US20050147784A1 - Process for preparing poly(trimethylene terephthalate) fiber - Google Patents
Process for preparing poly(trimethylene terephthalate) fiber Download PDFInfo
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- US20050147784A1 US20050147784A1 US10/752,399 US75239904A US2005147784A1 US 20050147784 A1 US20050147784 A1 US 20050147784A1 US 75239904 A US75239904 A US 75239904A US 2005147784 A1 US2005147784 A1 US 2005147784A1
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- -1 poly(trimethylene terephthalate) Polymers 0.000 title claims abstract description 60
- 229920002215 polytrimethylene terephthalate Polymers 0.000 title claims abstract description 28
- 239000000835 fiber Substances 0.000 title description 16
- 238000004519 manufacturing process Methods 0.000 title description 4
- 238000000034 method Methods 0.000 claims abstract description 66
- 230000008569 process Effects 0.000 claims abstract description 52
- 239000000155 melt Substances 0.000 claims abstract description 19
- 238000009987 spinning Methods 0.000 claims abstract description 11
- 229920000642 polymer Polymers 0.000 claims description 34
- 238000001816 cooling Methods 0.000 claims description 20
- 239000012530 fluid Substances 0.000 claims description 8
- 230000009477 glass transition Effects 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000009998 heat setting Methods 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 20
- 238000012360 testing method Methods 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 238000012546 transfer Methods 0.000 description 8
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 241000446313 Lamella Species 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 238000004804 winding Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 229920000728 polyester Polymers 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000002093 peripheral effect Effects 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 238000001542 size-exclusion chromatography Methods 0.000 description 3
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 2
- 229920001283 Polyalkylene terephthalate Polymers 0.000 description 2
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 2
- 238000000149 argon plasma sintering Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000013529 heat transfer fluid Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229920001707 polybutylene terephthalate Polymers 0.000 description 2
- 238000012667 polymer degradation Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- BYEAHWXPCBROCE-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropan-2-ol Chemical compound FC(F)(F)C(O)C(F)(F)F BYEAHWXPCBROCE-UHFFFAOYSA-N 0.000 description 1
- CHRJZRDFSQHIFI-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;styrene Chemical compound C=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C CHRJZRDFSQHIFI-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
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- 238000012937 correction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
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- 230000007717 exclusion Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000013374 right angle light scattering Methods 0.000 description 1
- UYCAUPASBSROMS-AWQJXPNKSA-M sodium;2,2,2-trifluoroacetate Chemical compound [Na+].[O-][13C](=O)[13C](F)(F)F UYCAUPASBSROMS-AWQJXPNKSA-M 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
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- 239000006200 vaporizer Substances 0.000 description 1
Images
Classifications
-
- 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
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
- D02G1/02—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
- D02G1/20—Combinations of two or more of the above-mentioned operations or devices; After-treatments for fixing crimp or curl
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/08—Interlacing constituent filaments without breakage thereof, e.g. by use of turbulent air streams
-
- 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
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
-
- 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
- D10B2503/00—Domestic or personal
- D10B2503/04—Floor or wall coverings; Carpets
Definitions
- the present invention relates to a polyester yarn and its manufacture. More particularly, the invention relates to a process for producing poly(trimethylene terephthalate) fibers having good physical properties.
- Polyethylene terephthalate (“2GT”) and polybutylene terephthalate (“4GT”), generally referred to as “polyalkylene terephthalates”, are common commercial polyesters.
- Polyalkylene terephthalates have excellent physical and chemical properties, in particular, chemical, heat and light stability, high melting points and high strength. As a result they have been widely used for resins, films and fibers.
- Polyesters prepared by condensation polymerization of the reaction product of a diol with a dicarboxylic acid can be spun into yarn.
- U.S. Pat. No. 3,998,042 describes a process for preparing poly(ethylene terephthalate) yarn in which the extruded fiber is drawn at high temperature (160° C.) with a steam jet assist, or at a lower temperature (95° C.) with a hot water assist.
