Note: Descriptions are shown in the official language in which they were submitted.
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TITLE OF INVENTION
PROCESS FOR PREPARING POLY(TRIMETHYLENE
TEREPHTHALATE) FIBER
FIELD OF THE INVENTION
The present invention relates to a polyester yarn and its
manufacture. More particularly, the invention relates to processes for
producing poly(trimethylene terephthalate) fibers having good physical
properties.
BACKGROUND OF THE INVENTION
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 polyethylene
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. Polyethylene 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. U.S. Pat. No. 4,877,572 describes a process for
preparing poly(butylene terephthalate) BCF yarn in which the extruded
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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.
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,,.-- ,~,.;~ ;. . ~~.. ...." ,.",. ,.".. . ..... ..... .. ..
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. According to this reference, 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. Although 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. Pat. 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. According to this reference,
poly(trimethylene terephthalate) with an intrinsic viscosity of 0.8 to 1.2 and
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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. Pat. Pub. No. 2003/0045611 relates to a process for
preparation of pigmented shaped articles (e.g., fibers). For fiber use,
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. 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 applications, 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.
SUMMARY OF THE INVENTION
According to a first aspect in accordance with the present
invention a process comprises:
(a) spinning 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) converging the filaments into yarn;
(c) cooling the filaments; and
(d) drawing the filaments at a speed of greater than 3000
meters per minute to produce filaments having a filament denier
greater than 1, and a yarn denier greater than 210.
Preferably, the filaments are drawn at a draw ratio of about
1.1 to about 4Ø
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Preferably, 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. Preferably,
the bulking comprises blowing and deforming the filaments in a hot-fluid jet
bulking unit.
According to another aspect, a process comprises:
(a) extruding molten poly(trimethylene terephthalate)
polymer having 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 per second shear rate through a spinneret
to form filaments;
(b) converging the filaments into yarn;
(c) cooling the extruded filaments;
(d) coating the cooled filaments with a spin finish; optionally
pre-intermingling the filaments;
(e) optionally heating the coated filaments to a temperature
greater than the glass transition temperature of the polymer
filaments, but less than about 200°C;
(f) drawing the optionally heated filaments at a speed of
greater than 3000 meters per minute to produce filaments
having a filament denier greater than 1 and yarn having a yarn
denier greater than 210;
(g) bulking the drawn filaments such that the filaments are
blown and deformed in three dimensions with a hot bulking fluid
to form bulked continuous filaments having random 3-
dimensional curvilinear crimp;
s
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(h) cooling the bulked continuous filaments to a temperature
less than the glass transition temperature of the polymer
filaments; and
(i) entangling the bulked continuous filaments.
Preferably, the bulked continuous filaments are entangled
before the cooling. In another aspect, the filaments can be ply-twisted and
heat set into a yarn. The ply-twisted, heat-set yarn can be made into
carpet.
BRIEF DESCRIPTION OF THE DRAWINGS
The drawings are provided for illustration purposes only, and
are not intended to limit the scope of the present invention.
Figure 1 schematically illustrates a chip dryer and melt
extruder system; and
Figure 2 schematically illustrates a spinning configuration
useful in this invention.
DETAILED DESCRIPTION
Unless stated otherwise, all percentages, parts, ratios, etc.,
are by weight. Trademarks are shown in upper case.
Further, when an amount, concentration, or other value or
parameter is given as either a range, preferred range or a list of upper
preferable values and lower preferable values, this is to be understood as
specifically disclosing all ranges formed from any pair of any upper range
limit or preferred value and any lower range limit or preferred value,
regardless of whether ranges are separately disclosed. Where a range of
numerical values is recited herein, unless otherwise stated, the range is
intended to include the endpoints thereof, and all integers and fractions
within the range. It is not intended that the scope of the invention be
limited to the specific values recited when defining a range.
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In accordance with a first aspect of the present invention, a
process comprises:
(a) spinning 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) converging the filaments into yarn;
(c) cooling the filaments; and
(d) drawing the filaments at a speed of greater than 3000
meters per minute to produce filaments having a filament denier
greater than 1 and yarn having a yarn denier greater than 210.
The filaments can be coated with a spin finish and,
optionally, preintermingled. Preferably, the process further comprises
bulking the drawn filaments. The drawn filaments can be bulked to form 3-
dimensional curvilinear crimp therein. Preferably, the bulking comprises
blowing and deforming the filaments in a hot-fluid jet bulking unit.
Preferably, the process further comprises entangling the
filaments.
