U.S. patent application number 13/882588 was filed with the patent office on 2013-10-03 for flame retarded textile and process for coating textile.
The applicant listed for this patent is Sergei V. Levchik, Jeffrey Stowell. Invention is credited to Sergei V. Levchik, Jeffrey Stowell.
Application Number | 20130260626 13/882588 |
Document ID | / |
Family ID | 45003059 |
Filed Date | 2013-10-03 |
United States Patent
Application |
20130260626 |
Kind Code |
A1 |
Stowell; Jeffrey ; et
al. |
October 3, 2013 |
FLAME RETARDED TEXTILE AND PROCESS FOR COATING TEXTILE
Abstract
The present invention relates to solid phosphate ester, which
can be used as a flame retardant in treatments for textile
substrates. More specifically, the treatments for textiles
substrates can be used as flame retardant formulations for
application on textile fabrics while substantially maintaining the
desired characteristics (aesthetic or textural properties) of the
textile. The present invention thus further provides for articles
having these phosphate ester formulations applied thereon, and of
processes of applying them onto various textile substrates.
Inventors: |
Stowell; Jeffrey; (Wingdale,
NY) ; Levchik; Sergei V.; (Croton-on-Hudson,
NY) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
Stowell; Jeffrey
Levchik; Sergei V. |
Wingdale
Croton-on-Hudson |
NY
NY |
US
US |
|
|
Family ID: |
45003059 |
Appl. No.: |
13/882588 |
Filed: |
November 1, 2011 |
PCT Filed: |
November 1, 2011 |
PCT NO: |
PCT/US11/58768 |
371 Date: |
June 6, 2013 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
|
61410195 |
Nov 4, 2010 |
|
|
|
Current U.S.
Class: |
442/141 ;
427/430.1 |
Current CPC
Class: |
D06M 13/244 20130101;
D06M 13/282 20130101; D06M 2200/30 20130101; Y10T 442/2672
20150401; D06M 13/292 20130101 |
Class at
Publication: |
442/141 ;
427/430.1 |
International
Class: |
D06M 13/282 20060101
D06M013/282 |
Claims
1. A textile comprising a flame retardant effective amount of a
flame retardant additive composition comprising a phosphate ester
of the general formula (I): ##STR00004## wherein R.sup.1, R.sup.2,
R.sup.3 and R.sup.4 each independently is aryl, or arylalkyl each
independently containing up to about 30 carbon atoms, optionally
interrupted with heteroatoms, X is a divalent aryl or arylalkyl
group, containing up to about 20 carbon atoms, and n has an average
value of from about 1.0 to about 2.0.
2. The textile of claim 1 wherein each of R.sup.1, R.sup.2, R.sup.3
and R.sup.4 are phenyl, X is a divalent phenylene group, and n is
one.
3. The textile of claim 1, wherein the textile which contains the
flame retardant additive composition passes the NFPA 701 and MVSS
302 tests.
4. A process comprising applying a flame retardant effective amount
of a flame retardant additive composition comprising a phosphate
ester of the general formula (I): ##STR00005## wherein R.sup.1,
R.sup.2, R.sup.3 and R.sup.4 each independently is aryl, or
arylalkyl each independently containing up to about 30 carbon
atoms, optionally interrupted with heteroatoms, X is a divalent
aryl or arylalkyl group, containing up to about 20 carbon atoms,
and n has an average value of from about 1.0 to about 2.0, to a
textile substrate.
5. The process of claim 4 wherein each of R.sup.1, R.sup.2, R.sup.3
and R.sup.4 are phenyl, X is a divalent phenylene group, and n is
one.
6. The process of claim 4 wherein the step of applying comprises
contacting the textile substrate with the flame retardant additive
composition comprising the phosphate ester (I).
7. The process of claim 4 wherein the step of applying comprises
backcoating the textile substrate with the flame retardant additive
composition comprising the phosphate ester (I).
8. The process of claim 4 wherein the step of applying comprises
immersing the textile substrate in a flame retardant additive
composition comprising the phosphate ester (I).
9. The process of claim 6, further comprising, subsequent to said
contacting, heating the textile substrate.
10. An article comprising the textile of claim 1.
11. The article of claim 10 wherein the article is selected from
the group consisting of furniture, a drapery, a garment, linen, a
mattress, a carpet, a tent, a sleeping bag, a toy, a decorative
fabric, an upholstery, a wall fabric, a curtain, carpeting, a
technical textile and combinations thereof.
12. A dispersion of a flame retardant additive composition
comprising a phosphate ester of the general formula (I):
##STR00006## wherein R.sup.1, R.sup.2, R.sup.3 and R.sup.4 each
independently is aryl, or arylalkyl each independently containing
up to about 30 carbon atoms, optionally interrupted with
heteroatoms, X is a divalent aryl or arylalkyl group, containing up
to about 20 carbon atoms, and n has an average value of from about
1.0 to about 2.0; and, water.
13. A process of treating a textile comprising applying the
dispersion of claim 12 to a textile substrate.
14. A textile that has been treated by the process of claim 13.
15. An article comprising the textile of claim 14.
16. The article of claim 15 wherein the article is selected from
the group consisting of furniture, a drapery, a garment, linen, a
mattress, a carpet, a tent, a sleeping bag, a toy, a decorative
fabric, an upholstery, a wall fabric, a curtain, carpeting, a
technical textile and combinations thereof.
