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Sommaire du brevet 1118163 

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Disponibilité de l'Abrégé et des Revendications

L'apparition de différences dans le texte et l'image des Revendications et de l'Abrégé dépend du moment auquel le document est publié. Les textes des Revendications et de l'Abrégé sont affichés :

  • lorsque la demande peut être examinée par le public;
  • lorsque le brevet est émis (délivrance).
(12) Brevet: (11) CA 1118163
(21) Numéro de la demande: 1118163
(54) Titre français: PROCEDE DE TRAITEMENT DE FIBRES SYNTHETIQUES PAR DES POLYDIORGANOSILOXANES CONTENANT DES AMINOALKYLES
(54) Titre anglais: METHOD FOR TREATING SYNTHETIC FIBERS WITH AMINOALKYL-CONTAINING POLYDIORGANOSILOXANES
Statut: Durée expirée - après l'octroi
Données bibliographiques
(51) Classification internationale des brevets (CIB):
  • D06M 15/643 (2006.01)
(72) Inventeurs :
  • KALINOWSKI, ROBERT E. (Etats-Unis d'Amérique)
(73) Titulaires :
  • DOW CORNING CORPORATION
(71) Demandeurs :
  • DOW CORNING CORPORATION (Etats-Unis d'Amérique)
(74) Agent: GOWLING WLG (CANADA) LLP
(74) Co-agent:
(45) Délivré: 1982-02-16
(22) Date de dépôt: 1977-09-16
Licence disponible: S.O.
Cédé au domaine public: S.O.
(25) Langue des documents déposés: Anglais

Traité de coopération en matière de brevets (PCT): Non

(30) Données de priorité de la demande:
Numéro de la demande Pays / territoire Date
764,674 (Etats-Unis d'Amérique) 1977-02-02

Abrégés

Abrégé anglais


Abstract of the Disclosure
Synthetic fibers such as polyethylene terephthalate
and nylon are treated with certain polydiorganosiloxanes to
provide improved properties such as "hand" and water
repellency. When the polydiorganosiloxanes contain
approximately two silicon-bonded amino radicals of the formula
-R'(NHCH2CH2)aNHR", such as -CH2CH2CH2NHCH2CH2NH2, they
provide a crosslinked siloxane on the surface of the
treated fiber, when heated, which does not diminish the
fire-retardancy rating of the fibers.

Revendications

Note : Les revendications sont présentées dans la langue officielle dans laquelle elles ont été soumises.


The embodiments of the invention in which an
exclusive property or privilege is claimed are defined as
follows:
1. A method for treating a synthetic fiber
comprising applying to the surface of said fiber a
liquid composition consisting essentially of a triorgano-
siloxane-endblocked polydiorganosiloxane containing an
average of at least two nitrogen-containing siloxane units
per molecule of polydiorganosiloxane, said nitrogen-containing
siloxane units bearing an aliphatically saturated radical
of the formula -R'(NHCH2CH2)aNHR" wherein a is 0 or 1,
R' denotes a divalent hydrocarbon radical and R" denotes
a hydrogen radical or a monovalent hydrocarbon radical,
any remaining organic radicals in the polydiorganosiloxane
being monovalent radicals, free of aliphatic unsaturation,
selected from the group consisting of hydrocarbon radicals
and fluorinated hydrocarbon radicals, and heating the applied
triorganosiloxane-endblocked polydiorganosiloxane, thereby
providing a treated synthetic fiber having durably affixed
to the surface thereof a crosslinked polydiorganosiloxane.
2. A method according to claim 1 wherein the
polydiorganosiloxane is heated to a temperature of from
50°C. to 250°C. after it has been applied to the
thermoplastic fiber.
21

Description

Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.