- Poly(ethylene terephthalate) can be spun into bulk continuous filament (BCF) yarn in a two-stage drawing process in which the first stage draw is at a significantly higher draw ratio than the second stage draw.
- BCF bulk continuous filament
- 4,877,572 describes a process for preparing poly(butylene terephthalate) BCF yarn in which the extruded fiber is drawn in one stage, the feed roller being heated to a temperature 30° C. above or below the Tg of the polymer and the draw roller being at least 100° C. higher than the feed roller.
- U.S. Pat. No. 6,254,961 relates to spinning poly(trimethylene terephthalate) into yarn suitable for carpets. According to this patent, drawing speeds of greater than 1000 m/min. are possible with the inventive process, with drawing speeds greater than 1800 m/min. desirable because of the high tenacity of the resulting yarn.
- U.S. Pat. No. 6,284,370 relates to a poly(trimethylene terephthalate) fiber which has a suitable thermal stress and a suitable boil-off shrinkage and which gives a fabric, when woven or knitted, showing less stiffness caused by excessive shrinkage, and manifesting softness and the excellent color developing property expected from the low elastic modulus characteristic of the fiber.
- the intrinsic viscosity of a polymer used in the invention is preferably from 0.4 to 1.5, more preferably from 0.7 to 1.2.
- the polyester fiber of the invention preferably is in the form of multifilament yarn when used for clothing applications. Although the total size of the yarn is not restricted, it is usually from 5 to 200 d (denier), preferably from 20 to 150 d.
- the single filament size is not restricted, it is from 0.1 to 10 d, preferably from 0.5 to 5 d, more preferably from 1 to 3 d. Also according to this patent, it is important that the peripheral speed of a first roll used to produce the fiber be from 300 to 3,500 m/min. The peripheral speed is preferably from 800 to 3,000 m/min, more preferably from 1,200 to 2,500 m/min. Although the peripheral speed of a second roll is determined by the draw ratio, it is usually from 600 to 6,000 m/min.
- U.S. patent Pub. No. 2003/0127766 relates, in general, to a poly(trimethylene terephthalate) BCF carpet modified cross-section yarn and a method for preparing the same and in particular, to a poly(trimethylene terephthalate) BCF carpet modified cross-section yarn and a method for preparing the same.
- poly(trimethylene terephthalate) with an intrinsic viscosity of 0.8 to 1.2 and a moisture content of 50 ppm or less is used as raw materials, and preferably melt-spun at a spinning rate of 1500 to 4000 m/min. Spun filaments are drawn at a rate of 1500 to 4000 m/min. and crimped.
- U.S. patent Pub. No. 2003/0045611 relates to a process for preparation of pigmented shaped articles (e.g., fibers).
- poly(trimethylene terephthalate) preferably has an intrinsic viscosity that is about 0.6 dl/g or higher, and typically is about 1.5 dl/g or less.
- Preferred viscosities for many end uses, and, particularly for fibers and films, are 0.8 dl/g or higher, more preferably 0.9 dl/g or higher.
- the viscosity of poly(trimethylene terephthalate) fibers and films is 1.4 dl/g or less, 1.2 dl/g or less, or 1.1 dl/g or less.
- the spinning speed is preferably at least about 1,000 meters/minute, and may be up to about 5,000 meters/minute or more, using roll 40 as reference speed.
- a process comprises:
- the filaments are drawn at a draw ratio of about 1.1 to about 4.0.
- the poly(trimethylene terephthalate) has an intrinsic viscosity of about 0.95 to about 1.10.
- the drawn filaments can be bulked and/or entangled. They can be bulked to form 3-dimensional curvilinear crimp therein.
- the bulking comprises blowing and deforming the filaments in a hot-fluid jet bulking unit.
- a process comprises:
- the bulked continuous filaments are entangled before the cooling.
- the filaments can be ply-twisted and heat set into a yarn.
- the ply-twisted, heat-set yarn can be made into carpet.
- FIG. 1 schematically illustrates a chip dryer and melt extruder system
- FIG. 2 schematically illustrates a spinning configuration useful in this invention.
