US20030164467A1

US20030164467A1 - Flashpointless textile treatment composition, preparation thereof and use thereof

Info

Publication number: US20030164467A1
Application number: US10/365,815
Authority: US
Inventors: Michael Gerle; Winfried Guth; Helmut-Martin Meier; Anton Hermanns; Jan-Dieter Wiechmann
Original assignee: Individual
Current assignee: Bayer AG
Priority date: 2002-02-20
Filing date: 2003-02-13
Publication date: 2003-09-04
Also published as: DE10207087A1; EP1338695A1

Abstract

Disclosed are a flashpointless textile treatment composition, a process for preparing it, its use for treating textile materials and also the treated textile materials.

Description

BACKGROUND OF THE INVENTION

1. Field of the Invention

The present invention relates to a flashpointless textile treatment composition, to a process for preparing it, to its use for treating textiles and to the treated textiles.

2. Brief Description of the Prior Art

Modern textile materials used, for example, as upholstery fabrics or as a textile floor covering are expected by the consumer to have favourable properties with regard to mechanical strength, i.e., their ability to withstand static and dynamic stresses. Especially in the case of pile materials, i.e., textiles which by virtue of loops or cut-open loops (cut pile) have a certain surface texture, it is important that this surface texture be maintained during their period of use. Pile carpet will frequently show signs of damage in the form of a change in surface constitution after a relatively short period of being subjected to foot traffic, the weight of heavy furniture or the movement of chairs equipped with castors. Carpets subjected to such wear exhibit pressure marks and grooves and form tracks of unevenly lying pile where people habitually tread. Upholstery fabrics suffer similar changes in surface constitution, especially in the most readily accessible and most heavily stressed areas. The consequence is a non-uniform appearance of the textile surface.

Textile auxiliaries used for finishing modern textile materials are expected by the user not only to be technically suitable but also to be unproblematical to handle from a safety standpoint. This applies especially to the transport of these auxiliaries. An important aspect of a chemical's safety profile is its flashpoint. The flashpoint is the lowest temperature, corrected to a barometric pressure of 101.3 kPa (760 Torr), at which application of an ignition source causes the vapors of a specimen of the sample to ignite under specified conditions of the test. The test used to determine the flashpoint of flammable liquids is the closed cup test of Pensky-Martens, DIN EN 22 719 (1993), ISO 2719 (1988).

Flammable liquids are defined by the German regulation on flammable liquids (Römpp Lexikon Umwelt, Version 1.0, Stuttgart, N.Y., Georg Thieme Verlag 1997, headwords: “Brennbare Flüssigkeiten” and “TRbF”) as having a flashpoint, being neither solid nor salvelike at 35° C., having a vapor pressure of 3 bar or less at 50° C. and belonging to one of the following hazard classes A or B:

A: Liquids having a flashpoint of 100° C. or less which do not have the properties of hazard class B with regard to water solubility.

A liquids are divided into:

A I: liquids having a flashpoint below 21° C.,

A II: liquids having a flashpoint of 21° C. to 55° C.,

A III: liquids having a flashpoint above 55° C. to 100° C.,

B: Liquids having a flashpoint below 21° C. which are soluble in water at 15° C. or whose flammable liquid constituents are soluble in water at 15° C.

This classification is also significant for the transport regulations governing flammable liquids. It is accordingly advantageous in the light of the transport regulations for a substance to be classified in hazard class A III at least.

DE-A 1 594 985 discloses giving fibrous materials, such as filaments, fibers, fabrics and carpets, antislip and dry-soiling resistance properties by treating these fibrous materials with textile auxiliaries which are colloidal suspensions of silasesquioxanes having the unit formula RSiO _3/2and a particle size in the range of 10 to 1000 angstrom, wherein R represents methyl, ethyl, vinyl, phenyl and/or 3,3,3-trifluoropropyl radicals. These silasesquioxanes are prepared by adding silanes of the formula RSi(OR″)₃, where R″ represents C₁-C₄-alkyl radicals or radicals of the formulae —CH₂CH₂OH, —CH₂CH₂OCH₃, —C(═O)CH₃or —CH₂CH₂OC₂H₅, to a mixture of water and surface-active agents under acidic or basic conditions. However, the silasesquioxane suspensions described there are relatively unstable, in no case suitable for use in pile-stabilizing finishing and what is more have a low flashpoint.