This invention relates to a method of treating
synthetic fibers with organosiloxane compositions and
to the treated fibers obtained therefrom. In one aspect,
this invention relates to a method of providing improved
properties such as improved " hand " to te~tiles consisting
of synthetic fibers without diminishing the fire-retardancy
rating of the textiles.
Organosilicon compositions are well known for
treating textiles to confer desirable properties thereto,
such as " hand ", antistatic behavior, oil repellency
and improved tear strength. For example, it has long
be known to apply a curable organopolysilo~ane composition
to a fabric or fiber and to subsequently cure the applied
organopolysilo~ane by the action of a curing component
to produce a fiber or fabric that is surrounded by,
i.e. encased in, a sheath of the cured organopolysiloxane
composition.
However, a two-component curable composition
has certain deficiencies. For example, the curable
compositions must often be prepared, shipped, and stored
in two or more non-curing packages, which are mixed shortly
before the intended time of use, in order to avoid
premature curing of the composition. This requirement is
costly, inconvenient, and time consuming. Further, relativeiy
large amounts of a two-component curable composition must
be added to a fabric or fiber in order JO provide suffic~ent
integrity for the cured composltion to resist mechanical
removal, such as by abrasioIl.
An increasingly imporl~rt de~ficier.cy ~f two-
compor,ert curab-le t-~tile treat~!ert3 i3 t;~e tendenc~ 3I`
~k

the cured organosiloxane, which is highly crosslinked,
to interfere with the flame-retardant p.operties of the
textile, particularly the flame-retardant property due
to melt-drip action of a thermoplastic textile. While
certain natural fibers such as wool have some inherent
flame-retardancy, many synthetic textiles such as
thermoplastics such as polyethylene terephthalate and
nylon rely on a melting of the ignited textile and a dripping
of flaming material to carry away fire and heat from
the textile and thus achieve reduced flammability. It has
been found that the presence of certain cured organosiloxanes
on the surface of such textiles interferes with this
melt-drip action and leads to a diminishing of the fire-
retardancy rating of the textile.
It is an object of this invention to provide
a process for durably treating synthetic fibers to improve
the characteristics, such as water repellency, resiliency
or ''loft " , and ''hand " , of a textile consisting of
said fibers without diminishing the fire-retardancy
rating of said textile.
It is a further objec~ of this invention to
provide a process for durably treating textiles comprising
a synthetic fiber with a polydiorganosiloxane which does
not require a curing component to cause crosslinking of
the polydiorganosiloxane.
These and other objects are achieved by the
process of this invention which comprises applying to
synthetic fibers certain polydiorganosiloxanes containing
silicon-bonded amino-containing radicals and heating
the applied polydiorganosiloxane. The resulting treated

i3
fiber has durably affixed to its surface a crosslinked
polydiorganosiloxane ~hich ~s resistant to removal by
washing. A fire-retardant fabric consisting of said
treated fibers has improved properties such as " hand"
without having its fire-retardancy rating diminished
when the polydiorganosiloxane is lightly crosslinked.
Textiles comprising synthetic fibers and other fibers
such as cotton may also be treated with the process of
this ~nvention.
The present invention relates to a method for -
treating a synthetic fiber and to the treated fiber
obtained thereby, said method comprising applying to the
surface of said fiber a liquid composition consisting
essentially of a triorganosiloxane-endblocked polydiorgano-
siloxane containing an average of at least two nitrogen-
containing siloxane units per molecule of polydiorgano-
siloxane, said nitrogen-containing siloxane units bearing
an aliphatically saturated radical of the formula
-R'(NHCH2C~2)aNHR" wherein a is 0 or 1, R' denotes a
divalent hydrocarbon radical and R " denotes a hydrogen
radical or a monovalent hydrocarbon radical, any
remaining organic radicals in the polydiorganosiloxane
being monovalent radicals, free of aliphatic unsaturation,
selected from the group consisting of hydrocarbon radicals
and fluorinated hydrocarbon radicals, and heating
the applied triorganosiloxane-endbloc~ed polydiorganosiloxane,
thereby providing a treated synthetic fiber having durably
aff'ixed to the surface thereof a crosslin~ed polydiorgano-
siloxane.
3~
-3-

