WO2014084470A1 - Fibre de polyéthylène et son procédé de préparation - Google Patents

Fibre de polyéthylène et son procédé de préparation Download PDF

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Publication number
WO2014084470A1
WO2014084470A1 PCT/KR2013/005782 KR2013005782W WO2014084470A1 WO 2014084470 A1 WO2014084470 A1 WO 2014084470A1 KR 2013005782 W KR2013005782 W KR 2013005782W WO 2014084470 A1 WO2014084470 A1 WO 2014084470A1
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Prior art keywords
polyethylene
gel
less
distribution
molecular weight
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PCT/KR2013/005782
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English (en)
Korean (ko)
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김승훈
박종훈
정상영
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주식회사 삼양사
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Publication of WO2014084470A1 publication Critical patent/WO2014084470A1/fr

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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
    • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/04—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins

Definitions

  • the present invention relates to polyethylene fiber and a method for producing the same, and more particularly, polyethylene fiber having excellent quality and physical properties obtained by using a polyethylene resin having a distribution ratio and a molecular weight distribution index satisfying a predetermined condition according to size, and such
  • the present invention relates to a method for producing a fiber.
  • Polyethylene resins are classified into high density polyethylene, low density polyethylene, linear low density polyethylene, etc. according to the comonomer content, and are used as engineering plastics and films, and the use of fibers is increasing for clothing and industrial purposes.
  • Ultra-high molecular weight polyethylene fibers with excellent strength and elastic modulus are manufactured by gel spinning using organic solvents because of their weight average molecular weight of millions, and bulletproof helmets, body armor, ropes, and reinforcing materials that require abrasion resistance, chemical resistance, and cut resistance. It leads to use for high strength applications, such as these.
  • Korean Patent Nos. 10-0308739 and 10-0459575 describe a method for producing fibers having strength of 30 g / d and elastic modulus of 900 g / d or more using ultra high molecular weight polyethylene having an extreme viscosity [ ⁇ ] of 5 or more.
  • the ultra high molecular weight polyethylene resin by the gel spinning method is dissolved in organic solvents such as decalin, paraffin oil, dodecane, xylene, and then extracted with fibers using a volatile solvent such as cyclohexanone.
  • Economic problems are emerging due to additional costs such as solvent recovery and auxiliary equipment for purification.
  • US Patent No. 4,228,118 discloses a polyethylene resin having a number average molecular weight of 20,000 or more and a weight average molecular weight of 125,000 or less, melted at a spinning temperature of 220 ° C. to 335 ° C., and extruded to an 8-hole nozzle to draw a thermal stretching temperature of 115 ° C. to 132 °. It was wound at a minimum spinning speed of 30m / min with a hot tube temperature of 200 °C to 335 °C and stretched 20 times or more to prepare a fiber of 10g / d to 20g / d.
  • this method has a production limit due to the odd number of nozzles in the commercial production of polyethylene fibers, it is difficult to produce polyethylene fibers having excellent uniformity and spinning work when producing hundreds to thousands of multifilaments, and hundreds during the stretching process.
  • By supplying uniform heat to thousands of multifilaments there is a problem in producing high quality polyethylene fibers having excellent quality due to fewer defects such as wool or loops.
  • an object of the present invention is to provide a method for producing a polyethylene fiber excellent in strength and elastic modulus through a high magnification and a multi-stage stretching process using an unstretched multifilament having excellent uniformity.
  • the gel having a size of 250 ⁇ m or more in the polyethylene resin is distributed in 10 / m 2 to 150 / m 2 , the gel having a size of less than 250 ⁇ m distributed in 500 / m 2 to 2,000 / m 2 or less It may be.
  • the polyethylene fiber may have up to 10 moles per 100,000 m.
  • the monofilament of the polyethylene fiber may have a density of 1 to 1.5 denier (denier), 16g / d or more, 400g / d or more.
  • a method for producing polyethylene fiber comprising melt spinning a polyethylene resin of? 0.075.
  • the melt spinning may include passing a hot tube of 200 ° C. to 300 ° C. with an air gap of 100 mm or less under the nozzle.
