US20200216980A1 - High-strength polyethylene terephthalate yarn and method for producing the same - Google Patents

High-strength polyethylene terephthalate yarn and method for producing the same Download PDF

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Publication number
US20200216980A1
US20200216980A1 US16/640,771 US201816640771A US2020216980A1 US 20200216980 A1 US20200216980 A1 US 20200216980A1 US 201816640771 A US201816640771 A US 201816640771A US 2020216980 A1 US2020216980 A1 US 2020216980A1
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Prior art keywords
spinning
polyethylene terephthalate
pet
yarn
intrinsic viscosity
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US16/640,771
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English (en)
Inventor
Ki Sub Lim
II Chung
Sung Ho Park
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Kolon Industries Inc
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Kolon Industries Inc
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Assigned to KOLON INDUSTRIES, INC. reassignment KOLON INDUSTRIES, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CHUNG, IL, LIM, Ki Sub, PARK, SUNG HO
Publication of US20200216980A1 publication Critical patent/US20200216980A1/en
Abandoned legal-status Critical Current

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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
    • D01D5/084Heating filaments, threads or the like, leaving the spinnerettes
    • 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
    • D01D5/098Melt spinning methods with simultaneous stretching
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00Physical properties
    • D10B2401/06Load-responsive characteristics
    • D10B2401/063Load-responsive characteristics high strength