According to a further aspect in accordance with the present
invention, a process comprises:
(a) extruding molten poly(trimethylene terephthalate)
polymer having 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 per second shear rate through a spinneret
to form filaments;
(b) converging the filaments into yarn;
(c) cooling the extruded filaments;
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(d) coating the cooled filaments with a spin finish; optionally
pre-intermingling the filaments;
(e) optionally heating the coated filaments to a temperature
greater than the glass transition temperature of the polymer
filaments, but less than about 200°C;
(f) drawing the optionally heated filaments at a speed of
greater than 3000 meters per minute to produce filaments
having a filament denier greater than 1 and yarn having a yarn
denier greater than 210;
(g) bulking the drawn filaments such that the filaments are
blown and deformed in three dimensions with a hot bulking fluid
to form bulked continuous filaments having random 3-
dimensional curvilinear crimp;
(h) cooling the bulked continuous filaments to a temperature
less than the glass transition temperature of the polymer
filaments; and
(i) entangling the bulked continuous filaments.
As noted, the bulked continuous filaments can be entangled
before the cooling.
According to a further aspect, the filaments are ply-twisted
and heat set into yarn. Carpet can be made from the ply-twisted and heat-
set yarn.
With specific reference to Fig. 1 of the drawing,
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. Preferably, the number average
molecular weight is at least about 26500, more preferable at least about
27500, most preferably, at least about 29000. Preferably, the number
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average molecular weight is up to about 50000, more preferably up to
about 45000, most preferably up to about 40000. 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 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. When the moisture content is at the
desired level at the dryer exit, remelting is started.
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.
By "remelter throat" reference is being made to a pipe
connecting the metering screw and the remelter.
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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 280° 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. Any
suitable pump may be used.
Polymer temperature should be monitored and controlled,
using techniques well within the skill of the art, to prevent polymer
degradation and possible generation of irritating and/or toxic byproducts.
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. By way of non-limiting example, 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,
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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.
With reference to Figure 2, 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. Following the finish application
and prior to the meter roll 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
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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.
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 4Ø 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.
In accordance with the present invention, 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
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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. In the bulking unit described in U.S. Pat. No. 3,525,134,
the filaments are both bulked and entangled. Other bulking units can be
used. With some units, 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.
Using methods known in the art, the filaments can be ply-
twisted and heat set into yarn. The yarn can then be made into carpet. Of
course, other uses will readily occur to one of ordinary skill in the art
having the benefit of the present disclosure. By way of example, the yarn
of the present invention could also be used in rugs, woven tiles,
automotive interiors and fabrics.
Experimental
Conditioning
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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. After drying, the moisture levels in the 3GT Sample 1 and 3GT
Sample 2 were 38 and 40 ppm, respectively.
Procedures
The 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 L/D, 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 ~ 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 acidldichloromethane 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 ~ 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.
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Melt Stability
Goodyear IV versus time from the extrudate samples is
shown in Table 1. Both 3GT resins degrade with time at the test
temperatures. The initial rapid loss up to ~ 500 s is believed to be due to
hydrolysis. At longer times (> 500 s), the loss in IV is likely a result of
thermal degradation. The rate of IV loss is about the same in both resins.
TABLE 1
Time 3GT 3GT 3GT 3GT
Sample Sample Sample Sample
(s) 1 1 2 2
250 C 260 C 250 C 260
C
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
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Melt Viscosity
Melt viscosity versus shear rate is shown in Table 2. The
viscosity of the 3GT Sample 1 is higher compared to the 3GT Sample 2,
consistent with a higher Goodyear IV.
Table 2.