- a process comprises:
- the filaments can be coated with a spin finish and, optionally, preintermingled.
- the process further comprises bulking the drawn filaments.
- the drawn filaments can be bulked to form 3-dimensional curvilinear crimp therein.
- the bulking comprises blowing and deforming the filaments in a hot-fluid jet bulking unit.
- the process further comprises entangling the filaments.
- a process comprises:
- the bulked continuous filaments can be entangled before the cooling.
- the filaments are ply-twisted and heat set into yarn.
- Carpet can be made from the ply-twisted and heat-set yarn.
- poly(trimethylene terephthalate) chips are loaded into dryer 10 to be dried.
- the intrinsic viscosity of the poly(trimethylene terephthalate) is preferably about 0.95 to about 1.10 dl/g.
- the intrinsic viscosity can be about 0.98 to about 1.04 or about 1.00 to about 1.02.
- the number average molecular weight is at least about 26500, more preferable at least about 27500, most preferably, at least about 29000.
- the number average molecular weight is up to about 50000, more preferably up to about 45000, most preferably up to about 40000.
- the melt viscosity of the polymer is at least about 350, more preferably at least about 400, even more preferably at least about 450 and most preferably at least about 500 Pascals at 250° C. and 48.65 per second shear rate. Also preferably, the melt viscosity is up to about 1000, more preferably up to about 900, even more preferably up to about 800 and most preferably up to about 700 Pascals at 250° C. and 48.65 per second shear rate.
- Drying is preferably carried out at about 80° C. or higher and about 180° C. or lower, most preferably at about 150° C.
- the poly(trimethylene terephthalate) chips are preferably dried until the moisture content is less than 100 ppm, more preferably about 50 ppm or less, and most preferably about 40 ppm or less. Drying time should be as long as required to reach the desired moisture content, preferably about 4 to about 10 hours, more preferably about 6 to about 8 hours.
- the operator should keep the moisture level steady in order to maintain consistent melt viscosity.
- Commercially available dehumidifiers can be used. Dry nitrogen, air or other inert gasses can be used.
- the dried chips are fed to an optional chip metering screw 12 and are metered in to the remelter throat 14 .
- the metering screw is optional since the screw can be used to control the amount of chips used.
- a chip metering screw is normally used with a screw remelter. Any commercially available metering screw can be used.
- remelter throat reference is being made to a pipe connecting the metering screw and the remelter.
- the remelter can be any suitable single or twin screw extruder.
- a nitrogen purge can be used to prevent oxygen from being carried along with the chips into the remelter. This will reduce oxygen-caused polymer degradation.
- Remelting is preferably carried out at about 200° C. or higher, preferably at least about 235° C., more preferably at least about 245° C., and at about 2800 C. or lower, preferably about 270° C. or lower, more preferably about 265° C. or lower. At temperatures above 280° C., the undesirable byproduct acrolein is generated.
- Polymer is fed to optional transfer line pump 20 , which provides sufficient pressure (about 2250-3000 psig) to overcome losses in the transfer line 22 , provide constant feed rate, and provide sufficient pressure to feed the polymer to the spin pack metering pump 24 .
- transfer line pump 20 provides sufficient pressure (about 2250-3000 psig) to overcome losses in the transfer line 22 , provide constant feed rate, and provide sufficient pressure to feed the polymer to the spin pack metering pump 24 . Any suitable pump may be used.
- Transfer line 22 is, preferably, surrounded by an outer pipe (not shown), which provides an outer jacket for the transfer line.
- the outer jacket can contain heat transfer fluid to help maintain the temperature of the polymer within acceptable limits.
- the temperature of the polymer transfer line 22 is preferably kept at least at about 220° C., more preferably at least at about 230° C., most preferably at least about 240° C.
- the temperature can be up to about 265° C., preferably up to about 260° C., most preferably up to about 255° C.
- the heat transfer fluid in the jacket could be paraffin kept, preferably, below 250° C.