Definitions

  • the present invention relates to a polyethylene terephthalate yarn and a method for producing the same, and more particularly to a polyethylene terephthalate yarn having higher strength than a conventional polyethylene terephthalate yarn and a method for producing the same.
  • PET industrial polyethylene terephthalate
  • the method of producing a PET yarn includes a spinning process of forming a multifilament and a process of drawing the multifilament at a predetermined draw ratio, wherein the spinning process includes melting a PET chip, discharging the PET melt through a nozzle of a spinning pack, and converging the filaments in a solidified state formed through cooling after the PET melt is discharged through the nozzle, thereby forming a multifilament.
  • the spinning speed and the draw ratio have a trade-off relationship
  • increasing the spinning speed ultimately limits the draw ratio that can be applied in the drawing step. That is, if the spinning speed is increased to 1500 m/min or more in order to improve the dimensional stability of the PET yarn, the draw ratio that can be applied in the drawing step is ultimately lowered to 2.0 or less. The lower the draw ratio, the lower the strength of the PET yarn.
  • the present invention relates to a PET yarn capable of preventing problems caused by the limitations and disadvantages of the related art as described above, and to a method for producing the same.
  • One aspect of the present invention provides a PET yarn having high strength compared to the existing PET yarn while having excellent dimensional stability.
  • Another aspect of the present invention provides a method for producing a PET yarn having high strength compared to the existing PET yarn while having excellent dimensional stability.
  • a PET yarn including 100 to 500 filaments each having fineness of 2 to 5 denier is provided, wherein the PET yarn has an intrinsic viscosity of 1.1 dl/g or more and a tensile strength of 10 g/d or more.
  • 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% at a 4.5 g/d load and dry heat shrinkage of 7 to 12%.
  • the PET yarn may have elongation at break of 13 to 14%.
  • the PET yarn may have elongation at break of 13.4 to 13.9%.
  • a method for producing a PET yarn including the steps of: melting a polyethylene terephthalate chip having an intrinsic viscosity of 1.4 to 1.7 dl/g to prepare a spinning melt; discharging the spinning melt through a nozzle of a spinning pack; heating the spinning melt just before discharging it from the nozzle by means of a heat source of 300 to 500° C. located immediately below the nozzle; converging a plurality of filaments formed by the discharging to form a multifilament; and drawing the multifilament, wherein a temperature of the spinning pack is maintained at 280 to 305° C.
  • a speed after drawing of 4000 to 6200 m/min and a draw ratio of 1.9 to 2.5 may be applied.
  • 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 spinning pack.
  • the heat source may include a hot wire.
  • the heat source may include a plurality of hot wires, and the hot wires may be respectively arranged between the filaments so as to not hinder the movement of the filaments.
  • the hot wires may be arranged at equal intervals.
  • Each of the hot wires may be arranged to be parallel to the lower surface of the nozzle.
  • the draw ratio in the drawing step may be 1.9 to 2.5.
  • the discharging step may be performed under a discharge pressure of 2400 psi or less.
  • the present invention by using a PET chip having a relatively high intrinsic viscosity (I.V.), and minimizing thermal decomposition of the polymer during the spinning process and a decrease in intrinsic viscosity (I.V. drop) resulting therefrom, it is possible to produce a PET yarn having a relatively high intrinsic viscosity (I.V.) of 1.1 dl/g or more and a relatively high tensile strength of 10 g/d or more.
  • I.V. intrinsic viscosity
  • the uniformity of mechanical properties of a large number of filaments constituting the polyester yarn can be improved.
  • FIG. 1 schematically illustrates an apparatus for producing a PET yarn according to one embodiment of the present invention.
  • FIG. 2 is an enlarged view of a portion A in FIG. 1 .
  • the present inventors found that the intrinsic viscosity (I.V.) of PET yarn is closely related to the strength of PET yarn. That is, as the intrinsic viscosity (I.V.) of the PET yarn increases, the strength of the PET yarn increases. Therefore, in order to produce a PET yarn having higher strength than a conventional PET yarn, it is required to produce a PET yarn having a higher intrinsic viscosity (I.V.) than the conventional PET yarn.
  • the spinning melt should be prepared using a PET chip having a higher intrinsic viscosity (I.V.) than the intrinsic viscosity (I.V.) of PET chips used in a conventional PET yarn manufacturing method, and (ii) thermal decomposition of polymers and a drop in intrinsic viscosity (I.V. drop) resulting therefrom should be minimized by applying a spinning temperature that is lower than the spinning temperature (i.e., the temperature of the spinning pack) that has been applied to a conventional PET yarn manufacturing method.
