U.S. patent number 3,763,644 [Application Number 05/251,628] was granted by the patent office on 1973-10-09 for flame retardant textiles.
Invention is credited to William R. Darnell, Winston J. Jackson, Jr..
United States Patent |
3,763,644 |
Jackson, Jr. , et
al. |
October 9, 1973 |
FLAME RETARDANT TEXTILES
Abstract
Disclosed are textile yarns comprising a plurality of
antimony-containing fibers and a plurality of bromine-containing
fibers. The antimony-containing fibers are formed from a polymer
having an antimony-containing compound dispersed therein and the
bromine-containing fibers are formed from a polyester having a
bromine-containing compound dispersed therein. The textile yarns of
this invention exhibit an unobvious combination of commercially
acceptable mechanical properties and commercially acceptable flame
retardancy. Blends of the fibers used to prepare the yarn are also
disclosed. Fabrics of the yarn are also disclosed.
Inventors: |
Jackson, Jr.; Winston J.
(Kingsport, TN), Darnell; William R. (Weber City, VA) |
Family
ID: |
22952765 |
Appl.
No.: |
05/251,628 |
Filed: |
May 9, 1972 |
Current U.S.
Class: |
428/357; 57/255;
57/257; 57/904; 252/609; 428/359; 428/396; 428/412; 428/480;
428/921; 524/409; 524/519 |
Current CPC
Class: |
D02G
3/443 (20130101); D01F 1/10 (20130101); D01F
1/07 (20130101); Y10S 57/904 (20130101); Y10S
428/921 (20130101); Y10T 428/2904 (20150115); Y10T
428/2971 (20150115); Y10T 428/31786 (20150401); Y10T
428/29 (20150115); Y10T 428/31507 (20150401) |
Current International
Class: |
D02G
3/44 (20060101); D01F 1/02 (20060101); D01F
1/10 (20060101); D01F 1/07 (20060101); D02g
003/04 (); D02g 003/44 () |
Field of
Search: |
;57/14R,14BY
;161/169,172,403 ;264/211 ;252/8.1 ;260/75R,4R,41B,28.5A
;106/15 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Petrakes; John
Claims
We claim:
1. A textile yarn comprising
A. a plurality of antimony-containing fibers formed from a polymer
selected from the group consisting of polyesters, modacrylics,
regenerated cellulose, polyamides and cellulose acetate, the fibers
having uniformly dispersed throughout the fiber, based on the
weight of the antimony-containing fibers, from 0.1-20 weight
percent of an antimony-containing compound, and
B. a plurality of bromine-containing fibers formed from a
polyester, the fibers having uniformly dispersed throughout the
fiber, based on the weight of the bromine-containing fibers, from
1-50 weight percent of a bromine-containing compound having a
molecular weight of at least 500 and containing from 40-80 weight
percent bromine, based on the weight of the bromine-containing
compound.
2. The yarn of claim 1 wherein
the antimony-containing and bromine-containing fibers are formed
from a dicarboxylic acid component which is at least 80 mole
percent terephthalic acid and a glycol component which is at least
80 mole percent ethylene glycol, 1,4-butanediol, or
1.4-cyclohexanedimethanol.
3. The yarn of claim 2 wherein
the antimony-containing fibers contain from 0.5-5 weight percent of
the antimony-containing compound, and
the bromine-containing fibers contain 3-30 weight percent of the
bromine-containing compound.
4. The yarn of claim 2 wherein
the bromine-containing compound has a molecular weight of at least
2,000 and is a linear bromopolycarbonate wherein at least 50
percent of the recurring units in the polymer chain are connected
by ##SPC8##
linkages and at least 50 percent of the recurring units include the
structure ##SPC9##
5. The yarn of claim 4 wherein
substantially 100 percent of said recurring units include the
structure ##SPC10##
and substantially 100 percent of the recurring units in the
bromopolycarbonate chain are connected by ##SPC11##
linkages.