18~3
By synthe~ic fiber it is meant a fiber or filament
consisting essentially of a synthetic polymer along with
any other of the components commonly used in synthetic fibers
such as delusterants, fire-control additives, and
colorants.
By synthetic fiber it is further meant a single
synthetic fiber or filament, or a plurality of fibers
comprising synthetic fibers such as a bundle or tow of
fibers or filaments, a yarn, a thread, a fiberfill or
a fabric such as a woven fabric, an agglomerated random
fabric and a knitted fabric.
Synthetic fibers include, but are not limited
to fibers of cellulose derivatives such as cellulose
acetate; vinylic fibers such as polyethylene, polypropylene
and polyacrylonitrile and condensation fibers such as
polyamides, polyesters, polyimides, and polycarbonates.
Of particular interest for the purposes of this
invention are the polyamides, such as the nylons and
polyesters such as polyethylene terephthalate that are
used to prepare oriented and non-oriented fibers used to
make filaments, threads, yarns, fiberfill, and fabrics such as
woven fabrics, knitted fabrics, and random or non-woven
fabrics.
The liquid composition that i~ applied to a
surface of a fiber in accordance with this invention
consists essentially of a triorganosiloxane~endblocked
polydiorganosiloxane. The liquid composition may consist
solely of a liquid pol~rdiorganosiloxane. Alternatively,
in those cases where the polydiorganosiloxane is not a
liquid under ambient conditions, a liquid composition may

be prepared by any suitable method. For example, a
liquid composition may be prepared by dissolving or
dispersing or emulsifying a non-liquid polydiorganosiloxane
in a suitable medium such as an organic liquid or water.
Of course, it should be understood that a liquid
polydiorganosiloxane may also be dissolved, dispersed or
emulsified in place of or in addition to a non-liquid
polydiorganosiloxane in said suitable method for preparing
a liquid composition.
By ambient conditions it is meant the conditions
of time, temperature and pressure that are used during
the treating of the fiber according to the process of
this invention. Thus, it is within the scope of this
invention to apply to a fiber a composition which may
be non-liquid at room temperature but which will be a
liquid at a higher temperature that may be used in the
method of this invention.
The liquid composition may also contain non-
essential components such as pigments, emulsifying
agents, fire-retardant additives, plasticizers,
anti-static agents and perfumes when desired.
In many instances it is desirable to apply
and durably affix a very small amount, for example,
less than 1 percent by weight, based on the weight of
the fiber, of polydiorganosiloxane to a surface of a
fiber. To this end it is ofterl desirable to prepare a
dilute solution or a suspension or an emulsion of the
polydiorganosiloxane and app y the resuiting dilute
liquid composition to the fiber.
3o
--5--

Çi3
~ he viscosity OI' the liquid composition is not
critical. The liquid composition should be su~ficiently
fluid to permit its use in the method of th~s lnvention,
i.e. it should be applicable to ~he desired surface
of the fiber at amblent conditions. The volatility of the
polydiorganosiloxane should be sufficiently low so that
at least a portion of it will remain in contact with the
surface of the fiber at ambient conditions so that it
is durably affixed to the surface of the fiber~
The triorganosiloxane-endblocked polydiorgano-
siloxane is preferably a liquid having a viscosity of
less than approximately 100 pascal-seconds (100,000 cp.)
at 25C. Desirable results with respect to the " hand "
of a textile comprising the treated fiber are obtained
when the viscosity of the polydiorganosiloxane at 25C. has
a value of less than 10 pascal-seconds, most preferably
from 0.1 to 5 pascal-seconds.
The triorganosiloxane-endblocked polydiorgano-
siloxane consists essentially of terminal triorganosiloxane
units of the formula R3SiO~/2 and backbone diorganosilo.{ane
units of the formula R2SiO2/2. Trace amounts of other
siloxane units in the polydiorganosiloxane, such as Si04/2
and RSiO3/2, which are normally present as impurities in
commercial polydiorganosiloxanes, are within the scope
of this invention. The R radicals of the above siloxane
units are bonded to silicon by a silicon-carbon bond and
are either nitrogen-containing radicals of the formula
-R'(NHCH2CH2)aNHR " or monovalent hydrocarbon radicals or
monovalent fluorine-containir.~ hydrocarbon radicals,
all of which are free of aliphati~ unsaturation.

