WO2019059560A1 - 고강도 폴리에틸렌테레프탈레이트 원사 및 그 제조방법 - Google Patents

고강도 폴리에틸렌테레프탈레이트 원사 및 그 제조방법 Download PDF

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Publication number
WO2019059560A1
WO2019059560A1 PCT/KR2018/010211 KR2018010211W WO2019059560A1 WO 2019059560 A1 WO2019059560 A1 WO 2019059560A1 KR 2018010211 W KR2018010211 W KR 2018010211W WO 2019059560 A1 WO2019059560 A1 WO 2019059560A1
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WIPO (PCT)
Prior art keywords
polyethylene terephthalate
spinning
nozzle
intrinsic viscosity
yarn
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PCT/KR2018/010211
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English (en)
French (fr)
Korean (ko)
Inventor
임기섭
정일
박성호
Original Assignee
코오롱인더스트리 주식회사
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Priority to CN201880061237.7A priority Critical patent/CN111148866A/zh
Priority to EP18858587.1A priority patent/EP3686326A4/de
Priority to US16/640,771 priority patent/US20200216980A1/en
Priority to JP2020531410A priority patent/JP2020531710A/ja
Publication of WO2019059560A1 publication Critical patent/WO2019059560A1/ko

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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
    • 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
    • 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
    • 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