Description
FIELD OF THE INVENTION
[0001] The present invention relates to the field of flame
retardants (FRs) and, more particularly, to a flame retarded
textile and a process of making the same.
BACKGROUND OF INVENTION
[0002] Textiles are an essential part of everyday life and are
found, for example, in draperies, cloths, furniture and vehicle
upholsteries, padding, toys, packaging material and many more
applications. Consequently, textile flammability is of concern.
[0003] The flammability of fabrics is typically determined by the
nature of the fiber comprising the fabric. Fabric flammability also
depends on the fabric thickness and/or looseness.
[0004] Several approaches have been proposed heretofore for
retarding the flammability of flammable textiles:
[0005] One approach involves fiber copolymerization: several fiber
monomers are mixed and copolymerized, thus improving the properties
of a certain fiber (e.g., a flammable fiber) through the enhanced
properties of another fiber (e.g., a fire resistant fiber).
However, this technique is limited by the number of existing fibers
and their properties, and cannot be tailor-made for any substrate
or requirements. Furthermore, fiber types and fiber polymerization
types are not necessarily compatible, thus further limiting the
applicability of this technique. An additional disadvantage of this
approach is the high cost of the fire resistant fibers.
[0006] Another approach involves the introduction of flame
retardant (FR) in or on the fabric, using one of three
methodologies: [0007] (i) Chemical post treatment: the fabric is
treated with flame retardant chemicals after it has been produced,
either by coating the fabric, or by the introduction of the FR into
the fabric during the final dyeing process. The flame retardant can
be applied to the back of the fabric (termed "back-coating") or to
its front (termed "front-coating"), depending on the specific
fabric application. For example, for draperies, furniture
upholstering garments and linen, where the aesthetic appearance of
the front side of the fabric is most important, back-coating is
desired. Backcoating treatment transfers the flame retardant
properties of the FR from the back side of the fibers/fabric, where
the backcoating is located to the area on the front face of the
fibers/fabric where a possible ignition source would present
itself; [0008] (ii) Fiber-additive matrix (also termed
"compounding"): the FR is linked to the fiber during the melt
spinning process, such that a fiber-additive molten plastic matrix
is formed. This methodology has many drawbacks: (a) degradation of
the FR agent due to the high extrusion temperatures, (b) reaction
of the FR agent with the extruded fiber, and subsequent
modification of the fiber properties, such as fiber dyeability,
fiber processability or other physical properties of the fiber, and
(c) reaction of the FR agent with the various polymeric additives,
such as dyes or catalysts; and, [0009] (iii) Finishing of flame
retardant additive onto fabric surface either directly or using
finish chemicals (resins) which chemically link flame retardant to
the fabric. Disadvantages of this method are (a) usually finishes
can be applied to cotton fibers, but they are not able to be
effectively applied to synthetic fibers because of the absence of
the necessary functional groups with which they would have to react
in such an application, (b) some finishes use toxic chemicals like
formaldehyde containing resins which can release formaldehyde, and
(c) in some finishes gaseous ammonia is used as a curing agent.
[0010] Selecting the suitable flame retardant and the suitable
methodology for applying it to the fabric largely depends on the
specific textile substrate which has to be protected, e.g., the
protection of a garment, or the protection of an electrical
appliance will inherently pose different requirements and
restrictions of the flame retardant used.
[0011] When used in textiles, an applied flame retardant should be:
(a) compatible with the fabric, (b) non-damaging to the aesthetical
and textural properties of the fabric, (c) transparent, (d) light
stable, (e) resistant to extensive washing and cleaning, (f)
environmentally and physiologically safe, (g) of low toxic gas
emission, and (h) inexpensive. Above all, a flame retardant should
pass the standard flammability tests in the field.
[0012] Properties of the FR such as stability to UV light, heat,
water, detergents and air-pollutants, as well as chemical
stability, may be summed-up under the term "durability". The most
durable textiles are those which are inherently flame retardant, or
which contain reactive (chemically bound) flame retardants ((iii)
above). In the latter, the degree of durability depends on the
strength of the bonds between the flame retardant formulation and
the fiber. Additive (mixed) flame retardants ((ii) above), or
chemically applied flame retardants ((i) above) which are
water-soluble, are considered less durable. Furthermore, topically
applied FR agents ((i) above) are generally not as durable as those
which are incorporated into the fabric during the extrusion of the
fiber ((ii) above). Thus, the topically applied FR agent ((i)
above) may be washed off during the laundry cycle, and in these
cases the expensive and burdensome dry cleaning of the textile has
to be used.
[0013] Among the main families of flame-retardant chemicals are
halogenated flame retardants, primarily based on bromine and
chlorine and phosphorus flame retardants.
[0014] Bromine-containing compounds and bromine/antimony-containing
compounds have been long established as flame retardants,
especially in the field of backcoating applications, the success of
which is primarily dependent on their ability to function as
effective vapor-phase flame retardants.
[0015] The use of aromatic bromines as flame retardants for
textiles, however, suffers disadvantages including, for example,
high bromine content demand, high dry add-on and/or binder demand,
and a need to add compounds which enhance the flame retardancy. It
is extremely undesirable to apply on a textile a flame retardant
formulation in large amounts (also termed "high add-on") since high
additive concentrations on the dry fabric results in inferior
fabric properties, as well as increased cost of production. In
addition, application of the noted flame retardants on fabrics may
result in streak marks on dark fabrics, excessive dripping during
combustion of thermoplastic fibers, relatively high level of
smoldering and a general instability of the flame retardant
dispersion which may prevent a uniform application thereof on the
fabric. Further still, there has been a drive in the industry to
either in part or wholly replace these halogenated flame
retardants. Most of these drawbacks are inherent to the aromatic
bromine compounds currently in use.
