한다.As such, the present invention adjusts the content of the free carboxyl group to 10 meq / kg or less by hydrolyzing the polyester by disintegrating or quenching the terminal free carboxyl group which catalyzes the decomposition of the polyester by adding polycarbodiimide as an additive. It is to prevent shortening of life. In other words, even when the polyester is used under high temperature and high humidity conditions, it exhibits an effect of delaying hydrolysis and stabilizes it.

또한, 본 발명에서 에틸렌-테트라플루오르에틸렌은 필수성분으로 사용하여 내오염성을 부여하는 것으로서, 상기와 같이 2성분 또는 3성분이 혼합된 모노필라멘트를 모두 사용할 수 있으며, 폴리카보디이미드를 추가로 첨가하는 경우에는 첨가하지 않은 경우에 비해 유리카르복실기의 함량을 감소시키는 효과에서 우수한 것이다.In addition, in the present invention, ethylene-tetrafluoroethylene is used as an essential component to impart pollution resistance, and both monofilaments mixed with two or three components as described above may be used, and additionally polycarbodiimide is added. If the case is excellent in the effect of reducing the content of the free carboxyl group compared to the case without addition.

따라서, 본 발명에 의해 얻어지는 폴리에스테르 모노필라멘트는 모노필라멘트의 표면특성을 개선하여 영구적으로 작용하게 됨에 따라 우수한 내오염성을 갖게 되며, 또한 고온 다습한 조건에서 장기간 사용할 수 있도록 내가수분해성도 동시에 갖기 때문에 제지업체에서 사용과정에 문제가 되는 오염물질의 부착을 방지해줄 수 있는 표면특성이 부염됨과 동시에 초지가 함유하는 수분에 대한 발수성이 우수하므로 장기간에 걸쳐 초지용구를 사용하여도 초지의 오염방지와 초지기구의 수명을 보장해주는 효과를 갖게 된다.Therefore, the polyester monofilament obtained by the present invention has excellent stain resistance as it permanently works by improving the surface properties of the monofilament, and also has hydrolysis resistance at the same time for long-term use at high temperature and high humidity conditions. Surface properties that can prevent the adhesion of contaminants, which are a problem in the process of use, are affected by the paper industry, and the water repellency of the paper is excellent. It has the effect of guaranteeing the life of the instrument.

이하, 본 발명을 실시예를 통해 더욱 상세히 설명하면 다음과 같다.Hereinafter, the present invention will be described in more detail with reference to Examples.

[제조예][Production example]

(중합체와 첨가제의 혼합방법)(Method of mixing polymer and additive)

중합체와 첨가제를 컴파운더(Compounder)를 이용하여 다음 표 1의 조성비에 따라 용융혼합하였으며, 이때 자동계량장치(dosing machine)을 이용하여 계량하여 혼합하였다. 이때 실린더 온도는 260 내지 320℃로 설정하여 혼합하였으며 혼합체는 냉각조를 통과시켜 펠레트 상태로 절단하여 사용하였다.The polymer and the additive were melt mixed using a compounder according to the composition ratio of Table 1 below, and then mixed by metering using a dosing machine. At this time, the cylinder temperature was set at 260 to 320 ° C. and mixed, and the mixture was cut and used in a pellet state by passing through a cooling bath.

이 방법에 사용된 중합체는 공지된 제조방법을 제조된 고유점도가 0.6 내지 1.2dl/g이고 말단 유리카르복실기의 함량이 20 내지 35meq/kg을 갖는 폴리에틸렌-테레프탈레이트 중합체와 융점이 250 내지 270℃를 갖고 에틸렌과 테트라플루오르에틸렌의 공중합비가 1:1인 공중합체를 사용하였으며, 첨가제는 융점이 130 내지 160℃를 갖는 폴리카보디이미드 화합물이 첨가된 컴파운딩펠레트를 사용하였다.The polymer used in this process is a polyethylene-terephthalate polymer having a intrinsic viscosity of 0.6 to 1.2 dl / g and a terminal free carboxyl group having a content of 20 to 35 meq / kg, and a melting point of 250 to 270 ° C. And a copolymer having a copolymerization ratio of ethylene and tetrafluoroethylene of 1: 1 was used, and an additive was used as a compounding pellet to which a polycarbodiimide compound having a melting point of 130 to 160 ° C was added.