Definitions

  • the present invention relates to a polyethylene terephthalate yarn having a high strength compared to a conventional polyethylene terephthalate yarn and a method for producing the same.
  • BACKGROUND OF THE INVENTION 1 Field of the Invention The present invention relates to a polyethylene terephthalate yarn and a production method thereof.
  • PET industrial polyethylene terephthalate
  • a method for producing a PET yarn includes a spinning process for forming a multifilament and a process for stretching the multifilament at a predetermined stretch ratio, wherein the spinning process includes melting the PET chip, And collecting the filaments in the solid state formed by cooling after the PET melt is discharged through the nozzle to form the multifilament.
  • PET yarns Since it is generally required that industrial PET yarns have excellent form stability (i.e. low specific load elongation (EASL) and low dry shrinkage), it is necessary to produce PET yarns, for example at high speeds of 1500 m / min or higher have. That is, by increasing the degree of orientation of the fiber before the stretching process, the morphological stability can be improved.
  • EASL specific load elongation
  • the stretching ratio applicable in the stretching step is inevitably limited. That is, if the spinning speed is increased to more than 1500 m / min to improve the morphological stability of the PET yarn, the stretching ratio applicable to the stretching step can not be lowered to 2.0 or less. The lower the stretching ratio, the lower the strength of the PET yarn.
  • the present invention is directed to a PET yarn and a manufacturing method thereof that can prevent the problems due to the limitations and disadvantages of the related art.
  • One aspect of the present invention is to provide a PET yarn having excellent shape stability and high strength compared to conventional PET yarns.
  • Another aspect of the present invention is to provide a method for producing a PET yarn having high strength compared to conventional PET yarn while having excellent shape stability.
  • a filament yarn comprising 100 to 500 filaments each having a fineness of 2 to 5 denier and having an intrinsic viscosity of 1.1 dl / g or more and a tensile strength of 10 g / d or more.
  • PET yarn is provided.
  • the PET yarn may have an intrinsic viscosity of 1.1 to 1.25 dl / g and a tensile strength of 10 to 10.6 g / d.
  • the PET yarn may have elongation of 3 to 6% or less at 4.5 g / d laod and dry heat shrinkage of 7 to 12% at a load of 4.5 g / d.
  • the PET yarn may have a cut elongation of 13 to 14%.
  • the PET yarn may have a cut elongation of 13.4 to 13.9%.
  • a method for producing a spinning melt comprising: melting a polyethylene terephthalate chip having an intrinsic viscosity of 1.4 to 1.7 dl / g; Discharging the spinning melt through a nozzle of a spinning pack; Heating the spinning melt immediately before being discharged from the nozzle by a heat source of 300 to 500 ° C located directly under the nozzle; Collecting a plurality of filaments formed by the discharging step to form a multifilament; And stretching the multifilament, wherein the temperature of the spinning pack is maintained at 280 to 305 ⁇ ⁇ .
  • the PET yarn manufacturing method may be applied with a stretching speed of 4000 to 6200 m / min and a stretching ratio of 1.9 to 2.5.
  • the distance between the nozzle and the heat source may be 5 to 50 mm.
  • the temperature of the heat source may be higher than the temperature of the radiation pack.
  • the heat source may include a hot wire.
  • the heat source may include a plurality of heat lines, and the heat lines may be arranged between the filaments so as not to interfere with the movement of the filaments.
  • the hot lines may be arranged at regular intervals.
  • Each of the hot lines may be arranged to be parallel to the lower surface of the nozzle.
  • the stretching ratio in the stretching step may be 1.9 to 2.5.
  • the discharging step may be performed at a discharging pressure of 2400 psi or less.
  • a relatively high intrinsic viscosity (IV) PET chip is used and the polymer pyrolysis during the spinning process and thus the drop of the intrinsic viscosity (IV drop) is minimized,
  • a PET yarn having a viscosity (IV) and a relatively high tensile strength of 10 g / d or more can be produced.
  • the uniformity of the mechanical properties of the plurality of filaments constituting the polyester yarn can be improved.
  • FIG. 1 schematically shows an apparatus for producing a PET yarn according to an embodiment of the present invention
  • FIG. 2 is an enlarged view of a portion A in Fig.
  • the inventors of the present application have found that the intrinsic viscosity (I.V.) of PET yarn is closely related to the strength of PET yarn. That is, the higher the intrinsic viscosity (I.V.) of the PET yarn, the greater the strength of the PET yarn. Therefore, in order to produce PET yarn having higher strength than conventional PET yarn, it is required to produce PET yarn having higher intrinsic viscosity (I.V.) than conventional PET yarn.
  • the low fluidity of the spinning melt increases the discharge pressure, increasing the risk of leaks in the spinning pack and damage to the spinning pack.
  • a relatively high intrinsic viscosity (IV) of from 1.4 to 1.7 dl / g is obtained to produce a PET yarn having a relatively high intrinsic viscosity (IV) of 1.1 dl / g or more and a relatively high strength of 10 g / ) PET chip and a relatively low radiation temperature of 280 to 305 DEG C is applied, it is possible to prevent the leakage phenomenon and the damage of the radiation pack in the above-mentioned radiation pack by applying high-temperature heat energy from directly underneath.
  • FIG. 1 a method of manufacturing a PET yarn according to an embodiment of the present invention will be described in detail with reference to FIGS. 1 and 2.
  • FIG. 1 a method of manufacturing a PET yarn according to an embodiment of the present invention will be described in detail with reference to FIGS. 1 and 2.