EP-A 0 036 475 describes a textile auxiliary for the pile-stabilizing finishing of textiles composed of manufactured or natural fiber materials and mixtures thereof, which is effective, durable and cleanable. This agent likewise contains colloidal suspensions of organosilasesquioxanes and of silica. The colloidal suspensions are prepared by condensation of silanes of the formula RSi(OR′) ₃together with silanes of the formula Si(OR′)₄. Here, R represents a substituted or unsubstituted C₁-C₇hydrocarbyl radical whose substituents can be halogen atoms or amino, mercapto or epoxy groups, up to 95 mol % of the R radicals being methyl. R′ denotes an alkyl radical of 1-4 carbon atoms. The colloidal suspensions formed in the course of the condensation are directly used as such for textile treatment, but regrettably have a low flashpoint.

It is an object of the present invention to provide a textile auxiliary which is useful as a pile-stabilizing finish, but at the same time is simple to handle safely and, more particularly, ideally is no problem to transport.

This object is achieved by providing flashpointless textile auxiliaries which are easy to store and transport safely.

SUMMARY OF THE INVENTION

The invention accordingly provides flashpointless textile auxiliaries containing aqueous colloidal suspensions of organosilasesquioxanes containing units of the general formula (I)

R¹Si(O)_3/2 (I)

where each

R ¹is the same or different and represents a straight-chain or branched C₁-C₁₈-alkyl radical which may be substituted by one or more identical or different halogen radicals, —NH₂, —SH or epoxy groups and/or in which one or more (CH)₂groups may be replaced by —O—, —S— or —N(H)—.

The flashpointless textile auxiliaries according to the invention are substantially free of an alcohol of the formula R ²OH, where R²represents a straight-chain or branched C₁-C₄-alkyl radical. By “substantially free” is meant that the alcohol content is such as would not adversely affect the nature or use of the flashpointless auxiliaries of the invention as described more fully hereinunder Typically, the flashpointless textile auxiliaries contain not more than 2.5% by weight, preferably not more than 2.2% by weight and especially not more than 2% by weight, each percentage being based on the total textile auxiliary, of an alcohol of the formula R²OH, where R²represents a straight-chain or branched C₁-C₄-alkyl radical.

DETAILED DESCRIPTION OF THE INVENTION

Preference is given to textile auxiliaries according to the invention wherein R ¹is the same or different and represents a straight-chain or branched C₁-C₇-alkyl radical which may be substituted by one or more identical or different halogen radicals, especially F, Cl or Br radicals, —NH₂, —SH or epoxy groups and/or in which one or more (CH)₂groups may be replaced by —O—, —S— or —N(H)—.

Particular preference is given to textile auxiliaries according to the invention wherein each R ¹is the same or different and represents a straight-chain or branched C₁-C₇-alkyl radical which may be substituted by one or more identical or different halogen radicals, especially F, Cl or Br radicals, —NH₂, —SH or epoxy groups and/or in which one or more (CH)₂groups may be replaced by —O—, —S— or —N(H)—.

When the organosilasesquioxanes of the flashpointless textile auxiliary according to the invention contain units of the formula R ¹Si(O)_3/2, where R¹has different meanings, it is customary for up to 95 mol %, preferably 50-94 mol % and more preferably 80-94 mol % of all the R¹radicals to be methyl.

Useful substituents for the R ¹radical, typically for the C₁-C₁₈-alkyl and preferably C₁-C₇-alkyl radical, include particularly the —NH₂radical and also epoxy groups. Useful epoxy groups are those of the formula (II)

where

n is an integer from 1 to 18 and preferably from 1 to 7, and

one or more of the alkylene groups —(CH ₂)— may be replaced by —O—, —S— or —N(H)—.

Particular preference is given to using epoxy groups of the formulae (III) or (IV):

where

x is O, S or NH.

