WO2018135714A2 - Methods for manufacturing polyethylene terephthalate yarn and car mat - Google Patents
Methods for manufacturing polyethylene terephthalate yarn and car mat Download PDFInfo
- Publication number
- WO2018135714A2 WO2018135714A2 PCT/KR2017/007154 KR2017007154W WO2018135714A2 WO 2018135714 A2 WO2018135714 A2 WO 2018135714A2 KR 2017007154 W KR2017007154 W KR 2017007154W WO 2018135714 A2 WO2018135714 A2 WO 2018135714A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- polyethylene terephthalate
- yarn
- phase polymerization
- polymer
- solid phase
- Prior art date
Links
- 229920000139 polyethylene terephthalate Polymers 0.000 title claims abstract description 49
- 239000005020 polyethylene terephthalate Substances 0.000 title claims abstract description 49
- -1 polyethylene terephthalate Polymers 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 29
- 239000007790 solid phase Substances 0.000 claims abstract description 21
- 238000009987 spinning Methods 0.000 claims abstract description 8
- 238000004804 winding Methods 0.000 claims abstract description 8
- 239000007791 liquid phase Substances 0.000 claims abstract description 6
- 238000002844 melting Methods 0.000 claims abstract description 4
- 230000008018 melting Effects 0.000 claims abstract description 4
- 229920000642 polymer Polymers 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000005299 abrasion Methods 0.000 abstract description 8
- 229920000728 polyester Polymers 0.000 abstract description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 abstract 1
- 238000001816 cooling Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 238000005886 esterification reaction Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- LLLVZDVNHNWSDS-UHFFFAOYSA-N 4-methylidene-3,5-dioxabicyclo[5.2.2]undeca-1(9),7,10-triene-2,6-dione Chemical group C1(C2=CC=C(C(=O)OC(=C)O1)C=C2)=O LLLVZDVNHNWSDS-UHFFFAOYSA-N 0.000 description 1
- QDQVOCDLPGGZBQ-UHFFFAOYSA-N OCCC=1C(=C(C(=O)O)C=CC1C(=O)O)CCO.C(C1=CC=C(C(=O)O)C=C1)(=O)OCCO Chemical compound OCCC=1C(=C(C(=O)O)C=CC1C(=O)O)CCO.C(C1=CC=C(C(=O)O)C=C1)(=O)OCCO QDQVOCDLPGGZBQ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/80—Solid-state polycondensation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
- C08L67/03—Polyesters derived from dicarboxylic acids and dihydroxy compounds the dicarboxylic acids and dihydroxy compounds having the carboxyl- and the hydroxy groups directly linked to aromatic rings
-
- 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
Definitions
- the present invention relates to a method for producing a polyethylene terephthalate yarn having improved abrasion resistance by using a polyethylene terephthalate chip having improved viscosity through liquid phase polymerization or solid phase polymerization, and a carpet comprising a polyethylene terephthalate yarn prepared by the above method. .
- polyester resins especially polyethylene terephthalate resins, are linear polymers synthesized from dicarboxylic acids or their ester-forming derivatives and diols or their ester-forming derivatives, and are inexpensive, yet have excellent mechanical and chemical properties. In addition to excellent gas barrier properties, it is widely used in the manufacture of various containers, films, fibers and the like.
- polyester is produced by the condensation polymerization method, the equilibrium reaction according to external conditions to obtain a commercially available viscosity through the conditions of high temperature, high vacuum, wherein a certain amount of oligomers remain in the final polymer.
- the carpet mat market is composed of PET Needle Punch and Nylon BCF.
- the price is cheaper than nylon carpet mats, but it has been limited to small cars due to the problem of abrasion resistance (300 times) required for automobile mats.
- Applicant proceeded to the above invention to express PET BCF with improved wear resistance than the existing PET Needle Punch to expand the market of PET carpet, succeeded in the commercialization by achieving more than 800 times of nylon wear resistance and the current market It is expanding.
- One aspect of the present invention for achieving the above object comprises the steps of melting a polyethylene terephthalate chip to prepare a polymer; And spinning the polymer with a spinning nozzle, stretching in multiple stages, and then winding the polymer to prepare a polyethylene terephthalate yarn, wherein the polyethylene terephthalate chip has a viscosity of 0.8 to 1.5 dl through liquid phase polymerization or solid phase polymerization. It is characterized in that / g and preferably provides a method for producing a high strength polyethylene terephthalate yarn through liquid phase polymerization or solid phase polymerization in the range of 0.85 to 1.30 dl / g.
- Solid phase polymerization of the esterification reaction through the solid phase polymerization is carried out by drying (batch) or continuous polymerization, drying for 4 to 6 hours water removal at 110 to 170 °C under vacuum conditions and 235 to 255 It is preferable to make solid-phase polymerization time into 20 to 30 hours by heating up over 4 to 6 hours and performing solid-phase polymerization in 235-255 degreeC range.
- the drying rate is drastically lowered when the temperature is lower than 110 ° C. during drying, and when the temperature is 170 ° C. or higher, physical properties fall.
- the solid phase polymerization temperature is less than 235 °C or the solid phase polymerization time is less than 20 hours, the reaction does not occur sufficiently, the wear resistance is inferior when the solid phase temperature exceeds 255 °C or the solid phase polymerization time exceeds 30 hours.
- the present invention provides a polyethylene terephthalate yarn characterized in that the fineness is 800 to 1500 denier, preferably 850 to 1350 denier.
- the strength, toughness, and density of the yarn may be improved, and thus the wear resistance of the mat may be improved.
- Method for producing a polyethylene terephthalate yarn comprises the steps of melting a polyethylene terephthalate chip to prepare a polymer; And spinning the polymer by a spinning nozzle, stretching in multiple stages, and then winding the polymer to prepare a polyethylene terephthalate yarn, wherein the polyethylene terephthalate chip increases viscosity through liquid phase polymerization or solid phase polymerization. do.
- a method for producing a high strength polyethylene terephthalate yarn characterized in that 0.8 to 1.5dl / g as described above.
- the intrinsic viscosity (I.V.) of the polyethylene terephthalate chip manufactured as described above is preferably at a level of 0.8 to 1.5 or less. When the intrinsic viscosity is less than 0.8, the strength of the yarn is low, and the radiation is not good when it exceeds 1.5.