  • An apparatus includes an extruder 110, a spinning pack 120, a heat source 130, a cooling unit 140, a focusing unit 150, a stretching unit 160, and a winder 170.
  • the radiation pack 120 includes main components such as a filter, a distribution plate, a nozzle 121, and the like, and a pack body 122 surrounding the main components.
  • the heat source 130 may be fixed to the nozzle 121 through a bolt 131. Alternatively, the heat source 130 may be secured to a spin block (not shown) surrounding the spinning pack 120.
  • the PET chip is put into the extruder 110 and then melted to produce a spinning melt (i.e., PET melt), and the spinning melt is extruded into the spinning pack 120.
  • a spinning melt i.e., PET melt
  • the PET chip used in the present invention has an intrinsic viscosity (I.V.) of 1.4 to 1.7 dl / g, which is higher than the intrinsic viscosity (I.V.) (less than 1.4 dl / g) of a PET chip used in the past.
  • I.V. intrinsic viscosity
  • the spinning melt transferred from the extruder 110 to the spinning pack 120 is discharged through the holes of the nozzle 121.
  • the nozzle 121 may have 100 to 500 holes, and L / D, which is a ratio of the length L to the diameter D of each hole, may be 2 to 5.
  • the radiation temperature that is, the temperature of the radiation pack 120 (more specifically, the temperature of the pack body 122) is maintained at 280 to 305 ⁇ when the radiation process is proceeding.
  • the temperature of the radiation pack 120 can be measured through a temperature sensor installed in a spinning block surrounding the radiation pack 120.
  • the spinning temperature is lower than 280 ⁇ ⁇ , the spinning melt is lowered in uniformity and fluidity of the spinning melt is excessively lowered to such an extent that a high discharge pressure outside the allowable range is required.
  • the spinning temperature of 280 to 305 ° C. which is much lower than the spinning temperature of 310 to 320 ° C., which is applied to the conventional PET yarn manufacturing method, is applied, IV drop
  • the spinning temperature of 280 to 305 ° C. which is much lower than the spinning temperature of 310 to 320 ° C., which is applied to the conventional PET yarn manufacturing method, is applied, IV drop
  • the higher the intrinsic viscosity (IV) of the PET chip and the lower the spinning temperature the lower the fluidity of the spinning melt and the lower fluidity of the spinning melt increases the discharge pressure, Thereby increasing the risk of leakage and the damage of the radiation pack 120.
  • the spinning melt immediately before being discharged from the nozzle 121 is heated by a heat source 130 located immediately below the nozzle 121.
  • the spinning process proceeds at a discharge pressure of 2400 psi or less, preferably 2350 psi or less, more preferably 2320 psi or less.
  • the distance between the nozzle 121 and the heat source 130 may be 5 to 50 mm in order to appropriately heat the spinning melt immediately before discharge.
  • the temperature of the heat source 130 is higher than the temperature of the radiation pack 120.
  • the temperature of the heat source 130 may be 300 to 500 ° C, preferably 320 to 490 ° C, more preferably 350 to 480 ° C.
  • the heat source 130 may include a heat ray.
  • the heat source 130 may include a plurality of heat lines, and the heat rays may be radiated through the plurality of semi-solid state filaments 10 formed by discharging the spinning melt from the holes of the nozzle 121
  • the filaments 10 may be arranged such that they do not interfere with each other.
  • the hot wires may be arranged at regular intervals and each of the hot wires may be arranged to be parallel to the lower surface of the nozzle 121.
  • each of the filaments 10 is uniformly spaced from the heat lines by a certain distance (for example, 3 to 10 mm), uniformity of physical properties between the filaments 10 can be ensured.
  • a plurality of hot wires constituting the heat source 130 are arranged at right angles to the nozzle 121 (IV) having a relatively high intrinsic viscosity (IV) of 1.4 to 1.7 dl / g is used to heat the spinning melt immediately before being discharged from the nozzle 121, Even though the temperature is applied, leakage phenomenon in the radiation pack due to an increase in discharge pressure and damage to the radiation pack can be prevented.
  • a plurality of semi-solid filaments 10 formed by discharging the spinning melt from the holes of the nozzle 121 are completely solidified while passing through the cooling part 140. Blowing the cooling wind at a proper temperature and speed to the filaments 10 for controlling the cooling process. The cooling behavior of the filaments 10 greatly affects the final properties of the fibers.
  • the fully-solidified filaments 10 are then converged by the focusing unit 150 to form the multifilament 20.
  • an emulsion may be applied to the multifilament 20. That is, the multifilament 20 forming step and the emulsion applying step may be performed simultaneously.
  • the emulsifying agent may be carried out through a method of MO (Metered Oiling) or RO (Roller Oiling).
  • the multifilament 20 formed through the focusing process is stretched by the stretching portion 160.
  • the extension portion 160 may include first to fifth godet rollers 161, 162, 163, 164, and 165.
  • the first godet roller 161 determines the spinning speed and the draft ratio.
  • the stretching of the multifilament 20 is performed between the first godet roller 161 and the fourth godet roller 164. That is, the draw ratio is determined by the ratio of the speed of the first godet roller 161 to the speed of the fourth godet roller 164.
  • the interval between the fourth godet roller 164 and the fifth godet roller 165 is a relaxation period and is defined by the length of the multifilament 167 drawn by the first to fourth godet rollers 161, 162, 163, (I) the excessive shrinkage of the multifilament 20, (ii) the distortion of the winder 170, and (iii) the unwinding of the multifilament 20, which can be understood as a contraction force immediately after being stretched, Can be prevented from being unstable.