  • the non-stretched polyethylene obtained by the melt spinning may further comprise the step of stretching in two or more stages using a heating chamber and a goblet roller that can be temperature-controlled in contact with the fibers.
  • Polyethylene fiber obtained by melt spinning the polyethylene resin according to the present invention is excellent in spinning workability and has a good quality that minimizes the occurrence of the swell or loop during the stretching process.
  • the polyethylene unstretched yarn having excellent uniformity by minimizing the gel distribution ratio obtained in accordance with the present invention obtains uniform thermal efficiency during the stretching process, thereby enabling high magnification and multistage stretching process to be made of high performance polyethylene fiber having excellent strength and elastic modulus. have.
  • FIG. 1 is a process diagram schematically showing a method for producing polyethylene fiber according to the present invention.
  • the present invention provides a polyethylene fiber obtained by using a polyethylene resin having a distribution ratio and a molecular weight distribution index of a gel according to size in a predetermined range and a method for producing the same.
  • the term 'gel' refers to a gel formed on a polymerized polyethylene resin, and the gel is formed in various sizes due to the incorporation of foreign substances and characteristics of the resin itself in the polyethylene resin manufacturing process.
  • the gel may be produced in a fine size due to the incorporation of foreign matters and the deterioration or oxidation in the process of manufacturing the powder in a semi-finished state in a pellet state.
  • a screen filter or a screen bag is installed inside the extruder to remove such a gel, thereby removing a gel that may be included in the polyethylene resin and may cause problems in future product production.
  • a gel of 250 ⁇ m or more based on the size of the gel is referred to as a “small gel”, and a gel of less than 250 ⁇ m is referred to as a “sand gel”.
  • the 'size' of the gel refers to the longest diameter of the gel.
  • Gels contained in polyethylene resins generally occur in a total of less than 3,000 pieces / m 2 , and may appear in sizes of several to several hundred ⁇ m, but are classified into gels of 250 ⁇ m or more and gels of less than 250 ⁇ m based on the gel size of 250 ⁇ m. do.
  • the gel contained in the polyethylene resin is used to control the pores of the metal mesh inside the twin extruder, the extruder temperature, and the pressure of the semi-finished resin. Are classified as less than sand gel.
  • a number of the polyethylene resin unit area of 1m 2 per small gel and sand gel is increased or decreased, and distribution of the small gel of polyethylene resin ( ⁇ 1) is less than 150 / m 2 in a proportional relationship, within a sand gel polyethylene resins distribution ( ⁇ 2) is preferably 2,000 / m 2 or less.
  • the ratio of the small gel distribution ( ⁇ 1 ) to the sand gel distribution ( ⁇ 2 ) in the polyethylene resin is referred to herein as a 'gel distribution ratio' or 'k', and the gel distribution ratio is a film forming facility using a blow method. After measuring the number of gels per unit area 1m 2 using the Equation 1 can be determined, but the method for evaluating the gel distribution ratio is not limited thereto:
  • Gel distribution ratio ( k ) affects the workability according to the cross-sectional uniformity of the undrawn yarn in the spinning process and the incidence of occurrence of single filaments and the rate of single yarn in the multifilament during the stretching process.
  • the gel distribution ratio is preferably 0.020 ⁇ k ⁇ 0.075 in order to produce a high quality multifilament by minimizing defects such as workability, uniform fiber cross-section and wool, loops in the spinning process.
  • the distribution of small gels is reduced and the distribution of sand gels is increased in the range of sand gel distribution of 2,000 / m 2 or less, which reduces the possibility of trimming undrawn yarn during spinning.
  • Sand gel softens between the multifilaments being stretched during the high magnification, multistage stretching process, thereby forcing a crosslinking role to the highly oriented crystallized fiber molecular chain, thereby increasing the homogeneity of the polyethylene multifilament and the yarn strength and elastic modulus.
  • the distribution of small gels tends to exceed 150 distributions / m 2 , which causes threading in the nozzle or hot tube section during spinning, which lowers the spinning workability and the spinning workability ratio. Even if this is high, there is a high possibility that the cross section becomes uneven, which leads to defects such as wool and loops in the stretching process, resulting in deterioration of the multifilament.