R ¹preferably represents methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, tert-butyl, n-pentyl or 2-ethylbutyl.

The silasesquioxanes in the textile auxiliaries according to the invention have an average particle size of 100-1000 angstrom and preferably 200-600 angstrom, determined by Mie light scattering. Typically, the particle size distribution is very narrow. The specified particle size is important to obtain a stable suspension. Especially higher particle sizes than those specified must be avoided, or the particles will precipitate.

In a further embodiment, the organosilasesquioxanes included in the colloidal suspensions can contain silica units of the formula Si(O ₄)₂as well as units of the formula (I).

The invention further provides a process for preparing these flashpointless textile auxiliaries by

(1) condensing one or more silanes of the general formula (V)

—R¹—Si(OR²)₃ (V)

and optionally one or more silanes of the general formula (VI)

Si(OR²)₄ (VI)

where each

R ¹is the same or different and represents a straight-chain or branched alkyl radical having 1 to 18 carbon atoms which may be substituted by one or more identical or different halogen radicals, —NH₂, —SH or epoxy groups and/or in which one or more (CH)₂groups may be replaced by —O—, —S— or —N(H)— and each

R ²is the same or different and represents a straight-chain or branched C₁-C₄-alkyl radical,

in a mixture of water, a buffer substance and a surface-active substance, and

(2) distilling the resulting mixture of (1) at 55° C. to 100° C. under a pressure of 950 to 250 mbar and under an inert gas stream of 5 to 50 l/h.

The process according to the invention utilizes one or more silanes of the general formula (V) and optionally one or more silanes of the general formula (VI).

Preference is given to using the following silanes of the general formula (V): methyltrimethoxysilane, methyltriethoxysilane, methyltriisopropoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, propyltrimethoxysilane, isobutyltrimethoxysilane, isobutyltriethoxysilane or 2-ethylbutyltriethoxysilane. A particularly useful silane of the general formula (VI) is tetraethoxysilane. These silanes are either commercially available or else preparable by prior art methods familiar to one skilled in the art.

The reaction according to the invention is customarily carried out in the presence of at least one surface-active substance. The surface-active substance used can be selected from cationic or anionic surface-active substances known from the prior art. As well as these cationic or anionic surface-active substances, it is also possible to use nonionic or amphoteric surface-active substances.

Useful anionic surface-active substances include aliphatic and/or aromatic sulphonic acids, for example decyl-, dodecyl-, cetyl-, stearyl-, myristyl- or oleylsulphonic acids and alkali metal salts thereof.

Useful cationic surface-active substances include for example ammonium salts of alkylamines, quaternary ammonium salts, alkylpyridinium salts, imidazole salts, imidazolinium salts, salts of alkyldiamines and of alkylpolyamines, salts of acylated diamines and polyamines, salts of acylated alkanolamines, salts of esters and ethers of alkanolamines, alkanolamine ether salts, alkylethyleneurea salts, sulphonium compounds, phosphonium compounds or amine oxides.

Cationic surface-active substances are advantageously used in the form of their halides and especially chlorides and bromides.

Useful surface-active agents further include for example those of a nonionic or amphoteric nature, which are preferably used in combination with anionic or cationic surface-active agents as long as neither their nature nor their amount adversely affect the stability of the colloidal suspension.

The amount of surface-active substances used should be as low as possible, since excessively high salt concentrations impair the stability of the sol formed in the course of the condensation in step (1). It will be advantageous to use 0.01 to 3% by weight and preferably 0.05-2% by weight of surface-active substance, based on the reaction mixture as a whole.

The surface-active substances mentioned have the function of additionally stabilizing the resulting particles of the colloidal suspension.

Successful practice of the process according to the invention further requires the presence of at least one buffer substance to control the pH value. Useful buffer substances include for example sodium tetraborate, ammonium bicarbonate, sodium bicarbonate or potassium bicarbonate. The buffer substance is used in an amount of 0.05 to 4% by weight and preferably of 0.1-2% by weight, based on the reaction mixture as a whole. The pH value of the reaction mixture in the course of the reaction is in the range of 5-12 and preferably in the range of 8-10. The addition of this buffer provides optimal control of the hydrolysis behaviour of the alkoxysilanes used and of the condensation of the silanol groups, which are both known to be pH dependent.

