KR20060123432A - Process for preparing poly(trimethylene terephthalate) fiber - Google Patents

Abstract

The present invention relates to processes using poly(trimethylene terephthalate) filaments (2)/yarn. The poly(trimethylene terephthalate) has a number average molecular weight of at least about 26500 and a melt viscosity of at least about 350 Pascals at 250°C and 48.65 per second shear rate. The poly(trimethylene terephthalate) is spun into filaments (2) and the filaments (2) are converged into yarn. The filaments have a denier greater than 1 and the yarn has a denier greater than 210.

Description

Process for Preparing Poly (Trimethylene Terephthalate) Fiber

The present invention relates to polyester yarns and their preparation. More specifically, the present invention relates to a process for producing poly (trimethylene terephthalate) fibers having good physical properties.

Polyethylene terephthalate ("2GT") and polybutylene terephthalate ("4GT"), commonly referred to as "polyalkylene terephthalates", are general commercial polyesters. Polyalkylene terephthalates have good physical and chemical properties, in particular chemical stability, thermal stability and light stability, high melting point and high strength. As a result, it has been widely used for resins, films and fibers.

Polyesters prepared by condensation polymerization of the reaction product of diols and dicarboxylic acids can be spun into yarns. U.S. Patent No. 3,998,042 describes a process for producing poly (ethylene terephthalate) yarns in which the extruded fibers are drawn at high temperatures (160 ° C.) with steam jet assistance or at lower temperatures (95 ° C.) with hot water assistance. Poly (ethylene terephthalate) can be spun into bulk continuous filament (BCF) yarns in a two-stage stretching process where the first stage stretching is at a significantly higher draw ratio than the second stage stretching. U.S. Patent No. 4,877,572 is a poly (butylene terephthalate) wherein the extruded fibers are stretched in one step, the feed roller is heated to a temperature 30 ° C. higher or lower than the Tg of the polymer, and the draw roller is 100 ° C. or more higher than the feed roller. Described are methods for making BCF yarns.

U.S. Patent No. 6,254,961 relates to spinning poly (trimethylene terephthalate) with a suitable yarn on the carpet. According to this patent, a stretching speed of more than 1000 m / min is possible in the process of the invention, and a stretching speed of more than 1800 m / min is preferred because it allows the resulting yarn to have high strength.

U.S. Patent No. 6,284,370 has poly (trimethylene terephthalate) which has a moderate thermal stress and a moderate boiling shrinkage, provides a fabric having lower stiffness caused by excessive shrinkage when weaving or knitting, and exhibiting excellent color development expected from the low modulus properties of the fibers. ) It is about fiber. According to this reference, the intrinsic viscosity of the polymer used in the invention is preferably 0.4 to 1.5, more preferably 0.7 to 1.2. The polyester fibers of the invention are preferably in the form of multifilament yarns when used for garment applications. The total size of the yarn is not limited but is usually 5 to 200 d (denier), preferably 20 to 150 d. The single filament size is not limited but is from 0.1 to 10 d, preferably from 0.5 to 5 d, more preferably from 1 to 3 d. Furthermore, according to this patent, it is important that the peripheral speed of the first roll used to make the fibers is 300 to 3,500 m / min. The ambient speed is preferably 800 to 3,000 m / min, more preferably 1,200 to 2,500 m / min. The peripheral speed of the second roll is determined by the draw ratio, but is mainly 600 to 6,000 m / min.

U.S. Patent publication publication No. 2003/0127766 generally relates to poly (trimethylene terephthalate) BCF carpet modified single-sided yarns and methods of making the same, in particular poly (trimethylene terephthalate) BCF carpet modified single-sided yarns and methods of making the same. According to this document, poly (trimethylene terephthalate) having an intrinsic viscosity of 0.8 to 1.2 and a water content of up to 50 ppm is used as raw material and is preferably melt spun at a spinning speed of 1500 to 4000 m / min. The spun filaments are drawn and crimped at a speed of 1500 to 4000 m / min.

U.S. Patent publication publication No. 2003/0045611 relates to a method of making colored shaped articles (eg, fibers). For fiber applications, the poly (trimethylene terephthalate) preferably has an intrinsic viscosity of at least about 0.6 dl / g, typically up to about 1.5 dl / g. Preferred viscosities for many end uses, in particular fibers and films, are at least 0.8 dl / g, more preferably at least 0.9 dl / g. Typically, 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. In commercial use, the spinning speed is preferably at least about 1,000 meters / minute and can reach up to at least about 5,000 meters / minute using the roll 40 as a reference speed.