Suitable nitrogen-contain~ng radicals of the
above formula are bonded to silicon by one valence
of a divalent R' radical, the other valence of said R'
radical being bonded to nitrogen. Divalent hydrocarbon
radicals R' may be saturated radicals such as alkylene
radicals of the general formula -CnH n~ such as -CHz-,
-CH2CH2-, -CH2CH2CH2 , -CH2CH(CH3)CH2-, and -(CH2) 4-
and cycloalkylene radicals of the general formula
-CnH n ~~ such as cyclohexylene-1,4; and aromatically
unsaturated radicals such as p-phenylene, m-phenylene,
-(CHz)nC6H4-, -(CX2)nC6H~(CHz)n- and ring-alkylated
derivatives thereof. In the above formulae n may have
a value of from l to 18, preferably 3 to 8, all inclusive.
Polydiorganosiloxanes wherein the silicon-bonded,
nitrogen-containing radicals have a propylene radical
such as -CH2CH2CH2- or an alkylated propylene radical
such as -CH2CH(CH3)CH2- as the R' radical are preferred
because of ease of synthesis and availability.
Suitable nitrogen-containing radicals of the
above formula also bear a nitrogen-bonded monovalent radical
R " which may be a hydrogen radical, which is preferred,
or a monovalent hydrocarbon radical free of aliphatic
unsaturation such as alkyl radicals of the general
formula -CmH m+ such as methyl, ethyl, propyl, butyl
and isobutyl and cycloalXyl radicals of the general
formula -CmH m such as cyclohexyl; and aromatically
unsaturated radicals such as phenyl, benzyl, and tolyl.
In the above formulae m may have a value of from l to 18,
preferably l tc o, all ir.clusi-Te-.
3o

Any R radica;s of said siloxane units which
are not nitrogen-containing radicals of the above formula
are monovalent radicals, free of aliphatic unsaturation,
selected from the group consisting of monovalent hydrocarbon
radicals, hereinabove delineated as R " , and monovalent
fluorinated hydrocarbon radicals such as 3~3,3-trifluoro-
propyl, pentafluorobutyl, pentafluorophenyl and a,a,a-tri-
fluorotolyl.
It is to be understood that trace amounts of
other monovalent radicals may be present as R radicals
in the polydiorganosiloxane as impurity radicals such
as radicals resulting from the particular method of preparation
of said polydiorganoslloxanes, hereinafter recited. For
example, a convenient method for preparing nitrogen-containing
siloxanes is to react a suitable amine with a siloxane or
silane which bears a chloropropyl radical. A large
percentage of the chloropropyl radicals are thereby
converted to amino-containing propyl radicals, any
unconverted chloropropyl radicals remaining as said
impurity radicals.
In accordance with the above, triorganosiloxane-
endblocked polydiorg~nosiloxanes suitable for use in the
process of this lnvention consist essentially of siloxane
units bearing nitrogen-containing radicals such as
R "NH(CX2CH2NH)aR'SiOl/2 and R"NH(CH2CHzNH)aR'SiO2/2 and
ni~rogen-free siloxane units such as -SiO 1/2 and -siO2/2
wherein the undesignated silicon valences are satisfied
by nitrogen-~ree R radicals. Preferred nitrogen-free
R radicals include methyl, phenyl, and 3,3,3-trifluoropropyl
and the preferred nit^ogen-containing R radical is
--8--