  • the spinning speed (that is, the speed of the first godet roller 161) is 1500 to 3300 m / min and the speed after stretching ] Is 4000 to 6200 m / min, and the stretching ratio is 1.9 to 2.5.
  • the inventive high form stability PET yarns produced at a spinning speed of 1500 to 3300 m / min and a drawing speed of 4000 to 6200 m / min have an elongation of 3 to 6% at 4.5 g / d load 6% at 4.5 g / d laod) and a dry heat shrinkage of 7 to 12%.
  • At least one of the second to fourth godet rollers 162, 163, 164 may be provided with heating means for performing heat treatment / heat setting of the drawn multifilament 20.
  • heating means for performing heat treatment / heat setting of the drawn multifilament 20. For example, by adjusting the number of times the multifilament 20 is wound on the fourth godet roller 164, the time for which the multifilament 20 stays in the fourth godet roller 164 can be adjusted, and the heat treatment / Fixation can be performed.
  • the stretched and heat-treated multifilament 20 is wound by a winder 170 to complete the PET yarn.
  • the PET yarn of the present invention comprises 100 to 500 filaments each having a fineness of 2 to 5 denier and has a relatively high intrinsic viscosity (IV) of 1.1 dl / g or more and a relative relative viscosity of 10 g / d or more And high tensile strength.
  • the PET yarn has a cut elongation of 13 to 14%.
  • the high strength PET yarn of the present invention can be applied to various industrial applications such as tire cord, airbag and the like.
  • a plurality of semi-solid filaments formed by discharging the spinning melt from the holes of the nozzles are completely solidified while passing through the cooling section, and the drawing process, the heat treatment process and the winding process are sequentially performed on the multifilament in which the filaments are gathered, PET yarn (total fineness: 1000 denier) containing 250 filaments each having a fineness of denier was obtained.
  • a discharge pressure of 2101 psi was applied, the rate after drawing was 5800 m / min, and the draw ratio was 2.0.
  • the PET yarn was obtained in the same manner as in Example 1, except that the spinning temperature and the temperature of the hot wires were 299 ° C and 420 ° C, respectively, and the spinning process was performed at a discharge pressure of 2181 psi.
  • the PET yarn was obtained in the same manner as in Example 1, except that the spinning temperature and the temperature of the hot wires were 304 ⁇ and 380 ⁇ , respectively, and the spinning process was performed at a discharge pressure of 2312 psi.
  • a PET chip with an intrinsic viscosity (IV) of 1.4 dl / g was used for the preparation of the spinning melt and the spinning temperature and hot wire temperatures were 298 ° C and 380 ° C, respectively, and the spinning process was performed at a discharge pressure of 2160 psi PET yarn was obtained in the same manner as in Example 1. The results are shown in Table 1.
  • Example 2 The same method as in Example 1 was applied except that the spinning temperature was 310 ⁇ ⁇ , heating by hot wire was omitted, and a discharge pressure of 2930 psi was applied. However, due to the excessively high discharge pressure, spinning melt leakage in the spinning pack is caused and winding is not possible.
  • a PET chip with an intrinsic viscosity (IV) of 1.4 dl / g was used for the preparation of the spinning melt, except that the spinning temperature was 306 ° C, heating by hot wire was omitted and a discharge pressure of 2370 psi was applied , A PET yarn was obtained in the same manner as in Example 1.
  • a PET chip with an intrinsic viscosity (IV) of 1.21 dl / g was used for the preparation of the spinning melt, except that the spinning temperature was 299 ° C, heating by hot wire was omitted and a discharge pressure of 1910 psi was applied , A PET yarn was obtained in the same manner as in Example 1.
  • a PET chip with an intrinsic viscosity (IV) of 1.21 dl / g was used for the preparation of the spinning melt and the spinning temperature and the temperature of the hot wires were 292 ° C and 380 ° C respectively and the spinning process was carried out at a discharge pressure of 1850 psi PET yarn was obtained in the same manner as in Example 1. The results are shown in Table 1.
  • PET yarns of Examples and Comparative Examples were measured for intrinsic viscosity (IV), tensile strength, cut elongation, elongation at a load of 4.5 g / d (EASL@4.5g/d), and dry heat shrinkage by the following methods (IV of the dropped solidified sample was measured and the tensile strength, cut elongation, EASL@4.5g/d, and dry heat shrinkage of the yarn were not measurable for Comparative Example 1, which was impossible to roll), and the result Table 1 shows the results.
  • the intrinsic viscosity (I.V.) (dl / g) of each PET yarn was measured by a capillary viscometer according to the ASTM D4603-96 method.
  • the solvent used was a mixture of phenol / 1,1,2,2-tetrachloroethane (60/40 wt%).
  • the tensile strength (g / d) and elongation (%) of the PET yarn were measured using an all-purpose tensile tester of Instron Engineering Corp. (Canton, Mass) according to the ASTM D885 method (initial load: 0.05 gf / d, sample length: 250 mm, tensile speed: 300 mm / min), and EASL@4.5 g / d of PET yarn was measured.
  • the dry heat shrinkage percentage (%) of the PET yarn was calculated by the following formula Respectively.
  • a PET chip having a relatively high intrinsic viscosity (IV) of 1.4 to 1.7 dl / g was used and by applying a relatively low radiation temperature of 295 to 304 DEG C to minimize polymer pyrolysis, PET yarns having a high intrinsic viscosity (IV) of 1.11 to 1.25 dl / g, a high tensile strength of 10.0 to 10.6 g / d, and a cut elongation of 13.4 to 13.9% could be obtained.
  • Examples 1 to 4 although a PET chip having a relatively high intrinsic viscosity (IV) of 1.4 to 1.7 dl / g was used and a relatively low radiation temperature of 295 to 304 ⁇ was applied, (Spinning speed: 5800 mm / min) with a discharge pressure of 2101 to 2312 psi, that is, an allowable discharge pressure (that is, 2400 psi or less) by heating the spinning melt just before discharging could.
  • IV intrinsic viscosity