  • a spinning temperature that is lower than the spinning temperature (i.e., the temperature of the spinning pack) that has been applied to a conventional PET yarn manufacturing method.
  • the low fluidity of the spinning melt increases the discharge pressure and thus increases the risk of leakage at the spinning pack and damage to the spinning pack.
  • the present invention in order to produce a PET yarn having a relatively high intrinsic viscosity (I.V.) of 1.1 dl/g or more and relatively high strength of 10 g/d or more, despite using PET chips with a relatively high intrinsic viscosity (I.V.) of 1.4 to 1.7 dl/g and applying a relatively low spinning temperature of 280 to 305° C., it is possible to prevent the occurrence of a leakage phenomenon in the spinning pack and the damage to the spinning pack by providing high-temperature thermal energy from immediately below the spinneret.
  • I.V. intrinsic viscosity
  • FIGS. 1 and 2 the method for producing a PET yarn according to one embodiment of the present invention will be described in more detail.
  • An apparatus includes an extruder 110 , a spinning pack 120 , a heat source 130 , a cooling unit 140 , a converging unit 150 , a drawing unit 160 , and a winder 170 .
  • the spinning pack 120 includes main parts such as a filter, a distribution plate, a nozzle 121 , and the like, and a pack body 122 surrounding the main parts.
  • the heat source 130 may be fixed to the nozzle 121 via a bolt 131 .
  • the heat source 130 may be fixed to a spin block (not shown) surrounding the spinning pack 120 .
  • the PET chip is put into an extruder 110 , and then melted to form a spinning melt (that is, a PET melt), and the spinning melt is extruded into a spinning pack 120 .
  • a spinning melt that is, a PET melt
  • the PET chip used in the present invention has an intrinsic viscosity (I.V.) of 1.4 to 1.7 dl/g that is higher than the intrinsic viscosity (I.V.) (less than 1.4 dl/g) of the PET chip that has been previously used.
  • I.V. intrinsic viscosity
  • the intrinsic viscosity (I.V.) of the PET chip is less than 1.4 dl/g, it is impossible to produce a PET yarn having an intrinsic viscosity (I.V.) of 1.1 dl/g or more, and as a result, it is also impossible to produce PET yarns having a tensile strength of 10 g/d or more.
  • the intrinsic viscosity (I.V.) of the PET chip exceeds 1.7 dl/g, the fluidity of the spinning melt is excessively low to the extent that a high discharge pressure outside the allowable range (2400 psi or less) is required (even if the method of the present invention is applied).
  • the spinning melt delivered from the extruder 110 to the spinning pack 120 is discharged through holes in the nozzle 121 .
  • the nozzle 121 may have 100 to 500 holes, and L/D, which is a ratio of the length L and the diameter D of each hole, may be 2 to 5.
  • the spinning temperature that is, the temperature of the spinning pack 120 (more specifically, the temperature of the pack body 122 ) is maintained at 280 to 305° C.
  • the temperature of the spinning pack 120 may be measured via a temperature sensor installed in a spinning block surrounding the spinning pack 120 .
  • the spinning temperature is less than 280° C., not only is the uniformity of the spinning melt lowered, but the fluidity of the spinning melt is excessively low to the extent that a high discharge pressure outside the allowable range is required.
  • the present invention by applying a spinning temperature of 280 to 305° C. which is much lower than the spinning temperature of 310 to 320° C. that has been applied to a conventional PET yarn manufacturing method, thermal decomposition of polymers during the spinning process and a drop in intrinsic viscosity (I.V. drop) resulting therefrom can be minimized.
  • the low fluidity of the spinning melt increases the discharge pressure and thus increases the risk of a leakage phenomenon in the spinning pack 120 and damage to the spinning pack 120 .
  • the spinning melt just before being discharged from the nozzle 121 is heated by a heat source 130 located immediately below the nozzle 121 .
  • the spinning process is performed at a discharge pressure of 2400 psi or less, preferably 2350 psi or less, and more preferably 2320 psi or less.
  • the distance between the nozzle 121 and the heat source 130 may be 5 to 50 mm.
  • the temperature of the heat source 130 is higher than the temperature of the spinning pack 120 .
  • the temperature of the heat source 130 may be 300 to 500° C., preferably 320 to 490° C., and more preferably 350 to 480° C.
  • the heat source 130 may include a hot wire.
  • the heat source 130 may include a plurality of hot wires, and the hot wires may be arranged between the filaments 10 so that the spinning melt does not hinder the movement of the plurality of semi-solid filaments 10 formed while being discharged from the holes of the nozzle 121 .
