U.S. patent number 3,695,025 [Application Number 05/059,383] was granted by the patent office on 1972-10-03 for fibrillated film yarn.
Invention is credited to John D. Gibbon.
United States Patent |
3,695,025 |
Gibbon |
October 3, 1972 |
FIBRILLATED FILM YARN
Abstract
There is provided a fibrillated continuous filament yarn
comprised of random-length fibrils of a synthetic organic high
polymer wherein: the average width/thickness ratio of cross
sections of the fibrils (the "aspect ratio") is from about 2/1 to
about 12/1, and the aspect ratios of the cross sections of the
fibrils range from about 0.5/1 to about 20/1; the fibrils in the
yarn exceeding 40 centimeters in length comprise at least 70
percent (by weight) of the yarn; the tenacity of the yarn is from
about 0.1 to about 10 grams per denier; the total denier of the
yarn is from 30 to about 10,000, and the average denier per fibril
of the fibrils comprising the yarn is from about 0.5 to about 60;
the elongation of the yarn is from about 0.5 to about 75 percent;
and the initial modulus of the yarn is from about 2 to about 300.
The yarn of this invention has high tenacity, a soft hand, and good
cover.
Inventors: |
Gibbon; John D. (Charlotte,
NC) |
Family
ID: |
22022604 |
Appl.
No.: |
05/059,383 |
Filed: |
July 30, 1970 |
Current U.S.
Class: |
428/85; 28/274;
57/31; 57/248; 57/260; 57/333; 57/907; 428/401; 428/17 |
Current CPC
Class: |
D01D
5/423 (20130101); Y10T 428/298 (20150115); Y10S
57/907 (20130101) |
Current International
Class: |
D01D
5/42 (20060101); D01D 5/00 (20060101); D02g
003/06 (); D02g 003/22 (); D02g 001/16 () |
Field of
Search: |
;57/14R,157R,157F,167,151,155,34B ;28/DIG.1,1.4,72R
;161/168,169 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Petrakes; John
Claims
WHAT IS CLAIMED IS:
1. A continuous filament fibrillated yarn comprised of
random-length fibrils of a synthetic organic high polymer wherein:
the aspect ratio of cross sections of the fibrils is from about 2/1
to about 12/1, and the aspect ratios of the cross sections of the
fibrils range from about 0.5/1 to about 20/1, the fibrils in the
yarn exceeding 40 centimeters in length comprise at least 70
percent (by weight) of the yarn; the tenacity of the yarn is from
about 0.1 to about 10 grams per denier; the total denier of the
yarn is from about 30 to about 10,000, and the average denier per
fibril of the fibrils comprising the yarn is from about 0.5 to
about 60; the elongation of the yarn is from about 0.5 to about 75
percent; and the initial modulus of the yarn is from about 2 to
about 300.
2. The yarn of claim 1, wherein said yarn is essentially comprised
of polymer selected from the group consisting of poly(ethylene
terephthalate) polymer, poly(trimethylene terephthalate) polymer,
and poly(tetramethylene terephthalate) polymer; said yarn contains
less than 4 free fibril ends per centimeter.
3. The yarn of claim 2, wherein said polymer is poly(ethylene
terephthalate).
4. The yarn of claim 3, wherein said polymer has an intrinsic
viscosity of from about 0.4 to about 0.8; the average aspect ratio
of the yarn is from about 2.5 to about 7.0 and the average aspect
ratio of fibrils comprising the yarn is from about 3/1 to about
5/1; the tenacity of the yarn is from about 0.5 to about 7 grams
per denier; the elongation of the yarn is from about 1 to about 20
percent; the initial modulus of the yarn is from about 30 to about
200 grams per denier; the fibrils comprising the yarn have a
tenacity of from about 2 to abOut 6 grams per denier and an
elongation at break of from about 2 to about 25 percent; and the
boiling water shrinkage of said yarn is up to about 20 percent.
5. The yarn of claim 4, wherein said initial modulus is from about
50 to about 120 grams per denier and said boiling water shrinkage
is from about 5 to about 10 percent.
Description
This invention relates to a novel fibrillated yarn with unique
properties.
Fibrillation processes, wherein filamentary articles are produced
from longitudinally oriented fibrillatable synthetic polymeric
tapes or films, are well known to the art. To applicant's
knowledge, however, there is no prior art which describes a
fibrillated yarn similar to applicant's continuous filament
fibrillated yarn.
It is an object of this invention to provide an economical
continuous filament fibrillated yarn with good cover, handle, and
tensile properties. In accordance with this invention, there is
provided a continuous filament fibrillated yarn comprised of
random-length fibrils of a synthetic organic high polymer wherein:
the average width/thickness ratio of cross sections of the fibrils
(the "aspect ratio") is from about 2/1 to about 12/1, and the
aspect ratios of the cross sections of the fibrils range from about
0.5/1 to about 20/1; the fibrils in the yarn exceeding 40
centimeters in length comprise at least 70 percent (by weight) of
the yarn; the tenacity of the yarn is from about 0.1 to about 10
grams per denier; the total denier of the yarn is from about 30 to
about 10,000, and the average denier per fibril of the fibrils
comprising the yarn is from about 0.5 to about 60; the elongation
of the yarn is from about 0.5 to about 75 percent; and the initial
modulus of the yarn is from about 2 to about 300.
The yarn of applicant's invention has many unique advantages; a few
of these are listed below.
1. Applicant's fibrillated yarn, for any given polymer, has a
higher tenacity (particularly at zero twist) than other known
fibrillated film yarns, produced from the same polymer.
2. This yarn has a softer handle than an equivalent denier per
filament continuous filament yarn (which it resembles in
appearance). This characteristic is particularly obvious (and
advantageous) when the yarn is used as a carpet face yarn.
3. This yarn has a crisp, dry hand which is beneficial in cordage
applications.
4. Fabrics produced from fibrillated polyester yarn of this
invention have good cover, good "breathability" , excellent wrinkle
resistance (even without the use of a resin finish), and excellent
printability.