6. The yarn of claim 1 wherein
the bromine-containing compound is an addition polymer which
comprises at least 35 mole percent units of the structure
##SPC12##
7. A textile yarn comprising
A. a plurality of antimony-containing fibers formed from
poly(ethylene terephthalate) having uniformly dispersed throughout
the fiber from 1 to 4 weight percent antimony trioxide, based on
the weight of the antimony-containing fibers, and
B. a plurality of bromine-containing fibers formed from
poly(ethylene terephthalate) having uniformly dispersed throughout
the fiber 5-12 weight percent of a bromine-containing compound
selected from the group consisting of addition polymers having at
least 95 mole percent units derived from poly(tribromoneopentyl
acrylate) and linear bromopolycarbonates wherein substantially 100
percent of the recurring units include the structure ##SPC13##
and substantially 100 percent of the recurring units in the
bromopolycarbonate chain are connected by ##SPC14##
linkages.
8. A fiber blend comprising
A. a plurality of antimony-containing staple fibers formed from a
polymer selected from the group consisting of polyesters,
modacrylics, regenerated cellulose, polyamides and cellulose
acetate, the fibers having uniformly dispersed throughout the
fiber, based on the weight of the antimony-containing fibers, from
0.1-20 weight percent of an antimony-containing compound, and
B. a plurality of bromine-containing staple fibers formed from a
polyester, the fibers having uniformly dispersed throughout the
fiber, based on the weight of the bromine-containing fibers, from
1-50 weight percent of a bromine-containing compound having a
molecular weight of at least 500 and containing from 40-80 weight
percent bromine, based on the weight of the bromine-containing
compound.
9. The fiber blend of claim 8 wherein
the antimony-containing and bromine-containing fibers are formed
from a dicarboxylic acid component which is at least 80 mole
percent terephthalic acid and a glycol component which is at least
80 mole percent ethylene glycol, tetramethylene glycol or
1,4-cyclohexanedimethanol.
10. The fiber blend of claim 9 wherein
the antimony-containing fibers contain from 0.5-5 weight percent of
the antimony-containing compound, and the bromine-containing fibers
contain 3-30 weight percent of the bromine-containing compound.
11. The fiber blend of claim 9 wherein
the bromine-containing compound has a molecular weight of at least
2,000 and is a linear bromopolycarbonate wherein at least 50
percent of the recurring units in the polymer chain are connected
by ##SPC15##
linkages and at least 50 percent of the recurring units include the
structure ##SPC16##
12. The fiber blend of claim 11 wherein
the bromine-containing compound is an addition polymer which
comprises at least 35 mole percent units of the structure
##SPC17##
13. The fiber blend of claim 11 wherein substantially 100 percent
of said recurring units include the structure ##SPC18## and
substantially 100 percent of the recurring units in the
bromopolycarbonate chain are connected by ##SPC19##
linkages.
14. A fiber blend comprising
A. a plurality of antimony-containing fibers formed from
poly(ethylene terephthalate) having uniformly dispersed throughout
the fiber from 1 to 4 weight percent antimony trioxide, based on
the weight of the antimony-containing fibers, and
B. a plurality of bromine-containing fibers formed from
poly(ethylene terephthalate) having uniformly dispersed throughout
the fiber 5-12 weight percent of a bromine-containing compound
selected from the group consisting of addition polymers having at
least 95 mole percent units derived from poly(tribromoneopentyl
acrylate) and linear bromopolycarbonates wherein substantially 100
percent of the recurring units include the structure ##SPC20##
and substantially 100 percent of the recurring units in the
bromopolycarbonate chain are connected by ##SPC21##
linkages.
15. A textile fabric of the yarn of claim 1.
16. A textile fabric of the yarn of claim 7.
Description
This invention relates to a textile yarn of a plurality of
antimony-containing fibers and a plurality of bromine-containing
fibers. The textile yarn of this invention exhibits a combination
of mechanical properties and flame retardancy necessary in a
commercially acceptable textile yarn.
The use of synthetic textile yarns has increased tremendously over
the last several decades. Although a synthetic textile yarn may
have any number of desirable properties, every textile yarn must
have a number of necessary properties to make the fiber
commercially acceptable for typical applications such as wearing
apparel, carpets and the like. Historically, certain mechanical
properties have been necessary in order to make a yarn commercially
acceptable.
