Title of Invention

A PROCESS FOR TREATING FIBERFILL FIBERS WITH AQUEOUS DISPERSIONS OF ORGANOPOLYSILOXANES

Abstract Treatment of fiberfill fibers with aqueous dispersions of organopolysiloxanes A process for treating fiberfill fibers with aqueous dispersions of organopolysiloxanes obtainable by reaction of organopolysiloxanes (1) comprising condensation-capable groups according to claim 1 with silanes (2) of the formula (R30)3SiCR22-Y (II) or their hydrolyzates, where R is. a hydrogen atom or a monovalent alkyl radical of 1 to 4 carbon atoms, R3 is. an alkyl radical having; 1 to. 8; carbon. . atoms per radical, Y is a ■"radical of the formula -NHR , -NR 2 or -NR5 , where R4 and R5 are each as defined in claim 1 in the presence of water (3), emulsifier (4) and optionally further silanes (5) of the formula (R30)xR3_xSi-R6-Z (III) or their hydrolyzates, where R6 is a divalent hydrocarbyl radical of 2 to 18 carbon atoms and Z is a radical selected from the group consisting of amino or aminoalkylamino radicals, epoxy radicals and (meth)-acryloyloxy radicals, and x is 1, 2 or 3, and optionally further materials (6) which do not take part in the reaction, with the proviso that no metal-containing catalysts are used and that the organopolysiloxanes (1) and silanes (2) are used in such amounts that the organopolysiloxanes after removal of water (3) form elastomeric films insoluble in toluene.
Full Text

Treatment of fiberfill fibers with aqueous dispersions of
organopolysiloxanes
This invention relates to a process for treating fiberfill fibers with aqueous dispersions of organopolysiloxanes.
Emulsions of crosslinked silicones are known. Catalysts comprising (heavy) metal or free of metal are required for crosslinking silicones as well as crosslinkers. In some cases,, inhibitors are also used to control reactivity and pot life in order that any unwanted, premature gelling may be prevented.
Metal-free aqueous RTV1 dispersions are described in
EP 828 794 A and EP 655 475 Al- They are obtainable using the
three starting components:
(A) organopolysiloxanes comprising condensation-capable groups,
(B) (amine-free) organosilicon compounds acting as crosslinkers in that they have at least 3 crosslinking-reactive groups,
(C) organosilicon compound comprising basic nitrogen, more preferably the alkali metal siliconates of the compound, which are catalytically active.
Component (C) confers a very high pH of the products, which presents difficulties in processing.
DE 102004038148 Al (equivalent WO 2006/015740 Al) describes the
preparation of high-viscosity silicones (10 000 to
50 000 000 mPa"s) in emulsion by reaction of silanol-terminated
organopolysiloxanes with α-aminomethylalkoxysilanes. However,
no elastomeric silicone films insoluble in toluene are
obtained.
EP 510 631 A describes the preparation and finishing of a fiber-finishing agent based on copolyesters grafted with polyorganosiloxanes, for a soft featherlike hand for polyester fiberfill fibers. The lateral grafting of polyorganosiloxanes

onto the polyester backbone gives a finishing agent which produces a smooth, low-friction hand on fibers, in particular polyester fiberfill fibers.
GB 1 458 319 A (= DE 24 20 151 A) describes novel manufactured fibers and a process for their production wherein a reactive polysiloxane is used in combination with aminoalkoxysilane and a curing agent, a metal salt of 2- to 4-valent metal ions, such as dibutyltin diacetate or zinc acetate, under heat treatment of 120 to 200°C.
DE 35 03 457 A discloses a process for impregnating organic fibers wherein an organopolysiloxane having amino groups, such as aminoethylaminopropyl groups, is crosslinked with hydrosiloxane in the,presence of metal-containing catalysts, such as dibutyltin dilaurate.
EP 1 096 059 A describes an aqueous emulsion for treating polyester fibers which contains a mixture of an emulsion of an amino-functional organopolysiloxane having alkoxy groups and an emulsion of an amino-functional organopolysiloxane having hydroxyl groups. The two organopolysiloxanes first have to be conveniently prepared by reaction of a,co-dihydroxydimethyl-polysiloxanes with N-(2-aminoethyl)(3-aminopropyl)methyldi-methoxysilane or by reaction of a,co-dihydroxydimethylpoly-siloxanes or cyclic dimethylpolysiloxanes with the hydrolysis or condensation product of N-(2-aminoethyl)(3-aminopropyl)-methyldimethoxysilane, respectively.
High molecular weight linear polysiloxanes are obtained, but not crosslinked films insoluble in toluene.
The present invention has for its object to provide a process for treating fiberfill fibers with aqueous dispersions of organopolysiloxanes without use of metal-containing catalysts. The present invention further has for its object to provide a

process for treating fiberfill fibers with aqueous dispersions of organopolysiloxanes wherein the aqueous dispersions of organopolysiloxanes form elastomeric films insoluble in toluene after the water has been removed and this treatment endows the fiberfill fibers with a permanent soft hand and good bulk. The present invention further has for its object to provide a process for treating fiberfill fibers with aqueous dispersions of organopolysiloxanes wherein the dispersions are obtained by a simple process, wherein no costly or inconvenient chemical reactions have to take place, wherein the treatment of the fiberfill fibers can be effected using short residence times and wherein the treatment of the fiberfill fibers can take place at low temperatures as well as at high temperatures and the fiberfill fibers thus treated exhibit less or lower
yellowing.
The present invention further has for its object to provide aqueous dispersions of organopolysiloxanes for treatment of fiberfill which are finely divided, stable and preferably pH-neutral (pH range about 5-9) and which are free or almost free of volatile organic compounds (VOCs).
We have found that this object is achieved by the present invention.
The present invention accordingly provides a process for treating fiberfill fibers with aqueous dispersions of organopolysiloxanes obtainable by reaction of
organopolysiloxanes (1) comprising condensation-capable groups and units of the general formula
where
R is a hydrogen atom or a monovalent hydrocarbyl radical of 1
to 18 carbon atoms which is optionally substituted with the
heteroatoms N and/or 0,
R1 is a hydrogen atom or an alkyl radical with 1 to 8 carbon