- the fineness of the polyethylene terephthalate yarn thus produced is preferably from 800 to 1500 denier, more preferably from 850 to 1350 denier. If the fineness of the yarn is less than 800 denier, the uprightness of the fabric pile is lowered during the forming of the mat, resulting in poor abrasion resistance, molding restoring power and appearance, and the density of the mat mat fabric becomes lower when the density exceeds 1500 demier, resulting in poor wear resistance and resilience. Done.
- polyethylene terephthalate yarn can be produced a carpet improved in the wear resistance.
- liquid polymerized or solid-phase polymerized polyethylene terephthalate chip according to the present invention is melt-spun at 245 to 335 ° C. to pass a spinneret.
- the polyethylene terephthalate resin underlying in the present invention contains 90 mol% or more of repeating units of ethylene terephthalate.
- the cooling temperature is adjusted to 10 ⁇ 35 °C.
- the speed of the cooling air is less than 0.2m / sec, the cooling effect is insufficient, if it exceeds 1.0m / sec, the shaking of the yarn is excessive, which is a problem in the spinning workability.
- the cooling temperature is less than 10 °C economically disadvantageous, if it exceeds 35 °C cooling effect is inferior.
- the first and second stages are oiled using neat or water-soluble emulsions to improve the cohesion, lubricity and smoothness of the yarn. Increase it.
- the feed roller is supplied to the stretching roller at a speed of 100 to 1,000 m / min, preferably 400 to 800 m / min, wherein the stretching roller is at a temperature of 100 to 230 ° C. and 2.5 to 6.0 of the feed roller speed.
- stretching is preferably from 3.5 to 5.0 fold.
- the filament passed through the stretching roller passes through a texturing unit with a texturing nozzle to impart bulkiness.
- the filament is irregularly formed by spraying a heating fluid of 150 to 270 ° C at a pressure of 3 to 10 kg / cm2 inside the texturing unit. It is crimped to a dimension and the crimp rate at this time is 3 to 50%.
- the temperature of the heating fluid is preferably 150 ⁇ 270 °C, which is less than 150 °C texturing effect and exceeds 270 °C causes damage to the filament.
- the pressure of the heating fluid is preferably 3 to 10 kg / cm 2, which is less than the texture effect of less than 3 kg / cm 2 and causes damage to the filament exceeds 10 kg / cm 2.
- the filament After passing through the texturing unit, the filament is cooled while passing through the cooling section.
- a slight twist and a knot are applied at a pressure of 2.0 to 8.0 kg / m 2.
- the range is 0 to 40 times / m, preferably 10 to 25 times.
- the rollers are passed through at a speed of 0.65 to 0.95 times the speed of the stretching roller to give a relaxation rate of 5 to 35%, and then wound up at the final winding machine.
- the speed of the winder is usually adjusted so that the tension of the thread is in the range of 50 to 350 g.
- the tension in the winding machine is less than 50g, the winding is impossible, and if it exceeds 350g, the bulkiness is reduced, the yarn shrinks greatly and causes high tension, which causes trouble in the work.
- the speed of the relaxation roller is less than 0.65 times of the stretching roller speed, it is not wound, and if it exceeds 0.95 times, the bulkiness is decreased, the yarn shrinks greatly, and high tension causes the work.
- the method relates to a BCF made of polyethylene terephthalate resin only, the step-by-step process is the same as above when producing the primary yarn according to the carpet application.
- the raw material supply it is also possible to prepare the yarn by adding a predetermined amount of colorant to the base chip input amount.
- the polyethylene terephthalate multifilament prepared according to the present invention as described above is produced into a carpet through a post-process.
- Carpets made with the BCF company of the present invention can be produced in any manner known to those skilled in the art.
- Preferably a plurality of BCF yarns are cable twisted and heat set together and then weave to the primary back side.
- the latex adhesive and the secondary backside are then applied. Cut pile style carpets or loop pile style carpets with pile heights of approximately 2-20 mm can be made.
- the yarn is left for 24 hours in a constant temperature and humidity room under standard conditions, that is, 25 ° C. and 65% RH relative humidity, and the sample is measured by a tensile tester using the ASTM 2256 method.
- TYT-EW Textured Yarn Tester
- the wear resistance of the mat was measured under the following conditions, and the wear resistance of the mat was evaluated based on the final wear at the time when the mat floor was exposed at the level equivalent to the grade 2.5 of the external appearance. It was.
- the polyethylene terephthalate polymer produced through spinneret having 128 holes and having a Y-shaped cross section is melt-spun at 290 ° C.
- the polymer exiting the spinneret is cooled by 0.5 m / s at 20 ° C. cooling air at the bottom of the nozzle and then passed through the emulsion feeder.
- the emulsified yarn is subjected to a feed roller maintained at 90 ° C. at a speed of 598 m / min, and then drawn at a speed of 190 ° C. and 2,840 m / min in a drawing roller.
- the yarn passed through the stretching roller passes through the texturing nozzle and is crimped.
- the hot air temperature is 200 °C
- the pressure is 7kg / cm2
- the back pressure is 5kg / cm2.
- 20 times / m of entanglement is applied at a pressure of 4.0 kg / m2 in the post-concentrator cooled by cooling water. It passes through the relaxation roller at 2250m / min and is relaxed by 21% and then wound up on a winding machine. Denier, strength and crimp values of polyethylene terephthalate BCF yarns prepared in this process were measured and shown in Table 1 below.
- a polymer, a yarn and a carpet were prepared in the same manner as in Example 1 except that the intrinsic viscosity and the fineness of the yarn of the polyethylene terephthalate polymer were changed as shown in Table 1 below.
- a polymer, a yarn, and a carpet were prepared in the same manner as in Example 1 except for a solid phase polymerization process of increasing the viscosity of a liquid polymer by utilizing a solid phase polymerization in preparing a polyethylene terephthalate polymer.
- a polymer, a yarn, and a carpet were prepared in the same manner as in Comparative Example 1, except that the intrinsic viscosity and the fineness of the yarn of the polyethylene terephthalate polymer were changed as shown in Table 1 below.