One undesirable property of most synthetic yarns is a lack of flame
retardancy. The growing significance of this property has now
caused many textile yarns to be regarded as commercially
unacceptable for many applications because of the lack of flame
retardancy, even though the textile yarns exhibit the mechanical
properties necessary for commercial acceptance. One particular and
significant instance where textile yarns must be flame retardant is
the children's sleepwear field where polyester/cotton blends enjoy
popularity. Therefore, to meet current standards for many
applications, the properties that have been historically necessary
for commercially acceptable textile yarns must be revised to
include at least a moderate degree of flame retardancy, and in some
cases a substantial degree of flame retardancy.
Efforts to produce polyester yarns which will meet many of the more
stringent standards of flame retardancy and still exhibit
mechanical properties necessary for commercial acceptance have
generally been unsatisfactory. The failure to produce the desired
yarn has not generally resulted from an inability to impart flame
retardancy to the yarn, but instead has resulted from an inability
of the yarn to exhibit a combination of the mechanical properties
historically necessary for commercial acceptance and a level of
flame retardancy suitable for current commercial acceptance.
Specifically, it is well known in the art that commercially
acceptable levels of flame retardancy can be achieved in a
polyester yarn by dispersing a bromine-containing compound and an
antimony-containing compound in the same fiber in the yarn.
Representative of this art are U. S. Pat. Nos. 3,419,518;
3,285,965; 3,347,822; 2,669,521 and 2,480,298, wherein it is
disclosed that a combination of antimony-containing compounds and
bromine-containing compounds are suitable for imparting flame
retardancy to yarns of polyesters. Commercially acceptable flame
retardancy in these yarns has been regarded to be a consequence of
the well-known phenomenon that when an antimony-containing compound
and a bromine-containing compound are dispersed in the same ploymer
they act synergistically and produce a yarn with an excellent level
of flame retardancy which is greater than the level of flame
retardancy that can be achieved through use of either of the
compounds by themselves. Thus, the prior art teaches that the
bromine-containing compound and the antimony-containing compound
must be in intimate contact within the same polymer matrix in order
for the synergistic effect to occur. Although polyester yarns of
fibers having both an antimony-containing compound and
bromine-containing compound dispersed in the same fiber exhibit
excellent commercially acceptable levels of flame retardancy, the
mechanical properties of the melt-spun yarns are, quite
unfortunately, commercially unacceptable.
Thus, in summary, the state of the art is that yarns with
commercially acceptable flame retardancy, but commercially
unacceptable mechanical properties, can be prepared by dispersing
in the same melt-spun polyester fiber of the yarn both an
antimony-containing compound and a bromine-containing compound.
We have now discovered a textile yarn that exhibits commercially
acceptable mechanical properties as well as a commercially
acceptable level of flame retardancy. In broad summary we have
achieved this result by forming a textile yarn of
A. a plurality of textile fibers that contain an
antimony-containing compound but do not contain a
bromine-containing compound, and
B. a plurality of textile fibers that contain a bromine-containing
compound but do not contain an antimony-containing compound.
Stated another way, we have discovered that, entirely contrary to
the teaching of the prior art, the antimony-containing compound and
the bromine-containing compound do not have to be in intimate
contact within a single polymer matrix for the above noted
synergistic effect to occur. Stated even more simply, in our
invention we put the antimony-containing compound in one fiber and
the bromine-containing compound in another fiber instead of putting
both compounds in one fiber as is taught by the prior art. Thus, we
have at least discovered a textile yarn that exhibits not only the
mechanical properties necessary for commercial acceptability, but
also exhibits a commercially acceptable level of flame
retardancy.
Accordingly, an advantage of the textile yarn of this invention is
a commercially acceptable level of flame retardancy.
Another advantage of the textile yarn of this invention is the
commercially acceptable mechanical properties.
Another advantage of the textile yarn of this invention is the
combination of commercially acceptable mechanical properties and
commercially acceptable flame retardancy.
Other advantages and features of this invention will be readily
apparent to those skilled in the art from the following description
and appended claims.