- Polymer holdup time in transfer pipe 22 should be kept at a minimum, for example, below 20 minutes, preferably below 10 minutes, most preferably below 2 minutes. This can be accomplished, for example, by reducing the length and/or diameter of the piping and/or increasing throughput by using a booster pump.
- the metering pump 24 meters the polymer composition to the spinneret or die 26 .
- the polymer is extruded through the spinneret or die 26 to form filaments 2 .
- Spun filaments are cooled in cooling zone 3 by a radial flow or cross flow of gas to below the polymer glass transition temperature.
- a spin finish or oil can be applied to the solidified filaments by finish applicator 4 .
- the filaments can be treated with turbulent air in the optional preintermingling device 5 to even out the finish on the filaments.
- the polymer is extruded through the spinneret or die at a temperature of at least about 200° C., preferably at least about 235° C., more preferably at least about 245° C., and up to about 275° C., preferably up to about 270° C., more preferably up to about 265° C.
- the spin pack metering pump and spinneret or die may be heated through conventional means (e.g., Dow fluid or hot oil).
- the throughput is a function of the number of spin positions and typically is anywhere from about 2 pounds/hour (about 0.9 kg/hour) to commercial scales of about 2,000 pounds/hour (about 907 kg/hour) to about 3,000 pounds/hour (about 1,361 kg/hour) per spinning machine (i.e., per one remelter) or higher.
- the cooling zone 3 cools the filaments by a radial flow or cross flow of gas, typically humidified air at a temperature preferably of about 10° C. or above and preferably about 30° C. or below applied at about 0.2 m/sec or more and about 0.8 m/sec or less. As shown, the filaments are converged into yarn at roller 6 .
- gas typically humidified air
- the filaments are then drawn by use of a supplying roller 6 and a set of drawing rollers 7 .
- the filaments are preferably drawn at a draw ratio of about 1.1 to about 4.0.
- the draw ratio can be about 1.2 to about 3.0 or even 1.4 to 2.2.
- the filaments can then be crimped through a bulking unit 8 with a texturing nozzle after the filaments are passed through the drawing rollers 7 .
- the filaments can then be cooled through a cooling drum 9 , and passed through intermingler 11 via roller 17 , where the filaments are entangled. Thereafter, the filaments are wound with the use of a wind-up machine 15 via roller 13 and a yarn guide 16 .
- the filaments are drawn at a speed of greater than 3000 meters per minute (m/min.).
- the draw speed can be greater than 3500 m/min., greater than 4000 m/min., greater than 5000 m/min., at least 5100 m/min. or even at least 5500 m/min.
- the draw ratio of the filaments is controlled by adjusting the speeds of the supply roller 6 and/or draw rolls 7 until the break elongation of the filaments is preferably at least about 10%, more preferably at least 20% and preferably no more than about 90%, more preferably no more than 70%.
- the drawn filament denier is greater than 1, preferably at least 3, more preferably at least 10, most preferably at least about 15 dl/g.
- the yarn denier is preferably greater than 210, more preferably at least about 250, even more preferably at least about 500 and most preferably at least about 1000.
- a jet-bulking unit 8 where the filaments can be blown and deformed in three directions with hot bulking fluid such as air or steam can be used in practicing the invention.
- a suitable unit is described in U.S. Pat. No. 3,525,134, the disclosure of which is hereby incorporated herein by reference.
- the filaments are both bulked and entangled.
- a separate entangling step may be necessary prior to the windup. Any method common in the trade may be used to entangle the yarn.
- the resultant BCF yarn having randomly spaced 3-dimensional curvilinear crimp, is then preferably cooled below the glass transition temperature of the filaments (approximately 45-50° C.) while the yarn is in a state of approximately 0 gpd tension so as not to pull out a significant amount of crimp. Cooling may be accomplished by a variety of commercially available means, preferably by air or water flow, spray or mist.
- the filaments can be ply-twisted and heat set into yarn.
- the yarn can then be made into carpet.
- the yarn of the present invention could also be used in rugs, woven tiles, automotive interiors and fabrics.