- Example 1 Example 2 Example 3
- Example 4 Example 5
- Example 6 Comparative Example 1 Comparative Example 2 Comparative Example 3
- Polymer Intrinsic Viscosity 1.25 0.80 0.93 1.05 1.05 1.08 0.55 0.60 0.65
- Denier 851 917 954 978 1291 964 1299 1299 1304
- Wear-resistant (carmat) 900 500 600 750 700 850 200 250 300
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Artificial Filaments (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The present invention relates to a method for manufacturing a polyester terephthalate yarn with improved abrasion resistance by melting, spinning, stretching, and then winding a polyethylene terephthalate chip with improved viscosity through liquid-phase polymerization or solid-phase polymerization. In addition, a car mat with improved abrasion resistance comprising a polyethylene terephthalate yarn manufactured by the manufacturing method can be provided.
Description
본 발명은 액상중합 또는 고상중합을 통해 점도가 향상된 폴리에틸렌테레프탈레이트 칩을 이용하여 내마모성이 향상된 폴리에틸렌테레프탈레이트 원사를 제조하는 방법과 상기 제조방법으로 제조된 폴리에틸렌테레프탈레이트 원사를 포함하는 카매트에 관한 것이다.The present invention relates to a method for producing a polyethylene terephthalate yarn having improved abrasion resistance by using a polyethylene terephthalate chip having improved viscosity through liquid phase polymerization or solid phase polymerization, and a carpet comprising a polyethylene terephthalate yarn prepared by the above method. .
일반적으로, 폴리에스테르 수지, 특히 폴리에틸렌테레프탈레이트 수지는 디카르복실산 또는 이의 에스테르 형성성 유도체 및 디올 또는 이의 에스테르 형성성 유도체로부터 합성되는 선상 고분자로, 가격이 저렴하면서도, 기계적 특성과 화학적 물성이 우수할 뿐만 아니라 가스 차단성 또한 우수하여 각종 용기, 필름, 섬유 등의 제조에 폭 넓게 사용되고 있다. 한편, 폴리에스테르는 축합 중합법으로 제조되는데, 외부 조건에 따른 평형반응으로 고온, 고진공의 조건을 통해 상업적으로 사용 가능한 점도를 얻게 되며, 이때 최종 중합물 내에 일정량의 올리고머가 잔류하게 된다.Generally, polyester resins, especially polyethylene terephthalate resins, are linear polymers synthesized from dicarboxylic acids or their ester-forming derivatives and diols or their ester-forming derivatives, and are inexpensive, yet have excellent mechanical and chemical properties. In addition to excellent gas barrier properties, it is widely used in the manufacture of various containers, films, fibers and the like. On the other hand, polyester is produced by the condensation polymerization method, the equilibrium reaction according to external conditions to obtain a commercially available viscosity through the conditions of high temperature, high vacuum, wherein a certain amount of oligomers remain in the final polymer.
한편, 카매트 시장은 현재까지 크게 PET Needle Punch와 Nylon BCF로 이루어진 시장으로 구성되어 있다. 기존 PET 카매트의 경우, Nylon 카매트 대비 가격은 저렴하나 자동차 카매트에서 요구되는 내마모성이 떨어지는 문제(300회 수준)로 소형 자동차에 한정되어 사용되어 왔다.Meanwhile, the carpet mat market is composed of PET Needle Punch and Nylon BCF. In the case of existing PET carpet mats, the price is cheaper than nylon carpet mats, but it has been limited to small cars due to the problem of abrasion resistance (300 times) required for automobile mats.
본 출원인은 PET 카매트의 시장 확대를 위하여 기존의 PET Needle Punch 보다 내마모성이 개선된 PET BCF의 발현하고자 상기 발명을 진행하여, Nylon 수준의 내마모성인 800회 이상을 달성하여 제품화에 성공하였고 현재 시장을 확대 중이다.Applicant proceeded to the above invention to express PET BCF with improved wear resistance than the existing PET Needle Punch to expand the market of PET carpet, succeeded in the commercialization by achieving more than 800 times of nylon wear resistance and the current market It is expanding.
본 발명의 목적은 폴리에틸렌테레프탈레이트 액상 및 고상 중합체를 이용하여 내마모성이 개선된 폴리에틸렌테레프탈레이트 원사 및 이를 포함하는 카매트를 제조하는 방법을 제공하는 것이다.It is an object of the present invention to provide a polyethylene terephthalate yarn having improved abrasion resistance using a polyethylene terephthalate liquid and solid polymer and a method for producing a carpet comprising the same.
상술한 목적을 달성하기 위한 본 발명의 하나의 양상은, 폴리에틸렌테레프탈레이트 칩을 용융하여 폴리머를 제조하는 단계; 및 상기 폴리머를 방사노즐에 의해 방사하고, 다단 연신한 후, 권취하여 폴리에틸렌테레프탈레이트 원사를 제조하는 단계;를 포함하고, 상기 폴리에틸렌테레프탈레이트 칩은 액상중합 또는 고상중합을 통해 점도가 0.8 내지 1.5 dl/g 인 것을 특징으로 하며 바람직하게는 0.85내지 1.30 dl/g 범위의 액상중합 또는 고상중합을 통한 고강도 폴리에틸렌테레프탈레이트 원사의 제조방법을 제공한다.One aspect of the present invention for achieving the above object comprises the steps of melting a polyethylene terephthalate chip to prepare a polymer; And spinning the polymer with a spinning nozzle, stretching in multiple stages, and then winding the polymer to prepare a polyethylene terephthalate yarn, wherein the polyethylene terephthalate chip has a viscosity of 0.8 to 1.5 dl through liquid phase polymerization or solid phase polymerization. It is characterized in that / g and preferably provides a method for producing a high strength polyethylene terephthalate yarn through liquid phase polymerization or solid phase polymerization in the range of 0.85 to 1.30 dl / g.
상기 고상중합을 통해 에스테르화 반응물을 고상중합하는 단계는 배치(batch) 또는 연속중합의 방법을 이용하여, 진공조건하에서 110 내지 170℃에서 4 내지 6시간 수분 제거를 위한 건조를 진행하고 235 내지 255℃까지 4 내지 6 시간에 걸쳐 승온을 실시하여 235 내지 255℃ 범위에서 고상중합을 실시하는 것으로 고상중합시간을 20 내지 30시간으로 하는 것이 바람직하다.Solid phase polymerization of the esterification reaction through the solid phase polymerization is carried out by drying (batch) or continuous polymerization, drying for 4 to 6 hours water removal at 110 to 170 ℃ under vacuum conditions and 235 to 255 It is preferable to make solid-phase polymerization time into 20 to 30 hours by heating up over 4 to 6 hours and performing solid-phase polymerization in 235-255 degreeC range.