atoms, preferably a hydrogen atom or a methyl or ethyl radical,
a is 0, 1, 2 or 3, and
b is 0, 1 or 2,
with the proviso that the sum a+b is organopolysiloxane (1) contains on average at least one OR1
radical, preferably in the meaning of R1 as a hydrogen atom,
per molecule,
with silanes (2) of the general formula
(R30)3SiCR22-Y (II) or their hydrolyzates,
where R2 is a hydrogen atom or a monovalent alkyl radical of 1
to 4 carbon atoms, preferably a hydrogen atom,
R3 is an alkyl radical having 1 to 8 carbon atoms per radical,
Y is a radical of the formula -NHR4,-NR42 OR -NR5, where R4 is a
monovalent hydrocarbyl radical of 1 to 18 carbon-atoms which
optionally contains nitrogen and/or oxygen atoms, and
R5 is a divalent hydrocarbyl radical of 3 to 12 carbon atoms
which optionally contains nitrogen and/or oxygen atoms,
in the presence of water (3),
emulsifier (4)
and optionally further silanes (5) of the general formula
(R30)xR3_xSi-R6-Z (III) or their hydrolyzates,
where R6 is a divalent hydrocarbyl radical of 2 to 18 carbon
atoms and
2 is a radical selected from the group consisting of amino or
aminoalkylamino radicals, epoxy radicals and (meth)acryloyloxy
radicals, and
x is 1, 2 or 3, preferably 2 or 3,
and optionally further materials (6) which do not take part in
the reaction of organopolysiloxane (1) with silane (2),
with the proviso that no metal-containing catalysts are used
and that the organopolysiloxanes (1) and silanes (2) are used

in such amounts that the organopolysiloxanes after removal of water (3) form elastomeric films insoluble in toluene.
It is surprising that a simple reaction of just 2 components -unlike the two reactions in EP 1 096 059 A and also unlike the reaction described in DE 10 2004 038 148 A - provides aqueous dispersions of high molecular weight, partially crosslinked particles of polymer which, after removal of water, preferably by evaporation, provide an elastic film with formation of a high molecular weight elastic network and endow the fiberfill fibers treated therewith with a permanent soft hand.
In the process of the present invention, the reaction of organopolysiloxane (1) with silane (2) can be carried out not only before the emulsion is produced but also by initially emulsifying the organopolysiloxane (1) which then reacts in emulsion droplets with the silane (2).
The dispersions of the present invention contain precrossiinked organopolysiloxanes which, after removal of water, form elastomeric films containing crosslinked organopolysiloxanes comprising high molecular weight branched or dendrimerlike ultrabranched structures. No viscosity measurement is possible on these elastomeric films. The polymeric siloxane networks of the elastomeric films are typically insoluble in organic solvents, such as toluene, although they may possibly swell therein, which for the purposes of this invention is likewise to be understood as insoluble. This is in contrast to uncrosslinked organopolysiloxanes which can also be highly viscous but for which a viscosity measurement is possible and which are soluble in organic solvents, such as toluene.
It is surprising that aqueous dispersions of crosslinked organopolysiloxanes are obtainable by this process because it is stated in A. Adima et.al., Eur. J. Org. Chem. 2004, 2582-

2588 that α-aminomethyltrialkoxysilanes decompose in the presence of water to form Si02 and the corresponding methylated amine.
Preferably, the dispersions of the present invention are aqueous suspensions or aqueous emulsions of organopolysiloxanes .
The dispersions of the present invention form an elastic network of silicone as they dry - without addition of catalyst or change in pH. Preferably only two (mutually reacting) components are required to prepare the crosslinked organopolysiloxanes of the present invention:
organopolysiloxanes (1) having condensation-capable groups, and crosslinkers (2). These components preferably react with each other at as low a temperature as room temperature. No metal-containing additional catalysts are required to support this reaction. The reaction further preferably proceeds in the neutral range, i.e., in the pH range of about 5 to 9, which results autogenously due to the components themselves. Moreover, the high reactivity means that there is no need for specific management of the chemical reaction, nor preferably for any heating.
The dispersion of the present invention is notable for its high stability in storage, even at elevated temperature, and for its high stability to shearing. The process of the present invention has the advantage that dispersions of high solids content and filler content can be obtained. The nonvolatiles content of the dispersion is preferably about 1% to 99% by weight, preferably 3 0% to 95% by weight and more preferably greater than 50% by weight, based on the total weight of the dispersion.
The process of the present invention does not utilize any

metal-containing catalysts; that is, preferably no transition metals of transition group VIII of the periodic table and their compounds and no metals of main groups III/ IV and V of the periodic table and their compounds are used. The elements C, Si, N, and P do not count as metals in this definition.
Examples of hydrocarbyl radicals R are alkyl radicals, such as methyl, ethyl, n-propyl, isopropyl, 1-n-butyl, 2-n-butyl, isobutyl, tert-butyl, n-pentyl, isopentyl, neopentyl, tert-pentyl; hexyl, such as n-hexyl; heptyl, such as n-heptyl; octyl, such as n-octyl and isooctyl, such as 2,2,4-trimethyl-pentyl; nonyl, such as n-nonyl; decyl, such as n-decyl; dodecyl, such as n-dodecyl; octadecyl, such as n-octadecyl; cycloalkyl, such as cyclopentyl, cyclohexyl, cycloheptyl and methylcyclohexyl; alkenyl, such as vinyl, 5-hexenyl, cyclohexenyl, 1-propenyl, allyl, 3-butenyl and 4-pentenyl; aryl, such as phenyl, naphthyl, anthryl and phenanthryl; alkaryl, such as o-, m-, p-tolyl; xylyl and ethylphenyl; and aralkyl, such as benzyl, α-phenylethyl and (i-phenylethyl.
Preference for use as R radical is given to methyl, ethyl, octyl and phenyl, with methyl and ethyl being particularly preferred.
Examples of N- or O-substituted hydrocarbon radicals R are hydrocarbyl radicals substituted with amino groups and polyethoxy or polypropoxy or polyethoxy-polypropoxy groups. Examples of amino-substituted radicals R are radicals of the formula -R6-NR72,
where R6 is as defined above and each R7 is the same or different and represents a hydrogen atom or an alkyl or aminoalkyl or iminoalkyl radical. N-(2-Aminoethyl) (3-aminopropyl) is a preferred example.
Preferably, R1 is a hydrogen atom. Examples of alkyl R1 are the

alkyl radicals recited above for R, and methyl or ethyl is preferred.
Preferably, R2 is a hydrogen atom.
Examples of alkyl radicals R having 1 to 8 carbon atoms also apply in full to alkyl radicals R3. Preferred examples of alkyl radicals R3 are the methyl and ethyl radical.
Examples of hydrocarbyl radicals R, such as alkyl, cycloalkyl,
aryl, alkaryl and aralkyl radicals, hold in full for
hydrocarbyl radicals R4. Preferred examples of alkyl radicals R4
are methyl, ethyl, butyl, hexyl, and octyl radicals, and a
preferred example of cycloalkyl radicals R4 is the cyclohexyl
radical.
A preferred example of R5 is the radical of the formula -CH2-CH2-0-CH2-CH2- .
Preferred examples of Y radicals are morpholino, piperazino, piperidino and cyclohexylamino radicals,
Preferably, R6 is an alkylene radical, more preferably a radical of the formula -CH2CH2CH2-.
Preference for use as organopolysiloxanes (1) is given to siloxanes of the general formula
(R10)R2SiO(SiR20)eSiR2(OR1) (IV) ,
where R and R1 are each as defined above and
e is an integer from 1 to 1000,
with the proviso that 25 to 100% and preferably 50 to 100% of
all R1 radicals are hydrogen atoms.