We have accomplished the remarkable objective of obtaining a
textile yarn that exhibits a desirable combination of mechanical
properties and flame retardancy necessary for commercial acceptance
by discovering a textile yarn broadly comprising
A. a plurality of antimony-containing fibers formed from a polymer
selected from the group consisting of polyesters, modacrylics,
regenerated cellulose, polyamides and cellulose acetate, the fibers
having uniformly dispersed through the fiber, based on the weight
of the antimony-containing fibers, from 0.1-20 weight percent of an
antimony-containing compound, and
B. a plurality of bromine-containing fibers formed from a
polyester, the fibers having uniformly dispersed throughout the
fiber, based on the weight of the bromine-containing fibers, from
1-50 weight percent of a bromine-containing compound having a
molecular weight of at least 500 and containing from 40-80 weight
percent bromine, based on the weight of the bromine-containing
compound.
In this disclosure the term "antimony-containing fiber", and terms
of similar import, is defined to mean a fiber that contains an
antimony-containing compound, and optionally other materials, but
does not contain a bromine-containing compound, except perhaps in
very minute trace, or impurity amounts. Thus, because the
antimony-containing fiber of this invention does not contain a
bromine-containing compound, applicants regard the
antimony-containing fiber of their invention as literally
distinguishable over the prior art disclosing a single fiber that
contains both an antimony-containing compound and a
bromine-containing compound.
In this disclosure the term "bromine-containing fiber", and terms
of similar import, is defined to mean a fiber that contains a
bromine-containing compound, and optionally other materials, but
does not contain an antimony-containing compound, except perhaps in
very minute trace, or impurtiy amounts. Thus, because the
bromine-containing fiber of this invention does not contain an
antimony-containing compound, applicants regard the
bromine-containing fiber of their invention as literally
distinguishable over the prior art disclosing a single fiber that
contains both an antimony-containing compound and a
bromine-containing compound.
As noted above, one desirable characteristic of the textile yarns
of this invention is their mechanical properties. More
specifically, the mechanical properties of the fibers of the
textile yarns of this invention, such as tenacity, elongation and
modulus, are quite similar to a yarn of fibers containing no
additives or only an antimony-containing compound or,
alternatively, only a bromine-containing compound. In contrast
however, the mechanical properties of the yarn of this invention
are quite superior to a yarn wherein the fibers contain both an
antimony-containing compound and a bromine-containing compound in
the same fiber. In one embodiment of this invention the toughness
is more than 30 percent geater, and in another embodiment is more
than 50 percent greater, than a control yarn of fibers having both
an antimony-containing compound and a bromine-containing compound
in the same fiber.
Another desirable characteristic of the textile fibers of this
invention is the excellent and commercially acceptable level of
flame retardancy. Typically, the levels of flame retardancy of the
yarns of this invention are equal to the levels of flame retardancy
of yarns containing both a bromine-containing compound and an
antimony-containing compound in the same fiber. In one embodiment
of this invention textile fabrics of the yarn of this invention
pass the Children's Sleepwear test (DOC FF 3-71).
According to this invention the antimony-containing fibers are
formed from a polymer selected from the group consisting of
polyesters, modacrylics, regenerated cellulose, polyamides and
cellulose acetate. The bromine-containing fibers are formed from a
polyester.
The polyesters of this invention can be prepared from one or more
aliphatic, alicyclic, or aromatic diols containing from two to 40
carbon atoms and one or more aromatic, alicyclic or aliphatic
dicarboxylic acids containing from two to 40 carbon atoms. In one
preferred embodiment the antimony-containing fibers are formed from
a polyester of a dicarboxylic acid component which is at least 80
mole percent terephthalic acid and a glycol component which is at
least 80 mole percent ethylene glycol, 1,4-butanediol, or
1,4-cyclohexanedimethanol. In one especially preferred embodiment
the antimony-containing fibers are formed from poly(ethylene
terephthalate).