5. Fabrics produced from the fibrillated yarns of this invention
have a unique, desirable luster.
6. Fabrics produced from the fibrillated polyester yarns of this
invention show excellent resistance to dry heat degradation; gas
and ozone fading; mildew, moth larvae, and household insects;
mineral and organic acids, alcohols, bleaching agents, dry-cleaning
solvents, halogenated hydrocarbons, ketones, soap and synthetic
detergents, water (including sea water), weak acids, and weak
alkalies (most of these compounds have little or no effect on these
fabrics); perspiration (which has no significant effect upon the
strength of these fabrics); sunlight (no appreciable deterioration
or discoloration occurs); and the like.
7. The durability of the folded edge of draperies produced from the
fibrillated polyester yarn of this invention is very good.
8. The cover effect of the fibrillated polyester yarns of this
invention is greater than the cover effect of the same denier
round-cross-section filament yarn produced by the conventional
process.
9. The fabrics produced from the fibrillated polyester yarn of this
invention will withdraw from a flame; thus, they do not flash burn.
If ignition does take place, the molten fiber tends to drop off and
prevent propagation of the flame. 10. Textile processing of the
fibrillated yarn of this invention (such as twisting, coning,
quilling, warping, slashing, and weaving) can be carried out using
standard textile equipment. Dyeing procedures for said yarn are the
same as those used for regular filament yarn. Not only does
applicant's fibrillated yarn have the aforementioned unique,
advantageous combination of properties, but it is substantially
cheaper to make than regular filament yarn.
The fibrillated yarn of this invention is comprised of
random-length fibrils of a crystalline synthetic organic high
polymer, i.e., any polymer capable of possessing an appreciable
amount of crystallinity which will retain orientation on relaxation
after stretching. Thus, e.g., polymers such as polyethylene;
polypropylene; polybutene; polymethyl-3-butene; polystyrene;
polyamides such as polyhexamehtylene adipamide, poly (ethylene
sebacamide), poly(methylene bis-p-cyclohexyleneadipamide), and
polycaprolactam; acrylics such as polymethyl-methacrylate and
methyl methacrylate; polyethers such as polyoxymethylene;
halogenated polymers such as polyvinyl chloride, polyvinylidene
chloride, tetrafluoroethylene, hexafluoropropylene, and the like;
polyurethanes; cellulose esters of acetic acid, propionic acid,
butyric acid, and the like; polycarbonates; polyacetals; polyesters
of the formula
(wherein n is from 2 to about 10 and preferably is 2, 3, or 4 );
and the like, can be used to prepare the yarn of this invention.
Other materials such as delustrants, incompatible polymers, etc.,
may comprise the yarns of this invention. Thus the yarns of this
invention are "essentially comprised" of the polymers described,
i.e., at least 80 percent (by weight) of the yarn consists of one
or more of said polymers.
The fibrillated yarn of applicant's invention is virtually
indistinguishable in appearance from a continuous filament yarn.
This is largely due to the fact that the average width/thickness
ratio (the "aspect ratio") of cross sections of the fibrils
comprising applicant's novel yarn is from about 2/1to about 12/2,
and the aspect ratios of the cross sections of the fibrils range
from about 0.5/1 to about 20/1. The preferred yarn of applicant's
invention is essentially comprised of poly(ethylene terephthalate)
yarn, and the average aspect ratio of the fibrils of this yarn is
from about 3/1 to about 5/1, the aspect ratios of the cross
sections of the fibrils ranging from about 2.5/1 to about 7/1.
The tenacity of the fibrillated yarns of applicant's invention are
relatively high, ranging from about 0.1 to up to about 10 grams per
denier (as determined by a modified ASTM D 2256/69 test wherein the
strain rate is held at 100 percent). The most preferred embodiment,
poly(ethylene terephthalate) fibrillated yarn, has a tenacity of
from about 0.5 to about 7 grams per denier.
There are many long fibrils in the yarns of applicant's invention.
The fibrils exceeding 40 centimeters comprise at least 70 percent
(by weight) of these yarns.
The fibrillated yarns of this invention have a denier of from about
30 to about 10,000, and the average denier per fibril of the fibril
comprising the yarn is from about 0.5 to about 60. The elongation
of these yarns is from about 0.5 to about 75 percent, and the
initial modulus of these yarns is from about 2 to about 300.
Applicant's novel fibrillated yarns do not need to be twisted as do
some of the web-like "yarns" described in the prior art.
The preferred yarns of applicant's invention contain less than four
free fibril ends per centimeter and thus generally are not as hairy
as are the fibrillated products of the prior art; this property
contributes to the continuous yarn-like appearance of the yarns of
this invention. A free fibril end is a fibril which is unattached
on one end, proturdes from the yarn bundles, and is visible to the
naked eye.
The polymer from which the yarns of this invention are made should
have a sufficiently high molecular weight so that the polymer is
fiber forming. When fibrillated yarn essentially comprised of
poly(ethylene terephthalate) is made via the processes of this
invention, it is preferred that it be made from a polymer with an
intrinsic viscosity of from about 0.4 to about 0.8. Unrelaxed
poly(ethylene terephthalate) fibrillated yarns of this invention
made from polymer with an intrinsic viscosity of from about 0.4 to
about 0.8 preferably will have an initial modulus of from about 50
to about 120 grams per denier and a boiling water shrinkage of from
about 5 to about 10 percent. The poly(ethylene terephthalate) yarns
of this invention generally have an elongation of from about 1 to
about 20 percent, an initial modulus of from about 30 to about 200
grams per denier and a boiling water shrinkage of up to about 20
percent; fibrils comprising the poly(ethylene terephthalate) yarn
of this invention have a tenacity of from about 2 to about 6 grams
per denier, an elongation at break of from about 3 to about 25
percent, and a denier per fibril of from about 0.1 to about 60.