Summary of the Invention

According to a first aspect according to the invention, the method is

(a) spinning a molten poly (trimethylene terephthalate) polymer having a number average molecular weight of at least about 26500 and a melt viscosity of at least about 350 Pascals at 250 ° C. and 48.65 per second shear rate;

(b) converge the filaments into yarns;

(c) cool the filament;

(d) stretching the filament at a rate of more than 3000 meters / minute to produce a filament having more than one filament denier and more than 210 yarn denier

It includes.

Preferably, the filaments are drawn at a draw ratio of about 1.1 to about 4.0.

Preferably, the poly (trimethylene terephthalate) has an intrinsic viscosity of about 0.95 to about 1.10.

Elongated filaments may be bulked and / or entangled. It can be bulked to form three-dimensional curved crimps therein. Preferably, the bulking comprises blowing and deforming the filaments in the hot fluid jet bulking unit.

According to the other side, the way

(a) an intrinsic viscosity in the range of about 0.95 to about 1.10, a water content of less than about 100 ppm, a number average molecular weight of about 26500 to about 50000, and a melt viscosity of about 350 to about 1000 pascals at 250 ° C. and 48.65 shear rates per second Extruding the molten poly (trimethylene terephthalate) polymer having a spinneret to form a filament;

(b) converge the filaments into yarns;

(c) cool the extruded filaments;

(d) coating the cooled filaments with a spin finish; Optionally preintermingling the filaments;

(e) optionally coated filaments are heated to a temperature above the glass transition temperature of the polymer filament and below about 200 ° C .;

(f) stretching the optionally heated filament at a rate of more than 3000 meters / minute to produce a filament having more than one filament denier and more than 210 yarn denier;

(g) bulking the stretched filaments to blow and deform the filaments in three dimensions with a hot bulking fluid to form bulked continuous filaments with random three-dimensional curved crimps;

(h) cooling the bulked continuous filament to a temperature below the glass transition temperature of the polymer filament;

(i) entangle bulked continuous filaments

It includes.

Preferably, the bulked continuous filaments are entangled before cooling. In another aspect, the filaments can be joined and heat fixed with yarns. The combined and heat set yarns can be made into carpets.

The drawings are provided for purposes of illustration only and are not intended to limit the scope of the invention.

1 schematically illustrates a chip dryer and a melt extruder system;

2 schematically illustrates a radiation configuration useful for the present invention.

Unless stated otherwise, all percentages, parts, ratios, etc., are by weight. The trademark is capitalized.

In addition, where an amount, concentration, or other value or parameter is presented as a list of one range, preferred range, or preferred upper limit and preferred lower limit, this means that any range upper limit or It is to be understood that the specific values and all ranges formed by any pair of lower limit values or preferred values are specifically disclosed. Where a range of numerical values is cited herein, unless stated otherwise, the range is intended to include the endpoint and all integers and fractions within that range. The scope of the present invention is not intended to be limited to the specific values recited in limiting the range.

According to a first aspect of the invention, the method is

(a) spinning a molten poly (trimethylene terephthalate) polymer having a number average molecular weight of at least about 26500 and a melt viscosity of at least about 350 Pascals at 250 ° C. and a shear rate of 48.65 per second;

(b) converge the filaments into yarns;

(c) cool the filament;

(d) stretching the filament at a rate of more than 3000 meters / minute to produce a filament having more than one filament denier and more than 210 yarn denier

It includes.

The filaments are coated with a spin finish and can optionally be premixed. Preferably, the method further comprises bulking the drawn filaments. The stretched filaments can be bulked to form three-dimensional curved crimps therein. Preferably, the bulking comprises blowing and deforming the filaments in the hot fluid jet bulking unit.

Preferably, the method further comprises entanglement of the filaments.

According to another aspect of the invention, the method is

(a) an intrinsic viscosity in the range of about 0.95 to about 1.10, a water content of less than about 100 ppm, a number average molecular weight of about 26500 to about 50000, and a melt viscosity of about 350 to about 1000 pascals at 250 ° C. and 48.65 shear rates per second Extruding the molten poly (trimethylene terephthalate) polymer having a spinneret to form a filament;

(b) converge the filaments into yarns;

(c) cool the extruded filaments;

(d) coating the cooled filaments with a spin finish; Optionally premixing the filaments;

(e) optionally coated filaments are heated to a temperature above the glass transition temperature of the polymer filament and below about 200 ° C .;

(f) stretching the optionally heated filament at a rate of more than 3000 meters / minute to produce a filament having more than one filament denier and more than 210 yarn denier;

(g) bulking the stretched filaments to blow and deform the filaments in three dimensions with a hot bulking fluid to form bulked continuous filaments with random three-dimensional curved crimps;

(h) cooling the bulked continuous filament to a temperature below the glass transition temperature of the polymer filament;

(i) entangle bulked continuous filaments

It includes.