[0016] In recent years there has been a significant effort made to
develop and commercialize phosphorus-based flame retardants in
textile coating formulations.
[0017] Ongoing research has therefore been conducted in order to
obtain flame-retardants with improved performance, which are less
detrimental to textile properties.
[0018] There is thus a widely recognized need for flame retardant
formulations devoid of the above limitations.
SUMMARY OF THE INVENTION
[0019] It is thus a purpose of this invention to provide a textile
comprising a flame retardant effective amount of a flame retardant
additive composition comprising a phosphate ester.
[0020] It is still another purpose of this invention to provide
stable dispersions or suspensions of the target solid phosphate
esters, or of mixtures thereof, thereby allowing the application of
these solid phosphate esters to substrates via an aqueous
application methodology commonly known to those skilled in the art
(e.g., knife, spray, foam, froth, pad, etc.).
[0021] It has been surprisingly found that a textile can be
rendered flame retardant with a solid phosphate ester.
[0022] In one embodiment herein there is provided a textile
comprising a flame retardant effective amount of a flame retardant
additive composition comprising a phosphate ester of the general
formula (I):
##STR00001##
wherein R.sup.1, R.sup.2, R.sup.3 and R.sup.4 each independently is
aryl, or arylalkyl each independently containing up to about 30
carbon atoms, optionally interrupted with heteroatoms, X is a
divalent aryl or arylalkyl group, containing up to about 20 carbon
atoms, and n has an average value of from about 1.0 to about
2.0.
[0023] In another embodiment herein there is provided a process
comprising applying a flame retardant effective amount of a flame
retardant additive composition comprising the above-identified
phosphate ester of the general formula (I) to a textile
substrate.
[0024] The term "fiber" as used hereinafter refers to a natural or
synthetic filament capable of being spun into a yarn or made into a
fabric.
[0025] The terms "fabric", "textile", "textile fabric" and "textile
substrate" are used herein interchangeably to describe a sheet
structure made from fibers.
[0026] Fabric durability, as it is commonly defined, is a fabric
meeting its performance standard after 5, 10 or 50 washes.
[0027] The term "carrier", as used herein, describes an inert
material with which the composition is mixed or formulated to
facilitate its application, or its storage, transport and/or
handling. The carrier can be, for example, an organic carrier
(e.g., alcohols, ketones, petroleum fractions, aromatic or
paraffinic hydrocarbons, chlorinated hydrocarbons, or liquefied
gases) or an aqueous carrier.
[0028] Since the flame retardant formulations described herein are
particularly useful for the treatment of textiles, the carrier is
preferably a textile acceptable carrier (e.g., water).
[0029] The term "textile acceptable carrier" as used herein refers
to an inert, preferably environmentally acceptable carrier, which
is not harmful to the textile.
[0030] As used herein, the term "flame retardant", describes a
compound, a composition or a formulation which is capable of
reducing or eliminating the tendency of a substance to sustain
combustion when exposed to a small match-like or candle-like
flame.
[0031] The "textile substrate" described herein can be a textile,
film, laminant or other similar treatable surface which has a
surface that can be beneficially coated (either wholly or
partially) with the flame retardant additive composition, which may
include interior surfaces of fibers of the textile as well as the
interior of textile fibers in the textile.
[0032] As is used herein, the term "flammable substrate" describes
a textile substrate that easily ignites when exposed to a small
flame. The flammability of different textile substrates or of
articles made of these textile substrates is typically tested and
determined according to flammability test methods. Representative
examples include the NFPA 701, MVSS 302 and BS5852, Part 1, a
standard test method for flammability of upholstered furniture.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0033] In one embodiment herein there is provided a textile
comprising a flame retardant effective amount of a flame retardant
additive composition comprising a phosphate ester of the general
formula (I):
##STR00002##
wherein R.sup.1, R.sup.2, R.sup.3 and R.sup.4 each independently is
aryl, or arylalkyl each independently containing up to about 30
carbon atoms, preferably up to 20 carbon atoms, most preferably up
to about 15 carbon atoms, optionally interrupted with heteroatoms,
the aryl group may be phenyl, cresyl, 2,6 xylenyl and the like, X
is a divalent aryl or arylalkyl group, such as a divalent aryl or
arylalkyl group containing up to about 20 carbon atoms, preferably
up to about 16 carbon atoms, and n has an average value of from
about 1.0 to about 2.0. Heteroatoms can comprise halogen, oxygen,
nitrogen and sulfur. In one embodiment each of R.sup.1, R.sup.2,
R.sup.3 and R.sup.4 are phenyl. In one embodiment X is a divalent
phenylene group, preferably X is a divalent phenylene group so that
the molecule of the general formula (I) is a hydroquinone
bisphosphate, e.g., hydroquinone bisdiphenyl phosphate. X can
comprise a divalent arylene group derived from a dihydric compound,
for example, resorcinol, bisphenol-A, 4,4'-biphenol and the
like.