Futher examples of organopolysiloxanes (1) are resins of the general formula
[(R3SiO1/2)f (R2Si02/2)g (R1Si03/2)h (Si04/2)k] (V)
where R is as defined above and additionally R in formula (V)
can also be (OR1) as defined above, with the proviso that at
least one -OR1, where R1 is a hydrogen atom, is present per
molecule,
f, g, h and k are each an integer from 0 to 100 0 and
h/(f+g+h+k) is preferably > 0.2.
Examples of siloxanes (1) are commercially available . polydimethylsiloxanes having terminal .silanol groups and polydimethylsiloxanes having terminal alkoxy groups.
Further examples of siloxanes (1) are commercially available functionalized siloxanes, such as amine oils, for example amine oils having 3- (2-aminoethyl)aminopropyl functions, glycol oils, phenyl or phenylmethyl oils containing silanol or alkoxy groups.
Further examples of organopolysiloxanes (1) are resinous siloxanes, such as methylsilicone resins, having 80 mol% of CH3S103/2 and 20 mol% of (CH3)2Si02/2 and a molar mass of about 5000 g/mol or 98 mol% of CH3Si03/2 and 2 mol% of (CH3) 2Si02/2 and a molar mass of about 5000 g/mol, or for example methylphenyl silicone resins having 65 mol% of C6H5Si03/2 and 35 mol% of (CH3) 2Si02/2/ whose remaining free valences bear R10- groups of the abovementioned meanings.
These compounds are commercially manufactured in large volumes, and are available at very low cost, so that the dispersions used in the process of the present invention can likewise be produced at low cost.

These dispersions can be produced using one kind of organopoly-siloxane (1) or different kinds of organopolysiloxane (1) .
The organopolysiloxanes (1) used preferably have viscosities in the range from 1 mPa.s to 5 000 000 mPa.s at 25°C, preferably 50 mPa.s to 100 000 mPa.s at 25°C and more preferably 100 mPa.s to 10 000 mPa.s at 25°C.
The present invention's process for preparing the dispersion can utilize one kind of silane (2) or different kinds of silane (2).
Preferably, the -CR 2-Y radical in silane (2) of formula (II) is a radical of formula -CH2-Y.
Examples of -CR22-Y radicals in silane' (2) of formula(ll) are' aminomethyl, methylaminomethyl, dimethylaminomethyl, diethylaminomethyl, dibutylaminomethyl, cyclohexylaminomethyl, morpholinomethyl, piperidinomethyl, piperazinomethyl, ( (diethoxymethylsilyl) methyl) eye lohexyl aminomethyl, ((triethoxysilyl)methyl)cyclohexylaminomethyl, anilinomethyl, 3-dimethylaminopropylaminomethyl and bis(3-dimethylaminopropyl)aminomethyl.
Examples of silanes (II) are
dibutylaminomethyltriethoxysilane,
dibutylaminomethyltributoxysilane,
eyelohexylaminomethyltrimethoxysilane,
cyclohexylaminomethyltriethoxysilane,
anilinomethyltriethoxysilane,
morpholinomethyltriethoxysilane,
morpholinomethyltrimethoxysilane,
morpholinomethyltriisopropoxysilane,
3-dimethylaminopropylaminomethyltrimethoxysilane,
ethylcarbamoylmethyltrimethoxysilane,
morpholinomethyltributoxysilane,

morpholinomethyltrialkoxysilane, where the alkoxy radical is a
C1-C4-alkoxy radical, in particular a mixture of methoxy and
ethoxy, bis (dimethylaminopropyl) aminomethyltriethoxysilane,
diisopropylaminomethyltriethoxysilane,
piperazinomethyltriethoxysilane,
piperidinomethyltriethoxysilane
bis(diethoxymethylsilylmethyl)cyclohexylamine,
bis(triethoxysilylmethyl)cyclohexylamine,
morpholinomethyltri(2-hydroxyethoxy)silane
Preference is given to silanes (2) of formula (II) wherein the (R30)- radical is an ethoxy group.
The silanes (2) of formula (II)- may contain up' to 30% by weight of difunctional silanes of formula
(R30)2RSiCR22-Y (II') or their hydrolyzates.
The silane of formula (II7) has a chain-extending effect for organopolysiloxanes (1), but does not disrupt the crosslinking reaction of silane of formula (II) with the chain-extended organopolysiloxane (1). Crosslinked organopolysiloxanes in accordance with the present invention are obtained.
The degree of crosslinking depends on the starting ratio of the equivalents of -OR3 in silane (2) of formula (II) to -OR1 in organopolysiloxane (1) of formula (I).
The dispersions of the present invention are prepared from organopolysiloxane (1) and silane (2) by using silane (2) or its partial hydrolyzates preferably in amounts of at least 0.6 equivalent of -OR3, preferably at least 0.7 equivalent .of -OR3, more preferably 0.6 to 2 equivalents of -OR3, especially 0.65 to 1 equivalent of -OR3, and even more preferably 0.7 to 0.99

equivalent of -OR3, per equivalent of -OR1 in organopolysiloxane (1) , where R1 in (1) is preferably a hydrogen atom.
The crosslink frequency depends not only on the chain lengths of the organopolysiloxanes (1) but also on the stoichiometry of the mutually reacting SiOR1 groups of organopolysiloxane (1) and the SiOR3 groups of silane (2) . High degrees of crosslinking are achieved when equal numbers of the SiOR1-groups of organopolysiloxane (1) and SiOR3 groups of silane (2) react with each other. Losses due to volatility or secondary reactions may for this purpose require a stoichiometric ratio other than 1.0:1.0. If desired, a stoichiometric excess of SiOR3 groups from silane (2) to SiOR1 groups from organopolysiloxane (1) can be used. It.was determined that, surprisingly, elastic films are obtainable even from a stoichiometric deficiency of SiOR3 groups from silane (2) to SiOR1 groups from organopolysiloxane (1), for example 0.7:1.0.
The dispersions of the present invention are produced by
intensive mixing of organopolysiloxanes (1) with
silanes (2),
water (3),
emulsifiers (4),
if appropriate further silanes (5),
and if appropriate, further materials (6). Production can be
batchwise or continuous, as described for example in
DE 102004023911 A or equivalently WO 2005100453.
Technologies for producing dispersions or emulsions of organopolysilpxanes are known. The intensive mixing and dispersing can take place in rotor-stator stirrers, colloid mills, high-pressure homogenizers, microchannels, membranes, jet nozzles and the like, or ultrasonically. Homogenizing instruments and processes are described for example in Ullmann's Encyclopedia of Industrial Chemistry, CD-ROM edition