One process that the applicant has discovered for producing the
yarns of his invention (and which he believes to be patentable by
itself) relates to fibrillating a fibrillatable tape at a windup
speed of greater than about 500 feet per minute comprising the step
of subjecting said fibrillatable tape to the action of at least two
(and preferably four) fluid twisting means wherein the direction of
twist imparted to the tape is completely and shraply reversed
between adjacent twisting means and the tape is maintained under a
tension of from about 0.05 to about 0.2 grams per denier. This
process is a distinct improvement over prior art processes which
suffer from the disadvantage that they generally can only be
operated at relatively low "throughput speeds" and filament yarn
thus cannot be produced via them which can compete in price with
filament yarn produced by conventional processes. The throughput
speeds used in these processes are generally about 300 feet per
minute, and the maximum throughput speed which can be used in these
processes is about 500 feet per minute. "Throughput speed" is often
referred to as "windup speed" and is the speed at which the
fibrillated yarn is taken through the last fluid twisting means
and/or wound up.
In the aforementioned process it is preferred to work at throughput
speeds in excess of 1000 feet per minute. A suprising advantage of
this process is that the fibrillated yarn produced thereby has very
good uniformity even when very high throughput speeds are used.
This process is applicable to any fibrillatable tape, i.e. any tape
showing a readiness to split in the lateral direction (a tape
wherein the bonds in the lateral direction are weak when compared
to the bonds in the longitudinal direction). Various fibrillatable
tapes are disclosed, e.g., in U. S. Pat. Nos. 2,185,789; 3,214,899;
3,242,035; 3,323,978; and the like.
In this process the fibrillatable tape is subjected to the action
of at least two (and preferably four) fluid twisting means so that
the direction of twist imparted to the tape is completely reversed
between adjacent twisting means and there is substantially no
change in the longitudinal direction of movement of the tape
between successive twisting means.
FIG. 1 is a view in perspective of the fluid twister used in this
invention.
FIGS. 2 and 3 are views taken along lines 2--2 and 3--3 of FIG.
1.
The fluid twisting means known to the art may be used in
applicant's process. Thus, e.g., the fluid twisting means disclosed
in abandoned application Ser. No. 563,234 (filed July 6, 1966) may
be used. Thus, e.g., the fluid twisting means disclosed in U. S.
Pat. No. 2,515,299 (wherein air or water is supplied to a small,
cylindrical, receptacle having a central axial passage therethrough
through which the textile strand may pass freely, and twist is
imparted to the strand by a vortex of whirling fluid which rotates
about the axis of travel of the strand in direct contact therewith)
work well in applicant's invention. Thus, e.g., the apparatus shown
in FIGS. 1, 2, and 3 may be used in applicant's invention. This
apparatus is comprised of two cooperating opposite rotating
twisting means. Apparatus 10 is comprised to a U-shaped member with
co-axial bores 12 and 14 through the legs of the "U" and slots 16
and 18 which communicate with bores 12 and 14 respectively. Fluid
is supplied to manifold box 20 by connector 22 (which is supplied
with a pressurized fluid such as, e.g. water or air), and this
fluid then passes through fluid passageways 24 and 26 into bores 12
and 14 respectively. Said fluid passageways are essentially
tangential to bores 12 and 14 with axes in planes perpendicular to
the axis of bores 12 and 14, respectively. They are thus positioned
with respect to bores 12 and 14 so as to produce respectively
therein fluid vortices rotating in opposite directions.
In apparatus 10 because the axes of fluid passageways 24 and 26 lie
in a plane perpendicular to the axes of bores 12 and 14 the
vortices generated at the intersections of said passageways 24 and
26 with bores 12 and 14 respectively are propagated equally along
the axes of bores 12 and 14 from the points of vortex generation.
In another useful embodiment a preferential direction and intensity
of vortex propagation may be obtained by placing the axes of fluid
passageways 24 and 26 in planes intersecting the axes of bores 12
and 14 at angles which are other than perpendicular. In these
embodiments the twisting of the vortices not only fibrillate the
tape but also tension the tape in a preferred direction. It is
preferred that the planes in which the fluid passageways lie make
an angle of from 15 to 70 degrees to the axis of the bores. It is
more preferred that this angle be from 30 to 60 degrees and most
preferred that this angle be from 45 to 60 degrees.
In applicant's process it is preferred that the perimeter of the
tape in the yarn passageway be from about 4 to about 12
millimeters, the perimeter of the yarn passageway (which, in the
apparatus described above, would be bores 12 and 14) be from about
5 to about 20 millimeters, the perimeter of the air passageway
(which would be passageways 24 and 26 in the apparatus described
above) be from 1.25 to about 10 millimeters, and the ratio of the
tape perimeter/yarn passageway perimeter be from about 0.1 to 1.5
(and most preferably from about 0.3 to about 0.7). If the yarn
passageway and air passageway are cylindrical, it is preferred that
the ratio of the yarn passageway diameter/air passageway diameter
be from about 0.1 to about 0.7 (and most preferably from about 0.2
to about 0.5).
Any series of at least two (and preferably four) fluid twisting
means wherein the direction of twist imparted to the tape is
completely reversed between adjacent twisting means and there is
substantially no change in the longitudinal direction of movement
of the tape between successive twisting means will work well in
this process. The fluid used in said twisting means may be
virtually any gas which approaches ideal gas behavior and does not
react with the tape to be fibrillated. Thus, e.g., air, steam,
nitrogen, oxygen, carbon dioxide, etc., may be used in the process
of this invention; because it is one of the cheapest gasses, it is
preferred to use air as said fluid. In said twisting means the
fluid velocity should reach from about 0.5 to about 1.0 sonic
velocity at the point of contact with the strand.
The direction of twist imparted to the tape is reversed between
adjacent twisting means. Thus, e.g., if the fibrillatable tape is
passed through the apparatus shown in FIG. 1, it will have a
clockwise twist imparted to it in bore 12 and counter-clockwise
twist imparted to it in bore 14; the tape may then be subjected to
a third fluid twisting means wherein clockwise twist is imparted to
it and a fourth twisting means wherein counter-clockwise twist is
imparted to it.