[0034] In one embodiment herein, the solid phosphate ester is
hydroquinone bis-phosphate flame retardant having the structure of
formula (I), wherein preferably R.sup.1, R.sup.2, R.sup.3 and
R.sup.4 each independently is a phenyl group, preferably a phenyl
group of general formula (II):
##STR00003##
wherein each R independently is alkyl of 1 to 4 carbon atoms, each
Z independently is chlorine or bromine, p is 0 to 3 and q is 0 to 5
with the sum of p and q being 0 to 5 and n has an average value of
from about 1.0 to about 2.0, preferably from about 1.0 to less than
or equal to about 1.2, and more preferably from about 1.0 to about
1.1. A particularly preferred oligomeric bis-phosphate within
formula (I) above is hydroquinone bis(diphenyl phosphate), i.e.,
R.sup.1, R.sup.2, R.sup.3 and R.sup.4 are each phenyl.
[0035] In one embodiment herein the phosphate ester of the general
formula (I) is selected from the group consisting of hydroquinone
bis(diphenyl phosphate), resorcinol bis(di-2,6-xylyl phosphate),
4,4'-biphenol bis(2,6-xylenol phosphate); and, combinations of any
of the herein described phosphate esters.
[0036] In one embodiment the phosphate ester of the general formula
(I) is present in an amount of from about 10 to about 90,
specifically from about 20 to about 80 weight percent based on the
total weight of the flame retardant additive composition.
[0037] According to one aspect of the invention, the flame
retardant additive composition is in the form of a dispersion, e.g,
an aqueous dispersion. In one embodiment herein, the flame
retardant additive composition further comprises a carrier which
can be selected from the group consisting of an aqueous carrier, an
organic carrier and a combination thereof. Some non-limiting
examples of organic carriers are alcohols, ketones, petroleum
fractions, aromatic or paraffinic hydrocarbons, chlorinated
hydrocarbons, or liquefied gases. Preferably the carrier is an
aqueous carrier. More preferably the carrier is water. The amount
of carrier can vary greatly provided that the carrier provides for
a dispersion of the phosphate ester (I) which can be effectively
coated onto a textile substrate to provide for reduced flammability
of the textile. Generally the amount of carrier can be from about
20 to about 90 weight percent, most preferably from about 30 to
about 60 weight percent based on the total weight of the flame
retardant additive composition. It will be understood herein that
all ranges recited for phosphate ester, carrier and binder mean
that the flame retardant additive composition cannot contain more
than 100 weight percent of all of the components therein, and thus,
all ranges of weight percents being recited herein can be adjusted
accordingly if there is present binder and/or carrier as well as
other additional ingredients. In one embodiment the amount of
binder and/or carrier and any optional additional ingredients (e.g.
the endpoints of the herein recited ranges) will be adjusted
accordingly based on the amount of phosphate ester (I) present in
the flame retardant additive composition.
[0038] According to one embodiment herein, the flame retardant
additive composition further comprises a binding agent (also termed
herein interchangeably as a "binder"). The use of a binder is
utilized to improve adhesion of the molecules of the phosphate
ester, to the textile substrate.
[0039] A suitable binder can be selected depending on the specific
application. For example, different binders may be suitable to
attach the FR additive composition described herein to different
textiles. Preferably, when the flame retardant additive
compositions described herein are applied to the textile, the
binder is selected to be most suitable for use on the specific
textile being employed, i.e., it is selected to be both
non-damaging to the aesthetical and textural properties of the
fabric, and durable (to washing, drying, UV light etc.). The binder
used in the formulations described herein is also selected to be
compatible with the phosphate ester (I) and any additional
additives in the flame retardant additive composition.
[0040] The binder can thus be selected from a large variety of
materials, including, but not limited to, synthetic polymers, such
as styrene-butadiene (SBR) copolymers, carboxylated-SBR copolymers,
melamine resins, phenol-aldehyde resins, polyesters, polyamides,
polyureas, polyvinylidene chloride, polyvinyl chloride (PVC),
acrylic acid-methylmethacrylate copolymers, acetal copolymers,
polyurethanes, mixtures thereof and cross-linked versions thereof.
Preferably, the binding agent is selected from the group comprising
of an acrylate, a polyurethane, a polyvinyl chloride (PVC) and
combinations thereof. Most preferably, the binder used in the
formulations described herein is an acrylate.
[0041] Examples of acrylates that are suitable for use as binders
in the context of the present invention include, but are not
limited to, 2-phenoxyethylacrylate, propoxylated 2 neopentyl glycol
diacrylate, polyethylene glycol diacrylate, pentaerythritol
triacrylate, 2-(2-ethoxyethoxy)ethyl acrylate, butyl acrylate,
styrene acrylate copolymers, and others.
[0042] While the exact amount of binder used depends on the
phosphate ester (I) and concentration, as well as the textile
substrate onto which the flame retardant additive is applied, it
has been shown that in the case of various textile substrates, the
concentration of the binding agent in the flame retardant additive
compositions described herein can be low, i.e., lower than 30
weight percent of the total weight of the flame retardant additive
composition, preferably lower than 20 weight percent of the total
weight of the flame retardant additive composition and most
preferably less than 10 weight percent of the total weight of the
flame retardant additive composition.
[0043] According to a still further aspect of the invention, the
flame retardant additive composition further comprises at least one
additional ingredient selected from the group consisting of an
additional flame retardant, a smoldering suppressant, surface
active agent, a wetting agent, a dispersing agent, a suspending
agent, a thickening agent, a defoaming and/or antifoaming agent, a
preservative and/or a stabilizing agent, a pH buffer, an additional
solvent, a salt and, an oxide.