  • the filament surface is damaged in the process of stretching each filament is sprayed from the multifilament bundle, which is multi It can cause filament fever and single yarn occurrence.
  • the molecular weight distribution index (Mw / Mn, MWD) of the polyethylene resin is preferably greater than 0 and 2.5 or less, and more preferably greater than 0 and 2.3 or less in view of high strength physical properties.
  • the molecular weight distribution index is greater than 2.5, it means that the molecular weight distribution index is increased as the low molecular weight polyethylene increases, which may impede molecular orientation in the spinning process or cause gel formation by deterioration or oxidation. In the stretching process, high magnification multistage stretching is difficult. For this reason, when the molecular weight distribution index is larger than 2.5, it is difficult to obtain a polyethylene yarn having high strength and elastic modulus.
  • the polyethylene resin preferably has a weight average molecular weight of 50,000 to 150,000, more preferably 80,000 to 120,000. If the weight average molecular weight is less than 50,000, the spinning workability is good at the spinning stage, but it is difficult to have high strength properties. Also, if the weight average molecular weight is more than 150,000, the melt viscosity becomes high, and thus the flowability during melting decreases, making the spinning process difficult. Occurs, failing to increase the draw ratio in the draw and heat setting stages, or reduce workability due to trimming during drawing.
  • the polyethylene resin as described above is melted in an extruder of 220 ° C. to 320 ° C., and a non-drawn yarn is wound at a low speed of 1,000 m / min or less by installing a hot tube of 200 ° C. to 300 ° C. at 100 mm or less from the nozzle. Taking steps.
  • the non-stretched polyethylene obtained in the above may include the step of stretching 15 times or more through a plurality of high-pressure rollers using a non-contact uniform heating chamber, thereby generating loops and wool, single yarn, etc. of the multifilament in the stretching process Defects can be minimized to improve the quality of the final product polyethylene fiber.
  • the stretched polyethylene yarn is characterized by having a strength of 16 g / d or more, an elastic modulus of 400 g / d or more, a spinning workability of 95% or more, and a stretch and moor occurrence of 10 times / 100,000 m or less.
  • the strength may be 16 to 21 g / d
  • the modulus of elasticity may be 400 to 500 g / d.
  • the polyethylene resin is polymerized according to the weight average molecular weight and the molecular weight distribution index, and the polyethylene resin is formed using a blowing type film forming equipment in the pre-spinning step to evaluate the small gel and sand gel included in the polyethylene resin.
  • the size of the gel is measured with a phase optical counter and the number of occurrences per unit area is converted.
  • the melt spinning step by the extruder is carried out, the undrawn yarn is wound up, and the prepared undrawn yarn is manufactured into the drawn yarn through a high magnification drawing and heat setting step through a non-contact uniform heating chamber and a plurality of rollers.
  • the polyethylene resin is usually melted at 220 ° C. to 320 ° C. in an extruder.
  • the temperature is not specifically limited according to each part of the extruder, but at a temperature of 320 ° C. or higher, high density polyethylene resins may form fine gels by pyrolysis, oxidation, and deterioration, so that they are melted at 320 ° C. or lower for a smooth spinning process. It is preferable to make it.
  • the unstretched yarn that has passed through the hot tube section of 200 °C to 300 °C at 100mm or less from the nozzle is cooled and solidified by a quenching device that controls the wind temperature and the wind speed, and the spinning speed of the unstretched yarn is lower than 1,000m / min. This is preferred.
  • the high-strength expression of the fiber it is preferable for the high-strength expression of the fiber to be stretched in a high magnification and multistage through a non-contact heating chamber and a plurality of high-pressure rollers that can be temperature controlled, and to be stretched in the range of 110 ° C to 125 ° C.
  • the non-contact heating chamber used in the stretching process reduces the defects of yarn by minimizing surface friction instead of the heated roller as hundreds to thousands of polyethylene multifilament strands pass and delivers uniform thermal efficiency to the multifilament for high multistage stretching. Make it possible.