건조 시 온도가 110℃ 미만인 경우 건조 속도가 급격히 저하되며, 170℃ 이상인 경우 물성이 떨어지게 된다.The drying rate is drastically lowered when the temperature is lower than 110 ° C. during drying, and when the temperature is 170 ° C. or higher, physical properties fall.
고상중합온도가 235℃미만이거나 상기 고상중합시간이 20시간 미만인 경우 반응이 충분히 일어나지 않으며, 고상온도가 255℃를 초과하거나 상기 고상중합시간이 30시간을 초과하는 경우 내마모성이 떨어지게 된다.If the solid phase polymerization temperature is less than 235 ℃ or the solid phase polymerization time is less than 20 hours, the reaction does not occur sufficiently, the wear resistance is inferior when the solid phase temperature exceeds 255 ℃ or the solid phase polymerization time exceeds 30 hours.
본 발명은 섬도가 800 내지 1500 denier인 것, 바람직하게는 850 내지 1350denier인 것을 특징으로 하는 폴리에틸렌테레프탈레이트 원사를 제공한다.The present invention provides a polyethylene terephthalate yarn characterized in that the fineness is 800 to 1500 denier, preferably 850 to 1350 denier.
또한, 상기 폴리에틸렌테레프탈레이트 원사를 포함하는 카매트도 제공한다.In addition, there is also provided a carpet comprising the polyethylene terephthalate yarn.
본 발명에서의 고점도 폴리에틸렌테레프탈레이트 중합체를 이용하여 원사 및 카매트를 제조할 경우, 원사의 강도, Toughness, 밀도가 향상되어 카매트의 내마모성이 향상될 수 있다.When the yarn and the carpet are manufactured using the high viscosity polyethylene terephthalate polymer in the present invention, the strength, toughness, and density of the yarn may be improved, and thus the wear resistance of the mat may be improved.
본 발명에 따른 폴리에틸렌테레프탈레이트 원사의 제조방법은 폴리에틸렌테레프탈레이트 칩을 용융하여 폴리머를 제조하는 단계; 및 상기 폴리머를 방사노즐에 의해 방사하고, 다단 연신한 후, 권취하여 폴리에틸렌테레프탈레이트 원사를 제조하는 단계;를 포함하고, 상기 폴리에틸렌테레프탈레이트 칩은 액상중합 또는 고상중합을 통해 점도를 높이는 것을 특징으로 한다. 전술한 바와 같이 0.8 내지 1.5dl/g 인 것을 특징으로 하는 고강도 폴리에틸렌테레프탈레이트 원사의 제조방법을 제공한다.Method for producing a polyethylene terephthalate yarn according to the present invention comprises the steps of melting a polyethylene terephthalate chip to prepare a polymer; And spinning the polymer by a spinning nozzle, stretching in multiple stages, and then winding the polymer to prepare a polyethylene terephthalate yarn, wherein the polyethylene terephthalate chip increases viscosity through liquid phase polymerization or solid phase polymerization. do. Provided is a method for producing a high strength polyethylene terephthalate yarn, characterized in that 0.8 to 1.5dl / g as described above.
전술한 바와 같이 제조된 폴리에틸렌 테레프탈레이트 칩의 고유점도(I.V.)는 0.8 내지 1.5 이하의 수준이 바람직한데, 고유점도가 0.8 미만인 경우에는 원사의 강력이 낮게 되고 1.5을 초과하게 되면 방사성이 좋지 않다.The intrinsic viscosity (I.V.) of the polyethylene terephthalate chip manufactured as described above is preferably at a level of 0.8 to 1.5 or less. When the intrinsic viscosity is less than 0.8, the strength of the yarn is low, and the radiation is not good when it exceeds 1.5.
이와 같이 제조되는 폴리에틸렌테레프탈레이트 원사의 섬도는 바람하게는800 내지 1500 denier이며, 850 내지 1350 denier인 것이 보다 바람직 하다. 원사의 섬도가 800 denier 미만이면 카매트 성형 시, 원단 파일의 직립도가 낮아져 내마모성, 성형복원력 및 외관이 불량하게 되고, 1500 demier 초과 시에는 카매트 원단의 밀도가 낮아지게 되어 내마모성 및 복원력이 불량하게 된다.The fineness of the polyethylene terephthalate yarn thus produced is preferably from 800 to 1500 denier, more preferably from 850 to 1350 denier. If the fineness of the yarn is less than 800 denier, the uprightness of the fabric pile is lowered during the forming of the mat, resulting in poor abrasion resistance, molding restoring power and appearance, and the density of the mat mat fabric becomes lower when the density exceeds 1500 demier, resulting in poor wear resistance and resilience. Done.
또한, 상기 폴리에틸렌테레프탈레이트 원사를 이용하여 내마모성이 향상된 카매트를 제조할 수 있다.In addition, by using the polyethylene terephthalate yarn can be produced a carpet improved in the wear resistance.
이하, 본 발명에 따른 폴리에틸렌테레프탈레이트 원사를 제조하는 방법에 대해 상세하게 설명한다.Hereinafter, the method for producing the polyethylene terephthalate yarn according to the present invention will be described in detail.
우선 본 발명에 따른 액상중합 또는 고상중합된 폴리에틸렌테레프탈레이트칩을 245∼335℃로 용융방사하여 방사구금을 통과시킨다.First, the liquid polymerized or solid-phase polymerized polyethylene terephthalate chip according to the present invention is melt-spun at 245 to 335 ° C. to pass a spinneret.
본 발명에서 기본이 되는 폴리에틸렌테레프탈레이트 수지는 에틸렌테레프탈레이트의 반복단위를 90몰 % 이상 함유한다.The polyethylene terephthalate resin underlying in the present invention contains 90 mol% or more of repeating units of ethylene terephthalate.