As discussed above, the bulked continuous filaments may be entangled before cooling.

According to another aspect, the filaments are joined with a yarn and heat fixed. Carpets can be made from joined and heat fixed yarns.

With particular reference to FIG. 1 of the drawing, the poly (trimethylene terephthalate) chip is transferred to a dryer 10 and dried. The intrinsic viscosity of the poly (trimethylene terephthalate) is preferably from 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. Preferably, the number average molecular weight is at least about 26500, more preferably at least about 27500 and most preferably at least about 29000. Preferably, the number average molecular weight is about 50000 or less, more preferably about 45000 or less, most preferably about 40000 or less. Preferably, 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 Pascal at 250 ° C. and 48.65 shear rates. Also preferably, the melt viscosity is about 1000 or less, more preferably about 900 or less, even more preferably about 800 or less, most preferably about 700 Pascal or less at 250 ° C. and 48.65 shear rates per second.

Drying is preferably performed at about 80 ° C. or higher and about 180 ° C. or lower, most preferably at about 150 ° C. The poly (trimethylene terephthalate) chip is preferably dried until the moisture content is less than 100 ppm, more preferably about 50 ppm or less, most preferably about 40 ppm or less. The drying time should be as long as necessary to reach the desired moisture content, preferably about 4 to about 10 hours, more preferably about 6 to about 8 hours. The actuator must maintain a constant moisture level to maintain a consistent melt viscosity. Commercially available dehumidifiers can be used. Dry nitrogen, air or other inert gases can be used. If the moisture content is at the desired level at the dryer outlet, remelting is initiated.

The dried chips are fed to an optional chip metering screw 12 and metered into the remelter throat 14.

The metering screw is optional because it can be used to control the amount of chips used. Chip metering screws are normally used with screw remelting machines. Any commercially available metering screw can be used.

The expression "remelter neck" refers to the piping connecting the metering screw and the remelting machine.

The remelting machine may be any suitable single screw or twin screw extruder. A nitrogen purge may be used to prevent oxygen from being loaded into the remelt with the chip. This will reduce the polymer degradation caused by oxygen.

The remelting is preferably at about 200 ° C. or higher, preferably about 235 ° C. or higher, more preferably about 245 ° C. or higher, and about 280 ° C. or lower, preferably about 270 ° C. or lower, more preferably about 265 ° C. or lower. Is performed. At temperatures above 280 ° C., acrolein is generated which is an undesirable byproduct.

The polymer is fed to an optional delivery line pump 20 providing sufficient pressure (about 2250 to 3000 psig) to overcome losses in the delivery line 22, to provide a constant feed rate, and to spin pack metering pump 24 Sufficient pressure to feed the polymer). Any suitable pump can be used.

In order to prevent polymer degradation and the possible occurrence of irritation and / or toxic by-products, the polymer temperature should be monitored and controlled using techniques that fall within the scope of the art. The delivery line 22 is preferably surrounded by external piping (not shown), which provides an outer jacket for the delivery line. The outer jacket may contain a heat transfer fluid to help maintain the temperature of the polymer within acceptable limits. The temperature of the polymer delivery line 22 is preferably maintained at about 220 ° C. or higher, more preferably at least about 230 ° C. and most preferably at least about 240 ° C. The temperature may be about 265 ° C. or less, preferably about 260 ° C. or less, most preferably about 255 ° C. or less. As a non-limiting example, the heat transfer fluid in the jacket may be paraffin, preferably maintained below 250 ° C.

The polymer retention time in the delivery tubing 22 should be kept to a minimum, for example less than 20 minutes, preferably less than 10 minutes and most preferably less than 2 minutes. This can be achieved, for example, by using a booster pump to reduce the length and / or diameter of the tubing and / or increase the yield.

Metering pump 24 metered the polymer composition into spinneret or die 26.

In connection with FIG. 2, the polymer is extruded through a spinneret or die 26 to form a filament 2. The spun filaments are cooled below the polymer glass transition temperature in the cooling zone 3 by radial or transverse flow of gas. The spin finish or oil may be applied to the filaments solidified by the finish applicator 4. After the finish application and also before the meter roll, the filaments can be treated with turbulence in the optional premixing device 5 to even out the finish on the filaments.

The polymer is roomed at a temperature of about 200 ° C. or higher, preferably about 235 ° C. or higher, more preferably about 245 ° C. or higher, and about 275 ° C. or lower, preferably about 270 ° C. or lower, more preferably about 265 ° C. or lower. Extrude through sand dunes or dies.

The spin pack metering pump and spinneret or die may be heated via conventional means (eg, Dow fluid or hot oil).