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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)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)
PCT/KR2018/010211 2017-09-22 2018-09-03 고강도 폴리에틸렌테레프탈레이트 원사 및 그 제조방법 WO2019059560A1 (ko)

Priority Applications (4)

Application Number Priority Date Filing Date Title
CN201880061237.7A CN111148866A (zh) 2017-09-22 2018-09-03 高强度聚对苯二甲酸乙二醇酯纱线及其制造方法
EP18858587.1A EP3686326A4 (de) 2017-09-22 2018-09-03 Hochfestes polyethylenterephthalatgarn und verfahren zu seiner herstellung
US16/640,771 US20200216980A1 (en) 2017-09-22 2018-09-03 High-strength polyethylene terephthalate yarn and method for producing the same
JP2020531410A JP2020531710A (ja) 2017-09-22 2018-09-03 高強度ポリエチレンテレフタレート原糸およびその製造方法

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KR10-2017-0122246 2017-09-22
KR20170122246 2017-09-22

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US (1) US20200216980A1 (de)
EP (1) EP3686326A4 (de)
JP (2) JP2020531710A (de)
KR (1) KR20190034083A (de)
CN (1) CN111148866A (de)
WO (1) WO2019059560A1 (de)

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CN111575817A (zh) * 2019-02-19 2020-08-25 海宁新高纤维有限公司 一种热塑性聚氨酯纤维的制造方法
CN113430656B (zh) * 2021-06-25 2022-05-06 江苏恒力化纤股份有限公司 一种制备超高强聚酯工业丝的方法
CN113430657B (zh) * 2021-06-25 2022-05-24 江苏恒力化纤股份有限公司 一种降低聚酯工业丝纺丝温度的方法

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JP2021120501A (ja) 2021-08-19
JP2020531710A (ja) 2020-11-05
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