이후 냉각구역에서 속도 0.2∼1.0m/sec의 공기로 냉각시킨다. 이때 냉각온도는 10∼35℃로 조절한다. 이때 냉각 공기의 속도가 0.2m/sec 미만이면 냉각효과가 불충분하며, 1.0m/sec를 초과하면 사의 흔들림이 과도하여 방사 작업성에 문제가 된다. 또한 냉각 온도가 10℃ 미만이면 경제적인 측면에서 불리하고 35℃를 초과하면 냉각 효과가 떨어진다.After cooling in the cooling zone with air at a speed of 0.2 ~ 1.0m / sec. At this time, the cooling temperature is adjusted to 10 ~ 35 ℃. At this time, if the speed of the cooling air is less than 0.2m / sec, the cooling effect is insufficient, if it exceeds 1.0m / sec, the shaking of the yarn is excessive, which is a problem in the spinning workability. In addition, if the cooling temperature is less than 10 ℃ economically disadvantageous, if it exceeds 35 ℃ cooling effect is inferior.
냉각 후 오일링을 하는 스핀 피니쉬(spin finish)단계를 거치는데 피니쉬 어플리케이터에서 1차, 2차 두 단계로 니트(neat)타입 유제 혹은 수용성 유제를 사용하여 오일링함으로써 사의 집속력, 윤활성 및 평활성을 높여준다.After cooling, it goes through a spin finish step of oiling. In the finish applicator, the first and second stages are oiled using neat or water-soluble emulsions to improve the cohesion, lubricity and smoothness of the yarn. Increase it.
이후 공급롤러에서 100∼1,000m/min의 속도로, 바람직하게는 400 내지 800m/min 속도로 필라멘트를 연신롤러에 공급하며, 이때 연신롤러는 100∼230℃의 온도이고 공급롤러 속도의 2.5∼6.0배의 속도로, 바람직하게는 3.5 내지 5.0배로 연신한다. 상기 연신속도가 2.5배보다 작을 경우 충분히 연신되지 못하며 6.0배보다 클 경우 폴리에틸렌테레프탈레이트 소재 특성상 연신을 견디지 못하고 사절된다.Thereafter, the feed roller is supplied to the stretching roller at a speed of 100 to 1,000 m / min, preferably 400 to 800 m / min, wherein the stretching roller is at a temperature of 100 to 230 ° C. and 2.5 to 6.0 of the feed roller speed. At a rate of fold, stretching is preferably from 3.5 to 5.0 fold. When the stretching speed is less than 2.5 times, it is not stretched sufficiently, and when the stretching speed is greater than 6.0 times, the polyethylene terephthalate material is not able to withstand the stretching and is trimmed.
연신롤러를 통과한 필라멘트는 벌키성을 부여하기 위해 텍스처링 노즐이 있는 텍스처링 유니트를 통과하며, 이때 텍스처링 유니트 내부에서 150∼270℃의 가열 유체를 3∼10kg/cm2의 압력으로 분사하여 필라멘트가 불규칙한 3차원으로 권축되게 하며, 이때의 크림프율은 3∼50%가 되도록 한다.The filament passed through the stretching roller passes through a texturing unit with a texturing nozzle to impart bulkiness.In this case, the filament is irregularly formed by spraying a heating fluid of 150 to 270 ° C at a pressure of 3 to 10 kg / cm2 inside the texturing unit. It is crimped to a dimension and the crimp rate at this time is 3 to 50%.
이때 가열 유체의 온도는 150∼270℃가 바람직하며, 이는 150℃ 미만에서는 텍스처링 효과가 떨어지고 270℃를 초과하면 필라멘트에 손상을 초래한다. 또한 가열 유체의 압력은 3∼10kg/cm2가 바람직하며, 이는 3kg/cm2 미만에서는 텍스처링 효과가 떨어지고 10kg/cm2를 초과하면 필라멘트에 손상을 초래한다.At this time, the temperature of the heating fluid is preferably 150 ~ 270 ℃, which is less than 150 ℃ texturing effect and exceeds 270 ℃ causes damage to the filament. In addition, the pressure of the heating fluid is preferably 3 to 10 kg / cm 2, which is less than the texture effect of less than 3 kg / cm 2 and causes damage to the filament exceeds 10 kg / cm 2.
텍스처링 유니트를 통과한 필라멘트는 냉각구간을 거치면서 냉각되어 교락기를 통과한다. 이 부분에서는 사의 집속력을 좋게 하기 위해 2.0∼8.0kg/m2의 압력으로 약간의 꼬임과 매듭을 주게 되는데 0∼40회/m의 범위로, 바람직하게는 10 내지 25회로 부여한다. 40회를 초과하여 교락을 줄 때는 염색, 후가공을 거쳐도 교락이 풀리지 않은 상태가 그대로 유지되어 카펫의 외관을 손상시킨다.After passing through the texturing unit, the filament is cooled while passing through the cooling section. In this part, in order to improve the focusing force of the yarn, a slight twist and a knot are applied at a pressure of 2.0 to 8.0 kg / m 2. The range is 0 to 40 times / m, preferably 10 to 25 times. When the entanglement is given more than 40 times, the entanglement of the entanglement remains unchanged even after dyeing and post-processing.
이후 릴렉스 롤러에서 연신롤러 속도의 0.65∼0.95배의 속도로 통과시켜 릴렉스율을 5∼35%로 준 후, 최종 권취기에서 권취한다. 권취기의 속도는 보통 실의 장력이 50∼350g범위가 되도록 속도를 조절한다. 이때 권취기에서 장력이 50g 미만이면 권취가 불가능하고, 350g을 초과하면 벌키성이 감소되며 원사의 수축이 크게 일어나고 높은 장력을 유발하여 작업에도 지장을 초래한다. 또한, 릴렉스 롤러의 속도가 연신롤러 속도의 0.65배 미만으로 하면 권취가 되지 않고, 0.95배를 초과하면 벌키성이 감소되며 원사의 수축이 크게 일어나고 높은 장력을 유발하여 작업에도 지장을 초래한다.Thereafter, the rollers are passed through at a speed of 0.65 to 0.95 times the speed of the stretching roller to give a relaxation rate of 5 to 35%, and then wound up at the final winding machine. The speed of the winder is usually adjusted so that the tension of the thread is in the range of 50 to 350 g. At this time, if the tension in the winding machine is less than 50g, the winding is impossible, and if it exceeds 350g, the bulkiness is reduced, the yarn shrinks greatly and causes high tension, which causes trouble in the work. In addition, if the speed of the relaxation roller is less than 0.65 times of the stretching roller speed, it is not wound, and if it exceeds 0.95 times, the bulkiness is decreased, the yarn shrinks greatly, and high tension causes the work.