It is preferred, for reasons of economy and efficiency, to have a
pair of twisting means embodied in the same apparatus. Such
apparatus are illustrated, e.g., in FIGS. 1, 2, and 3.
In each apparatus which is comprised of a pair of twisting means it
is preferred that the adjacent twisting means be no further than
about 3 inches apart so that the direction of twist will be sharply
reversed, and it is most preferred that said adjacent twisting
means be no further than about 1 inch apart. When four fluid
twisting means are used, the distance between each apparatus which
is comprised of two twisting means may be as great as is practical;
thus, e.g., two such apparatus may be from about 6 to about 1000
inches apart. It is preferred that the two adjacent apparatus, each
of which are comprised of two adjacent twisting means, be from
about 12 to about 500 inches apart, and it is more preferred that
they be from about 15 to about 72 inches apart. In the most
preferred embodiment, they are about 24 inches apart.
As the fibrillatable tape is being subjected to the action of at
least two fluid twisting means, it should be maintained under a
tension of from about 0.05 to about 0.2 grams per denier to insure
good fibrillation of the tape, although it is preferred to maintain
it at a tension of from about 0.05 to about 0.15 grams per denier,
and it is most preferred to maintain it at a tension of about 0.1
grams per denier. The tape may be maintained at the prescribed
tension by godet rolls or winding apparatus pulling the tape
through the fluid twisting means. Alternatively, if the passageways
of the twisting means are at an angle of from about 1 to about 89
degrees with respect to the axis of the passageway through which
the tape travels, the tape may be maintained under the prescribed
tension by the action of the fluid twisting means.
In the preferred embodiment air supplied to the fluid twisting
means will be under a pressure of from about 10 to about 250
p.s.i.g., although it is preferred that said pressure be from about
20 to about 100 p.s.i.g. and it is most preferred that said
pressure be from about 40 to about 80 p.s.i.g. When said preferred
pressure and the fluid twisting means shown in FIG. 3 are used in
the process of this invention, a poly(ethylene terephthalate) tape,
e.g., will have a twist of greater than 20,000 turns/minute
imparted to it.
Via this process from about 5 to about 300 fibrils per tape will be
produced, although it is preferred to adjust the operating
conditions of this invention so that from about 25 to about 200
fibrils per tape will be produced.
This process is applicable to any fibrillatable tape such as, e.g.,
fibrillatable tape essentially comprised of poly (ethylene
terephthalate), poly(trimethylene terephthalate), poly
(tetramethylene terephthalate), polypropylene, nylon, etc. Inasmuch
as a fibrillated film yarn produced from tape essentially comprised
of poly(ethylene terephthalate) has the desirable properties of
poly(ethylene terephthalate) yarn (such as high modulus,
susceptibility to texturing, etc.) and is cheaper and has better
aesthetic characteristics than yarn currently available, it is
preferred to apply this process to produce fibrillated yarn
comprised of poly(ethylene terephthalate).
Another process that the applicant has discovered (which may be
used together with applicant's "fluid twisting means process" but
can also be used with any fibrillating means), affords an
especially advantageous means of fibrillating poly(ethylene
terephthalate). It is very difficult to drew and fibrillate
poly(ethylene terephthalate) in accordance with the procedure the
art discloses for polypropylene fibrillation, for when this is done
a weak, non-uniform, commercially useless yarn is usually produced.
The following process solves this problem.
In this latter process a tape essentially comprised of polyester
with specified properties is fibrillated. The spun tape is from
about 0.0002 to about 0.0005 inches thick. The thickness of the
tape may be controlled by extruding a film and slitting a tape to
the required dimensions or by extruding a tape and controlling the
dimensions of the die through which it is extruded and/or the
quench height (the distance from the die face to the quenching
medium). It is preferred to extrude the tape through a slit die
which measures about 1 inch by from about 0.003 to about 0.015
inches and to have a quench height of from about 0.2 to about 2
inches, and it is most preferred to extrude the tape through a slit
die measuring about 1 inch .times. about 0.0006 inch and to use a
quench height of about 0.5 inches. Any quenching medium can be
used. The preferred quenching medium is water, and when it is used
the quench temperature (i.e., the temperature of the quench medium)
is about 0 to about 60 degrees centigrade, although it is preferred
that it be about 30 degrees centigrade. One may, alternatively,
quench on chill rollers, e.g.. The aforementioned parameters may be
varied to obtain the desired tape thickness of from about 0.0002 to
about 0.005 inches; any of the infinite combination of variables by
which one obtains the aforementioned tape thickness is within the
scope of applicant's discovery.
After said polyester tape is extruded and quenched, it may be dried
to a moisture content of less than about 2 percent (by weight of
tape), although when this step is employed it is preferred to dry
the tape to a moisture content of less than about 1 percent. Drying
should be used if a hot air drawing step is employed.
The tape used in this latter process may or may not be comprised of
from about 0.1 to about 25 percent (by weight of polyester) of
incompatible polymer. If incompatible polymer is used in said
latter process, it must be non reactive and be dispersed finely in
the polyester so that the average particle size of the dispersed
incompatible polymer is less than about 8 microns. POlymer selected
from the group consisting of polyethylene and polypropylene is the
preferred incompatible polymer, although other polymers, which can
be extruded with polyester without undergoing serious degradation
of themselves which adversely affect (e.g. degrade) the polyester,
may be used (e.g. nylon 6, nylon 6.6, polystyrene, etc.).
The most preferred incompatible polymer is polypropylene, and it is
preferred to use at least about 0.5 weight percent of it and
incorporate it into the tape. It is more preferred to use from
about 1 to about 3 percent of polypropylene, and it is most
preferred to use about 2 percent of polypropylene.