-CHzCH?CH2NHCHzCH2NH~ thereby giving rise to preferred
siloxane units of the formulae (CH3)3SiO~/~, C~3CH2CH2-
(CH3)2SiOl/2, CH3(C5H5)2SiO1/2, C6H,(CH3)2SiOl/2,
(CH3)2SiO2/2~ CF3CH2CH2(CH3)SiO2/2, CH3(C~H~)SiO2/2,
(C6H3)2SiO2/2, Z(CH3)2SiOl~2, Z(C6H,)2SiOl/2, Z(C6~)(CH3)-
SiOl/2, Z(CF3CH2CH2)(CH3)SiOL/2, Z(C~3CH2CH2)SiO2/2,
Z(CX3)SiO2/2 and Z(C6H,)SiO2/2, wherein Z denotes the
preferred -CH2CH2CH2NHCH2CH2NHz radical. Polydiorgano-
siloxanes wherein at least 50 percent of the R radicals
are the methyl radical are preferred for modifying a
synthetic fiber. Polydiorganosiloxanes wherein a majority,
preferably greater than 90 percent, of the siloxane units
are dimethyl siloxane units are preferred for providing
improved " handt' to textiles comprising synthetic
fibers treated therewith.
The triorganosiloxane-endblocked polydiorgano-
siloxane bears at least two siloxane units which have a
-R~(NHCH2CH2)aNHR " radical. Polydiorganosiloxanes having
greater amounts of the amino-containing siloxane units,
such as 3, 4, 5, 10, and more, are also operable in the
method of this invention, giving rise to more tightly
crosslinked polydiorganosiloxanes durably affixed to
the surface of the textile. As noted above, the amino-
containing siloxane units of the triorganosiloxane-
endblocXed polydiorganosiloxane may be terminal
triorganosiloxane units or backbone diorganosiloxane
units or both terminal and backbone siloxane units.
When it is desired tc treat a synthetic fiber
or a textile consisting of said synthetic fiber according
to the method of this ~nvention, without changing t~e

fire-retardancy rating of the fiber or textile, the
polydiorganosiloxane should contain no more than an average
of approximately two amino-containing siloxane units,
delineated above, per molecule. For example, a poly-
diorganosiloxane having up to 100 siloxane units per
molecules should contain only two amino-containing siloxane
units in order to preserve the fire-retardancy rating
of the treated fiber or fabric. A polydiorgano-
siloxane having more than 100 siloxane units may contain
from two to approximately 4 amino-containing
siloxane units per molecule to preserve said fire-
retardancy rating.
The flammability of a textile is often determined
by the Department of Commerce Test No. FF 3-71, 'lStandard
for the Flammability of Children's Sleepware.'' To
pass the DOC FF 3-71 test, a specified textile sample
must not burn its entire length of 254 mm. and the
length of the char must not exceed 177.8 mm. Furthermore,
any material fal~ing from the burning sample must not
burn (residual ~ire) for more than 10 seconds. For
the purposes of this invention9 the flame-retardancy
rating of a textile is determined by the char length and
the burning length requirements of DOC FF 3-71 as embodied
in DOC FF 5-74, and does not consider the residual fire
rating of the sample. ~hus, if none of five samples
burns its entire length and the average length of the
char of five samples does not exceed 177.~ mm., the
sample has a Pass fire-retardancy rating. If a
textile, unmodified by the process of this invention,
has a Pass rating accordlng tc ~OC FF 5-74, an
--10--

i3
identical textile, mGdified according to the method
of this invention, may also have a Pass rating according
to DOC FF 5-74, depending on whether or not the number
of amino-containing siloxane units in the polydiorgano-
siloxane is greater than approximately two. By
identical textile, it is meant that the test samples
have been taken from the same textile and have been
exposed to the same conditions, such as scouring, rinsing,
drying, heating, and the method of this invention except
that the modified textile was in contact with a liquid
composition consisting essentially of the polydiorgano-
siloxane polymer during at least a portion of the heating
step whereas the unmodified textile was not in said
contc t during said heating step.
Methods for preparing the triorganosiloxane-
endblocked polydiorganosiloxane polymers that are employed
according to this invention are well known in the art.
~hus, a triorganosiloxane-endblocked polydiorganosiloxane
bearing a limited number of suitably reactive groups
such as -SiX or -SiCH2CH2CH2Cl may be reacted with
CH2=C(CH3)CHzNH2CH2NX~ or H2NCH2CH2NH2~ respectively to
provide an analogous polydiorganosiloxane where in the
reactive groups have been converted to -CH2CH(CH3)CH2-
NHCH2CH2NH2 groups and CHzCH2CX2NHCH2CH2NHz groups,
respectively. Small amounts of unreacted -SiH
or -SiCH2CH2CHzCl groups may remain as impurity groups,
hereinbefore discussed. Al~ernately, a suitable
triorganosil3xane-end~locked polydiorganosiloxane ma~
be prepared from amino-containirlg silanes or siloxar.es
using well-kno-~n methods of hydrolysis and equilibration.
For example, P~ke, et al., ~J.S. Patent No. 3,033,815,
--11--