[0044] Examples of suitable optional additional flame retardants in
the flame retardant additive composition include at least one of
aromatic phosphates like triphenyl phosphate or alkylated triphenyl
phosphates, dicyandiamide, melamine, melamine salts like melamine
phosphate, melamine pyrophosphate, melamine polyphosphate and
melamine cyanurate.
[0045] Examples of suitable smoldering suppressants include, but
are not limited to urea, melamine and phosphate salts.
[0046] The surface active agents and/or wetting agents can be
nonionic and/or ionic (cationic or anionic) agents.
[0047] Examples of nonionic surface active and/or wetting agents
that are suitable for use in the context of the present invention
include, but are not limited to, polyoxyethylene (POE) alkyl
ethers, preferably NP-6 (Nonylphenol ethoxylate, 6 ethyleneoxide
units) such as DisperByk.RTM. 101.
[0048] Examples of anionic surface active and/or wetting agents
that are suitable for use in the context of the present invention
include, but are not limited to, free acids or organic phosphate
esters or the dioctyl ester of sodium sulfosuccinic acid.
[0049] Examples of dispersing agents and/or suspending agents
and/or thickening agents that are suitable for use in the context
of the present invention include, but are not limited to, acrylic
acids, acrylic acids ester copolymer neutralized sodium
polycarboxyl such as naphthalene sulfonic acid-formaldehyde
condensate sodium salt, alginates, cellulose derivatives and
xanthan. In one non-limiting embodiment the thickening agent is
carboxymethyl cellulose.
[0050] Examples of defoaming and/or antifoaming agents that are
suitable for use in the context of the present invention, include,
but are not limited to, mineral oil emulsions, natural oil
emulsions, and preferably are silicon oil emulsions, such as
AF-52..TM..
[0051] Examples of preserving and/or stabilizing agents that are
suitable for use in the context of the present invention, include,
but are not limited to, formaldehyde and alkyl hydroxy benzoates;
preferably the preserving or stabilizing agents is a mixture of
methyl and propyl hydroxy benzoates.
[0052] An optional additional solvent in the flame retardant
additive composition can comprise any one or more of the carriers
described above other than any initial carrier that is used in the
flame retardant additive composition.
[0053] The textile can be selected from the non-limiting group
consisting of synthetic textiles, natural textiles and blends
thereof. Non-limiting examples of textile substrates that can be
beneficially used in the context of the present invention include
wool, silk, cotton, linen, hemp, ramie, jute, acetate fabric,
acrylic fabric, latex, nylon, polyester, rayon, viscose, spandex,
metallic composite, carbon or carbonized composite, and any
combination thereof. Preferable non-limiting examples of textile
fabrics which were shown to be suitable for use in the context of
the present invention include, without limitation, cotton,
polyester, and combinations thereof.
[0054] The textile utilized according to embodiments of the present
invention may be used as a single layer or as part of a multi-layer
protective garment.
[0055] A textile of the invention herein may be incorporated in
various articles, where it is desired to reduce the flammability of
textiles used in such articles.
[0056] Exemplary articles according to the present invention
include any industrial product that comprises one or more textile,
film, laminant or other similar treatable substrates and hence
application of the FR additive composition described herein thereon
is beneficial. Preferably, some exemplary non-limiting articles
which comprise the textile containing the flame retardant additive
composition described herein include, without limitation,
furniture, toys, electrical appliances, a drapery, a garment,
linen, bedding, a mattress, a carpet, a tent, a sleeping bag, a
toy, a decorative fabric, an upholstery, a wall fabric and a
curtain. One non-limiting article can be a technical textile.
Technical textiles are textiles used in industrial, automotive,
construction, agricultural, aerospace, hygiene, and similar
applications.
[0057] Some articles, such as garments, linen and some decorative
or technical textiles, are subject to harsh usage (abrasion,
exposure to various environmental conditions etc.) and therefore
may need extensive, sometimes daily, cleaning and washing. So far,
fire proofing these articles involved either using the few
available non-flammable fabrics; coating flammable fabrics with
large amounts of FR, thus often damaging the fabric properties; or
applying low amounts of FR on the flammable fabric, but limiting
its cleaning method to the expensive and burdensome dry cleaning
method. Using the FR additive compositions presented herein, these
garments or technical textiles may be fire proofed while
maintaining the feel and look of the fabric, as a result of
applying relatively small amounts of the flame retardant additive
composition described herein. The other types of articles in the
list provided above, such as the non-limiting examples of
draperies, carpets, tents, sleeping bags, toys, wall fabrics,
decorative fabrics, mattresses and upholsteries, are not washed as
much as garments or linen. However, these articles also call for
efficient fire proofing thereof, while maintaining their durability
during periodic cleaning. These articles may easily be made fire
proof, either by using a textile treated by the flame retardant
additive composition described herein during the manufacturing
process, or by easily applying the flame retardant additive
composition described herein onto the final product textile or
article made therefrom.
[0058] According to another aspect of the invention the article
comprising a textile substrate which contains the flame retardant
additive composition described herein, is a flammable article prior
to being contacted with the flame retardant additive composition
described herein.