The yield is a function of the number of spin positions and is typically about 2 pounds / hour (about 0.9 kg / hour) per spinner (ie per remelter) to about 2,000 pounds / hour (about 907 kg / hour) on a commercial scale ) To about 3,000 pounds / hour (about 1,361 kg / hour), or more.

Cooling zone 3 is at least about 0.2 m / sec and about 0.8 m / sec or less, preferably at a temperature of at least about 10 ° C. and preferably at most about 30 ° C., in which radial flow of gas, typically moist air, Or cool the filament by cross flow. As shown, the filaments converge into the yarns at the roller 6.

The filaments are then stretched using a feed roller 6 and a set of stretching 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.

Subsequently, after the filament has passed through the stretching roller 7, the filament can be crimped through the bulking unit 8 to the texturing nozzle. The filaments are then cooled through the cooling drum 9 and can pass through the blending device 11 through the rollers 17, where the filaments are entangled. Then, the filament is wound up using the winding machine 15 via the roller 13 and the yarn guide 16.

According to the invention, the filaments are drawn at a speed of more than 3000 meters / minute (m / minute). The stretching speed may be greater than 3500 m / min, greater than 4000 m / min, greater than 5000 m / min, greater than 5100 m / min, or even greater than 5500 m / min.

The stretching ratio of the filament is preferably about 10% or more, more preferably 20% or more, and preferably about 90% or less, more preferably 70% or less, until the elongation at break of the filament is increased. And / or by adjusting the speed of the stretching roll 7.

The drawn filament denier is greater than 1 dl / g, preferably at least 3 dl / g, more preferably at least 10 dl / g, most preferably at least about 15 dl / g. Yarn denier is preferably greater than 210, more preferably at least about 250, even more preferably at least about 500, most preferably at least about 1000.

A jet-bulking unit 8 that can blow the filament and deform in three directions using a hot bulking fluid such as air or steam can be used in the practice of the present invention. One suitable unit is U.S. Patent No. 3,525,134. U.S. Patent No. In the bulking units described in 3,525,134, the filaments are entangled in bulk. Other bulking units may be used. For some units, a separate entanglement step may be necessary before winding up. Any method conventional in the art can be used to entangle the yarns.

The resulting BCF yarns, preferably with randomly spaced three-dimensional curved crimps, are then cooled to below the glass transition temperature of the filament (approximately 45-50 ° C.), while the yarns are at approximately 0 gpd tension so that no significant amount of crimps are released. Stay in the state. Cooling may be accomplished by various commercially available means, preferably by air or water flow, spray or mist.

Using methods known in the art, the filaments can be joined and heat fixed with yarns. The yarn can then be made into a carpet. Of course, other uses that benefit from the present disclosure will readily occur to those of ordinary skill in the art. By way of example, the yarns of the present invention may also be used in rugs, woven tiles, automotive interiors and fabrics.

Experiment

Conditioning

The poly (trimethylene terephthalate) (3GT) resin was dried at 120 ° C. for 50 hours under vacuum with heated dry nitrogen discharge using a VWR model 1430M vacuum oven. The moisture level in the dried resin was measured at 180 ° C. with a 10 minute delay using a Mitsubishi Moisture Analyzer Model CA100 with an evaporator model VA100. After drying, the moisture levels in 3GT Sample 1 and 3GT Sample 2 were 38 and 40 ppm, respectively.

step

Melt stability and melt viscosity were measured at 250 and 260 ± 0.1 ° C using a Dynisco LCR 7002 capillary rheometer with 1 mm diameter, 30: 1 L / D, 180 ° incidence die according to test method ASTM D3835-02. Measured at

Procedure 10.8.1 Melt stability was measured according to ASTM D3835-02. A constant speed test at 48.6 s ⁻¹ was used with a delay time of at least 1200 seconds. Extruded samples were collected at 40, 120, 180, 250, 360, 600, 900 and 1200 seconds. The Goodyear IV of the resin and the extrudate as received was subjected to 50 ° C./50 wt% trifluoroacetic acid / dichloromethane at 19 ° C. using Viscotek forced flow viscometer model Y-900, version 5.7. It was measured at a concentration of 0.4 g / dl.

Procedure 10.8.2. Melt viscosity was measured according to ASTM D3835-02. A multi-rate test (procedure × 2) using the stationary software detection of ASTM D3835-02 was used, with a melt time of 300 seconds and a shear rate of 48.6 s ⁻¹ repeatedly at the beginning, middle and end of each test. The melt viscosity stability was determined from the slope of the optimal line through a plot of repeat viscosity values versus residence time (procedure x 1.4) of ASTM D3835-02. Using melt viscosity stability, the data at each shear rate were corrected to zero residence time.