c;3
Speier, TJ.S. Patent No. 3,146,250 and Brown, U.S. Patent
No. 3,35~,424 contain teachings ~^lhich may be adapted
to prepare polydiorganosiloxanes which are suitable
for use in the method of this invention.
In general, it i5 preferred to prepare suitable
polydiorganosiloxanes by equilibration of the hydrolyzate
of a silane such as R''NH(CH2CH2NH)~R'Si(R'')Yz with a
cyclic siloxane of the formula (R2SiO)X and a source
of endblocking units such as R3SiY wherein Y is a hydrolyzable
group or atom, x has a value of three or more and R and R'
are as hereinbefore delineated.
A highly preferred triorganosiloxane-endblocked
polydiorganosiloxane for the method of this invention may
be prepared by hydrolyzing H2NCH2C~2NHCH2CH2CH2Si(CH3)(OCH3) 2
in excess water and equilibrating the resulting hydrolyzate
with dimethylcyclopolysiloxane and decamethyltetrasiloxane
using a base catalyst such as KOH, to provide a poly-
diorganosiloxane having about 100 siloxane units, 2 of which
bear aminoethylaminopropyl radicals.
A highly preferred liquid composition for the
method of this invention may be prepared by preparing
a dilute aqueous emulsion of the above highly preferred
polydlorganosiloxane, using a suitable emulsifying
agent such as a non-ionic emulsifying agent.
In the process of this invention, the liquid
composition may be applied to a surface of the fiber in
any suitable manner such as by brushing, rinsing~
padding, dipping, spraying, dusting, by thermal transfer
processes and by fluid-bed methods The liquid composition
-12-

may be applied to the entire surface of the fiber
or to any portion of the surface as desired.
The applied liquid composition may be crosslinked
by heating to a temperature of from above room
temperature to less than the melting or decomposing
temperature of the synthetic fiber. Any heating may
be done at any convenient time providing the
fiber is in contact with at least the polydiorgano-
siloxane for an effective length of time. An
effective length of time means a span of time
at the particular heating temperature that is sufficient
to allow the polydiorganosiloxane to be crosslinked and
durably affixed to the surface of the fiber. Thus,
the liquld composition must be exposed to said temperature
during or after the applying of the liquid composition
to the surface of the fiber.
Heating the composition may be done by any
suitable method or combination of methods such as
with infrared radiation; a suitable hot fluid such
as hot air or steam; electrical heating elements and
microwave heating. Alternately, the liquid may be
applied to a hot fiber. The fiber or polydiorganosiloxane
should not be heated so hot as to melt the fiber or to
adversely effect, such as by decomposing, the fiber and/or
the polydiorganosiloxane.
It has been found that the preferred poly-
diorganosiloxanes described above will crosslink
on the surface of synthetic fibers at temperatures
as low as approximately 50C. For example~ the method of
this invention is useful as a fabric softening