  • a polyethylene resin having a weight average molecular weight of 110,000 g / mol, a molecular weight distribution index (MWD) of 2.5 and a k of 0.020 was melted and extruded, and then an undrawn yarn was obtained at 100 mm or less through a 280 ° C. hot tube section at a nozzle. It was wound at 300 m / min and stretched a total of 18 times through a non-contact heating chamber of 115 °C in the first stretching process, 125 °C in the second stretching process to produce a polyethylene yarn.
  • Polyethylene yarns were prepared in the same manner as in Example 1 except that K was 0.034.
  • a polyethylene yarn was prepared in the same manner as in Example 1 except that k was 0.036.
  • a polyethylene yarn was prepared in the same manner as in Example 1 except that k was 0.064.
  • a polyethylene yarn was prepared in the same manner as in Example 1 except that k was 0.071.
  • a polyethylene yarn was prepared in the same manner as in Example 1 except that the molecular weight distribution index (MWD) was 2.3 and k was 0.020.
  • MFD molecular weight distribution index
  • a polyethylene yarn was prepared in the same manner as in Example 1 except that the weight average molecular weight was 110,000 g / mol, the molecular weight distribution index (MWD) was 3.5, k was 0.020, and the draw ratio was 15. Since the raw material having a molecular weight distribution index of 3.5 cannot work up to 18 times the draw ratio, a maximum draw ratio of 15 is applied.
  • a polyethylene yarn having a weight average molecular weight of 125,000 g / mol, a molecular weight distribution index (MWD) of 3.5 and a k of 0.020 was melted and extruded to obtain an undrawn yarn, which was drawn 15 times in total through a non-contact heating chamber to produce a polyethylene yarn. It was.
  • Polyethylene yarn was prepared in the same manner as in Example 1 except that the total draw ratio was 16 times using polyethylene resin having k of 0.076.
  • a polyethylene yarn was prepared in the same manner as in Example 1 except that the total draw ratio was 10 times using a polyethylene resin having k of 0.100.
  • the gel distribution ratio ( k ) was defined as the ratio of the small gel distribution ( ⁇ 1 ) and the sand gel distribution ( ⁇ 2 ) per unit area, according to Equation 1 below:
  • the machine rotated 90 degrees, wound 90m of yarn, measured the weight, and converted to 9,000m of the denier (denier, de ') standard.
  • the strength, elongation and elastic modulus of the fibers were measured in accordance with ASTM D-2256 using Universal Testing Mechine (INSTRON), a universal testing machine, and measured 10 times at a speed of 300 mm / min at 20 ° C and 65% relative humidity. One value was defined as the mean value for each of strength, elongation and elastic modulus.
  • the strength is defined as the stress-strain curve when the fiber is held in the universal testing machine and loaded at the above speed to tension, and the load when the fiber is cut is divided by denier divided by g / d.
  • Elongation is defined as the percentage of the initial length to the length that is stretched until cut, and modulus of elasticity is the tangential slope of the curve in g / d near the origin of the stress-strain curve displayed when tensioning.
  • This measurement method is defined in terms of the average value of each measured value for 10 measurements.
  • the total number of yarns produced and the number of yarns trimmed were calculated and evaluated as a percentage.
  • the incidence frequency was evaluated according to the number of mowers measured per 100,000 m for the total produced yarn.
  • 'yarn' is understood to mean a polyethylene fiber that is finally manufactured by multi-stretching in an unstretched yarn, that is, a manufactured polyethylene multifilament or polyethylene stretched yarn.
  • Example 1 Example 2
  • Example 3 Example 4
  • Example 6 Weight average molecular weight (Mw) g / mol 110,000 110,000 110,000 110,000 110,000 110,000 Molecular Weight Distribution Index (MWD) - 2.5 2.5 2.5 2.5 2.5 2.5 2.3 Distribution ratio ( k ) - 0.020 0.034 0.036 0.064 0.071 0.020 Elongation ratio - 18 18 18 18 18 18 18 Radiation workability % 98.6 97.8 97.5 95.5 96.3 98.6 Mouth occurrence frequency Ten thousand meters 6 6 8 8 10 6 Island de ' 400 400 400 400 400 400 400 400 400 400 400 400 400 400 400 400 burglar g / d 18.2 17.8 17.6 16.5 16.2 18.6 Modulus g / d 435.5 432.2 422.8 410.9 415.3 452.1
  • the distribution ratio k of the gel is in the range of 0.020 ⁇ k ⁇ 0.075 and the molecular weight distribution index is greater than 0 and less than 2.5, the occurrence of the moor in the spinning workability and the stretching process is minimized and the physical properties are excellent and the strength and High performance polyethylene fibers with excellent modulus of elasticity can be obtained.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)