The amount of silanes of the general formulae (V) and optionally (VI) which is used in the process according to the invention is 0.1-30% by weight and preferably 5-22% by weight, based on the reaction mixture as a whole.

Simultaneous hydrolysis of the silanes of the general formula (V) and optionally (VI) gives rise to interpolymers of the silasesquioxanes, in which the respective R ¹Si(O)_3/2and optionally Si(O₄)₂units can be present in block form or in random distribution. The preferred amount added of silane of the general formula (VI) is in the range of 0-50% by weight, based on the total amount of the employed silanes of the formula (V) and (VI), preferably in the range of 0-20% by weight and particularly preferably in the range of 0-15% by weight.

Water can be employed in an amount of 99.84-63% by weight and preferably 97.94-81.1% by weight based on the reaction mixture as a whole.

The condensation in step (1) of the process according to the invention is customarily carried out by adding the silanes of the general formula (V) and optionally (VI) to a mixture of water, buffer substance and surface-active substance. This mixture of water, buffer substance and surface-active substance is generally prepared by charging the water initially and then adding the buffer substance and surface-active substance. The silanes of the general formula (V) and optionally (VI) are advantageously added to the mixture in a uniform and gradual manner. This is a particularly good way of achieving the aforementioned low average particle size of 100-1000 angstrom and a very narrow particle size distribution. The reaction itself is preferably carried out with stirring for a period of up to 6 hours and preferably up to 4 hours. The process is carried out in the absence of organic solvents.

Step (1) of the inventive process for preparing the colloidal suspensions is customarily carried out at temperatures in the range of 20 to 80° C. This process step is preferably carried out in the range of 30 to 70° C. and particularly preferably in the range of 50 to 70° C.

In the reaction, the silanes condense to release alcohols of the formula R ²OH from the alkoxy groups OR²of the employed silanes of the general formulae (V) and (VI). Their presence has an appreciable influence on the flashpoint. It is of decisive importance for the present invention that these alcohols be substantially removed by distillation. Accordingly the flashpointless textile auxiliaries according to the invention are substantially free of, and typically contain not more than 2.5% by weight, preferably not more than 2.2% by weight and especially not more than 2% by weight, each percentage being based on the total textile auxiliary, of an alcohol of the formula R²OH, where R²represents a straight-chain or branched C₁-C₄-alkyl radical.

Surprisingly, the textile auxiliary according to the invention is obtained when the distillation is carried out under specific conditions. This distillation in step (2) of the process according to the invention is carried out at a temperature in the range from 55° C. to 100° C., preferably from 60 to 80° C. and particularly preferably from 70 to 75° C., under a pressure of 950 to 250 mbar and preferably of 900 to 300 mbar, and under an inert gas stream, preferably a nitrogen stream, of 5 to 50 l/h and preferably of 20 to 40 l/h. The duration of this distillation is 4 to 8 hours and preferably 5 to 7 hours.

The distillation can be started for example immediately following completion of the addition of the silanes (V) and optionally (VI) to the mixture of water, buffer substance and surface-active substance. However, it is also possible initially to continue the condensation beyond the silane addition, for a period of up to 6 hours and preferably 4 hours, and only then to start the distillation.

Without further work-up, the textile auxiliary according to the invention will customarily still contain at least one of the surface-active agents mentioned and also at least one of the buffer substances mentioned in the colloidal suspension of the organosilasesquioxanes.

Illustratively, the reaction mixture used for preparing the Textile auxiliary according to the invention has the following composition:

0.01-3% by weight of at least one surface-active agent,

0.05-4% by weight of a buffer substance,

0.1-30% by weight of silanes of the formula (V) and optionally (VI),

99.84-63% by weight of water,

all the components mentioned adding up to 100% by weight.

Preferably, the reaction mixture used for preparing the Textile auxiliary according to the invention has the following composition:

0.01-3% by weight at least one surface-active agent,

0.05-4% by weight of a buffer substance,

5-22% by weight of silanes of the formula (V) and optionally (VI),

94.94-71% by weight by weight of water,

all the components mentioned adding up to 100% by weight.