- Poly(trimethylene terephthalate) (3GT) resins were dried at 120° C. for 50 hours under vacuum with a heated, dry nitrogen sweep using a VWR Model 1430M vacuum oven.
- the moisture level in the dried resins was measured at 180° C. with 10 minute delay time using a Mitsubishi Moisture Analyzer Model CA100 with a Vaporizer Model VA100.
- the moisture levels in the 3GT Sample 1 and 3GT Sample 2 were 38 and 40 ppm, respectively.
- melt stability and melt viscosity were measured at 250 and 260 ⁇ 0.1° C. using a Dynisco LCR 7002 capillary rheometer with a 1 mm diameter, 30:1 LID, 180° entrance angle die in accordance with test method ASTM D3835-02.
- the melt stability was measured following procedure 10.8.1 ASTM D3835-02. A constant rate test at 48.6 s ⁇ 1 was used with a delay time of at least 1200 seconds. Extrudate samples were collected at 40, 120, 180, 250, 360, 600, 900, and 1200 seconds. The Goodyear IV of the as-received resins and extrudates were measured in 50/50 wt % trifluoroacetic acid/dichloromethane at 19° C. and a concentration of 0.4 g/dl using a Viscotek Forced Flow Viscometer Model Y-900, V5.7.
- the melt viscosity was measured following procedure 10.8.2. ASTM D3835-02. A multiple rate test with software detection of steady state (procedure X2) of ASTM D3835-02.was used with a melt time of 300 seconds and a shear rate of 48.6 s ⁇ 1 repeated at the beginning, middle and end of each test.
- the melt viscosity stability was determined from the slope of the best-fit line through a plot of the repeated viscosity values versus dwell time (procedure X1.4) of ASTM D3835-02. The melt viscosity stability was used to correct the data at each shear rate to zero dwell time.
- Polymer solutions were injected into size exclusion chromatography system.
- the system included size exclusion chromatography system Model Alliance 2690TM from Waters Corporation (Milford, Mass.), with a Waters 410TM refractive index detector (Differential Refractive Index) and Viscotek Corporation (Houston, Tex.) Model T-60ATM dual detector module incorporating static right angle light scattering and differential capillary viscometer detectors.
- Columns for seperation were Two Shodex GPC HFIP-80M TM styrene-divinyl benzene columns with exclusion limit 2 ⁇ 107 and 8,000/30 cm theoretical plates. Chromatographic conditions were at 35° C. temperature, 1.00 ml/min flow-rate, 0.1 ml injection volume and 50 minute run time.
- Poly(trimethylene terephthalate)polymer (3GT, PTT) in chip form was dried in a rotary dryer. Drying was done under vacuum at 160 degrees centigrade (° C. ) for 6 hours, cooled with nitrogen gas to 25° C. and stored in a sealed vessel to maintain a moisture level less than 50 ppm. For remelting, the chip was fed to a dry nitrogen supply hopper at room temperature and then gravity fed into the throat of the extruder.
- An alternative method is to have a drier mounted above the extruder and continuously dry chip at 160° C. for 6-8 hours using dry nitrogen or air. A dry nitrogen purge was located at the extruder throat to remove oxygen from the down coming chip when using dry air.
- the single screw extruder was set at: Zone 1 230° C. Zone 2 240° C. Zone 3 250° C. Zone 4 250° C. Zone 5 250° C. Extruder speed 14 rpm Melt Pressure 80 bar
- the extruder discharge melt temperature was 250° C.
- the transfer line and spin beam temperature was maintained at about 250° C.
- the melted polymer was fed to a 2-pack spin beam.
- the spin beam metering gear pumps provided 76 bar pressure to the spin pack. Each pump had a capacity of 30 cubic centimeters per revolution (cm 3 /rev). The pumps were run at 12.10 rpm.
- Each pack had a 1 layer metal screen filter with a screen mesh size of 10,000 M/cm 2 .
- the spinnerets each had 68 trilobal (Y) holes with capillary diameter of 0.35 ⁇ 0.66 mm with a length of 0.6 mm.