[0059] The article (as well as the textile contained in the
article) described herein can be characterized by an after flame
time of less than 120 seconds (sec), smoldering time of less than
15 minutes (min) and charring distance of less than 100 millimeters
(mm), as defined by BS 5852 Part 1 of the 20 seconds ignition test,
which is considered a pass of this test.
[0060] According to a still further feature of the invention there
is provided a textile substrate (e.g., a flammable textile
substrate) in the article, which textile contains the flame
retardant additive composition, wherein the textile is
characterized by at least one aesthetic or textural property which
aesthetic or textural property is identical to that of a textile
substrate which does not contain the flame retardant additive
composition.
[0061] Preferably, such an aesthetic or textural property is
selected from the group consisting of flexibility, smoothness,
color vivacity, and lack of streakiness. More preferably, these
properties remain substantially unchanged upon subjecting the
article to one or more washing cycles, and more preferably, to five
or more washing cycles, and even more preferably to 25 or more
washing cycles.
[0062] The flame retardant additive composition can be used in a
flame retardant effective amount in the textile. A flame retardant
effective amount will vary depending on the specific phosphate
ester and textile, and other parameters.
[0063] According to still further aspects of the invention, the
flame retardant effective amount of the flame retardant additive
composition is characterized in that the dry amount of the flame
retardant additive composition (dry add-on) is less than 100 weight
percent of the textile substrate's dry weight. Preferably, the dry
add-on is less than 75 weight percent of the textile substrate's
dry weight. More preferably, the dry add-on is less than 50 weight
percent of the textile substrate's dry weight, and most preferably
the dry add-on is less than 30 weight percent of the textile
substrate's dry weight. Thus, it should be appreciated that the
textile substrates treated with the flame retardant additive
compositions described herein are characterized by a relatively low
dry add-on.
[0064] With regard to dry add-on calculation, the phrase "amount of
the flame retardant additive composition" refers to the amount of
non-volatile components within the flame retardant additive
composition, which remain on the fabric after curing and drying.
The dry add-on value is determined by calculating the difference in
weight of the dry fabric before application of the flame retardant
additive composition and after drying and curing of the applied of
the flame retardant additive composition.
[0065] Examples of non-volatile components within the flame
retardant additive composition, include, but are not limited to,
phosphate ester(s) and binder(s).
[0066] According to yet an additional aspect herein there is
provided a process of applying any of the flame retardant additive
compositions described herein, to a textile substrate, the process
comprising contacting the textile substrate with the flame
retardant additive composition described herein. Preferably, the
contacting is effected by any industrially acceptable manner,
preferably by spreading, padding, foaming and/or spraying
means.
[0067] The process described herein of applying a flame retardant
effective amount of a flame retardant additive composition
comprising a phosphate ester of the general formula (I) described
herein to a textile substrate may include wherein applying
comprises contacting the textile substrate with the flame retardant
additive composition described herein.
[0068] In one embodiment the step of applying can comprise
immersing the textile substrate in the flame retardant additive
composition described herein.
[0069] In one embodiment in the process described herein, following
applying (e.g., contacting) the textile substrate with the flame
retardant additive composition described herein, the process can
further comprise subsequent to said applying, heating the textile
substrate.
[0070] In one specific embodiment, the flame retardant additive
composition described herein is contained in a layer such as a
backing, back layer, or back-coating, referred to collectively
herein as back-coating, that is applied to a surface of the
textile. The back-coating is typically derived from a polymer
compound ("binder" as described herein) and suitable liquid carrier
material (as described herein) in which the selected phosphate
ester (I) is dispersed. The selection of the polymer used in the
back-coating is readily achievable by one having ordinary skill in
the art. Typically the polymer of the back-coating can be selected
from any of a large number of stable polymeric dispersions known
and used for binding, coating, impregnating or related used, and
may be of a self crosslinking type or externally crosslinked type.
The polymeric constituent can be an addition polymer, a
condensation polymer or a cellulose derivative. Alternatively, the
back-coating may comprise conventional thermoplastic polymers,
which can be applied to the textile by hot melt techniques known in
the art.
[0071] The back-coating (and the flame retardant additive
composition described herein) can optionally include additional
components, such as other fire retardants, synergists, dyes,
wrinkle resist agents, foaming agents, buffers, pH stabilizers,
fixing agents, stain repellants such as fluorocarbons, stain
blocking agents, soil repellants, wetting agents, softeners, water
repellants, stain release agents, optical brighteners, emulsifiers,
thickeners, and surfactants.
[0072] The back-coating (and the flame retardant additive
composition described herein) is typically formed by combining the
polymer, liquid carrier material, optional components, if any, and
selected flame retardant in any manner and order known, and the
method and order is not critical to the instant invention.
[0073] Further, the back-coating (and the flame retardant additive
composition described herein) can be applied to the surface of the
textile through any means known in the art. For example, the use of
coating machines such as those utilizing pressure rolls and chill
rolls can be used, "knife" coating methods, by extrusion, coating
methods, transfer methods, coating spraying, foaming or the like.
The amount of back-coating (or flame retardant additive
composition) applied to the textile is generally that amount
sufficient to provide for a textile having a flame retarding amount
of the designated phosphate ester (I). A flame retarding amount of
the designated phosphate ester (I) is from about 80 to about 10
weight percent, specifically from about 70 to about 20 weight
percent and, most specifically from about 60 to about 30 weight
percent of phosphate ester (I) based on the weight of the flame
retarded textile.