Abstract

La présente invention concerne une fibre de polyéthylène et son procédé de préparation, la fibre de polyéthylène, obtenue en utilisant une résine de polyéthylène ayant un taux de distribution de gel qui dépend de la taille et de l'indice de distribution du poids moléculaire dans une certaine plage, présentant une excellente uniformité et aptitude au filage, ce qui lui confère d'excellentes qualités de filaments multiples et propriétés physiques pendant le tirage.
PCT/KR2013/005782 2012-11-29 2013-06-28 Fibre de polyéthylène et son procédé de préparation WO2014084470A1 (fr)

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KR10-2012-0137261 2012-11-29
KR1020120137261A KR101440570B1 (ko) 2012-11-29 2012-11-29 폴리에틸렌 섬유 및 그의 제조방법

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3241931A4 (fr) * 2014-12-31 2018-07-04 HUVIS Co., Ltd. Fibre de polyéthylène, son procédé de fabrication et son appareil de fabrication

Families Citing this family (5)

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KR101945943B1 (ko) * 2017-04-27 2019-02-11 주식회사 휴비스 고강도 폴리에틸렌 멀티필라멘트 섬유 및 그의 제조방법
KR101973772B1 (ko) * 2017-12-28 2019-04-30 주식회사 휴비스 백색도가 향상된 고강도 폴리에틸렌 섬유
KR101981760B1 (ko) * 2018-01-05 2019-05-27 주식회사 휴비스 공정성이 향상된 고강도 폴리에틸렌 섬유
KR101981759B1 (ko) * 2018-01-05 2019-05-27 주식회사 휴비스 공정성이 향상된 고강도 폴리에틸렌 섬유
WO2020138971A1 (fr) 2018-12-28 2020-07-02 코오롱인더스트리 주식회사 Fil texturé multifilament de polyéthylène et procédé de fabrication de celui-ci

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JP2001316939A (ja) * 2000-05-02 2001-11-16 Toyobo Co Ltd 高強度ポリエチレン繊維およびその製造方法
JP3832614B2 (ja) * 1999-03-18 2006-10-11 東洋紡績株式会社 高強度ポリエチレン繊維およびその製造方法
KR20060106058A (ko) * 2005-04-06 2006-10-12 동양제강 주식회사 초고강도 폴리에틸렌섬유의 제조방법
KR20100003373A (ko) * 2002-04-09 2010-01-08 도요 보세키 가부시키가이샤 폴리에틸렌 섬유 및 그의 제조 방법

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TW200504093A (en) 2003-05-12 2005-02-01 Dow Global Technologies Inc Polymer composition and process to manufacture high molecular weight-high density polyethylene and film therefrom
DE602005015741D1 (de) 2004-09-03 2009-09-10 Honeywell Int Inc Gezogene gelfaserpolyethylengarne und ziehverfahren
EP2316990B1 (fr) * 2008-08-20 2013-01-16 Toyobo Co., Ltd. Fibre de polyéthylène hautement fonctionnelle, tissu tissé/tricoté le comprenant et gant en celui-ci

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Publication number Priority date Publication date Assignee Title
JP3832614B2 (ja) * 1999-03-18 2006-10-11 東洋紡績株式会社 高強度ポリエチレン繊維およびその製造方法
JP2001316939A (ja) * 2000-05-02 2001-11-16 Toyobo Co Ltd 高強度ポリエチレン繊維およびその製造方法
KR20100003373A (ko) * 2002-04-09 2010-01-08 도요 보세키 가부시키가이샤 폴리에틸렌 섬유 및 그의 제조 방법
KR20060106058A (ko) * 2005-04-06 2006-10-12 동양제강 주식회사 초고강도 폴리에틸렌섬유의 제조방법

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3241931A4 (fr) * 2014-12-31 2018-07-04 HUVIS Co., Ltd. Fibre de polyéthylène, son procédé de fabrication et son appareil de fabrication

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KR101440570B1 (ko) 2014-09-17

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