상기 방법은 폴리에틸렌테레프탈레이트 수지만으로 제조한 BCF에 관한 것이며, 카펫 용도에 따라 원착사 제조 시에는 단계별 공정은 상기와 동일하다. 다만 원료 공급에 있어 베이스 칩 투입량에 일정량의 착색제를 투입하여 방사함으로써 원착사를 제조하는 것도 가능하다.The method relates to a BCF made of polyethylene terephthalate resin only, the step-by-step process is the same as above when producing the primary yarn according to the carpet application. However, in the raw material supply, it is also possible to prepare the yarn by adding a predetermined amount of colorant to the base chip input amount.
상기와 같이 본 발명에 따라 제조된 폴리에틸렌테레프탈레이트 멀티필라멘트는 후공정을 거쳐 카펫으로 제조된다. 본 발명의 BCF사로 제조된 카펫은 당업자에게 공지된 임의의 방식으로 제조할 수 있다. 바람직하게는 다수의 BCF사를 함께 케이블 가연 및 열고정시킨 다음, 이어서 1차 배면으로 직조한다. 이어서 라텍스 접착제 및 2차 배면을 도포한다. 대략 2 내지 20mm의 파일 높이를 갖는 컷 파일 스타일 카펫 또는 루프 파일 스타일의 카펫을 제조할 수 있다.The polyethylene terephthalate multifilament prepared according to the present invention as described above is produced into a carpet through a post-process. Carpets made with the BCF company of the present invention can be produced in any manner known to those skilled in the art. Preferably a plurality of BCF yarns are cable twisted and heat set together and then weave to the primary back side. The latex adhesive and the secondary backside are then applied. Cut pile style carpets or loop pile style carpets with pile heights of approximately 2-20 mm can be made.
이하, 본 발명을 하기 실시예에 의거하여 좀더 상세하게 설명한다. 단, 하기 실시예는 본 발명을 예시하기 위한 것일 뿐 한정하지는 않으며, 본 발명의 실시예 및 비교예에서 제조된 사의 물성 평가는 다음과 같은 방법으로 실시하였다.Hereinafter, the present invention will be described in more detail based on the following examples. However, the following examples are not intended to limit the present invention, but are not limited thereto. The physical properties of the yarns manufactured in Examples and Comparative Examples of the present invention were evaluated by the following method.
1. 원사의 강신도 측정방법1. How to measure the elongation of yarn
원사를 표준상태인 조건, 즉 25℃ 온도와 상대습도 65%RH인 상태인 항온 항습실에서 24시간 방치한 후 ASTM 2256 방법으로 시료를 인장 시험기를 통해 측정한다.The yarn is left for 24 hours in a constant temperature and humidity room under standard conditions, that is, 25 ° C. and 65% RH relative humidity, and the sample is measured by a tensile tester using the ASTM 2256 method.
2. 크림프율 및 표준편차2. Crimp rate and standard deviation
TYT-EW(Textured Yarn Tester) 측정기기에 의해 측정, 측정 길이는 20m, 2m간격으로 5회 측정하며 가열 구역(Heating zone)의 온도는 130℃, 측정 속도는 20m/min이다.Measured by TYT-EW (Textured Yarn Tester) measuring device, measuring length is measured 5 times at 20m and 2m intervals. Temperature of heating zone is 130 ℃ and measuring speed is 20m / min.
3. 카매트의 내마모 평가방법3. How to evaluate the wear resistance of the mat
카매트의 내마모성은 하기와 같은 조건으로 측정하였으며, 카매트의 내마모횟수는 한계 내마모수로 외관 평가 2.5급에 해당되는 수준에서 카매트 바닥면이 노출되는 시점의 최종 마모수를 기준으로 평가하였다.The wear resistance of the mat was measured under the following conditions, and the wear resistance of the mat was evaluated based on the final wear at the time when the mat floor was exposed at the level equivalent to the grade 2.5 of the external appearance. It was.
관련 시험방법규격 : ASTM D3884Related Test Method Standard: ASTM D3884
시험방법 : 현대자동차 MS300-35Test method: Hyundai Motor MS300-35
시험장비 : Taber 내마모 시험기Test equipment: Taber wear tester
시료크기 : 지름 130mm 원형 시료Sample size: 130mm diameter round sample
시험조건Exam conditions
1) 마모륜 : H-181) Abrasion Wheel: H-18
2) 회전속도 : 70회/분2) Speed: 70 times / min
3) 하중 : 1000g3) Load: 1000g
4) 평가방법 : 외관평가 1~5급 (현대자동차 MS343-15 규격 3급 이상(3,4,5급) 합격4) Evaluation Method: Appearance Evaluation Level 1 ~ 5 (Hyundai Motors MS343-15 Standard Level 3 or higher (3, 4, 5) passed
5) 평가기준 : 5급 마모가 전혀 보이지 않음5) Evaluation criteria: No grade 5 wear
4급 마모가 약간 보이거나 거의 눈에 띄지 않는 것 Slight or almost inconspicuous class 4 wear
3급 마모가 약간 있으나 보이는 것 Some grade 3 wear but visible
2급 마모가 약간 심한 것 Slightly severe class 2 wear
1급 상당히 심한 것 Class 1 quite severe
실시예 1Example 1
테레프탈산 100 중량부에 대하여 에틸렌 글리콜 50 중량부를 혼합하여 제조한 슬러리를 에스테르화 반응기에 투입하고, 250℃에서 4시간동안 0.5torr의 압력으로 가압하여 물을 반응기 밖으로 유출시키면서 에스테르화 반응을 진행시켜 비스(2-하이드록시에틸) 테레프탈레이트[bis(2-hydroxyethyl) terephthalate]를 제조하였다. 이때, 인계 내열안정제를 에스테르화 반응 말기에 300ppm 투입하였다. 또한, 에스테르화 반응 후, 중합 촉매로서 안티몬 촉매를 중축합반응 초기에 300ppm을 투입하고, 250℃에서 285℃까지 60℃/hr로 승온함과 동시에, 압력을 0.5torr까지 감압하여 중축합 반응을 진행하였다. 상기 중합물을 고상중합을 실시하여 액상중합물의 점도를 올린다. 일반적인 고상중합의 과정 중, Batch 고상중합기를 이용하여 진공조건하에서 140도에서 4시간 수분 제거를 위한 건조를 진행하고 235도까지 4시간에서 6시간에 걸쳐 승온을 실시하며 235도~245도의 온도 범위에서 최종 목표 점도까지 고상중합을 실시한다.Slurry prepared by mixing 50 parts by weight of ethylene glycol with respect to 100 parts by weight of terephthalic acid was added to an esterification reactor, pressurized at a pressure of 0.5torr for 4 hours at 250 ° C, and water was passed out of the reactor to proceed with the esterification reaction. (2-hydroxyethyl) terephthalate [bis (2-hydroxyethyl) terephthalate] was prepared. At this time, 300 ppm of the phosphorus heat stabilizer was added at the end of the esterification reaction. After the esterification reaction, 300 ppm of the antimony catalyst was initially added to the antimony catalyst as a polymerization catalyst, the temperature was raised from 250 ° C to 285 ° C at 60 ° C / hr, and the pressure was reduced to 0.5torr to carry out the polycondensation reaction. Proceeded. Solid polymerization of the polymer is carried out to increase the viscosity of the liquid polymer. During the general solid state polymerization process, Batch solid state polymerizer is used to perform drying for 4 hours of water removal at 140 ° C under vacuum condition, and the temperature is increased from 4 hours to 6 hours up to 235 ° C. The solid phase polymerization is carried out from to the final target viscosity.