이 공정에서 특정한 색상을 부여하기 위하여 여러 색상의 안료(Pigment)를 사용하였으며 이 색상부여 방법은 통상의 방법으로 진행하였다.In this process, various colors of pigments were used to impart a specific color, and this coloration method was performed in a conventional manner.

(모노필라멘트 제조방법)(Method of manufacturing monofilament)

컴파운팅 작업으로 얻어진 펠레트를 100 내지 140℃ 정도의 온도조건으로 결정화한 다음, 제습 드라이어에서 160 내지 180℃에서 5 내지 10시간에 걸쳐 수분율이 0.003% 이하가 되도록 건조시킨 다음 용융방사에 사용하였다.The pellets obtained by the compounding operation are crystallized at a temperature of about 100 to 140 ° C., and then dried in a dehumidifying dryer at 160 to 180 ° C. for 5 to 10 hours to have a moisture content of 0.003% or less, and then used for melt spinning. It was.

용융방사 작업은 건조된 펠레트를 용융방사장치의 호퍼로 이송하여 280 내지 320℃ 범위에서 실시하였으며 이때 사용된 방사구금은 2.2mm의 구경을 갖고 구멍수가 45개인 원형의 구금을 사용하였다. 방사구금을 통하여 사출된 용융상태의 모노필라멘트는 60 내지 90℃를 유지하고 있는 냉각조를 통과하여 충분히 굳어진 모노필라멘트를 얻게 된다.The melt spinning operation was carried out in a 280 to 320 ℃ range of the dried pellets transferred to the hopper of the melt spinning apparatus, the spinneret used was a circular mold having a diameter of 2.2mm and 45 holes. The molten monofilament injected through the spinneret passes through a cooling tank maintained at 60 to 90 ° C to obtain a sufficiently hardened monofilament.

이와같은 미연신 상태의 모노필라멘트를 단계적으로 연신과 열처리를 실시하여 최종 완성된 폴리에스테르 모노필라멘트를 권취하게 되어 제품이 생산하게 된다. 이때 연신비는 3 내지 6 정도로 실시되며 열처리 온도는 80에서 200℃까지 단계적으로 실시한다.The unstretched monofilament is stretched and heat-treated step by step to wind up the finished polyester monofilament to produce a product. At this time, the stretching ratio is performed to about 3 to 6 and the heat treatment temperature is carried out step by step from 80 to 200 ℃.

이러한 방법으로 얻어지는 폴리에스테르 모노필라멘트는 직경이 0.7mm이고 섬도가 약 4780 데니어를 갖으며 진원율이 98% 이상을 갖는 원형 횡단면 형태가 얻어진다.The polyester monofilament obtained in this way has a circular cross sectional shape with a diameter of 0.7 mm, a fineness of about 4780 denier and a roundness of 98% or more.

[실시예 1~4]EXAMPLES 1-4

고유점도가 0.64dl/g이고 말단 유리카르복실기의 함량이 30meq/kg인 폴리에틸렌 테레프탈레이트와 용융온도가 270℃인 에틸렌-테트라플루오르에틸렌 공중합체를 다음 표 1의 비율에 따라 혼합된 컴파운딩펠레트를 사용하여 얻어진 모노필라멘트의 물성과 내오염성을 평가하여 그 결과를 다음 표 1에 나타내었다.A polyethylene terephthalate having an intrinsic viscosity of 0.64 dl / g and a terminal free carboxyl group having a content of 30 meq / kg and an ethylene-tetrafluoroethylene copolymer having a melting temperature of 270 ° C. were mixed according to the ratio of Table 1 below. To evaluate the physical properties and stain resistance of the monofilament obtained using the results are shown in Table 1 below.