Melt stability

The time from the extrudate sample versus Goodyear IV is shown in Table 1. Both 3GT resins decompose over time at the test temperature. The initial rapid loss up to ˜500 seconds is believed to be due to hydrolysis. At longer times (> 500 seconds), the loss of IV is likely a result of thermal decomposition. The IV loss rate is approximately the same for both resins.

Time in seconds 3GT Sample 1 3GT Sample 1 3GT Sample 2 3GT Sample 2 250 ℃ 260 ℃ 250 ℃ 260 ℃ 0 1.031 1.031 0.936 0.936 40 1.016 1.014 0.928 0.926 120 1.006 1.000 0.927 0.897 180 1.004 0.985 0.914 0.897 250 0.987 0.980 0.895 0.879 360 0.980 0.960 0.884 0.858 600 0.963 0.932 0.874 0.849 900 0.943 0.908 0.854 0.827 1200 0.940 0.897 0.847 0.814

Melt viscosity

Melt viscosity versus shear rate is shown in Table 2. The viscosity of 3GT Sample 1 is higher than 3GT Sample 2, consistent with the higher Goodyear IV.

3GT Sample 1-Calibrated Melt Viscosity 250 ℃ 260 ℃ Shear rate (s ^-1 ) Test 1 Test 2 Test 3 Average (Pa.s) CV (%) Test 1 Test 2 Test 3 Average (Pa.s) CV (%) 24.32 636.8 639.9 668.6 648.4 2.7 48.65 621.8 623.9 634.5 626.7 1.1 495.6 505.0 499.9 500.2 0.9 72.97 612.4 612.0 618.2 614.2 0.6 492.5 494.5 493.0 493.4 0.2 97.29 584.1 603.0 608.8 598.6 2.2 484.9 485.0 487.1 485.7 0.3 121.61 586.9 585.3 594.5 588.9 0.8 476.1 476.4 479.7 477.4 0.4 182.42 556.9 541.8 564.9 554.5 2.1 457.9 458.5 459.4 458.6 0.2 243.23 531.6 535.7 540.9 536.1 0.9 441.4 441.3 437.9 440.2 0.5 364.84 492.3 494.6 495.7 494.2 0.4 412.0 410.1 411.2 411.1 0.2 486.45 387.9 390.4 389.2 0.5

3GT Sample 2-Calibrated Melt Viscosity

250 ℃ 260 ℃ Shear rate (s ^-1 ) Test 1 Test 2 Test 3 Average (Pa.s) CV (%) Test 1 Test 2 Test 3 Average (Pa.s) CV (%) 24.32 314.8 317.3 308.5 313.6 1.4 258.4 247.3 273.8 259.8 5.1 48.65 308.9 309.1 317.4 311.8 1.6 251.8 243.7 262.1 252.5 3.0 72.97 298.1 300.6 299.4 0.6 241.2 241.5 260.2 247.6 3.6 97.29 300.2 300.1 303.8 301.4 0.7 247.2 238.4 258.8 248.1 3.4 121.61 297.1 294.6 306.9 299.5 2.2 247.1 234.6 255.9 245.9 3.5 182.42 242.9 230.9 250.6 241.5 3.3

Size Exclusion Chromatography Method to Determine Molecular Weight Distribution in Soluble Polymers in HFIP

The polymer sample was dissolved for 2 hours in the mobile phase at 50 ° C. under moderate agitation (automated sample preparation system system PL 260 ^™ (manufactured by Polymer Laboratories)). All concentrations are milligrams / milliliters (mg / ml) The mobile phase solvent was 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) with 0.01 molar sodium trifluoroacetate.

The polymer solution was injected into a size exclusion chromatography system. The system includes a Waters 410 ^TM Refractive Index Detector (Differential Refractive Index), and a Viscotek Corporation (Houston, Texas) Model T-60A ^TM Dual Detector Module with Static Rectangular Light Scattering and Differential Capillary Viscometer Detector Together with the size exclusion chromatography system model Alliance 2690 ^TM (Waters Corporation, Milford, Miami, USA) The separation column included exclusion limits 2 × 10 7 and 8,000 / 30 cm theory. Two Shodex GPC HFIP-80M ^™ Styrene-Divinyl Benzene columns with Chromatography conditions were 35 ° C. temperature, 1.00 ml / min flow rate, 0.1 ml injection volume and 50 min operating time.