128홀(Hole)이며 Y형 단면을 갖는 방사구금을 통하여 제조된 폴리에틸렌테레프탈레이트 중합체를 290℃로 용융방사한다. 방사구금을 빠져나온 폴리머는 노즐 하부에서 0.5m/s, 20℃의 냉각 공기에 의해 냉각된 후 유제 공급 장치를 통과한다. 유제를 부여받은 원사는 90℃ 온도로 유지되는 공급롤러를 598m/min의 속도로 거친 후 연신롤러에서 190℃, 2,840m/min의 속도로 연신된다. 연신롤러를 통과한 원사는 텍스처링 노즐을 통과하며 크림프를 부여받는다. 이때 Hot air 온도는 200℃, 압력은 7kg/cm2이며 배압은 5kg/cm2이다. 이 후 냉각수에 의해 냉각된 후집속장치에서 4.0kg/m2의 압력으로 교락을 20회/m부여한다. 릴렉스 롤러를 2250m/min으로 통과하며 21%정도 릴렉스된 후 와인딩 머신(Winding Machine)에서 권취된다. 이러한 공정으로 제조된 폴리에틸렌테레프탈레이트 BCF 원사의 데니어, 강도 및 크림프 값을 측정하여 하기 표 1에 나타내었다.The polyethylene terephthalate polymer produced through spinneret having 128 holes and having a Y-shaped cross section is melt-spun at 290 ° C. The polymer exiting the spinneret is cooled by 0.5 m / s at 20 ° C. cooling air at the bottom of the nozzle and then passed through the emulsion feeder. The emulsified yarn is subjected to a feed roller maintained at 90 ° C. at a speed of 598 m / min, and then drawn at a speed of 190 ° C. and 2,840 m / min in a drawing roller. The yarn passed through the stretching roller passes through the texturing nozzle and is crimped. At this time, the hot air temperature is 200 ℃, the pressure is 7kg / cm2 and the back pressure is 5kg / cm2. Afterwards, 20 times / m of entanglement is applied at a pressure of 4.0 kg / m2 in the post-concentrator cooled by cooling water. It passes through the relaxation roller at 2250m / min and is relaxed by 21% and then wound up on a winding machine. Denier, strength and crimp values of polyethylene terephthalate BCF yarns prepared in this process were measured and shown in Table 1 below.
제조된 폴리에틸렌테레프탈레이트 BCF 원사를 이용하여 카매트를 제조하여 내마모성을 측정하였으며, 그 결과를 하기 표 1에 나타내었다.Carpets were prepared using the prepared polyethylene terephthalate BCF yarn to measure wear resistance, and the results are shown in Table 1 below.
실시예 2 내지 6Examples 2-6
폴리에틸렌테레프탈레이트 중합체의 고유점도와 원사의 섬도를 하기 표 1에 기재한 바와 같이 변경한 것을 제외하고는, 실시예 1과 동일한 방법으로 중합체, 원사 및 카매트를 제조하였다.A polymer, a yarn and a carpet were prepared in the same manner as in Example 1 except that the intrinsic viscosity and the fineness of the yarn of the polyethylene terephthalate polymer were changed as shown in Table 1 below.
비교예 1Comparative Example 1
폴리에틸렌테레프탈레이트 중합체 제조 시 고상 중합을 활용하여 액상의 중합체의 점도를 높이는 고상 중합 공정을 제외하고는, 실시예 1과 동일한 방법으로 중합체, 원사 및 카매트를 제조하였다.A polymer, a yarn, and a carpet were prepared in the same manner as in Example 1 except for a solid phase polymerization process of increasing the viscosity of a liquid polymer by utilizing a solid phase polymerization in preparing a polyethylene terephthalate polymer.