The mere addition of polypropylene in the latter process will not,
in and of itself, promote fibrillation: the polypropylene should be
finely dispersed throughout the poly(ethylene terephthalate) so
that the average size of the polypropylene particles therein is
less than about 8 microns, although it is preferred that they be
less than about 4 microns, and best results are obtained when they
are less than about 1 micron. Many methods well known to the art
may be used to obtain the required degree of dispersion.
One method applicant has used to obtain the required degree of
dispersion is to mix poly(ethylene terephthalate) and polypropylene
and extrude the mixture at a high temperature (e.g., about 285
.degree. centigrade) through a slit die. It is believed that, for
this method to work well, the viscosities of the poly(ethylene
terephthalate) and the polypropylene should be about equal.
Polypropylene is relatively non-newtonian, i.e., its viscosity is
dependent upon shear rate, whereas poly(ethylene terephthalate) is
nearly newtonian; thus it is believed that, with the use of the
proper conditions, at some stage during the extrusion process the
apparent viscosities of the two polymers will be matched. It is
believed that, in order to get good dispersion with this method,
the following conditions should exist; (1 ) the poly(ethylene
terephthalate) should have an intrinsic viscosity of from about
0.45 to about 0.75, although it is preferred that it has an
intrinsic viscosity of from about 0.61 to about 0.67; (2 ) the
polypropylene should have a melt flow index (as measured by ASTM
D-1238 62T, condition E or condition L) of from about 8 to about
22, although it is preferred that it have a melt flow index of
about 15; (3 ) a mixture comprised of from about 0.5 to about 5
percent of polypropylene (by weight of poly[ethylene
terephthalate]) and poly(ethylene terephthalate) should be
prepared; (4 ) this mixture should be extruded via a pack which
imposes a shear force of from about 60 to about 150 sec.sup.-.sup.1
for from about 1 to about 2 seconds; and (5 ) the extrusion
temperature should be from about 280 to about 300 degrees
centigrade, it being preferred to use an extrusion temperature of
about 285 degrees centigrade. Under these conditions good
dispersion of polypropylene results. It is to be understood that
this is merely one means of obtaining the desired degree of
dispersion, and any polyester tape comprised of the desired amount
of polypropylene with the desired degree of dispersion as well as
the process of using said tape to produce fibrillated polyester
yarn are within the scope of this invention.
This latter process, which utilizes the polyester tape described
hereinabove, can make yarn with denier of from about 30 to about
10,000; this yarn is useful for knitting, weaving and tufting.
The polyester tape applicant has discovered should, prior to the
time it is fibrillated, be subjected to a step which applicant has
found to be important for good fibrillation: it is hot drawn to a
draw ratio of from about 3.3 to about 4.2 while being subjected to
a temperature of from about 80 to about 140 degrees centigrade, and
thereafter it is subjected to a temperature of from about 120 to
about 230 degrees centigrade for from about 0.01 to about 0.2
seconds. It is preferred that the polyester tape be hot drawn to a
draw ratio of about 3.5 while it is being subjected to a
temperature of from about 80 to about 140 degrees centigrade for
from about 0.08 to about 0.8 seconds and that it thereafter be
subjected to a temperature of from about 200 to about 230 degrees
centigrade for from about 0.02 to about 0.1 seconds preferably by
passing it over a hot plate or a hot air oven, the use of the hot
plate being most preferred. The "residence time", the period of
time during which said tape is being hot drawn and subjected to a
temperature of from about 80 to about 140 degrees centigrade, is a
function of, e.g., the speed at which the process is being run; it
generally is from about 0.1 to about 1 second, and it most
preferably is from about 0.2 to about 0.4 seconds.
The polyester tape may be drawn in hot air at a preferred hot air
drawing temperature of from about 80 to about 150 degrees
centigrade, it being more preferred to use a hot air drawing
temperature of about 80 degrees centigrade; hot air drawing is the
preferred drawing method. Alternatively the polyester tape may be
drawn in hot water at a preferred hot water drawing temperature of
from about 80 to 100 degrees centigrade, it being more preferred to
use a hot water drawing temperature of about 90 degrees centigrade.
The temperatures described hereinabove are the temperatures of the
tape and not those of the drawing medium.
It is preferred that said polyester tape, after it has been
subjected to the aforementioned step of hot drawing it and
thereafter subjecting it to a temperature of from about 120 to
about 230 degrees centigrade, have been drawn to a total draw ratio
of from about 4 to about 5.5. Although the tape may be drawn to a
draw ratio of from about 5.5 in one stage, it is preferred that it
be so drawn in two stages. In the first stage, which corresponds to
the first part of the aforementioned step, the tape may be drawn to
a draw ratio of from about 3.3 to about 4.2 while being subjected
to a temperature of from about 80 to about 120 degrees centigrade
for from about 0.1 to about 1 second. In the second stage, which
corresponds to the second part of the aforementioned step, the tape
may be further drawn to increase the total draw ratio to from about
4 to about 5.5 while being subjected to a temperature of from about
120 to about 230 degrees centigrade for from about 0.02 to about
0.2 seconds.
The drawn tape can be fibrillated by any of the processes well
known to the art which will provide sufficient stress to fibrillate
it. Thus, e.g., the tape may be fibrillated as taught in British
Pat. 1,118,912 by contacting it with a roller having on its
periphery a plurality of grooves of equal pitch and cutting edges
of equal pitch disposed substantially in spiral form. Thus, e.g.,
the tape may be fibrillated as taught in U. S. Pat. No. 3,302,501
by passing it over a stationary brush or a similar shredding means
or, alternatively, by piercing the film through its thickness in a
plurality of points without shredding the film by, e.g., moving the
piercing means longitudinally or laterally through the film as it
is pierced. Thus, e.g., the tape may be fibrillated as taught in U.
S. Pat. No. 3,177,557 by passing it through a zone of high
turbulence provided by a high velocity jet of stream of air or
other gas.