삼중 검출기 SEC³ 버전 3.0(비스코텍)이었다. 데이터 축약 방법은, 3개 모든 검출기, 즉 굴절계, 점도계 및 광산란 광도계(직각)으로부터의 데이터를 포함하는 3중 검출 방법을 통한 것이었다. 각 비대칭 광산란 보정을 위해 플로리-폭스(Flory-Fox) 방정식을 사용한다. 데이터 처리에는 칼럼 보정이 포함되지 않았다. HFIP 내 3GT 중합체에 대한 샘플 농도를 굴절율 증가분[(dn/dc) = 0.235]에 기초하여 독립적으로 입증하였다. 수 평균 분자량을 계산하여, 표 3에 나타냈다.The software used for data reduction is Trisec

Triple detector SEC ³ version 3.0 (BISCOTECH). The data abbreviation method was through a triple detection method that included data from all three detectors: refractometer, viscometer and light scattering photometer (right angle). The Flory-Fox equation is used for each asymmetric light scattering correction. Data processing did not include column correction. Sample concentration for 3GT polymer in HFIP was independently verified based on refractive index increment [(dn / dc) = 0.235]. The number average molecular weight was calculated and shown in Table 3.

Number average molecular weight Suzy Measure 1 Measure 2 Average 3GT Sample 1 33200 33200 33200 3GT Sample 2 26800 25300 26050

Example 1 (3742 mpm draw roll speed)

Poly (trimethylene terephthalate) polymer (3GT, PTT), in particular 3GT sample 1, in chip form was dried in a tumble dryer. Dry under vacuum at 160 ° C. for 6 hours, cool to 25 ° C. with nitrogen gas, and store in a sealed container to maintain moisture levels below 50 ppm. For remelting, the chips were fed into a dry nitrogen feed hopper at room temperature and then gravity was applied to the extruder throat. One alternative is to have a dryer mounted on the extruder at 160 ° C. for 6-8 hours using dry nitrogen or air, followed by drying chips. A dry nitrogen purge was placed in the neck of the extruder to remove oxygen from the chip descending when using dry air.

The single screw extruder was set as follows:

Band 1 230 ℃

Band 2 240 ℃

Band 3 250 ℃

Band 4 250 ℃

Band 5 250 ℃

Extruder speed 14 rpm

Melt pressure 80 bar

The extruder discharge melt temperature was 250 ° C. The delivery line and spin beam temperatures were maintained at about 250 ° C. The molten polymer was fed to a two pack spin beam. In the spin beam, the metering gear pump provided 76 bar pressure to the spin pack. Each pump had a capacity of 30 cubic centimeters per revolution (cm ³ / rev). The pump was run at 12.10 rpm. Each pack had a one layer metal screen filter with a screen mesh size of 10,000 M / cm ² . The spinneret had 68 triangular (Y) holes each having a capillary diameter of 0.35 × 0.66 mm and 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 crossflow was 0.35 meters / second (m / s). The filament was pulled down through the 1-floor high interfloor tube (part of the 3-floor instrument) towards the Neumag bulk continuous filament (BCF) spinner. At the bottom of the interfloor tube, two sets of 68 filaments were converged using a finish applicator. The contact width of the top applicator was 5 millimeters (mm) and the bottom reverse phase finish applicator was 2 mm. Two four-stream 0.8 cm ³ / rev finish pumps set at 35 rpm pumped 18% standard finish to the finish applicator.

The threadline was sent to the inlet roller (roller) with a surface speed of 1950 meters / minute (m / minute) and then sent to the quantitative piston duo set at 40 ° C. at a surface speed of 1970 m / minute. The filaments were then spatially stretched by advancing to a set of enclosed heated duo sets set at 165 ° C. at a surface speed of 3742 m / min. The filaments were heated by a feed fed to a Pneumatic texturing chamber having a lamellar cone of 3 / 4.5 mm and a length of 80 mm. Eighteen lamella pieces formed a cone. Hot air set at 7.0 bar and 225 ° C. impacted the yarn bundle. The lamella exhaust cone had a vacuum set point of -70 millibars (mbar). The textured or bulked yarn flowed out of the bottom of the chamber and entered the cooling drum at a surface speed of 60 m / min.

The cooled threadline was removed from the cooling drum using a furnace having a cooling rate of 3010 m / min. From the furnace, the threadline was passed through a tack or horn sum box with an air jet having a yoke width and diameter of 6 mm. The threadline collided with air pressure of 5.5 bar. Correct tension was adjusted by release force with a surface velocity of 3030 m / min. This strain isolated the winding tension from the necessary adhesion tension.

The threadline was sent to a two-cot winder with a tube diameter of 79 millimeters (mm). The drive roll or pressure roll (set to 100 Newtons (N)) surface speed was 3015 m / min, which yielded a winding tension of about 150 grams. The transverse stroke was 250 mm and operated at a speed that yielded a 13 degree winding angle. The traversing mechanism was adjusted to an amplitude of 0.1% at 0.1 / second. The final package diameter was 215 mm, which yielded a package weight of 5.1 kilograms.