2003, Wiley-VCH, under the headword of "Emulsions".
Although the silanes (2) are known to contain hydrolysis-sensitive groups, particularly when R3 is a hydrogen atom or a methyl or ethyl radical, surprisingly crosslinked organopoly-siloxanes are obtained even in the presence of water by reaction with two or more organopolysiloxanes (1).
The manner of mixing the components to produce the dispersions of the present invention is not very critical, and can be performed in various orders. However, depending on the components (1), (2), (3), (4), if appropriate (5) and if appropriate (6), there may be preferred procedures which should be examined in the individual case.
For example, components (1) and (2) can be premixed with each other, then the emulsifier(s) (4) added and thereafter the water (3) and if appropriate further materials (5) and (6) be incorporated. It is also possible to meter the components (1) and (2) and also (3) to (6) into the emulsifying apparatus in succession. In particular cases, it can be advantageous, for example owing to the siloxane viscosity or reactivity, to mix silane (2) with an organopolysiloxane (1) and thereafter to incorporate another organopolysiloxane (1), or vice versa, depending on what results in better rheological properties for processing the components.
In the case of very reactive silanes (2), it can be advantageous first to convert component (1) with emulsifier (4) and the water (3) into a stiff phase and thereafter to meter the silane (2) pure or diluted in an inert material (6) before, if appropriate, further dilution with water.
It is also possible to add silane (2) into the final emulsion of organopolysiloxanes (1) in order that the desired reaction

and crosslinking of the organopolysiloxane (1) in the emulsion may thereby be achieved. The silane (2) may further be partially or completely hydrolyzed beforehand, by addition of water. To obtain VOC-free hydrolyzate of silane (2), the byproduct alcohol R3OH can be partially or completely removed by suitable known measures such as distillation, membrane processes or other separation processes.
The process of the present invention employs water (3) in amounts of preferably 1% to 99% by weight and more preferably 5% to 95% by weight, all based on the total weight of all ingredients of the dispersion.
Preferably, the process for producing dispersions can be carried out continuously. Preferably, the organopolysiloxanes (1) required for preparing the dispersion are prepared continuously and forwarded continuously to the emulsifying apparatus and, before emulsification, are mixed continuously with silanes (2), emulsifiers (4) and at least some of the water as dispersion medium (3), and this mixture is fed continuously to a first high-shear mixer and a viscous phase is formed in the mixer, the pressure and temperature downstream of the mixture being measured and closed-loop controlled such that a qualitatively high-value and very finely divided dispersion is produced. Further silanes (5) and further materials (6) can be added upstream or downstream of the first high-shear mixer. If appropriate, the emulsion downstream of the first high-shear mixer can be further diluted by admixture of water.
The process of the present invention may utilize as emulsifiers (4) any previously known, ionic and nonionic emulsifiers (not only individually but also as mixtures of different emulsifiers) with which aqueous dispersions, in particular aqueous emulsions of organopolysiloxanes, have hitherto been obtainable.

Examples of anionic emulsifiers are:
1. Alkyl sulfates, particularly those having a chain length of 8 to 18 carbon atoms, alkyl and alkaryl ether sulfates having 8 to 18 carbon atoms in the hydrophobic radical and 1 to 40 ethylene oxide (EO) or propylene oxide (PO) units.
2. Sulfonates, particularly alkyl sulfonates having 8 to 18 carbon atoms, alkylaryl sulfonates having 8 to 18 carbon atoms, taurides, esters and monoesters of sulfosuccinic acid with monohydric alcohols or alkylphenols having 4 to 15 carbon atoms; if appropriate, these alcohols or alkylphenols may also be ethoxylated with 1 to 40 EO units.
3. Alkali metal and ammonium salts of carboxylic acids having 8 to 2 0 carbon atoms in the alkyl, aryl, alkaryl or aralkyl radical.
4. Phosphoric partial esters and their alkali metal and ammonium salts, particularly alkyl and alkaryl phosphates having 8 to 2 0 carbon atoms in the organic radical, alkyl ether or alkaryl ether phosphates having 8 to 2 0 carbon atoms in the alkyl or alkaryl radical and 1 to 40 EO units.
Examples of nonionic emulsifiers are:
5. Polyvinyl alcohol still having 5 to 50% and preferably 8 to 2 0% of vinyl acetate units and a degree of polymerization in the range from 500 to 3000.
6. Alkyl polyglycol ethers, preferably those having 3 to 40 EO units and alkyl radicals of 8 to 20 carbon atoms.
7. Alkyl aryl polyglycol ethers, preferably those having 5 to

4 0 EO units and 8 to 2 0 carbon atoms in the alkyl and aryl radicals.
8. Ethylene oxide/propylene oxide(EO/PO) block copolymers, preferably those having 8 to 40 EO and/or PO units.
9. Addition products of alkylamines having alkyl radicals of 8 to 22 carbon atoms with ethylene oxide or propylene oxide.

10. Fatty acids having 6 to 24 carbon atoms.
11. Alkylpolyglycosides of the general formula R*-0-Zo, where R* is a linear or branched, saturated or unsaturated alkyl radical having on average 8-24 carbon atoms and Z0 is an oligoglycoside radical having on average o = 1-10 hexose or pentose units or mixtures thereof.
12. Natural materials and their derivatives, such as lecithin, lanolin, saponines, cellulose; cellulose alkyl ethers and carboxyalkylcelluloses whose alkyl groups each have up to 4 carbon atoms.
13. Linear organo(poly)siloxanes containing polar groups, containing in particular the elements 0, N, C, S, P, Si, particularly those linear organo(poly)siloxanes having alkoxy groups with up to 24 carbon atoms and/or up to 4 0 EO and/or PO groups.
Examples of cationic emulsifiers are:
14. Salts of primary, secondary and tertiary fatty amines
having 8 to 24 carbon atoms with acetic acid, sulfuric acid,
hydrochloric acid and phosphoric acids.
15. Quaternary alkyl- and alkylbenzeneammonium salts, in

particular those whose alkyl groups have 6 to 24 carbon atoms, particularly the halides, sulfates, phosphates and acetates.
16. Alkylpyridinium, alkylimidazolinium and alkyloxazolinium
salts, in particular those whose alkyl chain has up to 18
carbon atoms, specifically the halides, sulfates, phosphates
and acetates.
Useful ampholytic emulsifiers include in particular:
17. Amino acids with long-chain substituents, such as N-alkyl-di(aminoethyl)glycine or N-alkyl-2-aminopropionic acid salts.
18. Betaines, such as N- (3-acylamidopropyl) -N,N-dimethyl-ammonium salts having a C8-C18-acyl radical and alkylimidazoliuir
betaines.
Preference for use as emulsifier is given to nonionic emulsifiers, in particular the alkyl polyglycol ethers recited above under 6.
The constituent (4) can consist of one of the abovementioned emulsifiers or of a mixture of two or more of the abovementioned emulsifiers, it can be used in pure form or as solutions of one or more emulsifiers in water or organic solvents.
The process of the present invention utilizes the emulsifiers (4) in amounts of preferably 0.1% to 60% by weight and more preferably 0.5% to 30% by weight, all based on the total weight of organopolysiloxanes (1) and silanes (2) .
When the organopolysiloxane (1) or the silane (2) or the resulting crosslinked organopolysiloxane itself acts as an emulsifier, the addition of separate emulsifier (4) can be dispensed with.