3~3
method in a slothes washing procedure at 50 to 70C.
such as in the rinse and dry cycle of an automatic washer.
An article whose fibers may be modified by
the process of this invention may consist solely of the
synthetic fibers or said article may comprise other
components which are not synthetic fibers. For
example, it is within the scope of this invention to
treat the surface of a textile which comprises
components such as â wool or cotton~ The surface
of these other components may or may not be concurrently
modified during the process of this invention.
After the fiber has been treated, i.e.
having the liquid composltion applied and having been
heated to a suitable temperature as described above,
the polydiorganosiloxane is crosslinked and ~s durably
affixed to the surface of the fiber.
By durably affixed it is meant that the crosslinked
polydiorganosiloxane cannot be washed from the surface of
the fiber to a non-detectable level by 10 machine washings
according to AATCC 124-1973 test method.
By crosslinked polydiorganosiloxane it is meant
that the durably affixed polymer cannot be dissolved in
toluene using one or more of the following methods.
Thus, the polydiorganosiloxane is crosslinked (i) if it
cannot be dissolved from the surface of the fiber
at a temperature below the melting temperature
of the fiber or (ii) if, when the fiber is
dissolved, leaving a polydiorganosiloxane polymer, said
poiymer is insoluble in toluene, or (iiii if the
combination cf fiber and the durably affixed
-14-

i3
polydiorganosiloxane cannot be dissolved in toluene
or (iv) if when the fiber is melted~ leaving a
polydiorganosiloxane polymer, said polymer is
insoluble in toluene. Solvents for synthetic fibers
and polydlorganosiloxane polymers are well known
to those skilled in the synthetic polymer art.
It should be understood that the method of this
invention may be used to modify an end-product comprising
a synthetic fiber or said fiber may be so modified and
subsequently fabricated to an end-product. For example,
it is within the scope of this method to modify a
synthetic fiber or filament at any suitable point in its
manufacturing process or thereafter and subsequently
fabricate an article such as a yarn or a fabric from
said modified fiber or filament. Alternatively, a fabric
may be fashioned comprising a synthetic fiber or
filament and, subsequently, at least the synthetic
fiber portion of said fabric may be modified by said
process.
The process of this invention is further
illustrated by the following examples which teach the
best mode for carrying out the invent~on; however,
said examples should not be regarded as limiting the
invention which is delineated by the appended claims.
All parts are parts by weight.
Example 1
A siloxane having the formula Me3SiO(Me2SiO)~ 8-
(MeZSiO)2SiMe3, wherein Me denotes CH3 and Z denotes
-CH2CH2CH2NHCH2CH2NH2 was emuisified using a blend
of 66 9 parts water~ 1.8 parts of Te--gitol~ TMN-6 non-ionic

;3
surfactant and 1.3 parts Igepal3 CA-897 non-ionic surfactant
for every 30 parts of the siloxane. The siloxane
was mixed with the blend using mechanical mixing and
the mixture was homogenized twice at 6000 psi.
The resulting 30 weight percent siloxane emulsion was
diluted with water as needed for the following examples.
Weighed samples of prewashed and dried polyethylene
terephthalate (PET) and nylon knit fabrics were padded
using the above emulsions of varying concentration.
The padded samples were heated at 204C. for 90 seconds,
washed for 15 minutes at 77C. with a 0.1 percent Triton~
X-100 solution, rinsed3 air dried and reweighed to determine
the percent of siloxane add-on. Table I summarizes these
data. All treated samples exhibited good " hand~' and
AATCC spray ratings of 70 to 80.
Example 2
Nylon and PET samples of Example l having 4.5
weight percent add-on were tested for flame retardancy
according to DOC FF 5-74. Although the melt-drip
behavior of these samples was reduced, compared to the
untreated fabrics, the samples were self-extinguishing
by a combination of melt-drip behavior and charring,
thereby retaining a PASS fire-retardancy rating. The
treated samples were extracted with an equal volume
mixture of phenol and o-dichlorobenzene which dissolved
the fibers and left a crosslinked, insoluble polydiorgano-
siloxane residue which could not be melted at temperatures
as h~gh as 350C.
-16-