The ratio between the two silanes (V) and optionally (VI) in these reaction mixtures is subject to the previous remarks.

The Textile auxiliary according to the invention then illustratively has the following composition:

0.01-3% by weight of at least one surface-active agent,

0.05-4% by weight of a buffer substance,

2-9% by weight of the organosilasesquioxane,

0-0.4% by weight of silica,

0-2.5% by weight of an alcohol R ²OH and

97.94-81.1% by weight of water,

all the components mentioned adding up to 100% by weight.

The invention further provides for the use of the flashpointless textile auxiliary for finishing textile materials.

Useful textile materials include all manufactured fiber materials, whether organic or inorganic, and also natural fiber materials. It is preferable to use a pile material from the aforementioned fiber materials.

The reaction mixture remaining after the distillation can directly be used for treating the textile materials. If desired, it can also be diluted still further.

The Textile auxiliary can be applied before, during or after the coloration of the textile material or before, during or after subsequent further finishing steps or subsequently after processing into cover, upholstery or floorcovering textile and its use, by treatment in the liquor, padding or spraying.

A further way to apply the colloidal suspensions to the fiber material is to use them together with a cleaning agent, particularly when the textile to be treated has been soiled by use, or preceding processing steps. It is preferred for the Textile auxiliary to be sprayed onto the material after the material has been wet cleaned but before it has been finished by the manufacturer.

The textile auxiliary according to the invention is notable for having no flashpoint and yet provides a good pile-stabilizing effect at the same time. No flashpoint can be measured even at a temperature of 98-100° C.; no ignition of sample vapors is observed; the system just boils. The textile auxiliary according to the invention is thus safe to transport. In addition, the suspensions possess excellent stability.

The invention is further illustrated but is not intended to be limited by the following examples in which all parts and percentages are by weight unless otherwise specified.

EXAMPLES

Example 1

22 g of disodium tetraborate and 75 g of a cationic surfactant (N-C[0090] _12/14-alkyl-N,N-dimethyl-N-benzylammonium chloride) are dissolved in 1098 g of distilled Water at room temperature and the solution is heated to 70° C. On attainment of this temperature, 1980 g of methyltriethoxysilane are added over 4 hours, during which the temperature of the reaction mixture is maintained at 70° C. On completion of the addition, the resulting sol is stirred at 70° C. for 3 hours.

500.0 g of this condensation product (ethanol content determined via GC: 11% by weight) are distilled via stillhead and cold trap at 70° C. under the pressure reported in Table 1 and while simultaneously stripping with 30 l/h of N2 (policed via attached bubble counter) for 6 hours.

TABLE 1


				Ethanol content
Reaction	Reaction		Amount of	of suspension
time	temperature	Pressure	distillate	[% by weight]
[h]	[° C.]	[mbar]	[g]	(by GC)

6	70	380-450	74.9	1.25

The Mie particle size measurement does not give a result, with the emulsion being too fine. The particle size is thus less than 0.1 μm. The solids content is determined twice as 7.16 and 7.17% by weight. [0092]
382.0 g of this condensation product having a GC ethanol content of 1.25% by weight are adjusted to a solids content of 6.2% by weight by stirring at room temperature with 59.46 g of added water for 10 minutes. This suspension has an ethanol content of 1.09% by weight of ethanol (determined by GC) and a doubly determined solids content of 6.01 and 6.27% by weight. The suspension is a freely mobile, fluid, slightly opaque liquid. The test to DIN EN 22719 (1993), ISO 2719 (1988) indicates no flashpoint. [0093]

Example 2

22 g of disodium tetraborate and 75 g of a cationic surfactant (N-C[0094] _12/14-alkyl-N,N-dimethyl-N-benzylammonium chloride) are dissolved in 1098 g of distilled water at room temperature and the solution is heated to 70° C. On attainment of this temperature, 1980 g of methyltriethoxysilane are added over 4 hours, during which the temperature of the reaction mixture is maintained at 70° C. On completion of the addition, the resulting sol is stirred at 70° C. for 3 hours.