Textile measurements were as follows:

Denier 1242

Strength, gm / denier 2.63

Elongation,% 50

Modulus, gm / denier 13.3

TYT,% TR ¹ 16.

TYT,% CO ² 14.5

TYT,% FS ³ 2.4

¹ TYT = bulk measuring instrument (made by Lawson-Hemphill) Electron Yarn Tester Model TYT-EW,% TR = total refractive index

² % CO = Crimp Out

³ % FS = fiber shrinkage

Example 2 (4100 m / min stretching roll speed)

Poly (trimethylene terephthalate) polymer (3GT, PTT), in particular 3GT sample 1, in chip form was dried in a tumble dryer. Dry under vacuum at 160 ° C. for 6 hours, cool to 25 ° C. with nitrogen gas, and store in a sealed container to maintain moisture levels below 50 ppm. For remelting, the chips were fed into a dry nitrogen feed hopper at room temperature and then gravity was applied to the extruder throat. One alternative is to have a dryer mounted on the extruder at 160 ° C. for 6-8 hours using dry nitrogen or air, followed by drying chips. A dry nitrogen purge was placed in the neck of the extruder to remove oxygen from the chip descending when using dry air.

The single screw extruder was set as follows:

Band 1 230 ℃

Band 2 240 ℃

Band 3 250 ℃

Band 4 250 ℃

Band 5 250 ℃

Extruder speed 15 rpm

Melt pressure 80 bar

The extruder discharge melt temperature was 250 ° C. The delivery line and spin beam temperatures were maintained at about 250 ° C. The molten polymer was fed to a two pack spin beam. In the spin beam, the metering gear pump provided 76 bar pressure to the spin pack. Each pump had a capacity of 30 cm ³ / rev. The pump was operated at 13.26 rpm. Each pack had a one layer metal screen filter with a screen mesh size of 10,000 M / cm ² . The spinneret had 68 triangular (Y) holes each having a capillary diameter of 0.35 × 0.66 millimeters (mm) and 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 crossflow was 0.25 meters / second (m / s). The filament was pulled down towards the Newmag spinner via a 1-floor high interfloor tube (part of the 3-floor instrument). At the bottom of the interfloor tube, two sets of 68 filaments were converged using a finish applicator. The contact width of the upper applicator was 5 mm and the lower reverse phase finish applicator was 2 mm. Two four stream 0.8 cm ³ / rev finish pumps set at 40 rpm pumped the P-7050T 18% fiber solution finish to the finish applicator.

The threadline was sent to the inlet well with a surface speed of 2390 m / min. It was then sent to a quantitative Gauze duo set at 40 ° C. at a surface speed of 2400 m / min. The filaments were drawn spatially without assistance by advancing to a set of enclosed heated duo sets set at 165 ° C. at a surface speed of 4100 m / min. The filaments were heated by a feed fed to a Pneumatic texturing chamber having a lamellar cone of 3 / 4.5 mm and a length of 80 mm. Eighteen lamella pieces formed a cone. Hot air set at 7.5 bar and 225 ° C. impacted the yarn bundle. The lamella exhaust cone had a vacuum setpoint of -97 m / bar. The textured or bulked yarn flowed out of the bottom of the chamber and entered the cooling drum at a surface speed of 65 m / min.

The cooled threadline was removed from the cooling drum using a furnace having a cooling rate of 3300 m / min. From the furnace, the threadline was passed through a tack or horn sum box with an air jet having a yoke width and diameter of 6 mm. The threadline collided with an air pressure of 7.0 bar. Correct tension was adjusted by release force with a surface velocity of 3340 m / min. This strain isolated the winding tension from the necessary adhesion tension.

The threadline was sent to a two-coat winder which required a tube diameter of 79 mm. The drive roll or pressure roll (set to 100 N) surface speed was 3305 m / min, which yielded a winding tension of about 150 grams. The transverse stroke was 250 mm and operated at a speed that yielded a 13 degree winding angle. The traversing mechanism was adjusted to an amplitude of 0.1% at 0.1 / second. The final package diameter was 215 mm, which yielded a package weight of 5.1 kilograms.