[0074] After application of the back-coating, the back-coating can
be cured on the textile by heating or drying or in any way
reacting/curing the back coating.
[0075] Padding is a process that is typically used for applying the
flame retardant additive composition onto a textile substrate and
is defined as a process in which the textile is first passed
through a padder containing the FR additive composition wherein the
composition is applied, and the textile is then squeezed between
heavy rollers to remove any excess of the flame retardant additive
composition.
[0076] The process described herein can be affected, for example,
either during the dying or the finishing stages of the textile
substrate manufacture.
[0077] In another more specific embodiment herein there is provided
a process comprising coating a textile substrate with the flame
retardant additive composition described herein, preferably by any
one or more of the aforementioned spreading, padding, foaming
and/or spraying means.
[0078] According to still further features in the described
preferred embodiments the processes described herein further
comprise, subsequent to the contacting (or coating), heating the
textile substrate. Preferably, the textile substrate is heated to a
temperature of from about 100.degree. C. to about 200.degree. C.,
preferably from about 150.degree. C. to about 170.degree. C.
whereby the temperature is dictated by the curing temperature of
the binder.
[0079] In one embodiment herein the flame retardant additive
composition is packaged in a packaging material and is identified
in print in or on the packaging material for use as a flame
retardant for application on a textile substrate.
[0080] According to another embodiment of this aspect of the
present invention, the process is conducted under basic pH
conditions.
[0081] According to another embodiment of the process according to
this aspect of the present invention, there is added to the flame
retardant additive composition at least one additional ingredient
as described herein.
[0082] Consequently, as previously delineated, the flame retardant
additive compositions prepared by the process described herein, are
characterized by an increased storage stability, being stable for
at least two weeks at about room temperature, and often being
stable for at least four weeks at that temperature. Stability is
defined as no visual separation of suspension being observed.
[0083] The flame retardant additive compositions described herein
can be efficiently used when applied on textiles, by avoiding the
need to use excessive amounts of the flame retardant, binders, and
other additives. Furthermore, these flame retardant additive
compositions are easily applied onto the textile substrate.
[0084] Hence, according to another embodiment of the present
invention, the article herein, which contains the textile
containing the flame retardant additive composition described
herein, is further characterized by at least one aesthetical or
textural property which property is equivalent to an equivalent
article which contains an equivalent textile which textile does not
contain the flame retardant additive composition described
herein.
[0085] As a result, articles having textile substrates, treated by
the flame retardant additive composition described herein have
superior properties compared with the presently known FR-treated
products.
[0086] According to the presently most preferred embodiments of the
present invention, the article herein comprises a flammable textile
which has been treated with the flame retardant additive
composition herein.
[0087] There is also provided herein a dispersion of a flame
retardant additive composition comprising a phosphate ester of the
general formula (I) described herein; and, water. Such a dispersion
can contain water in an amount of from about 20 to about 80 weight
percent, specifically from about 30 to about 70 weight percent
water based on the total weight of the aqueous dispersion. Such a
dispersion can contain flame retardant additive composition in an
amount of from about 20 to about 80 weight percent, specifically
from about 30 to about 60 weight percent based on the total weight
of the aqueous dispersion of flame retardant additive
composition.
[0088] Such a dispersion can be provided by known methods and
apparatus as are known in the art and will not be further described
herein.
[0089] In another embodiment there is provided a process of
treating a textile comprising applying the aqueous dispersion of
phosphate ester of formula (I) to a textile substrate; still
further there is provided a textile that has been treated by such a
process; and even further there is provided an article comprising
such a textile. Application of the aqueous dispersion of phosphate
ester (I) can be done in any of the manners of application
described herein and as is known in the art.
[0090] The formulations and processes described herein were
practiced so as to provide textile substrates having the FR
additive composition applied thereon. The resulting textile
substrate is characterized by enhanced flame retardancy, while
still maintaining its aesthetical and textural properties.
[0091] It is to be understood that the invention is not limited in
its application to the details of construction and the arrangement
of the components set forth in the description herein. The
invention is capable of other embodiments or of being practiced or
carried out in various ways. Also, it is to be understood that the
phraseology and terminology employed herein is for the purpose of
description and should not be regarded as limiting. Additional
objects, advantages, and novel features of the present invention
will become apparent to one ordinarily skilled in the art.
[0092] The following examples are offered to illustrate the general
nature of the invention. Those skilled in the art will appreciate
that they are not limiting to the scope and spirit of the invention
and various and obvious modifications will occur to those skilled
in the art.
EXAMPLE 1
[0093] A 53 wt % solids aqueous dispersion (4.4 wt % phosphorus)
containing hydroquinone bis(diphenyl phosphate) as the sole flame
retardant, an acrylic binder, dispersant and thickener was pad
applied to 100% cotton twill fabric samples (spec. wt.=168
g/m.sup.2).