- the extruded or spun filaments were quenched with 18° C. air maintained at 80% humidity with a quench zone length of 1600 mm. Average air cross flow was 0.35 meters/second (m/s).
- the filaments were pulled down through a one floor high interfloor tube (part of a 3 floor machine) to a Neumag Bulk Continuous Filament (BCF) spinning machine. At the bottom of the interfloor tube two sets of 68 filaments were converged using finish applicators. The contact width of the upper applicators was 5 millimeters (mm) and the lower reversed finish applicators were 2 mm. Two 4 stream 0.8 cm 3 /rev finish pumps set at 35 rpm pumped 18% standard finish to the finish applicators.
- the threadlines were led onto an inlet godet (roller) with a surface speed of 1950 meters per minute (m/min.), then, onto a metering godet duo set at 40° C. with a surface speed of 1970 m/min.
- the filaments were drawn in space by advancing to a set of enclosed heated duos set at 165° C. with a surface speed of 3742 m/min.
- the filaments were heated by the godets fed into a Neumag texturing chamber that had a lamella cone of 3/4.5 mm and length of 80 mm. 18 lamella pieces formed the cone.
- the lamella exhaust cone had a vacuum setting of ⁇ 70 millibars (mbar).
- the textured or bulked yarn flowed out of the bottom of the chamber and piddled onto a cooling drum with a surface speed of 60 m/min.
- the cooled threadlines were removed from the cooling drum with a godet with a surface speed of 3010 m/min. From the godet the threadlines went through a tacking or intermingling box that had an air jet with a yoke width and diameter of 6 mm. The threadlines were impinged with an air pressure of 5.5 bar. The correct tension was controlled by an exit godet with a surface speed of 3030 m/min. This godet isolated the winding tension from the required tacking tension.
- the threadlines were led to a two-cot winder that takes a tube diameter of 79 millimeters (mm).
- the drive roll or pressure roll (set at 100 newtons (N)) surface speed was 3015 m/min., which produced a winding tension of around 150 grams.
- the traversing stroke was 250 mm and was run at speed to produce a 13-degree winding angle.
- the traversing mechanism was modulated with an amplitude of 0.1% at 0.1/second.
- the final package diameter was 215 mm producing a package weight of 5.1 kilograms.
- Poly(trimethylene terephthalate)polymer (3GT, PTT) in chip form was dried in a rotary dryer. Drying was done under vacuum at 160 degrees centigrade (° C. ) for 6 hours, cooled with nitrogen gas to 25° C. and stored in a sealed vessel to maintain a moisture level less than 50 ppm. For remelting, the chip was fed to a dry nitrogen supply hopper at room temperature and then gravity fed into the throat of the extruder.
- An alternative method is to have a drier mounted above the extruder and continuously dry chip at 160° C. for 6-8 hours using dry nitrogen or air. A dry nitrogen purge was located at the extruder throat to remove oxygen from the down coming chip when using dry air in the drier.
- the single screw extruder was set at: Zone 1 230° C. Zone 2 240° C. Zone 3 250° C. Zone 4 250° C. Zone 5 250° C. Extruder speed 15 rpm Melt Pressure 80 bar
- the extruder discharge melt temperature was 250° C.
- the transfer line and spin beam temperature was maintained at 250° C.
- the melted polymer was fed to a 2-pack spin beam.
- the spin beam metering gear pumps provided 79 bar pressure to the spin pack. Each pump had a capacity of 30 cm 3 /rev. The pumps were run at 13.26 rpm.
- Each pack has a 1 layer metal screen filter with a screen mesh size of 10,000 M/cm 2 .
- the spinnerets each have 68 trilobal (Y) holes with capillary diameter of 0.35 ⁇ 0.66 millimeters (mm) with a length of 0.6 mm.
- the extruded or spun filaments were quenched with 18° C. air maintained at 80% humidity with a quench zone length of 1600 mm. Average air cross flow was 0.25 meter per second (m/s).