Further silanes (5) of formula (III) can be used in the preparation of the dispersions of the present invention. Silanes (5) act as adhesion-promoting silanes. They can be used in addition to silane (2) and in the case of x = 3 can act as additional crosslinkers.
Z in formula (III) is preferably a radical of formula -NR72, where each R7 is the same or different and represents a hydrogen atom or an alkyl or aminoalkyl or iminoalkyl radical. A preferred example of the Z radical is the radical of the formula -NH (CH2) 2NH2 . Preferably, x is 2.
Preferably, R6 in formula (III) is a radical of.formula -CH2CH2CH2- .
Examples of silane (5) are
(3-methacryloxypropyl)trimethoxysilane,
3-aminopropyltrimethoxysilane,
3-(cyclohexylamino)propyltrimethoxysilane
N-(2-aminoethyl)(3-aminopropyl)methyldimethoxysilane,
N- (2-aminoethyl) (3-aminopropyl) methyldiethoxysilane,
N-(2-aminoethyl)(3-aminopropyl)trimethoxysilane,
N-(2-aminoethyl)(3-aminopropyl)triethoxysilane and
(3-glycidoxypropyl)triethoxysilane.
Examples of water-miscible liquids useful as further materials (6) are acids, such as formic acid, acetic acid, propionic acid, oxalic acid and citric acid and silicone- or non-silicone-containing emulsions.
Useful further materials (6) further include commercially available preservatives for dispersions, such as isothiazolinones or parabens, or their aqueous formulations.

The dispersions can be produced as dispersions of undiluted crosslinked organopolysiloxanes, but a dilution with organic solvents or low-viscosity oligomers/polymers is sometimes advisable for handling reasons.
Examples of water-immiscible liquids useful as further materials (6) are therefore organic solvents, such as toluene, n-hexane, n-heptane and technical-grade benzine fractions and low-viscosity oligomers/polymers, such as silicone oils, preferably siloxanes, such as dimethylpolysiloxanes.
Examples of water-soluble solids useful as further materials (6) are ammonium phosphates and polyphosphates, ammonium formates and lithium formate, which can act, as antistats and/or flame-inhibitingly.
Examples of water-insoluble solids useful as further materials (6) are reinforcing and nonreinforcing flame-inhibiting fillers. Examples of reinforcing fillers, i.e., fillers having a BET surface area of at least 50 m2/g, are fumed silica, precipitated silica or silicon-aluminum mixed oxides having a BET surface area of more than 50 m2/g and silicone particles, such as MQ resins. The fillers mentioned may be in a hydrophobicized state. Examples of nonreinforcing and partly also flame-inhibiting fillers, i.e., fillers having a BET surface area of less than 50 m2/g, are powders of quartz, chalk, Cristobalite, diatomaceous earth, calcium silicate, zirconium silicate, montmorillonites, such as bentonites, zeolites, metal oxides, such as aluminum oxide or zinc oxide or mixed oxides thereof or titanium dioxide, metal hydroxides, such as aluminum hydroxide, barium sulfate, calcium carbonate, gypsum, silicon nitride, silicon carbide and boron nitride.
The emulsifying operation to produce the dispersion is preferably carried out at temperatures below 12 0°C, more preferably at 5°C to 100°C and even more preferably at 10°C to

80°C. The temperature increase preferably comes about through input of mechanical shearing energy, which is needed for the emulsifying operation. The temperature increase is not needed to speed a chemical process. The dispersion is preferably-carried out at the pressure of the ambient atmosphere, but can also be carried out at higher or lower pressures.
The dispersion used for the process of the present invention has the advantage that it can be obtained without addition of catalysts, in particular without addition of metal catalysts. The reaction of (1) with (2) preferably goes to completion within a few minutes to several hours, with methoxysilanes again reacting faster than ethoxysilanes. The condensation can be speeded by means of acids and bases.
The alcohols generated as condensation by-products in the course of the preparation of the dispersion can remain in the dispersion or else be removed, for example by vacuum distillation, membrane processes or by extraction.
The average particle size measured in the dispersions by means of light scattering is in the range from 0.001 to 100 µm, preferably in the range from 0.002 to 10 µm. The pH can vary from 1 to 14, preferably from 3 to 9 and more preferably from 5 to 9.
Examples of fiberfill fibers treated with the dispersions of
the present invention are those of polyester, polyamide,
polylactate(PLA), polybutyric acid, polyolefins, viscose, modal
and lyocell.
Preference is given to fiberfill fibers of polyester.
The fiberfill fibers are preferably staple fibers or crimpled
staple fibers from which a bulky wadding is produced by opening
and random-laying on cards. This bulky wadding can be used as
batting, fill material or cushioning/padding material in

cushions, pillows, padding, blankets, quilts, duvets, mattresses, sleeping bags, insulating apparel (examples being coats, sport anoraks).
The fiberfill fibers may be treated by contacting the fiberfill fibers with the dispersions of the present invention by dipping, spraying, rolling, printing, padding or curtain coating, preferably by applying the aqueous dispersions to the fiberfill fibers via spraying, dipping, padding or curtain coating. Thereafter, the water (3) is removed.
Preferably, the water is removed by allowing the fiberfill
fibers to dry at a temperature of 1 to 23 0°C, preferably 30 to
180°C and more preferably in the temperature range from 70 to
120°C.
The drying time is dependent on parameters such as, for
example, temperature, air circulation, substrate thickness and
add-on.
After drying, the dispersions of the present invention remain
as a film on the surface of the fiberfill fibers.
The process of the present invention has the advantage that the fiberfill fibers treated with the dispersions of the present invention have a permanent soft hand, enhanced elasticity, luster and smoothness, reduced frictional resistance and also improved hydrophobicity and soil rejection. The film obtained from the dispersion by the evaporation of water adheres firmly to the fiberfill fibers and endows the surface of the fiberfill fibers with a particularly soft smoothness and elasticity coupled with resiliency.
Owing to the good permanent adhesion to the fiber, the fiberfill fiber has good carding properties in that there is virtually no rub-off/deposition of silicone polymers on the card clothing which would require the cards to be switched off and an increased cleaning effort.