In this invention the antimony-containing fibers have uniformly
dispersed throughout the fiber, based on the weight of the
antimony-containing fibers, from 0.1-20 weight percent of an
antimony-containing compound. Although many types of
antimony-containing compounds are suitable for use in this
invention, antimony trioxide is especially preferred due to its
availability and effectiveness. In another embodiment, the
antimony-containing fibers can contain from 0.5-5 weight percent of
the antimony-containing compound, based on the weight of the
antimony-containing fiber, and in one still further embodiment the
antimony-containing fiber can contain 1 to 4 weight percent
antimony-containing compound, based on the weight of the
antimony-containing fibers.
In this invention the bromine-containing fibers have uniformly
dispersed throughout the fiber, based on the weight of the
bromine-containing fibers, from 1-50 percent of the
bromine-containing compound which has a molecular weight of at
least 500 and containing from 40-80 weight percent bromine, based
on the weight of the bromine-containing compound. In another
embodiment the bromine-containing fibers contain 3-30 weight
percent of the bromine-containing compound.
In one still further embodiment the bromine-containing compound is
an addition polymer which comprises at least 35 mole percent
poly(tribromoneopentyl acrylate) having units of the structure
##SPC1##
This compound is well known in the art and described in U. S. Pat.
No. 3,165,502. In another aspect of this embodiment the plurality
of bromine-containing fibers are formed from poly(ethylene
terephthalate) having uniformly dispersed throughout the fiber 5-12
weight percent of a bromine-containing compound selected from the
group consisting of addition polymers having at least 95 mole
percent units derived from poly (tribromoneopentyl acrylate) having
the above noted units.
In one still further embodiment, the bromine-containing compound
has a molecular weight of at least 2,000 and is a linear
bromopolycarbonate wherein at least 50 percent of the recurring
units in the polymer chain are connected by ##SPC2##
linkages and at least 50 percent of the recurring units include the
structure ##SPC3##
In another aspect of this embodiment substantially 100 percent of
the recurring units include the structure. ##SPC4##
and substantially 100 percent of the recurring units in the
bromopolycarbonate chain are connected by ##SPC5##
linkages. In a specific aspect of this embodiment the plurality of
bromine-containing fibers are formed from poly(ethylene
terephthalate) and have uniformly dispersed throughout the fiber
5-12 weight percent of a linear bromopolycarbonate wherein
substantially 100 percent of the recurring units include the
structure ##SPC6##
and substantially 100 percent of the recurring units in the
bromocarbonate chain are connected by ##SPC7##
linkages.
In another aspect this invention comprises a blend of the fibers
used to prepare the yarns of this invention. Although the fibers of
the blend can be either staple or continuous filament, staple is
preferred because of the ease of blending the antimony-containing
fibers and the bromine-containing fibers. In one approach the
blending of the fibers can be accomplished by a producer of both
the antimony-containing fiber and bromine-containing fiber and the
blend can then be sold to customers of the fiber manufacturer. In
another approach the customer of the fiber manufacturer can buy
antimony-containing fiber and bromine-containing fiber separately
and accomplish blending prior to spinning the fibers into yarn. In
another aspect of this invention the blends of staple fibers are
not spun into yarns but can be used in typical non-woven
applications such as fiberfill for pillows and blankets and
preparation of non-woven textile goods.
Textile fabrics of the yarn of this invention are also within the
scope of this invention.
The antimony-containing compound and bromine-containing compound
can be incorporated into the polymer melt before melt spinning by a
variety of means well known to the art, such as admixing the
compound with the melted polymer or slurrying a solution of the
compound with polymer powder and evaporating off the solvent.
The textile fibers used to prepare the yarn of this invention can
be spun by conventional spinning techniques such as melt spinning.
The fibers can then be drawn, crimped, heat-set and prepared into
yarn by conventional procedures. A conventional
phosphorus-containing stabilizer, such as tri(2-ethylhexyl)
phosphate, may be added to limit the thermal degradation of the
polyester during melt spinning. To reduce the spinning temperature
of high melting polyesters, a processing aid also may be blended
with the bromine-containing compound and polyester if desired. The
processing aid can consist of an aromatic compound which boils
above 300.degree.C., preferably above 350.degree.C., and is
compatible with the polyester. Examples include triphenyl
phosphate, tricresyl phosphate, tri(chlorophenyl) phosphate,
chlorinated biphenyls containing 35-70 percent chlorine,
chlorinated diphenyl ether containing 35-70 percent chlorine,
chlorinated terphenyls containing 0-70 percent chlorine, terphenyl,
benzophenone, triphenylmethane, dioctyl phthalate, and diphenyl
sulfone. The preferred processing aids are those which contain
phosphorus or halogen atoms and, therefore, contribute to the flame
resistance, e.g., triaryl phosphates and chlorinated aromatic
hydrocarbons containing 35-70 percent chlorine. The polyester
fibers may contain 5-30 percent by weight of the processing
aid.