It is preferred to fibrillate said poly(ethylene terephthalate)
tape by the "four fluid twisting means" process of this invention
wherein the tape is subjected to the action of at least four fluid
twisting means wherein the direction of twist imparted to the tape
is completely and sharply reversed between adjacent twisting means
and the tape is advanced from one fluid twisting means to another
while being maintained under a tension of from about 0.05 to about
0.2 grams per denier.
As was stated hereinabove, the latter process of this invention may
be advantageously used to fibrillate any fibrillatable tape. Thus,
e.g., it may be used to fibrillate poly(tetramethylene
terephthalate). Poly(tetramethylene terephthalate) tape can be
prepared in substantial accordance with the procedure described for
the preparation of poly(ethylene terephthalate) tape. The addition
of at least 0.5 percent of polypropylene (by weight) is not
essential to produce good fibrillation with poly(tetramethylene
terephthalate) tape, but said use of polypropylene is advantageous
in three respects: it makes the extruded poly(tetramethylene
terephthalate) film more stable and easier to process, it renders
said film slightly easier to fibrillate, and the fibrillated yarn
produced from said film is stronger than yarn produced from
poly(tetramethylene terephthalate) film which is not comprised of
polypropylene. Said poly(tetramethylene terephthalate), with or
without a minor amount of polypropylene, is extruded into a film or
tape which is uniaxially drawn to a draw ratio of from about 4.0 to
from about 6.0, although it is preferred to use a draw ratio of
about 5.0. The drawn film is then slit into the required denier,
which is generally from about 150 to about 600, and fibrillated in
accordance with the process of this invention. The yarn produced is
very similar to the poly(ethylene terephthalate) yarn produced via
the process of this invention.
In a typical process which may be used for the production of e.g.,
fibrillated poly(ethylene terephthalate) yarn, poly (ethylene
terephthalate) polymer and the required amount of polypropylene is
passed through an extruder, and through a tape die into a water
quench (alternatively, a chill roll may be used). Then it is wound
on a godet, passed through a hot air oven, wound over a second
godet, passed over a hot plate, passed over a third godet, and
subjected to the action of four fluid false twisting means in
apparatus. Thereafter the fibrillated yarn is wound by tension
controlled winders. Said typical process is only one of the many
which may utilize applicant's invention.
In order to better describe some of the preferred embodiments of
applicant's invention, the below mentioned examples are presented.
Unless otherwise mentioned, all parts are by weight and all
temperatures are in degrees centigrade.
In examples 1-4, a tape of the polymer under investigation was
prepared by extrusion and drawing under conditions which gave
favorable fibrillation at about 1000 feet per minute windup speed
with the process of this invention (four fluid twisting means).
This tape was then fibrillated over a range of speeds from 150 feet
per minute up to 2000 feet per minute in processes wherein it was
subjected to only two fluid twisting means and to four fluid
twisting means. A sample for each run was cross-sectioned (five
cross-sections for each sample at approximately 3 meter intervals),
and the number of fils was counted. The average of the five
cross-sections was then taken as the degree of fibrillation for a
sample.
In analyzing the results, the speed at which one need run the "two
twisting means" process with the "four twisting means" process was
compared. The results were averaged to reduce the degree of
uncertainty produced by the statistical variability of the fibril
count. In all runs the twisting means used was essentially the same
as that disclosed in FIGS. 3 and 4, wherein the apparatus disclosed
comprises 2 twisting means (and is referred to as a "jet" in these
Examples). When, e.g., other fluid twisting means, such as the
apparatus shown in FIGS. 1, 2a, and 2b, are used, similar results
are obtained.
EXAMPLE 1
Poly(ethylene terephthalate) with an intrinsic viscosity of 0.61
and 2 percent (by weight of polyethylene terephthalate) of
polypropylene with a melt flow index of 15 were mixed and then
subjected in a pack to a shear force of 120 sec.sup.-.sup.1 for
about 1 second and extruded via a pack through a slit die (which
was 1 inch .times. 0.0005 inch); the extrusion temperature was 280
degrees centigrade. The extruded tape was quenched in water (at a
quench height of 1.25 inch) and spun. The spun tape was 10 mm wide
and had a total spun denier of 3150. The spun tape was then drawn
in a first stage at a draw temperature of about 110 degrees
centigrade and a draw speed of 175 feet per minute to a draw ratio
of 3.5/1, and thereafter it was drawn in a second stage at a draw
temperature of about 200 degrees centigrade and a draw speed of 120
feet per minute to a draw ratio of 1.4/1.
This tape was then fibrillated with one "jet" (comprising two fluid
twisting means wherein the direction of twist imparted to the tape
is completely reversed between adjacent twisting means) and two
jets. The maximum speeds one could use to get any given degree of
fibrillation with one jet and two jets operated at the same
conditions (i.e., same as pressure and tension) are shown
below.
Number of Maximum speed one Maximum speed one Fils/Tape can use
with one can use with two jet to obtain the jets to obtain the
specified degree specified degree of fibrillation of ibrillation
(feet/minute) (feet/minute)
60 0 (i.e., at no 100 speed could the one jet give one this degree
of fibril- lation) 50 0 170 40 70 300 35 130 410 30 230 greater 600
than 25 500 greater 600 than
EXAMPLE 2
A poly(ethylene terephthalate) tape was prepared in substantial
accordance with the procedure described in Example 1, with the
exception that the first stage draw ratio was 3.6/1, the first
stage take up speed was 1080 feet per minute, the first stage draw
temperature was 127 degrees centigrade, the second stage draw
ration was 1.3/1, and the second stage take up speed was the same
speed as the fibrillation speed. The tape was comprised of
poly(ethylene terephthalate) with an intrinsic viscosity of 0.61
and 2 percent polypropylene with a melt flow index of 15.
This tape was then fibrillated with one jet and two jets. The
results are presented below.