Operative methods in lab:
Film formation test:
The amount of emulsion which produces about 1 g of residue is weighed out; for example about 1.5 g in the case of a 66% emulsion and about 2 g in the case of a 50% emulsion. This amount is diluted 1:1 with water and poured into a tinplate lid
(10 cm in diameter) . The product is distributed over the entire surface by tilting the lid and the sample is placed open in a fume hood (at room temperature for 24 h or in a drying cabinet at 120°C or 170°C for 20 min).
The evaluation is performed when the water or; solvent has completely evaporated. Ratings from 1 to 5 are awarded
(ratings: 1 = oily, uncrosslinked, 2 = oily, viscid, 3 = viscous, incipiently crosslinked, 4 = incipiently crosslinked, tacky, 5 = firm with tack-free dry surface).
Fiberfill finish:
For finishing, 117 g of the dispersions described in the inventive and comparative examples were diluted with completely ion-free water to 1000 g and 400 ml thereof were introduced as initial charge into all glass beaker. Crimped polyester staple fibers having a linear density of 61 dtex and a staple length of 50 mm are opened on a card or on a willowing machine to form bulky wadding. 20 g of this fiber are dipped into the glass beaker for 1 minute and completely wetted. The wet fiber is then removed and whizzed in a salad spinner to remove only sufficient liquid to keep a weight increase of 70%. To remove the rest of the water and to complete curing, the moist fibers are placed for 10 min in a drying cabinet (selectively at 120 or 170°C) or selectively the treated fibers were spread out and dried at 23°C for 24 hours.

Extraction with Soxhlet apparatus:
To investigate permanence, 10 g of fiberfill material (with or without silicone finish) were extracted for 3 hours in a 500 ml round-bottomed flask by refluxing with 22 0 g of hexane and the residue after the hexane had been evaporated was determined.
Production of film-forming silicone dispersions:
Example 1:
In an Ultra-Turrax T 50 emulsifying apparatus (from Janke & Kunkel/IKA), 5 g of isotridecyl decaethoxylate, 85% in water, commercially available under the trade name of Lutensol TO 109 (from BASF) and 8 g of ion-free water are combined to prepare an emulsifier mixture which is admixed with 100 g of a freshly prepared homogeneous siloxane polymer/silane mixture consisting of 99.65 g of polydimethylsiloxanediol containing 1100 weight ppm of terminal OH groups, as siloxane (1), and 0.39 g of N-morpholinomethyltriethoxysilane (molar mass 263 .4) as silane (2), by metered addition. This is followed by portionwise dilution with altogether 90.1 g of completely ion-free water to obtain a milkily white emulsion having an average particle size of 309 nm. The solids content of the emulsion is 50.7%, the pH is 6.0. The emulsion is homogeneous and stable even after 6 months of storage at room temperature.
When 0.5 g of this emulsion is poured into 8 g of tetrahydro-furan, a precipitate of the crosslinked and THF-insoluble organopolysiloxane elastomer forms immediately. Nor does the precipitate redissolve within 24 h.
Evaporating the emulsion gives after a drying time of 24h/25°C a gel-like elastic film which firmly adheres to glass or aluminum.

Examples 2 to 6:
Further emulsions are prepared similarly to Example 1, using the amounts reported in table 1.

The solids content is determined at 150°C to constant weight using a Mettler Toledo HR 73,
Particle size is determined using a Coulter N4 plus.
Example B6 utilizes two siloxanes (la, lb);
siloxane (lb) is a copolymer of 3-(2-aminoethylamino)propyl-
methylsiloxy and dimethylsiloxy units having an amine number of
0.145, a viscosity of 4700 mm2/s (at 25°C) and an OH/OMe end
group ratio = 54/46;
siloxane (la) used is:

polydimethylsiloxanediol containing 1100 weight ppm of terminal OH groups.
Silane (2) used is: N-Morpholinomethyltriethoxysilane
The elasticity of the films produced from the emulsion decreases with increasing amount of silane (2) from Bl to B5.
The elastomeric film produced from the dispersion B3 is cut apart and placed in toluene for 24 h. The cut edges are afterwards still sharp. The film has swollen, but has not dissolved in toluene.
Comparative test la-le to EP 828 794 A and EP 655 475 Al:
The procedure of Example B3 is repeated except that 0.60 g of morpholinomethyltriethoxysilane, the inventive silane (2), is replaced by the component reported in table 2 :
Comparison la:
0.60 g of vinyltrimethoxysilane (VTMO) as per Example 1 of
EP 828 794 A
Compari son lb:
0.34 g of vinyltrimethoxysilane (molar mass 148.2) (0.34 g = 1.1 equivalents of Si-OCH3 of vinyltrimethoxysilane based on 1 equivalent of SiOH of siloxane (1) similarly to Example B3)
Comparison lc:
0.60 g of a,αω—dimethoxypoly(N- (2-aminoethyl) -3-aminopropyl-
methylsiloxane) as per Example 1 of EP 828 794 A

Comparison Id:
0.60 g of a resin mixture as per Example 1 of EP 655 475 Al consisting of 16 parts of organopolysiloxane resin of formula [ (CH3) 3SiO1/2] [Si02] having an average molecular weight of 2000 and an average ethoxy content of 2.1 percent by weight, based on the resin molecule and 17 parts of organopolysiloxane resin of formula [(CH3)2SiO]0,2 [(CH3) Si03/2] 0,8 having an average molecular weight of 3 000 and an average ethoxy content of 2.6 percent by weight, based on the resin molecule.
Comparison le:
Similarly to Comparison V Id except that KOH is added to the
resin mixture and the pH is 11.
Comparison If:
0.60 g of a 1:1 mixture of vinyltrimethoxysilane (VTMO) and
a,to-dimethoxypoly (N- (2-aminoethyl) -3-aminopropylmethylsiloxane)
as per Example 1 of EP 828 794 A.
The results are summarized in table 2:


1) vinyltrimethoxysilane
2) GF95-H = a,co-dimethoxypoly (N- (2-aminoethyl) -3-
aminopropylmethylsiloxane)
3) resin mixture from Example 1 of EP 655 475 Al (see
description above under Comparison Id))
None of the emulsions form a film on drying. The oily silicones remaining behind are soluble in toluene (tested as 20% solution in toluene), i.e., they are not crosslinked.

Comparative test 2
The viscosity increase after mixing the components siloxane (1)
and silane (2) as per Example B3, i.e., α,ω-dihydroxypoly-
dimethylsiloxane with morpholinomethyltriethoxysilane, was
measured.
For comparison, morpholinomethyltriethoxysilane was replaced by
the component reported in table 3, in V2a-V2f (similarly to the
comparative tests Vla-Vlf) and again the increase in viscosity
was measured.
The results are summarized in table 3.
While the viscosity rises rapidly using the inventive components (1) and (2), similarly to Example 3, and has. doubled after 2 hours and is no longer measurable after just 5 hours, because an elastomer is formed, the viscosity in the case of comparative tests V2a-V2e rises only very gradually and even 7 days later crosslinked elastomeric particles are still to form.