- the filaments were pulled down through a one floor high interfloor tube (part of a 3 floor machine) to a Neumag spinning machine. At the bottom of the interfloor tube the two sets of 68 filaments were converged using finish applicators.
- the contact width of the upper applicators was 5 mm and the lower reversed finish applicators were 2 mm.
- Two 4 stream 0.8 cm3/rev finish pumps set at 40 rpm pumped P-7050T18 % Fiber Solutions finish to the finish applicators.
- the threadlines were led onto an inlet godet with a surface speed of 2390 m/min. Then, onto a metering godet duo set at 40° C. with a surface speed of 2400 m/min.
- the filaments were drawn in space with no assist by advancing to a set of enclosed heated duos set at 165° C. with a surface speed of 4100 m/min.
- the filaments were heated by the godets fed into a Neumag texturing chamber that had a lamella cone of 3/4.5 mm and length of 80 mm. 18 lamella pieces formed the cone. Hot air set at 7.5 bar and 225° C. impinged on the yarn bundles.
- the lamella exhaust cone had a vacuum setting of ⁇ 95 m/bar.
- the textured or bulked yarn flowed out of the bottom of the chamber and piddled onto a cooling drum with a surface speed of 65 m/min.
- the cooled threadlines were removed from the cooling drum with a godet with a surface speed of 3300 m/min. From the godet the threadlines went through a tacking or intermingling box that had an air jet with a yoke width and diameter of 6 mm. The threadlines were impinged with an air pressure of 7.0 bar. The correct tension was control by an exit godet with a surface speed of 3340 m/min. This godet isolated the winding tension from the required tacking tension.
- the threadlines were led to a two-cot winder that took a tube diameter of 79 mm.
- the drive roll or pressure roll (set at 100 N) surface speed was 3305 m/min., which produces a winding tension of around 150 grams.
- the traversing stroke was 250 mm and was run at speed to produce a 13-degree winding angle.
- the traversing mechanism was modulated with an amplitude of 0.1% at 0.1/ second.
- the final package diameter was 215 mm producing a package weight of 5.1 kilograms.
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Fluid Mechanics (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Polyesters Or Polycarbonates (AREA)
- Carpets (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
Priority Applications (9)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US10/752,399 US20050147784A1 (en) | 2004-01-06 | 2004-01-06 | Process for preparing poly(trimethylene terephthalate) fiber |
| PCT/US2005/000774 WO2005068695A1 (fr) | 2004-01-06 | 2005-01-06 | Procede de preparation d'une fibre de poly(trimethylene terephthalate) |
| JP2006549507A JP2007521422A (ja) | 2004-01-06 | 2005-01-06 | ポリ(トリメチレンテレフタレート)繊維の製造方法 |
| EP05711340A EP1702092A4 (fr) | 2004-01-06 | 2005-01-06 | Procede de preparation d'une fibre de poly(trimethylene terephthalate) |
| CA002552662A CA2552662A1 (fr) | 2004-01-06 | 2005-01-06 | Procede de preparation d'une fibre de poly(trimethylene terephthalate) |
| KR1020067013476A KR20060123432A (ko) | 2004-01-06 | 2005-01-06 | 폴리(트리메틸렌 테레프탈레이트) 섬유의 제조 방법 |
| CN200580001824XA CN1906340B (zh) | 2004-01-06 | 2005-01-06 | 制备聚(对苯二甲酸1,3-丙二醇酯)纤维的方法以及用该纤维制成的地毯 |
| MXPA06007683A MXPA06007683A (es) | 2004-01-06 | 2005-01-06 | Proceso para preparar fibra de poli(trimetilentereftalato). |