Number of Maximum speed one Maximum speed one Fils/Tape can use
with one can use with two jet to obtain the jets to obtain the
specified degree specified degree of fibrillation of fibrillation
(feet/minute) (feet/minute) 50 0 300 45 75 450 40 225 650 35 400
1600 30 650 greater 2000 than
This example differs from Example 1 in that the tape was prepared
at much higher drawing speeds; this effect increases the
fibrillation for a given speed through the jets and at the higher
speeds make the fibrillation less sensitive to changes in
speed.
It was observed that the use of the two jets decrease the number of
large filaments, thus contributing to the uniformity of the yarn.
To quantify this observation the cross sections made for Example 2
were examined and the number of fils with a breadth to thickness
ratio greater than 6 were tabulated. On averaging, the following
results were obtained.
Wide Fil Count
(Average) 1 jet 2 jets Temp. of 140 4.5 2.2 Speed effect averaged
Hot Plate, 170 -- 2.2 .degree.C 200 -- 0.6 Speed 400 3.8 0.6
Temperature effects 800 4.0 1.6 average fpm 1200 3.8 2.0 1600 5.0
2.2 Overall average 3.7 1.5 Temp and speed effects Total
averaged
This experiment shows that the addition of the second jet is very
effective in reducing the number of wide fils. Another effective
method of reducing wide fils is to increase the hot plate
temperature to 200 degrees centigrade. With the use of two jets and
a hot plate temperature of 200 degrees centigrade, the incidence of
wide fils was almost eliminated.
EXAMPLE 3
In substantial accordance with Example 1, a nylon fibrillatable
tape comprised of 2 percent of polypropylene was prepared. The
nylon 6.6 had a relative viscosity of 40, and the polypropylene had
a melt flow index of 15. Total spun denier of the spun tape was
2000.
The term "relative viscosity" as employed in conjunction with the
nylon polymers may be defined as a measure of the ratio of the
viscosity of a solution of a given strength of the polyamide in a
given solvent to the viscosity of the solvent itself at the same
prescribed temperature. The relative viscosity values noted herein
utilize 90 percent by weight of aqueous formic acid as the solvent.
The efflux time t of an 8.4 percent by weight solution of the
polyamide in the formic acid solvent is determined and the ratio of
said viscosity to the efflux time t of the solvent itself is the
measure of relative viscosity as determined by the equation:
RV = t/t.degree.
The temperature employed for the determination of these viscosities
is 25 degrees centigrade.
The nylon tape was then fibrillated with one and two jets; the
results are shown below.
Number of Fils/ Maximum speed Maximum speed Tape (f.p.m., one jet)
(f.p.m., two jets) 50 75 250 45 150 325 28 750 1600 26 950 2500
EXAMPLE 4
In substantial accordance with Example 1, a tape comprised of
poly(tetramethylene terephthalate) with an intrinsic viscosity of
0.67 and 2 weight percent of polypropylene (with a melt flow index
of 15 ) was prepared. The term "intrinsic viscosity" as used with
reference to polyester polymers may be defined as the limit of the
ratio of solution viscosity to solvent viscosity taken from one 1
divided by the concentration of the polymer in solution as the
concentration approaches zero
units are in deciliters/gram. Measurements may be made of relative
viscosity (on an 8 percent solution polyester in orthochlorophenol)
and converted to intrinsic viscosity by an empirical formula. The
tape was 8 mm wide and had a total spun denier of 400. The draw
ration used was 5/1 and the draw speed was 1500 feet per minute.
The tape was fibrillated with one jet and two jets, and the results
are shown below.
Number of Maximum speed one Maximum speed one Fils/Tape can use
with one can use with two jet to obtain the jets to obtain the
specified degree specified degree of fibrillation of fibrillation
(feet/minute) (feet/minute) 90 0 375 80 200 550 60 550 1200 58 625
1500 56 700 2500
EXAMPLE 5
In substantial accordance with Example 1, a tape 9 mm wide of total
denier 3000 was extruded from a polymer mix of 2 percent
polypropylene (M. F. I. 15 ) and 98 percent poly (ethylene
terephthalate) (0.61 intrinsic viscosity). This tape was drawn into
hot air in two stages to a total draw ratio of 4.9/1. The drawn
tape was then fibrillated by passing it through one of the "jets"
disclosed in FIGS. 1, 2a, and 2b at a rate of 50 feet per minute
with an applied air pressure of 60 p.s.i.g. and a yarn tension of
75 grams. A fibrillated yarn with an average of 45 filaments was
obtained. The yarn was then passed through another such jet at a
rate of 200 feet per minute with an applied air pressure of 60
p.s.i.g. and a yarn tension of 50 grams. The yarn obtained had an
average of about 100 filaments per tape (as determined by a fibril
count of microscopically prepared cross-sections of the yarn). The
length/breadth distribution of the yarn, estimated from this
cross-section, was as follows:
Length/Breadth Ratio Percent Frequency 0- 1 1 1- 2 22 2- 3 27 3- 4
21 4- 5 16 5-6 10 6-7 3
The average length/breadth ratio is 3.2. The yarn, has a total
denier of 600 and an average denier per filament of about 6, has a
tenacity of 2.4 grams per denier, and an elongation of 12.5
percent. This yarn, as well as the other yarns described herein,
are useful in polyester shaped articles; more particularly, said
yarns are useful in textile fabrics and garments.
EXAMPLE 6
In substantial accordance with Example 5, an 800 denier drawn tape
was prepared and fibrillated through two of said jets at a rate of
100 feet per minute with a yarn tension of 50 grams and an air
pressure of 60 p.s.i.g. The yarn has an average of 68 filaments,
with an average length/breadth ratio of 4.3.
EXAMPLE 7
In substantial accordance with Example 5, a poly(ethylene
terephthalate) tape was drawn uniaxially in two stages to a total
draw ratio of 4.9; the dimensions of the drawn tape were
approximately 15 microns thick and 4.5 mm wide. The tape was
subjected to the action of two of the aforementioned jets at a rate
of 280 feet per minute with a yarn tension of 55 grams and an air
pressure of 40 p.s.i.g. The resulting fibrillated yarn had a
tenacity of 2.45 grams per denier, an elongation of 4.7 percent,
and an initial modulus of 84 grams per denier. On average, about 51
filaments could be counted at a cross-section of the yarn. From
microscopic examination the cross-section of an average filament
could be described as essentially rectangular and had an average
aspect ratio of 4.7/1. The total denier of the yarn was 684,with an
average denier per filament of 13.4. The yarn was very slightly
hairy in appearance.