[실시예 5~13]EXAMPLES 5-13

융점이 145℃인 폴리카보디이미드를 다음 표 2의 비율에 따라 혼합한 다음 이 컴파운딩펠레트를 건조공정에서 건조한 다음 용융방사공정을 거쳐 얻어진 모노필라멘트의 물성과 내오염성과 내가수분해성을 평가하여 그 결과를 다음 표 1에 나타내었다.Polycarbodiimide having a melting point of 145 ° C was mixed according to the ratio of the following Table 2, and then the compounding pellet was dried in a drying process and then evaluated for physical properties, fouling resistance and hydrolysis resistance of the monofilament obtained through the melt spinning process. The results are shown in Table 1 below.

[실시예 14]Example 14

고유점도가 0.64dl/g이고 말단 유리카르복실기의 함량이 30meq/kg인 폴리에틸렌 테레프탈레이트와 용융온도가 270℃인 에틸렌-테트라플루오로에틸렌 공중합체를 다음 표 1과 같은 일정비율로 혼합한 다음, 시아닌 블루 안료 0.3 중량%를 컴파운딩 과정에서 투입하여 펠레트를 제조하고, 이 착색된 컴파운딩 펠레트를 사용하여 건조고정을 거쳐 용융방사공정으로 얻어진 모노필라멘트의 물성과 내오염성과 내가수분해성을 평가하여 다음 표 1에 나타내었다.Polyethylene terephthalate having an intrinsic viscosity of 0.64 dl / g and a content of terminal free carboxyl group of 30 meq / kg and an ethylene-tetrafluoroethylene copolymer having a melting temperature of 270 ° C. were mixed at a predetermined ratio as shown in Table 1 below. 0.3 wt% of blue pigment was added in the compounding process to prepare pellets, and the colored compounding pellets were used to evaluate the physical properties, fouling resistance and hydrolysis resistance of the monofilament obtained by the melt spinning process. It is shown in Table 1 below.

[실시예 15]Example 15

융점이 145℃인 폴리카보디이미드를 표 3의 비율에 따라 혼합한 다음 시아닌 블루 안료 0.3 중량%를 첨가하여 컴파운딩 과정으로 펠레트를 제조한 다음, 건조공정에서 건조하여 용융방사공정을 거쳐 얻어진 모노필라멘트의 물성과 내오염성과 내가수분해성을 평가하여 다음 표 1에 나타내었다.Polycarbodiimide having a melting point of 145 ° C. was mixed according to the ratio of Table 3, and 0.3 wt% of cyanine blue pigment was added to prepare a pellet by compounding, followed by drying in a drying step to obtain a melt spinning step. The physical properties, fouling resistance and hydrolysis resistance of the monofilament were evaluated and shown in Table 1 below.

[실시예 16]Example 16

고유점도가 1.01dl/g이고 말단 유리카르복실기의 함량이 35meq/kg인 폴리부틸렌 테레프탈레이트와 용융온도가 270℃인 에틸렌-테트라플루오로에틸렌 공중합체를 다음 표 1의 비율에 따라 혼합한 컴파운딩펠레트를 사용하여 얻어진 모노필라멘트의 물성과 내오염성과 내가수분해성을 평가하여 다음 표 1에 나타내었다.Compounding a polybutylene terephthalate having an intrinsic viscosity of 1.01 dl / g and a content of terminal free carboxyl group of 35 meq / kg and an ethylene-tetrafluoroethylene copolymer having a melting temperature of 270 ° C. according to the ratio of Table 1 below. The physical properties, fouling resistance and hydrolysis resistance of the monofilament obtained using the pellets were evaluated and shown in Table 1 below.

[실시예 17]Example 17

내가수분해성을 강화하기 위하여 융점이 145℃인 폴리카보디이미드를 다음 표 1의 비율에 따라 혼합한 다음 이 컴파운딩펠레트를 건조공정에서 건조한 다음 용융방사공정을 거쳐 얻어진 모노필라멘트의 물성과 내오염성과 내가수분해성을 평가하여 다음 표 1에 나타내었다.In order to enhance hydrolysis resistance, polycarbodiimide having a melting point of 145 ° C was mixed according to the ratio of the following Table 1, and then the compounding pellet was dried in a drying process and then subjected to melt spinning process. The contamination and hydrolysis resistance were evaluated and shown in Table 1 below.