[0094] The fabric samples were then dried and cured in an oven at
160.degree. C. for 4 minutes. The treated fabric samples were then
tested and passed the criteria of the NFPA 701 (2010 version). The
NFPA 701 is a small scale flammability test developed by the NFPA
to assess the flame propagation of textiles and films. Testing
measures the ignition resistance of a fabric after it is exposed to
a flame for 45 seconds. The weight loss of the sample and
observation of any burning fragments are the two main pass/fail
criteria of the test. The fabric will pass the test if all samples
meet the following criteria: [0095] The average weight loss of the
specimens shall be 40% or less [0096] No individual specimen's
percent weight loss can exceed the mean value for the specimens
plus 3 standard deviations [0097] Fragments and residues of
specimens that fall to the floor of the test chamber shall not burn
for more than an average of 2 seconds per specimen [0098] The data
for the evaluations are given in Table 1 [0099] Fabric: 100% White
Cotton Twill (spec. wt.=168 g/m.sup.2) [0100] Formula Residue
Content [wt %]=53%
TABLE-US-00001 [0100] TABLE 1 Results of evaluation of padded
textile according to NFPA 701 Dry FR P Mass Add-on Loading loading
Loss Burning Sample ID (grams) (wt %) (wt %) (wt %) Fragments P/F
Sample #1 -- -- -- 97.3 N Fail (untreated) Sample #2 10.28 60.55
6.48 34.0 N Pass Sample #3 10.78 63.49 6.79 31.1 N Pass Sample #4
10.63 62.61 6.70 32.8 N Pass Sample #5 10.88 64.08 6.86 29.3 N
Pass
EXAMPLE 2
[0101] A 50 wt % solids aqueous dispersion (4.0 wt % phosphorus)
containing hydroquinone bis(diphenyl phosphate) as the sole flame
retardant, an acrylic binder, dispersant and thickener was pad
applied to 100% cotton twill fabric samples (spec. wt.=168
g/m.sup.2). [0102] The data for the evaluations are given in Table
2 [0103] Fabric: 100% White Cotton Twill (spec. wt.=168 g/m.sup.2)
[0104] Formula Residue Content [wt %]=50%
TABLE-US-00002 [0104] TABLE 2 Results of evaluation of padded
textile according to NFPA 701 Dry FR P Mass Add-on Loading loading
Loss Burning Sample ID (grams) (wt %) (wt %) (wt %) Fragments P/F
Sample #6 -- -- -- 97.5 N Fail (untreated) Sample #7 6.48 32.3 3.45
72.7 N Fail Sample #8 6.26 31.2 3.33 73.1 N Fail Sample #9 6.48
33.3 3.45 72.6 N Fail Sample #10 6.41 31.9 3.41 74.0 N Fail
[0105] The dry add-on values for each sample above were determined
by measuring and then calculating the difference in weight of a
"bone-dry" (conditioned at 105.degree. C. for 30 minutes) fabric
sample and one that was coated and fully cured. The FR and
phosphorus loading levels were calculated based on the known level
of solid flame retardant (and % P in that flame retardant) added to
the aqueous dispersion formulation in relation to the solids
content in the final application dispersion (both calculated and
confirmed by performing a "% solids" determination on the final
dispersion). The dry add-on values shown above express the amount
of solid in the aqueous dispersion that were applied to each fabric
sample; and based on knowing the percent of solid flame retardant
in the overall formulation, the FR and phosphorus add-on levels
were calculated.
EXAMPLE 3
[0106] A 50 wt % solids aqueous dispersion (4.1 wt % phosphorus)
containing hydroquinone bis(diphenyl phosphate) as the sole flame
retardant, an acrylic binder, dispersant and thickener was pad
applied to 100% cotton twill fabric samples (spec. wt.=258
g/m.sup.2).
[0107] The fabric samples were then dried and cured in an oven at
160.degree. C. for 4 minutes. The finished fabric samples were
tested and passed the MVSS 302 with either an SE or SE/NBR rating.
The MVSS 302 test is a horizontal flame test that is used as a
guideline for automobile manufacturers. The sample size is 14
inch.times.4 inch.times.1/2 inch. There is a line 11/2 inch from
the ignition point. A flame is ignited for 15 seconds. The ignition
source is then turned off and the sample is rated. A "DNI" rating
indicates that the sample did not support combustion. A rating of
"SE" indicates that the sample ignited but did not burn to the
timing zone, which is a point starting from the 11/2 inch mark to
the 31/2 inch line. A rating of "SENBR" indicates that the sample
burned past the 11/2 inch line but was extinguished before the 31/2
inch mark. A rating of "SE/B" indicates that a sample burned past
the 31/2 inch mark but extinguished before the end point; an inch
per minute rate is then calculated. [0108] The data for the
evaluations are given in Table 3 [0109] Fabric: 100% White Cotton
Twill (spec. wt.=258 g/m.sup.2) [0110] Formula Residue Content [wt
%]=50%
TABLE-US-00003 [0110] TABLE 3 Results of evaluation of padded
textile according to MVSS 302 Dry FR P Burn Rate Add-on Loading
loading (inches/ Test Sample ID (grams) (wt %) (wt %) min)
Classification Sample #11 -- -- -- 3.33 SE/B (untreated) Sample #12
13.30 47.88 5.12 -- SE Sample #13 13.35 48.06 5.14 -- SE Sample #14
12.56 45.21 4.84 -- SE/NBR Sample #15 13.00 46.80 5.01 -- SE
[0111] While the process of the invention has been described with
reference to certain embodiments, it will be understood by those
skilled in the art that various changes may be made and equivalents
may be substituted for elements thereof without departing from the
scope of the invention. In addition, many modifications may be made
to adapt a particular situation or material to the teachings of the
invention without departing from the essential scope thereof.
Therefore, it is intended that the invention not be limited to the
particular embodiment disclosed as the best mode contemplated for
carrying out the process of the invention but that the invention
will include all embodiments falling within the scope of the
appended claims.
* * * * *