  • the hot wires may be arranged at equal intervals and each of the hot wires may be arranged so as to be parallel to the bottom surface of the nozzle 121 .
  • the filaments 10 are uniformly spaced apart from the hot wires at a predetermined distance (for example, 3 to 10 mm), uniformity of physical properties between the filaments 10 may be ensured.
  • a plurality of hot wires constituting the heat source 130 are arranged at equal intervals immediately below the nozzle 121 , and instantaneously heat the spinning melt just before being discharged from the nozzle 121 .
  • I.V. intrinsic viscosity
  • a plurality of semi-solid filaments 10 formed as the spinning melt is discharged from the holes of the nozzle 121 are completely solidified while passing through the cooling unit 140 .
  • cooling air of an appropriate temperature and speed is blown into the filaments 10 .
  • the cooling behavior of the filaments 10 has a great influence on the final physical properties of the fiber.
  • the completely solidified filaments 10 are converged by the converging unit 150 to form a multifilament 20 .
  • An emulsion may be applied to the multifilament 20 at the converging unit 150 . That is, the step of forming the multifilament ( 20 ) and the step of applying the emulsion can be performed simultaneously.
  • the application of the emulsion may be performed using a MO (Metered Oiling) or RO (Roller Oiling) method.
  • the multifilament 20 formed through the converging step is drawn in the drawing unit 160 .
  • the drawing unit 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 spinning draft ratio.
  • Drawing of the multifilament 20 is performed between a first godet roller 161 and a fourth godet roller 164 . That is, a draw ratio is determined by a ratio of the speed of the fourth godet roller 164 to the speed of the first godet roller 161 .
  • the fourth godet roller 164 and the fifth godet roller 165 is a relaxation section, and by imparting some relaxation to the multifilament 20 drawn by the first to fourth godet rollers 161 , 162 , 163 , and 164 , it is possible to prevent (i) excessive shrinkage of the multifilament 20 , (ii) distortion of the winder 170 , and (iii) instability of unwinding, which may be caused by contraction forces immediately after drawing.
  • the spinning speed i.e., the speed of the first godet roller 161
  • the speed after drawing i.e., the speed of the fourth godet roller 164
  • the draw ratio is 1.9 to 2.5
  • PET yarns having high dimensional stability according to the present invention produced at spinning speeds of 1500 to 3300 m/min and speeds after drawing of 4000 to 6200 m/min have elongation of 3 to 6% at 4.5 g/d load and dry heat shrinkage of 7 to 12%.
  • At least one of the second to fourth godet rollers 162 , 163 , and 164 may be provided with a heating means to perform heat treatment/heat fixing of the drawn multifilament 20 .
  • a heating means to perform heat treatment/heat fixing of the drawn multifilament 20 .
  • the number of windings on the fourth godet roller 164 the amount of time that the multifilament 20 stays in the fourth godet roller 164 can be adjusted, which allows for appropriate heat treatment/heat fixing for the drawn yarn.
  • the drawn and heat-treated multifilament 20 is wound by a winder 170 to thereby complete the PET yarn.
  • the PET yarn of the present invention includes 100 to 500 filaments each having fineness of 2 to 5 denier, and it has a relatively high intrinsic viscosity (I.V.) of 1.1 dl/g or more and a relatively high tensile strength of 10 g/d or more as mentioned above. According to one embodiment of the present invention, the PET yarn has elongation at break of 13 to 14%.
  • I.V. intrinsic viscosity
  • the high strength PET yarn of the present invention can be applied to various industrial applications such as tire cords, air bags, and the like.
  • the spinning melt just before being discharged from the holes of the nozzle was heated with hot wires at 450° C. located 10 mm away from the nozzle immediately below the nozzle. A plurality of semi-solid filaments formed as the spinning melt was discharged from the holes of the nozzle were completely solidified while passing through the cooling unit.
  • the drawing step, the heat treatment step, and the winding step were sequentially performed on the plurality of filaments formed by converging the filaments, and thereby, a PET yarn containing 250 filaments each having fineness of 4 denier (total fineness: 1000 denier) was obtained.
  • a discharge pressure of 2101 psi was applied, the speed after drawing was 5800 m/min, and the drawing ratio was 2.0.
  • a PET yarn was obtained in the same manner as in Example 1, except that the spinning temperature and the temperature of the hot wire were 299° C. and 420° C., respectively, and the spinning process was performed under a discharge pressure of 2181 psi.