[비교예 1]Comparative Example 1

고유점도가 0.64dl/kg이고 말단 유리카르복실기의 함량이 30meq/kg인 폴리에틸렌 테레프탈레이트를 그대로 사용하여 얻어진 모노필라멘트의 물성과 내오염성을 평가하여 다음 표 1에 나타내었다.The physical properties and fouling resistance of the monofilament obtained using the polyethylene terephthalate having the intrinsic viscosity of 0.64 dl / kg and the content of the terminal free carboxyl group of 30 meq / kg are shown in Table 1 below.

[비교예 2~4][Comparative Examples 2-4]

비교예 1의 폴리에틸렌 테레프탈레이트와 융점이 145℃인 폴리카보디이미드를 다음 표 2의 비율에 따라 혼합한 다음 용융방사공정을 거쳐 얻어진 모노필라멘트의 물성과 내오염성과 내가수분해성을 평가하여 그 결과를 다음 표 1에 나타내었다.The polyethylene terephthalate of Comparative Example 1 and polycarbodiimide having a melting point of 145 ° C. were mixed according to the ratio of the following Table 2, and then the physical properties, fouling resistance and hydrolysis resistance of the monofilament obtained through the melt spinning process were evaluated. Is shown in Table 1 below.

[비교예 5][Comparative Example 5]

폴리에틸렌 테레프탈레이트 45 중량%와 에틸렌-테트라플로로에틸렌 공중합체 40 중량%, 그리고 폴리카보디이미드 15 중량%를 혼합한 다음 시아닌 블루 안료 0.3 중량%를 컴파운딩 과정에서 투입하여 펠레트를 제조한 다음, 이 착색된 컴파운딩펠레트를 사용하여 건조공정을 거쳐 용융방사공정을 얻어진 모노필라멘트의 물성과 내오염성과 내가수분해성을 평가하여 그 결과를 다음 표 1에 나타내었다.45% by weight of polyethylene terephthalate, 40% by weight of ethylene-tetrafluoroethylene copolymer, and 15% by weight of polycarbodiimide were mixed, and 0.3% by weight of cyanine blue pigment was added during compounding to prepare a pellet. Using the colored compounding pellets, the properties of the monofilament obtained through the drying process and the melt spinning process were evaluated. The results are shown in Table 1 below.

[비교예 6]Comparative Example 6

고유점도가 1.01dl/g이고 말단 유리카르복실기의 함량이 35meq/kg인 폴리부틸렌 테레프탈레이트을 그대로 사용하여 얻어진 모노필라멘트의 물성과 내오염성과 내가수분해성을 평가하여 그 결과를 다음 표 1에 나타내었다.The physical properties, fouling resistance and hydrolysis resistance of the monofilament obtained by using polybutylene terephthalate having an intrinsic viscosity of 1.01 dl / g and a content of terminal free carboxyl group of 35 meq / kg are shown in Table 1 below. .

[표 1]TABLE 1

A : 폴리에스테르 중합체A: polyester polymer

B : 에틸렌-테트라플루오르에틸렌 공중합체B: ethylene-tetrafluoroethylene copolymer

C : 폴리카보디이미드 수지C: polycarbodiimide resin

D : 시아닌 블루(안료)D: Cyanine Blue (pigment)

상기의 방법에 의해 제조된 모노필라멘트의 물성 측정방법은 다음과 같다.The physical property measurement method of the monofilament manufactured by the above method is as follows.

(내오염성의 평가방법)(Evaluation method for pollution resistance)

오염물질의 일종인 윤활유에 모노필라멘트를 5분가 침적한 다음 접촉각 측정기를 사용하여 윤활유의 표면부착정도를 접촉각으로 평가하는 방법을 채택하였다.After 5 minutes of monofilament was immersed in lubricating oil, which is a kind of contaminant, the contact angle of the lubricating oil was evaluated by using the contact angle measuring device.

(내가수분해성 평가방법)(Hydrolysis resistance evaluation method)

모노필라멘트를 가수분해 측정장치인 가속수명 측정장치를 이용하여 130℃의 고압 수증기하에서 5일간 채류시킨 다음 섬유물성과 고유점도의 말단 유리카르복실기의 변화를 측정하여 평가하였다.The monofilament was collected for 5 days under high pressure steam at 130 ° C. using an accelerated life measuring apparatus, which is a hydrolysis measuring apparatus, and then evaluated by measuring the change in the terminal glass carboxyl group of fiber properties and intrinsic viscosity.