비교예 2 내지 3Comparative Examples 2 to 3
폴리에틸렌테레프탈레이트 중합체의 고유점도와 원사의 섬도를 하기 표 1에 기재한 바와 같이 변경한 것을 제외하고는, 비교예 1과 동일한 방법으로 중합체, 원사 및 카매트를 제조하였다.A polymer, a yarn, and a carpet were prepared in the same manner as in Comparative Example 1, except that the intrinsic viscosity and the fineness of the yarn of the polyethylene terephthalate polymer were changed as shown in Table 1 below.
| 실시예1Example 1 | 실시예2Example 2 | 실시예3Example 3 | 실시예4Example 4 | 실시예5Example 5 | 실시예6Example 6 | 비교예1Comparative Example 1 | 비교예2Comparative Example 2 | 비교예3Comparative Example 3 | |
| 중합체 고유점도Polymer Intrinsic Viscosity | 1.251.25 | 0.800.80 | 0.930.93 | 1.051.05 | 1.051.05 | 1.081.08 | 0.550.55 | 0.600.60 | 0.650.65 |
| DenierDenier | 851851 | 917917 | 954954 | 978978 | 12911291 | 964964 | 12991299 | 12991299 | 13041304 |
| 내마모 (카매트)Wear-resistant (carmat) | 900900 | 500500 | 600600 | 750750 | 700700 | 850850 | 200200 | 250250 | 300300 |
표 1에서 나타난 바와 같이, 중합체의 고유점도가 0.8 이상이며, 원사의 섬도가 850~1,350denier인 경우, 제조한 카매트(실시예 1 내지 6)의 내마모성이 향상된 것을 알 수 있었다.As shown in Table 1, when the intrinsic viscosity of the polymer is 0.8 or more, and the fineness of the yarn is 850 to 1,350 denier, it was found that the wear resistance of the manufactured mats (Examples 1 to 6) was improved.
반면, 점도가 낮은 일발 PET 액상 중합체를 사용한 경우(비교예 1 내지 3), 제조한 카매트의 내마모성이 저하된 것을 알 수 있었다.On the other hand, when a low viscosity primary PET liquid polymer was used (Comparative Examples 1 to 3), it was found that the abrasion resistance of the manufactured mat was decreased.
이상에서 본 발명의 바람직한 실시예에 대하여 상세하게 설명하였으나, 본 발명은 상술한 실시예에 국한되는 것은 아니고, 본 발명의 취지 또는 범위를 벗어나지 않고 본 발명을 다양하게 변경하고 변형할 수 있다는 사실은 당업자에게 자명할 것이다. 따라서, 본 발명의 보호범위는 첨부한 특허청구범위 및 그와 균등한 범위로 정해져야 할 것이다.Although the preferred embodiments of the present invention have been described in detail above, the present invention is not limited to the above-described embodiments, and the fact that the present invention can be variously changed and modified without departing from the spirit or scope of the present invention. It will be apparent to those skilled in the art. Therefore, the protection scope of the present invention should be defined in the appended claims and equivalents thereof.
Claims (4)
- 폴리에틸렌테레프탈레이트 칩을 용융하여 폴리머를 제조하는 단계; 및Melting a polyethylene terephthalate chip to produce a polymer; And상기 폴리머를 방사노즐에 의해 방사하고, 다단 연신한 후, 권취하여 폴리에틸렌테레프탈레이트 원사를 제조하는 단계;를 포함하고And spinning the polymer by a spinning nozzle, multistage stretching, and winding the polymer to prepare a polyethylene terephthalate yarn.상기 폴리에틸렌테레프탈레이트 칩은 액상중합 또는 고상중합을 통해 점도가 0.8 내지 1.5 dl/g 인 것을 특징으로 하는 고강도 폴리에틸렌테레프탈레이트 원사의 제조방법.The polyethylene terephthalate chip is a method of producing a high strength polyethylene terephthalate yarn, characterized in that the viscosity is 0.8 to 1.5 dl / g through liquid phase polymerization or solid phase polymerization.
- 제1항에 있어서,The method of claim 1,상기 고상중합은 배치(batch) 또는 연속중합의 방법을 이용하여, 진공조건하에서 110 내지 170℃에서 4 내지 6시간 수분 제거를 위한 건조를 진행하고 235 내지 255℃까지 4 내지 6 시간에 걸쳐 승온을 실시하여 235 내지 255℃ 범위에서 고상중합을 실시하는 것으로 고상중합시간을 20 내지 30시간인 것을 특징으로 하는 폴리에틸렌테레프탈레이트 원사의 제조방법.The solid phase polymerization is carried out using a batch or a continuous polymerization method, drying for 4 to 6 hours water removal at 110 to 170 ℃ under vacuum conditions and the temperature is raised to 235 to 255 ℃ over 4 to 6 hours Method for producing a polyethylene terephthalate yarn, characterized in that the solid phase polymerization time is 20 to 30 hours by performing a solid phase polymerization in the range of 235 to 255 ℃.
- 제1항에 있어서,The method of claim 1,원사의 섬도가 800 내지 1500 denier인 것을 특징으로 하는 폴리에틸렌테레프탈레이트 원사의 제조방법.The fineness of the yarn is 800 to 1500 denier, characterized in that the polyethylene terephthalate yarn production method.
- 제1항에 기재된 폴리에틸렌테레프탈레이트 원사를 포함하는 카매트.A carpet comprising the polyethylene terephthalate yarn according to claim 1.
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| EP3620557A1 (en) * | 2018-09-05 | 2020-03-11 | Hyosung Advanced Materials Corporation | Polyethyleneterephthalate bulked continuous filament and tufted carpet including the same |
| WO2020050450A1 (en) | 2018-09-04 | 2020-03-12 | 효성첨단소재 주식회사 | Tufted carpet, for vehicles, comprising polyethylene terephthalate bulked continuous filaments |
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| CN109563646A (en) * | 2018-09-04 | 2019-04-02 | 晓星高新材料株式会社 | Tufted carpet comprising polyethylene terephthalate bulked continuous filament |
| WO2020050450A1 (en) | 2018-09-04 | 2020-03-12 | 효성첨단소재 주식회사 | Tufted carpet, for vehicles, comprising polyethylene terephthalate bulked continuous filaments |
| EP3848493A4 (en) * | 2018-09-04 | 2021-11-03 | Hyosung Advanced Materials Corporation | TILED CARPET FOR VEHICLES WITH POLYETHYLENE TEREPHTHALATE CONTINUOUS YARN |
| EP3620557A1 (en) * | 2018-09-05 | 2020-03-11 | Hyosung Advanced Materials Corporation | Polyethyleneterephthalate bulked continuous filament and tufted carpet including the same |
| CN110878432A (en) * | 2018-09-05 | 2020-03-13 | 晓星高新材料株式会社 | Tufted carpet comprising bulked continuous polyethylene terephthalate filaments |
| US11634536B2 (en) | 2018-09-05 | 2023-04-25 | Hyosung Advanced Materials Corporation | Tufted carpet including polyethyleneterephthalate bulked continuous filament |
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