500.0 g of the condensation product (ethanol content thus obtained GC: 11% by weight) are distilled via stillhead and cold trap at 100° C. at 760 mbar without a nitrogen stream over 3 hours.

TABLE 2


			Ethanol
			content of
	Reaction		suspension
	temperature	Amount of	[% by weight]
Time course	[° C.]	distillate	(by GC)

after 1 h	90-92	31.2 g	7.0
after 2 h	92-95	59.2 g	3.83
after 3 h	95-97	75.9 g	2.36

The condensation product obtained after 3 hours is coarser than the condensation product of Example 1 (slight white sediment). The particle size as determined by the Mie method is 2.7 um. The solids content is determined twice and found to be 7.23 and 7.19% by weight. The test to DIN EN 22719 (1993), ISO 2719 (1988) reveals no flashpoint for the sample after a reaction time of 3 hours. [0096]
366.6 g of this condensation product (solids content: 7.21% by weight) are adjusted to a solids content of 6.2% by weight by adding 59.7 g of water and stirring at room temperature for 10 minutes. The suspension obtained has an ethanol content of 2.07% by weight by GC and is white and fluid. The solids content is determined twice and found to be 6.02 and 6.02% by weight. [0097]

Comparative Example 1

22 g of disodium tetraborate and 75 g of a cationic surfactant (N-C[0098] _12/14-alkyl-N,N-dimethyl-N-benzylammonium chloride) are dissolved in 1098 g of distilled water at room temperature and the solution is heated to 70° C. On attainment of this temperature, 1980 g of methyltriethoxysilane are added over 4 hours, during which the temperature of the reaction mixture is maintained at 70° C. On completion of the addition, the resulting sol is stirred at 70° C. for 3 hours.
366.6 g of the condensation product thus obtained (solids content: 7.21% by weight) are adjusted to a solids content of 6.2% by weight by adding 59.7 g of water and stirring at room temperature for 10 minutes. The suspension obtained has an ethanol content of 11% by weight by GC and is white and fluid. The test to DIN EN 22719 (1993), ISO 2719 (1988) reveals a flashpoint of 50° C. [0099]

Use Example 1

Laboratory Soiling Test on the Lines of DIN 54 324 (Chair Castor Test) [0100]
A “Holiday” style nylon-6,6 tufted cut-pile material (pile weight 450 g/m2) which has been dyed, but not dried, is padded to a wet pick-up of 100%. [0101]
The material is then dried at 120° C. for 5 minutes, uniformly sheared and backcoated with a commercially available flat latex foam. [0102]
Identical samples are taken from the resulting material. These samples are initially soiled with 10 g each of a synthetic soil of the following composition: [0103]

1932 g of chamotte,

40 g of black iron oxide,

20 g of yellow iron oxide,

8 g of carbon black and

1000 g of water.
The samples are stressed by the chair castor test of DIN standard 54 324 under a castor load of 60 kg in total and a change in the direction of rotation of the castors after every 50 revolutions. Following this chair castor test, the soiling is determined according to DIN 54002. The results are reported in Table 3. [0104]

TABLE 3

Example 2

(product after

Textile Reference 3 h reaction Comparative

auxiliary of sample Example 1 time) Example 1

Amount used 0 10 20 40 10 20 40 10 20 40

in g/l

Soiling 2 4 4 4 3 3 3 4 4 4

evaluation

grey scale

DlN 54002
(Scale: 1=very pronounced change; 5=no change) [0105]
In contrast to the textile auxiliary as per the comparative example, the textile auxiliaries according to the invention not only provide a good pile-stabilizing finish, but also have no flashpoint. [0106]

Comparative Example 2

22 g of disodium tetraborate and 75 g of a cationic surfactant (N-C[0107] _12/14-alkyl-N,N-dimethyl-N-benzylammonium chloride) are dissolved in 1098 g of distilled water at room temperature and the solution is heated to 70° C. On attainment of this temperature, 1980 g of methyltriethoxysilane are added over 4 hours, during which the temperature of the reaction mixture is maintained at 70° C. On completion of the addition, the resulting sol is stirred at 70° C. for 3 hours.