  • a PET yarn was obtained in the same manner as in Example 1, except that the spinning temperature and the temperature of the hot wire were 304° C. and 380° C., respectively, and the spinning process was performed under a discharge pressure of 2312 psi.
  • a PET yarn was obtained in the same manner as in Example 1, except that PET chips with an intrinsic viscosity (I.V.) of 1.4 dl/g were used for the production of the spinning melt, the spinning temperature and the temperature of the hot wire were 298° C. and 380° C., respectively, and the spinning process was performed under a discharge pressure of 2160 psi.
  • PET chips with an intrinsic viscosity (I.V.) of 1.4 dl/g were used for the production of the spinning melt, the spinning temperature and the temperature of the hot wire were 298° C. and 380° C., respectively, and the spinning process was performed under a discharge pressure of 2160 psi.
  • Example 2 The same method as in Example 1 was applied, except that the spinning temperature was 310° C., heating by the hot wire was omitted, and a discharge pressure of 2930 psi was applied. However, an excessively high discharge pressure caused a leakage of the spinning melt in the spinning pack, and thus winding was impossible.
  • a PET yarn was obtained in the same manner as in Example 1, except that a PET chip with an intrinsic viscosity (I.V.) of 1.4 dl/g was used for the preparation of the spinning melt, the spinning temperature was 306° C., heating by the hot wire was omitted, and a discharge pressure of 2370 psi was applied.
  • I.V. intrinsic viscosity
  • a PET yarn was obtained in the same manner as in Example 1, except that a PET chip with an intrinsic viscosity (I.V.) of 1.21 dl/g was used for the preparation of the spinning melt, the spinning temperature was 299° C., heating by the hot wire was omitted, and a discharge pressure of 1910 psi was applied.
  • I.V. intrinsic viscosity
  • a PET yarn was obtained in the same manner as in Example 1, except that a PET chip with an intrinsic viscosity (I.V.) of 1.21 dl/g was used for the preparation of the spinning melt, the spinning temperature and the temperature of the hot wires were 292° C. and 380° C., respectively, and the spinning process was performed under a discharge pressure of 1850 psi.
  • I.V. intrinsic viscosity
  • the PET yarns of the examples and comparative examples were measured for intrinsic viscosity (I.V.), tensile strength, elongation at break, elongation at 4.5 g/d load (EASL@4.5 g/d), and dry heat shrinkage by the following method, respectively.
  • I.V. intrinsic viscosity
  • EASL@4.5 g/d tensile strength
  • EASL@4.5 g/d dry heat shrinkage
  • the intrinsic viscosity (I.V.) (dl/g) of each PET yarn was measured by a capillary viscometer according to Test Method ASTM D4603-96.
  • the solvent used was a mixture of phenol/1,1,2,2-tetrachloroethane (60/40 wt %).
  • the initial length (L1) of the specimen and the length (L2) of the specimen after 2 minutes in an oven at 177° C. were respectively measured in accordance with Test Method ASTM D885, and then the dry heat shrinkage (%) of the PET yarn was calculated by the following Equation.
  • PET yarns with high intrinsic viscosity (I.V.) of 1.11 to 1.25 dl/g, high tensile strength of 10.0 to 10.6 g/d, and elongation at break of 13.4 to 13.9% could be obtained.
  • PET chips with an intrinsic viscosity (I.V.) of less than 1.4 dl/g were used as in Comparative Examples 3 and 4, although low spinning temperatures of 299° C. or 292° C. were applied and thus the thermal decomposition of the polymer would be less than that of Examples 1 to 4, the intrinsic viscosity (I.V.) and tensile strength of PET yarns did not reach 1.1 dl/g and 10 g/d, respectively.
  • PET chips having a relatively high intrinsic viscosity (I.V.) of 1.4 dl/g were used, but even when a high spinning temperature of 306° C. was applied and thermal decomposition of the polymer occurred, the intrinsic viscosity (I.V.) and tensile strength of PET yarns did not reach 1.1 dl/g and 10 g/d, respectively.

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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)
US16/640,771 2017-09-22 2018-09-03 High-strength polyethylene terephthalate yarn and method for producing the same Abandoned US20200216980A1 (en)

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KR10-2017-0122246 2017-09-22
KR20170122246 2017-09-22
PCT/KR2018/010211 WO2019059560A1 (ko) 2017-09-22 2018-09-03 고강도 폴리에틸렌테레프탈레이트 원사 및 그 제조방법

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

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Publication number Priority date Publication date Assignee Title
US20220145496A1 (en) * 2019-02-19 2022-05-12 Basf Se A process for producing a thermoplastic polyurethane fiber with low shrinkage, and the use of the fiber
CN113430657A (zh) * 2021-06-25 2021-09-24 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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