fi3
Example 3
Nylon 6 knitted and PET woven fabrics were washed
in an automatic clothes washer wherein from 10 to 50
grams of the 30 percent siloxane emulsion of Example 1
was automatically added to the washer during the rinse
cycle. The washed and treated samples had improved " hand "
and were self-e~tinguishing in the DOC FF 5-74 flammability
test.
Example 4
Several samples of a blue print, fire-retarded
PET woven fabric treat.ed as in Example 1 and having
approximately 2.8 weight percent add-on were sub~ected
to 10 machine washings according to AATCC 124-1973 ~est
method. Although the samples lost approximately 34 percent
of the siloxane add-on, they experienced no loss of ''hand " ,
water repellency or self-extinguishing characteristics.
Additonal samples of the treated PET fabric were rinsed
10 times with perchloroethylene to determine dry cleaning
durability. The rinsed samples lost approximately 80
percent of the siloxane add~on and consequently lost
" hand " and water repellency.
Example 5
PET fiberfill was treated as in Example 1
with siloxane bath concentrations of 0.5 and 2.0 percent
siloxane producin~ add-on of less than 0.1 and 4.5
weight percent respectively. The sample of fiberfill
having less than 0.1 weight pe~cent add-on possessed better
" hand " than Dacron~ II fiberfill. Flammability of the
untreated fiberfill, the two treated f berfill samples
and Dacron3 II fiberfill was ev~luaved in two ways. In

the Pan Burn test 0.3 g. of sample was placed in a 5.6 cm.
diameter x 2.0 cm. deep aluminum cup and the sample was
ignited with a 1'~ lazy yellow bunsen flame for 3 seconds.
The burn time of the sample after the burner was removed
was noted. In the Vertical Burn test 0,3 g. of sample
was fashioned into a 1" x 5" wad, suspended over an
aluminum cup to collect burning fragments and the sample
was ignited at the bottom end with a 1 " lazy yellow
bunsen flame for 3 seconds. Burn time for the sample
and the fragments after the burner was removed were noted.
Table II summarizes these data which show that fiberfill
which has been treated by the method of this invention
have flammability characteristics which are little
different from the flammability of untreated fiberfill.
3o

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Dessin représentatif

Désolé, le dessin représentatif concernant le document de brevet no 1118163 est introuvable.

États administratifs

2024-08-01 : Dans le cadre de la transition vers les Brevets de nouvelle génération (BNG), la base de données sur les brevets canadiens (BDBC) contient désormais un Historique d'événement plus détaillé, qui reproduit le Journal des événements de notre nouvelle solution interne.

Veuillez noter que les événements débutant par « Inactive : » se réfèrent à des événements qui ne sont plus utilisés dans notre nouvelle solution interne.

Pour une meilleure compréhension de l'état de la demande ou brevet qui figure sur cette page, la rubrique Mise en garde , et les descriptions de Brevet , Historique d'événement , Taxes périodiques et Historique des paiements devraient être consultées.

Historique d'événement

Description Date
Inactive : CIB désactivée 2011-07-26
Inactive : CIB de MCD 2006-03-11
Inactive : CIB dérivée en 1re pos. est < 2006-03-11
Inactive : Périmé (brevet sous l'ancienne loi) date de péremption possible la plus tardive 1999-02-16
Accordé par délivrance 1982-02-16

Historique d'abandonnement

Il n'y a pas d'historique d'abandonnement

Titulaires au dossier

Les titulaires actuels et antérieures au dossier sont affichés en ordre alphabétique.

Titulaires actuels au dossier
DOW CORNING CORPORATION
Titulaires antérieures au dossier
ROBERT E. KALINOWSKI
Les propriétaires antérieurs qui ne figurent pas dans la liste des « Propriétaires au dossier » apparaîtront dans d'autres documents au dossier.
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Description du
Document 
Date
(aaaa-mm-jj) 
Nombre de pages   Taille de l'image (Ko) 
Page couverture 1994-02-02 1 11
Abrégé 1994-02-02 1 15
Dessins 1994-02-02 1 8
Revendications 1994-02-02 1 31
Description 1994-02-02 20 644