Comparative test 3 as per DE 102004038148 Al
In an Ultra-Turrax emulsifying apparatus T 50 (from Janke & Kunkel/IKA), 9.38 g of isotridecyl decaethoxylate (Lutensol TO 109, from BASF AG), 3.90 g of castor oil ethoxylate G 1300 (from Atlas) and 4.55 g of water are combined to prepare a stiff emulsifier mixture, which is admixed with 125.28 g of a freshly prepared homogeneous polymer/silane mixture of 124.63 g of polydimethylsiloxanediol containing 765 weight-ppm of terminal OH groups as organopolysiloxane (1) and 0.86 g of N-morpholylmethylmethyldiethoxysilane, added by metering. This is followed by portionwise diluting with altogether 106.65 g of water to obtain a stable emulsion having an average particle size of 275 nm. The silicone content of- .the emulsion is 50%.
After standing for 24 h/25°C the emulsion is evaporated and the siloxane polymer is re-extracted with n-heptane to obtain, after evaporation of the solvent, a highly viscous polysiloxane having a viscosity of 3400 Pa.s (25°C), which is soluble in toluene and hence uncrosslinked. The dispersion containing this highly viscous polysiloxane is not in accordance with the present invention.
Example 7
In an Ultra-Turrax T 50 emulsifying apparatus (from Janke &
Kunkel/IKA), 6 g of isotridecyl decaethoxylate, 85% in water,
commercially available under the trade name of Lutensol TO 109
(from BASF), and 6 g of ion-free water are combined to prepare
an emulsifier mixture which is admixed with 60 g of a freshly
prepared homogeneous siloxane polymer/silane mixture consisting
of
33.2% of a polydimethylsiloxanediol (la) containing 1100
weight-ppm of terminal OH groups,
66.41% of a copolymer of 3-(2-aminoethylamino) propylmethyl-

iloxy and dimethylsiloxy units (lb) having an amine number of .145, a viscosity of 4700 mm2/s (25°C) and an OH/OMe end group 'atio = 54/46 and
.39% of N-morpholinomethyltriethoxysilane as silane (2), Ldded by metering. This is followed by portionwise dilution With altogether 23 g of completely ion-free water to obtain a lilkily white emulsion having an average particle size of 110 nm. The emulsion is admixed with 1 g of N-(2-aminoethyl) (3-iminopropyl) methyldimethoxysilane as component (5) and 0.4 g of 50% acetic acid as component (6) by metered addition and stirring. The solids content of the emulsion is 66%, the pH is 7.5. The emulsion is homogeneous and stable even after 6 months Of storage at room temperature.
Example 8
To 97 g of the emulsion of Example 7 are gradually metered, with vigorous stirring, 3 g of N-(2-aminoethyl)(3-aminopropyl)-methyldimethoxysilane as further component (5)- The solids content of the emulsion is about 66%, the pH is 10.5.
Comparative test 4
In an Ultra-Turrax T 50 emulsifying apparatus (from Janke & Kunkel/IKA), 6 g of isotridecyl decaethoxylate, 85% in water, commercially available under the trade name of Lutensol TO 109 (from BASF), and 6 g of ion-free water are combined to prepare an emulsifier mixture which is admixed with 60 g of a freshly prepared homogeneous siloxane polymer/silane mixture consisting of
33.2% of a polydimethylsiloxanediol (la) containing 1100 weight-ppm of terminal OH groups,
66.41% of a copolymer of 3-(2-aminoethylamino)propylmethyl-siloxy and dimethylsiloxy units (lb) having an amine number of 0.145, a viscosity of 4700 mm2/s (25°C) and an OH/OMe end group

ratio = 54/46.
This is followed by portionwise dilution with altogether 23 g of completely ion-free water to obtain a milkily white emulsion having an average particle size of 210 nm. The emulsion is admixed with 1 g of N-(2-aminoethyl)(3-
aminopropyDmethyldimethoxysilane as component (5) and 0.4 g of 80% acetic acid as further component (6) by metered addition and stirring. The solids content of the emulsion is 66%, the pH is 7.5. The emulsion is homogeneous and stable even after 6 months of storage at room temperature.
Comparative test 5
To 91 g of the emulsion of Comparative test 4 are gradually metered, with vigorous stirring, 3 g of N-(2-aminoethyl)(3-aminopropyl)-methyldimethoxysilane as further component (5) . The solids content of the emulsion is about 66%, the pH is 10.5.
Testing of film formation of emulsions of Examples 7 and 8 and Comparative tests 4 and 5:
In accordance with the film-testing method described above, the emulsions of Examples 7 and 8 and Comparative tests 4 and 5 were diluted, weighed into a lid and dried at 23°C/24 h or at 120 or 170°C for 20 min each. The results are summarized in table 4.
While the emulsions of Comparative tests 4 and 5, (even when the amount of N- (2-aminoethyl) (3-aminopropyl)methyl-dimethoxysilane is increased) dry to leave an oily residue, the inventive emulsions of Examples 7 and 8 form a firm film not only at 23°C, at 120°C and also at 170°C. Shortly after drying, the film comprising an increased proportion of N-(2-amino-

r
ethyl)(3-aminopropyl)methyldimethoxysilane (Example 8) is still
very slightly tacky, but becomes dry on storage.
When dried at 120°C, the films remain free of yellowing, while
at 170°C it is possible to observe slight yellowing or marked
yellowing in the case of an increased amount of N-(2-amino-
ethyl)(3-aminopropyl)methyldimethoxysilane.
The emulsions of Examples 7 and 8 thus achieve crosslinking at
low temperature without yellowing, and provide a higher
molecular weight network with film character than the emulsions
of Comparative tests 4 and 5.

*Ratings: 1 = oily, uncrosslinked, 2 = oily, viscid, 3 = viscous, incipiently crosslinked, 4 = elastic, incipiently crosslinked, tacky, 5 = elastic, crosslinked with tack-free dry
surface.
Films awarded a rating of 4 or 5 are insoluble in toluene.
Finishing of fiberfill fibers with the emulsions of Examples 7 and 8 and Comparative tests 4 and 5:
The emulsions of Examples 7 and 8 and Comparative tests 4 and 5 were each used to finish crimped polyester staple fibers having a linear density of 61 dtex and a staple length of 50 mm in accordance with the lab description, and the fibers were dried at 3 different temperatures of 23°, 120° and 170°. After drying, the finished fibers were conditioned for 24 hours

in a conditioning chamber at 23°C 50% relative humidity and manually assessed by 5 people for hand (dryness, softness, slippiness, bulk and resiliency) . To this end, the samples were lined up according to the hand appraisal and a rating scale was established from 1 to 5 where 5 is the softest, most gliding, springy hand with best resiliency and 1 is a dry hand with noticeable permanent deformation and low resiliency. The results are summarized in table 5.
The hand of the fibers finished with Examples 7 and 8 is judged to be soft, gliding, of low friction and full (bulky). More particularly, the good hand is distinctly improved over the noninventive Comparative tests 4 and 5 at room temperature, but in particular at 120°C drying.
Table 5: Comparison of hand of crimped polyester staple fibers
finished with the following emulsions:
i i ——i
The finished fibers were divided and one half of the samples
were enclosed in a laundry bag and washed with a mild detergent
at 40°C (colored setting).
After washing, the bags were emptied and the fibers were dried
and conditioned in a conditioning chamber at 23°C 50% relative
humidity.
The washed samples were then manually assessed for hand against
each other (ratings 1 to 5; 5 the most gliding, most bulky
hand) .