500.0 g of this condensation product (ethanol content determined via GC: 11% by weight) are distilled via stillhead and cold trap at 50° C. under a slightly reduced pressure (see Table 4) and while simultaneously stripping with 30 l/h of N2 (policed via attached bubble counter) for 6 hours.

TABLE 4


			Ethanol content of
	Reaction		suspension
	temperature	Pressure	[% by weight]
Time course	[° C.]	[mbar]	(by GC)

After 2 h	50	200	8.68
After 1 h	50	200	6.55

The distillation is discontinued after 4 hours, since it has been going very badly. The reaction mixture repeatedly foams over violently at a pressure of ≦200 mbar, while no sensible distillation is possible at a pressure ≧200 mbar. [0109]
Although the invention has been described in detail in the foregoing for the purpose of illustration, it is to be understood that such detail is solely for that purpose and that variations can be made therein by those skilled in the art without departing from the spirit and scope of the invention except as it may be limited by the claims. [0110]

Claims

What is claimed is:

1. Flashpointless textile auxiliaries containing aqueous colloidal suspensions of organosilasesquioxanes containing units of the general formula (I)

R¹Si(O)_3/2 (I)

where each

R¹is the same or different and represents a straight-chain or branched C₁-C₁₈-alkyl radical which is optionally substituted by one or more identical or different halogen radicals, —NH₂, —SH or epoxy groups and/or in which one or more (CH)₂groups is optionally replaced by —O—, —S— or —N(H)—.

2. Flashpointless textile auxiliaries according to claim 1, containing not more than 2.5% by weight, each percentage being based on the total textile auxiliary, of an alcohol of the formula R²OH, where R²represents a straight-chain or branched C₁-C₄-alkyl radical.

3. Flashpointless textile auxiliaries according to claim 2 containing not more than 2.2% by weight, each percentage being based on the total textile auxiliary, of an alcohol of the formula R²OH, where R²represents a straight-chain or branched C₁-C₄-alkyl radical.

4. Flashpointless textiles according to claim 3 containing not more than 2% by weight, each percentage being based on the total textile auxiliary, of an alcohol of the formula R²OH, where R²represents a straight-chain or branched C₁-C₄-alkyl radical.

5. Flashpointless textile auxiliaries according to claim 1 wherein each R¹is the same or different and represents a straight-chain or branched C₁-C₇-alkyl radical which is optionally substituted by one or more identical or different halogen radicals, NH₂, —SH or epoxy groups and/or in which one or more (CH)₂groups is optionally replaced by —O—, —S— or —N(H)—.

6. Flashpointless textile auxiliaries according to claim 5 wherein halogen radicals is F, Cl or Br radicals.

7. Flashpointless textile auxiliaries according to claim 1, wherein the organosilasesquioxanes contain units of the formula R¹Si(O)_3/2where R¹has different meanings subject to the proviso that up to 95 mol % of all of the R1 radicals are methyl.

8. Flashpointless textile auxiliaries according to claim 1, wherein the organosilasesquioxanes contain units of the formula R¹Si(O)_3/2where R¹has different meanings subject to the proviso that up 50-94 mol % of all of the R⁴are methyl.

9. Flashpointless textile auxiliaries according to claim 1, wherein the organosilasesquioxanes contain units of the formula R¹Si(O)_3/2where R¹has different meanings subject to the proviso that up to 80-94 mol % of all of the R⁴are methyl.

10. Flashpointless textile auxiliaries according to claim 1 wherein the substituents on the R¹radical are epoxy groups of the formula (II)

where

n is an integer from 1 to 18 and preferably from 1 to 7,

and one or more of the alkylene groups —(CH₂)— is optionally replaced by —O—, —S— or —N(H)—.

11. Flashpointless textile auxiliaries according to claim 10, wherein the epoxy groups are groups of the formulae (III) or (IV)

where

x is O, S or NH.

12. Flashpointless textile auxiliaries according to claim 1, wherein R¹is methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, tert-butyl, n-pentyl or 2-ethylbutyl.