Textile measurements were as follows:

Denier 1212

Strength, gm / denier 2.71

Elongation,% 51

Modulus, gm / denier 13.1

TYT,% TR 16.4

TYT,% CO 13.8

TYT,% FS 3.0

¹ TYT = bulk measuring instrument (made by Lawson-Hemfil) Electron Yarn Tester Model TYT-EW,% TR = total refractive index

² % CO = critical rate

³ % FS = fiber shrinkage

Claims (37)

(a) spinning a molten poly (trimethylene terephthalate) polymer having a number average molecular weight of at least about 26500 and a melt viscosity of at least about 350 Pascals at 250 ° C. and 48.65 per second shear rate; (b) converge the filaments into yarns; (c) cool the filament; Drawing a filament at a speed of more than 3000 meters / min to produce a filament having more than one filament denier and more than 210 yarn denier How to include. The method of claim 1 wherein the number average molecular weight is about 26500 to about 50000. The method of claim 1 wherein the number average molecular weight is about 27500 to about 45000. The method of claim 1 wherein the number average molecular weight is from about 29000 to about 40000. The method of claim 1 wherein the melt viscosity is about 350 to about 1000 Pascals at 250 ° C. and 48.65 shear rates per second. The process of claim 1 wherein the melt viscosity is about 400 to about 900 pascals at 250 ° C. and a shear rate of 48.65 per second. The method of claim 1 wherein the melt viscosity is about 450 to about 800 pascals at 250 ° C. and a shear rate of 48.65 per second. The method of claim 1, wherein the melt viscosity is about 500 to about 700 pascals at 250 ° C. and 48.65 shear rates per second. The method of claim 1 wherein the filament denier is at least three. The method of claim 1 wherein the filament denier is at least 10. The method of claim 1 wherein the filament denier is at least 15. The method of claim 1 wherein the yarn denier is at least 250. The method of claim 1 wherein the yarn denier is at least 500. The method of claim 1 wherein the yarn denier is at least 1000. The method of claim 1, further comprising coating the filament with a spin finish and optionally preintermingling the filament. The method of claim 1, further comprising bulking the drawn filaments. The method of claim 21, further comprising entangling the filaments. The method of claim 21, wherein the stretched filaments are bulked to form three-dimensional curved crimps therein. 24. The method of claim 23, wherein the bulking comprises blowing and deforming the filaments in the hot fluid jet bulking unit. The method of claim 1 wherein the filaments are drawn at a draw ratio of about 1.1 to about 4.0. The method of claim 20, wherein the draw ratio is about 1.2 to about 3.0. The method of claim 20, wherein the draw ratio is about 1.4 to about 2.2. The method of claim 1 wherein the poly (trimethylene terephthalate) has an intrinsic viscosity of about 0.95 to about 1.10. The method of claim 23 wherein the intrinsic viscosity is from about 0.98 to about 1.04. The method of claim 25, wherein the intrinsic viscosity is from about 1.00 to about 1.02. (a) has an intrinsic viscosity in the range of about 0.95 to about 1.10, a water content of less than about 100 ppm, a number average molecular weight of about 26500 to about 50000, and a melt viscosity of about 350 to about 1000 pascal at 250 ° C. and 48.65 shear rates per second Extruding the molten poly (trimethylene terephthalate) polymer through a spinneret to form a filament; (b) converge the filaments into yarns; (c) cool the extruded filaments; (d) coating the cooled filaments with a spin finish; Optionally premixing the filaments; (e) optionally, the coated filament is heated to a temperature above the glass transition temperature of the polymer filament but less than about 200 ° C .; (f) stretching the optionally heated filament at a rate of more than 3000 meters / minute to produce a filament having more than one filament denier and more than 210 yarn denier; (g) bulking the stretched filaments to blow and deform the filaments in three dimensions with a hot bulking fluid to form bulked continuous filaments with random three-dimensional curved crimps; (h) cooling the bulked continuous filament to a temperature below the glass transition temperature of the polymer filament; (i) entangle bulked continuous filaments How to include. The method of claim 26, wherein the water content is less than about 50 ppm. 27. The method of claim 26, wherein the water content is less than about 40 ppm. 27. The method of claim 26, wherein the bulked continuous filaments of (g) are entangled before cooling in (h). 27. The method of claim 1 or 26, wherein the filaments are drawn at a speed of at least 3000 meters / minute. 27. The method of claim 1 or 26, wherein the filament is stretched at a rate greater than about 3500 meters / minute. 27. The method of claim 1 or 26, wherein the filaments are drawn at a speed of at least about 4000 meters / minute. 27. The method of claim 1 or 26, wherein the filaments are drawn at a speed of at least 5000 meters / minute. 27. The method of claim 1 or 26, wherein the filaments are drawn at a speed of at least 5100 meters / minute. 27. The method of claim 1 or 26, wherein the filaments are drawn at a speed of at least 5500 meters / minute. 27. The method of claim 26, further comprising joining and heat fixing the filaments with a yarn. A carpet made from the combined and heat-set poly (trimethylene terephthalate) yarns of claim 26.

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