The polymers of this invention are well known in the art and can be
formed according to conventional well known polymerization
techniques.
The polyesters of this invention have an inherent viscosity of at
least 0.5, measured at 25.degree.C. using 0.23 grams of polymer per
100 ml. of a solvent composed of 60 volumes of phenol and 40
volumes of tetrachloroethane.
The following examples are intended to illustrate but not limit the
invention.
The children's sleepwear test referred to in these examples is
carried out as described in "Standard for the Flammability of
Children's Sleepwear" (DOC FF 3-71). Briefly, in the test five or
more conditioned specimens, 3.5 .times. 10 in., are suspended one
at a time vertically in holders in a prescribed cabinet and ignited
for 3 seconds using a standard flame along their bottom edge. Each
specimen contains an overlap seam (three plies) one-half in. wide
which runs the length of the specimen. The overlap seam is sewed
with two rows of conventional silicone lubricated polyester thread
spaced three-eighths in. apart. To pass the test, no specimen shall
be completely consumed, the average char length of the specimens
must be less than 7.0 in., and no burning fragments from any
specimen shall be present on the floor of the test cabinet more
than ten seconds after the removal of the ignition flame.
The oxygen index test is described in MODERN PLASTICS, March, 1970,
p. 124 and can be broadly described as the minimal volume percent
of oxygen in a slowly rising oxygen/nitrogen atmosphere that will
sustain the candle-like burning of the fabric when the fabric is
ignited at the top. To prevent dripping, pieces of knitted fabrics
are sewed with three vertical rows one-fourth in. apart of
double-stitched glass threads and clamped at the edges in a frame.
The oxygen index is a convenient, reproducible, numerical measure
of polymer flammability.
EXAMPLE 1
This example illustrates the commercially unacceptable mechanical
properties and commercially acceptable flame retardancy of yarns of
poly(ethylene terephthalate) fibers of the prior art which contain
both an antimony-containing compound and a bromine-containing
compound intimately dispersed in the same polyester fiber.
Into a drum are placed a quantity of poly(tribromoneopentyl
acrylate) I.V. 0.60, and, based on the total weight, a sufficient
quantity of poly(tribromoneopentyl acrylate) to comprise 6 weight
percent, and a sufficient quantity of antimony trioxide to comprise
1.5 weight percent. The drum is then placed on parallel rolls and
rolled for several hours to facilitate mixing. The physical mixture
is then dried in a vacuum oven at 95.degree.C. overnight and melt
extruded at 273.degree.C. into one-eighth inch rods and pelletized.
The pellets are then dried under vacuum at 110.degree.C. and melt
spun at 280.degree.C. The fibers are too brittle to draft
satisfactorily, thus indicating that the mechanical properties of
the fibers are commercially unacceptable. A sock is knitted from
the undrafted fibers, and scoured. When the children's sleepwear
test is carried out on the sock, it passes the test.
Similar results are obtained when other bromine-containing
compounds, such as brominated terphenyls, and other polyesters,
such as poly (1,4-cyclohexylenedimethylene terephthalate), are
used.
Thus, applicants have illustrated that yarns of polyester fibers
wherein both a bromine-containing compound and an
antimony-containing compound are intimately dispersed in the same
fiber exhibit commercially unacceptable mechanical properties, but
exhibit commercially acceptable flame retardancy.
EXAMPLE 2
This example illustrates the commercially acceptable mechanical
properties and the commercially acceptable flame retardancy of
yarns of this invention comprised of a plurality of poly(ethylene
terephthalate) fibers having a bromine-containing compound, but no
antimony-containing compound, dispersed therein, and a plurality of
poly(ethylene terephthalate) fibers having an antimony-containing
compound, but no bromine-containing compound, dispersed
therein.