This yarn was 4 ply twisted into a thick yarn and tufted, as a face
yarn, into a carpet. Tufting performance was exceptionally good
and, except for a pleasant sheen, performed similarly to continuous
filament carpets from which it was difficult to distinguish. It was
judged far superior to commercially available carpets of
fibrillated polypropylene.
EXAMPLE 8
In substantial accordance with Example 7, a poly(ethylene
terephthalate) tape was drawn to a draw ratio of 5.4; the tape was
4.5 mm wide and 16.5 microns thick. This tape was fibrillated by
passing it through 3 of the aforementioned jets at a speed of 232
feet per minute under a yarn tension of 60 grams with an applied
air pressure of 80 p.s.i.g. A fibrillated yarn was obtained with a
tenacity of 3.2 grams per denier, an elongation of 4.5 percent, and
initial modulus of 106 grams per denier. The yarn had an average of
71 filaments per tape. The average cross-section ratio was 3.1.
The continuous filament yarn was woven as filling yarn into a warp
of 70 denier polyester to give a fabric which would be suitable in
upholstery and drapery. After dyeing and heat setting, the fabric
had a soft and pleasant handle and exhibited good drape and a
pleasing and unusual surface sparkle.
EXAMPLE 9
In substantial accordance with Example 5, a poly(ethylene
terephthalate) tape was prepared which had a denier of 680 and a
film thickness of 15 microns. This tape was fibrillated by passing
it through two of the aforementioned jets at 285 feet per minute
under yarn tension of 55 grams with air pressure of 40 p.s.i.g.
being supplied to the jets. The tape fibrillated into a yarn
composed of an average 51 filaments, corresponding to an average
denier per filament of 13.4. The yarn had only three ends per
centimeter and a tenacity of 2.5 grams per denier. To produce
fibrillation of this quality with only one jet (comprised of only
two twisting means), it was necessary to lower the fibrillation
speed to 70 feet per minute.
EXAMPLE 10
In substantial accordance with Example 5, a poly(ethylene
terephthalate) tape was prepared and fibrillated through two of
said jets at a speed of 532 feet per minute under a yarn tension of
60 grams and with 80 p.s.i.g. of air pressure being furnished the
jets. The yarn produced was 393 denier, had 48 filaments and a
tenacity of 4.4 grams per denier, was comprised of very few broken
ends, and had an elongation of 6 percent and an initial modulus of
80 grams per denier.
This yarn was woven into a drapery fabric which had good drape,
soft hand, dyed uniformly, and had a pleasant, sparkly surface
effect. This yarn was also woven into a fabric suitable for
awnings, tents, etc., in which the fabric properties match or
surpass a similar fabric made from cotton.
EXAMPLE 11
Poly(tetramethylene terephthalate) polymer with a relative
viscosity of 37.5 was extruded at a temperature of 255 degrees
centigrade into a water quench to give a film 4.5 mm wide with a
denier of 1520. This tape was then drawn in hot air at a
temperature in excess of 80 degrees centigrade in two stages to a
total draw ratio of 5/1. The drawn tape was then fibrillated
through two jets similar to those shown in FIGS. 1, 2a, and 2b at a
speed of 50 feet per minute under a yarn tension of 50 grams with
an applied air pressure of 60 p.s.i.g. A fibrillated product was
obtained with an average filament count of 34 and an average dpf of
8.9. The filament cross-section is rectangular with the thin
dimension about 17 microns and the cross section range between 1/1
and 4.5/1 with about 70 percent of the filaments being in the 2.5/1
to 3/1 range. The yarn had an elongation of 12.6 percent, a
tenacity of 0.87 grams per denier, and an initial modulus of 12.0
grams per denier at 60 percent strain rate.
EXAMPLE 12
Poly(tetramethylene terephthalate) polymer with a relative
viscosity of 37.5 was blended with 3 weight/percent of
polypropylene (melt flow index 12) and extruded to give a film 7.5
mm wide with a denier of 4250 and a birefringence of 3.6.
The tape was drawn and fibrillated under the same conditions used
in Example 11. A fibrillated yarn was obtained with an average
filament count of 26, average denier per filament of 33, and very
few broken ends. The filament cross section was rectangular with
the thin dimension being 38 microns. The aspect ratio range is from
2/1 to 7/1. The surface of the filament was very smooth and in
appearance very like similarly processed poly(ethylene
terephthalate) yarns. The yarn had a tenacity of 2.0 grams per
denier, an elongation of 12 percent, and an initial modulus of 30
grams per denier at 60 percent strain rate.
It is preferred that the yarns of this invention be comprised of at
least 90 percent (by weight of yarn) of polymer selected from the
group consisting of poly(ethylene terephthalate), poly(trimethylene
terephthalate), poly(tetramethylene terephthalate), nylon, and
mixtures thereof. This invention comprehends combination yarns
wherein, e.g., one or more tapes are simultaneously fed to the
false twisting means and combined or where, e.g., fibrillated yarn
is combined with conventional filament or semicontinuous yarn. The
yarn of this invention may contain additional additives such as
dyes or colorants; delustrants such as titanium dioxide; or
particulate materials such as talc, china clay, or glass.
The tapes described in this invention have utility for, e.g., the
preparation of carpet backing materials. Furthermore, they can be
used as tufting materials for artificial grass constructions.
Although the above examples and descriptions of this invention have
been very specifically illustrated, many other modifications will
suggest themselves to those skilled in the art upon a reading of
this disclosure. These are intended to be comprehended within the
scope of this invention.
* * * * *