| TW094100397A TW200602525A (en) | 2004-01-06 | 2005-01-06 | Process for preparing poly(trimethylene terephthalate) fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US10/752,399 US20050147784A1 (en) | 2004-01-06 | 2004-01-06 | Process for preparing poly(trimethylene terephthalate) fiber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US20050147784A1 true US20050147784A1 (en) | 2005-07-07 |
Family
ID=34711624
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US10/752,399 Abandoned US20050147784A1 (en) | 2004-01-06 | 2004-01-06 | Process for preparing poly(trimethylene terephthalate) fiber |
Country Status (9)
| Country | Link |
|---|---|
| US (1) | US20050147784A1 (fr) |
| EP (1) | EP1702092A4 (fr) |
| JP (1) | JP2007521422A (fr) |
| KR (1) | KR20060123432A (fr) |
| CN (1) | CN1906340B (fr) |
| CA (1) | CA2552662A1 (fr) |
| MX (1) | MXPA06007683A (fr) |
| TW (1) | TW200602525A (fr) |
| WO (1) | WO2005068695A1 (fr) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080014403A1 (en) * | 2006-07-13 | 2008-01-17 | Chang Jing C | Substantially Flame Retardant-Free 3GT Carpet |
| US7913418B2 (en) * | 2005-06-23 | 2011-03-29 | Whirlpool Corporation | Automatic clothes dryer |
| US11479884B2 (en) * | 2017-01-12 | 2022-10-25 | Trützschler Group SE | Device and method for producing a multicolor yarn |
| US11535955B2 (en) | 2017-01-12 | 2022-12-27 | Trützschler Group SE | Draw device |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5431461B2 (ja) * | 2008-05-23 | 2014-03-05 | エーリコン テクスティル ゲゼルシャフト ミット ベシュレンクテル ハフツング ウント コンパニー コマンディートゲゼルシャフト | 溶融紡糸時にマルチフィラメント糸を引出しかつ延伸する方法並びにこの方法を実施する装置 |
| CN101735608B (zh) * | 2009-12-14 | 2011-07-20 | 杭州师范大学 | 吸湿性细旦/超细旦锦纶母粒、锦纶poy长丝及其制备方法 |
| AU2011352246B2 (en) * | 2010-12-28 | 2016-07-07 | E. I. Du Pont De Nemours And Company | Carpets prepared from yarns comprising a fluorinated polyester blend |
| CN102618947B (zh) * | 2012-04-06 | 2014-08-06 | 缪爱国 | Ptt螺旋型三维中空纤维的生产方法 |
| CN102758604B (zh) * | 2012-07-30 | 2014-12-17 | 中国石油集团川庆钻探工程有限公司长庆井下技术作业公司 | 压裂施工纤维的膨化技术 |
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- 2005-01-06 TW TW094100397A patent/TW200602525A/zh unknown
- 2005-01-06 JP JP2006549507A patent/JP2007521422A/ja not_active Abandoned
- 2005-01-06 KR KR1020067013476A patent/KR20060123432A/ko not_active Ceased
- 2005-01-06 CN CN200580001824XA patent/CN1906340B/zh not_active Expired - Fee Related
- 2005-01-06 WO PCT/US2005/000774 patent/WO2005068695A1/fr not_active Ceased
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- 2005-01-06 EP EP05711340A patent/EP1702092A4/fr not_active Withdrawn
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Also Published As
| Publication number | Publication date |
|---|---|
| EP1702092A1 (fr) | 2006-09-20 |
| CA2552662A1 (fr) | 2005-07-28 |
| KR20060123432A (ko) | 2006-12-01 |
| TW200602525A (en) | 2006-01-16 |
| WO2005068695A1 (fr) | 2005-07-28 |
| MXPA06007683A (es) | 2006-09-01 |
| CN1906340A (zh) | 2007-01-31 |
| CN1906340B (zh) | 2012-07-04 |
| EP1702092A4 (fr) | 2007-12-05 |
| JP2007521422A (ja) | 2007-08-02 |
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| AS | Assignment |
Owner name: E. I. DU PONT DE NEMOURS AND COMPANY, DELAWARE Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:CHANG, JING CHUNG;DOMMEL, RICHARD LEE;REEL/FRAME:014727/0904;SIGNING DATES FROM 20040521 TO 20040526 |
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Free format text: ABANDONED -- AFTER EXAMINER'S ANSWER OR BOARD OF APPEALS DECISION |