3GT Sample 1 - Corrected Melt Viscosity
250 260
C C
Shear Test Test Test Avg CV Test Test Test Avg CV
Rate 1 2 3 1 2 3
(s ~) (Pa.s)(%) (Pa.s)(%)
24.32 636.8639.9668.6648.4 2.7
48.65 621.8623.9634.5626.7 1.1 495.6505.0499.9 500.20.9
72.97 612.4612.0618.2614.2 0.6 492.5494.5493.0 493.40.2
97.29 584.1603.0608.8598.6 2.2 484.9485.0487.1 485.70.3
121.61 586.9585.3594.5588.9 0.8 476.1476.4479.7 477.40.4
182.42 556.9541.8564.9554.5 2.1 457.9458.5459.4 458.60.2
243.23 531.6535.7540.9536.1 0.9 441.4441.3437.9 440.20.5
364.84 492.3494.6495.7494.2 0.4 412.0410.1411.2 411.10.2
486.45 387.9390.4 389.20.5
3GT Sample 2 - Corrected Melt Viscosity
250 260
C C
Shear Test Test Test Avg CV Test Test Test Avg CV
Rate 1 2 3 1 2 3
(s ~) (Pa.s)(%) (Pa.s)(%)
24.32 314.8317.3308.5313.6 1.4 258.4247.3273.8 259.85.1
48.65 308.9309.1317.4311.8 1.6 251.8243.7262.1 252.53.0
72.97 298.1300.6299.4 0.6 241.2241.5260.2 247.63.6
97.29 300.2300.1303.8301.4 0.7 247.2238.4258.8 248.13.4
121.61 297.1294.6306.9299.5 2.2 247.1234.6255.9 245.93.5
182.42 242.9230.9250.6 241.53.3
Size Exclusion Chromatography Method to Measure Molecular
Weight Distribution in Polymers Soluble in HFIP
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Polymer samples were under dissolution for 2 hours in
mobile phase solvent at 50° C with moderate agitation (Automatic sample
preparation system PL 260 T"" from Polymer Laboratories). All
concentrations are in milligram per milliliter (mg/ml). Mobile phase solvent
was 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) with 0.01 molar sodium
trifluoroacetate.
Polymer solutions were injected into size exclusion
chromatography system. The system included size exclusion
chromatography system Model Alliance 2690TM from Waters Corporation
(Milford, MA), with a Waters 410TM refractive index detector (Differential
Refractive Index) and Viscotek Corporation (Houston, TX) Model T-60AT""
dual detector module incorporating static right angle light scattering and
differential capillary viscometer detectors. Columns for separation were
Two Shodex GPC HFIP-80M TM styrene-divinyl benzene columns with
exclusion limit 2 x 107 and 8,000/30cm 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.
Software used for data reduction was Trisec~ Triple
Detector SEC3 version 3.0 by Viscotek. Data reduction method was via
triple detection method incorporating data from all three detectors:
refractometer, viscometer and light scattering photometer (right angle).
Flory-Fox equation is used for angular assymetry light scattering
correction. No column calibration was involved in data processing. Sample
concentration for 3GT polymers in HFIP was verified independently based
on refractive index increment (dn/dc) = 0.235. Number average molecular
weight was calculated and reported as shown in Table 3.
Table 3.
Number Average Molecular Weight
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Resin Measurement Measurement Avera a
1 2
3GT Sample 33200 33200 _ 33200
1 ~
3GT Sample 26800 25300 26050
2
Example 1 (3742 mpm Draw Roll Speed)
Poly (trimethylene terephthalate) polymer (3GT, PTT) in chip
form, specifically 3GT Sample 1, 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:
Zone1 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. In 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 (cm3/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/cm2. The spinnerets each had 68
trilobal ( Y ) holes with capillary diameter of 0.35x0.66 mm with a length of
0.6 mm.
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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 cm3/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.
Hot air set at 7.0 bar and 225° C impinged on the yarn bundles.
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.
19
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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.
Textile measurements were:
Denier 1242
Tenacity, gm/den 2.63
Elongation, % 50
Modulus, gm/den 13.3
TYT, % TR ~ 16.
TYT, % CO 2 14.5
TYT, % FS 3 2.4
~ TYT=Bulk measurement instrument of Lawson-Hemphill
Electron Yarn Tester Model TYT-EW, %TR=Total Retraction
2 %CO=Crimp Out
3 %FS=Fiber Shrinkage
Example 2 (4100 m/min. Draw Roll Speed)
Poly (trimethylene terephthalate) polymer (3GT, PTT) in chip
form, specifically 3GTSample 1, 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.
CA 02552662 2006-07-04
WO 2005/068695 PCT/US2005/000774
The single screw extruder
was set at:
Zone1 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. In the spin beam metering
gear pumps provided 79 bar pressure to the spin pack. Each pump had a
capacity of 30 cm3/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/cm2. The
spinnerets each have 68 trilobal ( Y ) holes with capillary diameter of
0.35x0.66 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-7050T 18 % 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
2i
CA 02552662 2006-07-04
WO 2005/068695 PCT/US2005/000774
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 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 65 mlmin.
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.
Textile measurements were:
Denier 1212
Tenacity, gm/den 2.71
Elongation, % 51
Modulus, gm/den 13.1
TYT, % TR 16.4
TYT, % CO 13.8
TYT, % FS 3.0
~ TYT=Bulk measurement instrument of Lawson-Hemphill
Electron Yarn Tester Model TYT-EW, %TR=Total Retraction
2 %CO=Crimp Out
3 %FS=Fiber Shrinkage
22