(고유점도 측정방법)(Measurement of Intrinsic Viscosity)

중합체를 페놀과 테트라클로로에탄의 1:1혼합용매를 사용하여 0.5dl/g의 용해농도로 제조한 다음 20℃의 항온조에서 우벨로브드 점도계(Ubbelohde Viscometer)를 이용하여 용액이 모세관을 통과하는 시간을 측정한 다음 고유점도로 계산하여 얻었다.The polymer was prepared at a solubility of 0.5 dl / g using a 1: 1 mixed solvent of phenol and tetrachloroethane, and then the time for the solution to pass through the capillary using an Ubbelohde Viscometer in a 20 ° C thermostat. It was obtained by measuring the intrinsic viscosity.

(말단 유리카르복실기의 측정방법)(Measuring method of terminal free carboxyl group)

중합체를 분쇄기로 미쇄하게 분쇄시켜 0.1~0.2g을 테스트 튜브에 넣고 여기에 벤질 알콜을 넣은 다음 215℃의 온도에서 약 2분 동안 교반하여 용해시킨다. 이 용해물을 상온의 물에서 급냉시킨 다음 10ml의 클로로포름을 넣은 비이커에 첨가한다. 이 용액에 페놀프탈레인을 넣고 벤질알콜에 녹인 0.1N 가성소다용액을 이용하여 적정한다. 그리고 동일량의 벤질알콜과 클로로포름의 혼합액을 적정하는 공시험을 실시하여 계산하였다.Grind the polymer finely into a grinder, put 0.1-0.2 g into a test tube, add benzyl alcohol, and dissolve by stirring for about 2 minutes at a temperature of 215 ℃. The lysate is quenched in water at room temperature and then added to a beaker with 10 ml of chloroform. Phenolphthalein is added to this solution and titrated using 0.1N caustic soda solution dissolved in benzyl alcohol. And it calculated by performing the blank test which titrates the mixed solution of the same amount of benzyl alcohol and chloroform.

Claims (2)

폴리에스테르 중합체를 이용하여 용융방사에 의해 초지건조용 모노필라멘트를 제조함에 있어서, 폴리에스테르 중합체 50~99.9 중량%와 에틸렌-테트라플루오르에틸렌 공중합체 0.1~50 중량%를 혼합하여 용융방사하는 것을 특징으로 하는 초지건조용 폴리에스테르 모노필라멘트의 제조방법.In preparing the papermaking monofilament by melt spinning using a polyester polymer, 50 to 99.9 wt% of the polyester polymer and 0.1 to 50 wt% of the ethylene-tetrafluoroethylene copolymer are mixed and melt spun. Method for producing a polyester monofilament for papermaking drying. 폴리에스테르 중합체를 이용하여 초지건조용 모노필라멘트를 제조함에 있어서, 폴리에스테르 중합체 40~99.8 중량%와 에틸렌-테트라플로오로에틸렌 공중합체 0.1~50중량%, 그리고 폴리카보디이미드 0.1~10 중량%를 혼합하여 용융방사하여 제조하는 것을 특징으로 하는 초지건조용 폴리에스테르 모노필라멘트의 제조방법.In preparing a papermaking monofilament using a polyester polymer, 40 to 99.9% by weight of polyester polymer, 0.1 to 50% by weight of ethylene-tetrafluoroethylene copolymer, and 0.1 to 10% by weight of polycarbodiimide Method for producing a polyester monofilament for papermaking drying, characterized in that the melting and spinning by mixing.
KR1019910011459A 1991-07-06 1991-07-06 Producing process of polyester monofilament for drafting paper KR930007829B1 (en)

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US6136437A (en) * 1997-10-07 2000-10-24 Astenjohson, Inc. Industrial fabric and yarn made from an improved fluoropolymer blend

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KR20000017989A (en) * 1999-12-30 2000-04-06 이정민 Exhaust base for liquid container

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6136437A (en) * 1997-10-07 2000-10-24 Astenjohson, Inc. Industrial fabric and yarn made from an improved fluoropolymer blend

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