Two ends of poly(ethylene terephthalate) fibers containing 8 wt.
percent poly(tribromoneopentyl acrylate) (68 filaments and 166
denier) and two ends of poly(ethylene terephthalate) fibers
containing 3 wt. percent antimony trioxide (68 filaments and 162
denier) are plied to give 136 filaments and 328 denier. The
resulting plied fiber contains overall 4 wt. percent
poly(tribromoneopentyl acrylate) and 1.5 wt. percent antimony
trioxide. The 328 denier, plied fibers are knitted into a jersey
knit sock (8 oz/yd..sup.2), scoured, and tested according to the
children's sleepwear test. The sock passes the test.
The fibers of the yarn have the following commercially acceptable
properties: tenacity 4 g./denier, elongation 25 percent and elastic
modulus of 48 g./denier.
Socks of only the poly(ethylene terephthalate) fibers containing 4
wt. percent poly(tribromoneopentyl acrylate) fail the children's
sleepwear test. Socks of only the poly(ethylene terephthalate)
fibers containing antimony trioxide fail the children's sleepwear
test.
These results illustrate that, very surprisingly, a synergistic
effect obtains between an antimony-containing compound and a
bromine-containing compound in poly(ethylene terephthalate), even
though the antimony-containing compound and brominated-containing
compound are not present in the same fibers but are in separate
fibers.
A similar synergistic effect obtains when other bromine-containing
compounds, other antimony-containing compound and other polyesters,
such as poly(tetramethylene terephthalate) and
poly(1,4-cyclohexylenedimethylene terephthalate), are used. Also,
similar synergistic results are obtained when the polymer of the
antimony-containing fiber is modacrylic, regenerated cellulose,
polyamide or cellulose acetate. Of course the exact levels of
antimony-containing compound and bromine-containing compound
necessary to achieve any specific level of flame retardancy would
vary depending on the specific polymer, specific
antimony-containing compound and specific bromine-containing
compound selected.
Thus, applicants have demonstrated that yarns comprised of a
plurality of polyester fibers having a bromine-containing compound,
but no antimony-containing compound dispersed therein, and a
plurality of polyester fibers having an antimony-containing
compound, but no bromine-containing compound, dispersed therein,
exhibit commercially acceptable mechanical properties and
commercially acceptable flame retardancy.
Stated another way, applicants have demonstrated that quite
unobviously, commercially acceptable flame retardancy can be
achieved due to a synergistic effect that obtains when the
bromine-containing compound and the antimony-containing compound
are dispersed in different fibers in the same yarn.
EXAMPLE 3
This example also illustrates the commercially acceptable
mechanical properties and the commercially acceptable flame
retardancy of yarns of this invention.
Two ends of poly(ethylene terephthalate) fibers (68 filaments and
170 denier) containing 8 wt. percent brominated terphenyl (75
percent bromine) and two ends of poly(ethylene terephthalate)
fibers (68 filaments and 162 denier) containing 3 wt. percent
antimony trioxide are plied and knitted into a jersey knit sock (8
oz./yd..sup.2). Overall, the sock contains 4 wt. percent brominated
terphenyl and 1.5 wt. percent antimony trioxide. The mechanical
properties of the yarn are commercially acceptable. When the
children's sleepwear test is carried out on the sock, it passes the
test. Socks of the poly(ethylene terephthalate) fibers containing
only 4 wt. percent brominated terphenyl or only antimony trioxide
fail the children's sleepwear test.
These results further illustrate that, very surprisingly, a
synergistic effect obtains beteen an antimony-containing compound
and a bromine-containing compound in poly(ethylene terephthalate),
even though the antimony-containing compound and bromine-containing
compound are not present in the same fibers but are in separate
fibers.
Thus, applicants have again demonstrated that yarns comprised of a
plurality of polyester fibers having a bromine-containing compound,
but no antimony-containing compound dispersed therein, and a
plurality of polyester fibers having an antimony-containing
compound, but no bromine-containing compound, dispersed therein,
exhibit commercially acceptable mechanical properties and
commercially acceptable flame retardancy.