Table 6: Comparison of hand of finished polyester staple fibers after mild washing

After washing, the hand of the fibers treated with Examples 7 . and 8 is distinctly better than in the case of the fibers treated with Comparative tests 4 and 5.
The permanence of the finish on the fiber to hexane as organic cleaning agent was tested by extracting the fiber in a Soxhlet apparatus for 3 hours and determining the amount extracted. The results are summarized in table 7.
Table 7: Comparison of hexane extractables of finished
fibers.

The extractables are distinctly lower at 1.78% and 1.61% in the
















We claim:
1. A process for treating fiberfill fibers with aqueous
dispersions of organopolysiloxanes obtainable by reaction of organopolysiloxanes (1) comprising condensation-capable groups and units of the general formula
where
R is a hydrogen atom or a monovalent hydrocarbyl radical of
1 to 18 carbon atoms which is optionally substituted with
the heteroatoms N and/or 0,
R1 is a hydrogen atom or an alkyl radical with 1 to 8 carbon
atoms, preferably a hydrogen atom or a methyl or ethyl
radical,
a is 0, 1, 2 or 3, and
b is 0, 1 or 2,
with the proviso that the sum a+b is <_ and the> organopolysiloxane (1) contains on average at least one OR1
radical per molecule,
with silanes (2) of the general formula
(R30)3SiCR22-Y (II) or their hydrolyzates,
where R2 is a hydrogen atom or a monovalent alkyl radical of
1 to 4 carbon atoms,
R3 is an alkyl radical having 1 to 8 carbon atoms per
radical,
Y is a radical of the formula -NHR4, -NR42 or -NR5 , where R4
is a monovalent hydrocarbyl radical of 1 to 18 carbon atoms
which optionally contains nitrogen and/or oxygen atoms, and
R5 is a divalent hydrocarbyl radical of 3 to 12 carbon atoms
which optionally contains nitrogen and/or oxygen atoms,
in the presence of water (3),

emulsifier (4)
and optionally further silanes (5) of the general formula
(R30)xR3_xSi-R6-Z (III) or their hydrolyzates,
where R6 is a divalent hydrocarbyl radical of 3 to 18 carbon atoms and
Z is a radical selected from the group consisting of amino or aminoalkylamino radicals, epoxy radicals and (meth)-acryloyloxy radicals, and x is 1, 2 or 3,
and optionally further materials (6) which do not take part in the reaction of organopolysiloxane (1) with sila'ne (2.) , with the proviso that no metal-containing catalysts are used and that the organopolysil.oxanes (1) and silanes (2) are used in such amounts that the org'anopolysiloxanes, after removal of water (3) form elastomeric films insoluble in toluene.
The process according to claim 1 wherein silane (2) is used in such amounts that 0.6 to 2 equivalents of -OR3 are present per equivalent of -OR1 in organopolysiloxane (1) .
The process according to claim 1 or 2 wherein fiberfill fibers comprise fiberfill fibers of polyester, polyamide, polylactate (PLA), polybutyric acid, polyolefins, viscose, modal and lyocell.
The process according to claim 1, 2 or 3 wherein organo-polysiloxanes (1) have the general formula


where R and R1 are each as defined in claim 1 and
e is an integer from 1 to 1000,
with the proviso that 50 to 100% of all R1 radicals are
hydrogen atoms.
The process according to any one of claims 1 to 4 wherein R2 is a hydrogen atom.
The process according to any one of claims 1 to 5 wherein the aqueous dispersions are applied to the fiberfill fibers by spraying, dipping, padding or curtain coating.
The process according to any one of claims 1 to 6 wherein the aqueous dispersions are applied to the fiberfill fibers and the water (3) is subsequently removed from the dispersions whereupon they form elastomeric films insoluble in toluene.
The process according to claim 7 wherein the water (3) is removed by allowing the fiberfill fibers treated with the aqueous dispersions to dry at a temperature of 1 to 230°C/ preferably 30 to 180°C and more preferably 70 to 120°C.
Fiberfill fibers treated by the process according to claims 1 to 8.
Dated this 7 day of November 2007

Documents:

2569-CHE-2007 AMENDED PAGES OF SPECIFICATION 19-01-2012.pdf

2569-CHE-2007 AMENDED CLAIMS 19-01-2012.pdf

2569-CHE-2007 CORRESPONDENCE OTHERS 16-05-2011.pdf

2569-CHE-2007 EXAMINATION REPORT REPLY RECEIVED 19-01-2012.pdf

2569-CHE-2007 FORM-3 19-01-2012.pdf

2569-CHE-2007 OTHER PATENT DOCUMENT 19-01-2012.pdf

2569-CHE-2007 POWER OF ATTORNEY 19-01-2012.pdf

2569-CHE-2007 FORM-3 16-04-2012.pdf

2569-CHE-2007 CORRESPONDENCE OTHERS 16-04-2012.pdf

2569-che-2007-abstract.pdf

2569-che-2007-claims.pdf

2569-che-2007-correspondnece-others.pdf

2569-che-2007-description(complete).pdf

2569-che-2007-form 1.pdf

2569-che-2007-form 18.pdf

2569-che-2007-form 3.pdf

2569-che-2007-form 5.pdf


Patent Number 255471
Indian Patent Application Number 2569/CHE/2007
PG Journal Number 09/2013
Publication Date 01-Mar-2013
Grant Date 25-Feb-2013
Date of Filing 07-Nov-2007
Name of Patentee WACKER CHEMIE AG
Applicant Address HANNS-SEIDEL-PLATZ 4 D-81737 MUNCHEN
Inventors:
# Inventor's Name Inventor's Address
1 WIERER, KONRAD, ALFONS HECKENWEG 2 D-84489 BURGHAUSEN
2 SCHNEIDER, OTTO CARL-BOSCH-STRASSE 6 D-84489 BURGHAUSEN
PCT International Classification Number D06M 13/46
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 102006052730.5 2006-11-08 Germany