13. Flashpointless textile auxiliaries according to claim 1, wherein the organosilasesquioxanes have an average particle size of 100-1000 angstrom.

14. Flashpointless textile auxiliaries according to claim 13, wherein the organosilasesquioxanes have an average particle size of 200-600 angstrom.

15. Flashpointless textile auxiliaries according to claim 1, wherein the organosilasesquioxanes, as well as the units of the formula (I), contain silica units of the formula Si(O₄)₂.

16. Flashpointless textile auxiliary according to claim 1, having the following composition:

0.01-3% by weight of at least one surface-active agent,

0.05-4% by weight of a buffer substance,

2-9% by weight of the organosilasesquioxane,

0-0.4% by weight of silica,

0-2.5% by weight of an alcohol R²OH and

97.94-81.1% by weight of water,

all the components mentioned adding up to 100% by weight.

17. Process for preparing the flashpointless textile auxiliaries according to claim 1 comprising

(1) condensing one or more silanes of the general formula (V)

R¹—Si(OR²)₃ (V)

and optionally one or more silanes of the general formula (VI)

Si(OR²)₄ (VI)

where each

R¹is the same or different and represents a straight-chain or branched alkyl radical having 1 to 18 carbon atoms which optionally is substituted by one or more identical or different halogen radicals, —NH₂, —SH or epoxy groups and/or in which one or more (CH)₂groups are optionally replaced by —O—, —S— or N(H)— and each

R²is the same or different and represents a straight-chain or branched C₁-C₄-alkyl radical,

in a mixture of water, a buffer substance and a surface-active substance, and

(2) distilling the reaction mixture of (1) at 55° C. to 100° C. under a pressure of 950 to 250 mbar and under an inert gas stream of 5 to 50 l/h.

18. Process according to claim 17, wherein the silanes of the general formula (V) are methyltrimethoxysilane, methyltriethoxysilane, methyltriisopropoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, propyltrimethoxysilane, isobutyltrimethoxysilane, isobutyltriethoxysilane or 2-ethylbutyltriethoxysilane.

19. Process according to claim 17, wherein the silane of the general formula (VI) is tetraethoxysilane.

20. Process according to claim 17, wherein the surface-active substances used are cationic.

21. Process according to claim 20, wherein the cationic surface-active substances are ammonium salts of alkylamines, quaternary ammonium salts, alkylpyridinium salts, imidazole salts, imidazolinium salts, salts of alkyldiamines and of alkylpolyamines, salts of acylated diamines and polyamines, salts of acylated alkanolamines, salts of esters and ethers of alkanolamines, alkanolamine ether salts, alkylethyleneurea salts, sulphonium compounds, phosphonium compounds or amine oxides

22. Process according to claim 17, wherein the buffer substance used is sodium tetraborate, ammonium bicarbonate, sodium bicarbonate or potassium bicarbonate.

23. Process according to claim 17, wherein the condensation in step (1) is carried out by adding the silanes of the general formula (V) and optionally (VI) to a mixture of water, buffer substance and surface-active substance.

24. Process according to claim 17, wherein the distillation in step (2) is carried out at a temperature in the range from 60 to 80° C., under a pressure of 900 to 300 mbar and under a nitrogen stream of 5 to 50 l/h.

25. Process according to claim 24, wherein the distillation in step (2) is carried out at a temperature in the range from 70 to 75° C., under a pressure of 900 to 300 mbar and under a nitrogen stream of 5 to 50 l/h.

26. Process according to claim 24, wherein the distillation in step (2) is carried out at a temperature in the range from 70 to 75° C., under a pressure of 900 to 300 mbar and under a nitrogen stream of 20 to 40 l/h.

27. Process according to claim 17, wherein the distillation is started immediately after completion of the addition of the silanes (V) and optionally (VI) to the mixture of water, buffer substance and surface-active substance.

28. A process for preparing textile materials comprising finishing the materials with the flashpointless textile auxiliary according to claim 1.

29. Textile material finished with a flashpointless textile auxiliary according to claim 28.