EXAMPLE 4
This example also illustrates the commercially acceptable
mechanical properties and the commercially acceptable flame
retardancy of yarns of this invention.
Two ends (178 denier) of a
poly(1,4-cyclohexylenedimethyleneterephthalate) fiber containing 15
wt. percent bis(pentabromophenyl)ether and one end (92 denier) of a
poly(1,4-cyclohexylenedimethylene terephthalate) fiber containing 5
wt. percent of a fused 70/30 mixture of antimony
trioxide/monosodium phosphate are plied to give 270 denier/15
filaments. The overall composition of the fibers is
poly(1,4-cyclohexylenedimethylene terephthalate) containing 10 wt.
percent bis(pentabromophenyl)ether and 1.7 wt. percent of the fused
70/30 mixture of antimony trioxide/monosodium phosphate. The plied
fibers are then knitted into a sock, scoured, and dried. The oxygen
index of the sock is 22.6. The mechanical properties of the yarn
are commercially acceptable.
These results offer still further illustration that, very
surprisingly, a synergistic effect obtains between an
antimony-containing compound and a bromine-containing compound in
poly(1,4-cyclohexylenedimethylene terephthalate) even though the
antimony-containing compound and bromine-containing compound are
not present in the same fibers but are in separate fibers.
EXAMPLE 5
This example further illustrates the commercially acceptable
mechanical properties and the commercially acceptable flame
retardancy of yarns of this invention.
One end (176 denier/30 filaments) of a poly(tetramethylene
terephthalate) fiber containing 20 wt. percent
tris[2,2-bis(bromomethyl)-3-bromopropyl] phosphate is plied with
one end (153 den./30 filaments) of a poly(tetramethylene
terephthalate) fiber containing 3 wt. percent antimony trioxide and
knitted into a sock. The overall composition of the sock is
poly(tetramethylene terephthalate) containing 10 wt. percent
tris[2,2-bis(bromomethyl)-3-bromopropyl] phosphate and 1.5 percent
antimony trioxide. The sock is scoured and its oxygen index is
determined to be 25.4. The mechanical properties of the yarn are
commercially acceptable.
These results offer still further illustration of the synergistic
effect that obtains in the yarns of this invention.
EXAMPLE 6
This example also illustrates the commercially acceptable
mechanical properties and the commercially acceptable flame
retardancy of yarns of this invention.
In the compositions listed below, FR polyester is poly(ethylene
terephthalate) fibers containing 12 wt. percent
poly[2,2-bis(bromomethyl)trimethylene carbonate]. Using plied yarn
blends, knit socks having the following compositions are
prepared:
a. 50 percent viscose rayon containing 5 wt. percent antimony
trioxide and 20 percent of mixed propoxyphosphazenes (preparation
described in Ind. Eng. Chem. Prod. Res. Develop., 9, No. 4, 426
(1970l )). 50 percent FR polyester.
b. 35 percent cellulose acetate containing 8 percent
tris(2,3-dibromopropyl) phosphate and 2 percent antimony trioxide.
65 percent FR polyester.
c. 30 percent of a modacrylic fiber containing 82.3 wt. percent of
the polymer prepared from 2 moles of acrylonitrile and 1 mole of
vinylidene chloride, 15.7 wt. percent poly(N-isopropyl acrylamide),
and 2 wt. percent antimony trioxide. 70 percent FR polyester.
d. 20 percent nylon 6 fibers containing 3 wt. percent antimony
trioxide. 80 percent FR polyester.
e. 50 percent poly(ethylene terephthalate) containing 3 wt. percent
antimony trioxide. 50 percent FR polyester.
Mechanical properties of these yarns are commercially acceptable.
Flammability characteristics of the yarns are similar to yarns
wherein the antimony-containing compound and bromine-containing
compound are in the same fiber.
The invention has been described in detail with particular
reference to preferred embodiments thereof, but it will be
understood that variations and modifications can be effected within
the spirit and scope of the invention.
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