Title of Invention	AQUEOUS DISPERSIONS OF ORGANOSILICON COMPOUNDS
Abstract	Abstrect Aqueous dispersicns of organosilicon compounds The invention relates to aquaocus dispersions of organosilicon compounds containing (A) at least one crganoEiilicon compound selected from (Al) silanes of the formula (I) and/or the partial hydrolysis products thereof and (A2) siloxanes containing units of the formula (II) (B) at least one nonioni.c emulsifier having an HLB value greater than or equal to 12, optionally as a mixture with nonionic emulsifiers having an HLB value of less than 12, (C) at least one cationd.c surfactant selected from (CI) compounds of the formula (III) and (C2) compounds of the formula (IV) where the radicals and indices have the meaning stated in claim 1, (D) water and optionally (E) further ccmponents, the preparation thereof and the use thereof, in particular for the hydrophobing impregnation and mass hydrophobing of mineral and organic building materials. 36

Title of Invention

AQUEOUS DISPERSIONS OF ORGANOSILICON COMPOUNDS

Abstract

Abstrect Aqueous dispersicns of organosilicon compounds The invention relates to aquaocus dispersions of organosilicon compounds containing (A) at least one crganoEiilicon compound selected from (Al) silanes of the formula (I) and/or the partial hydrolysis products thereof and (A2) siloxanes containing units of the formula (II) (B) at least one nonioni.c emulsifier having an HLB value greater than or equal to 12, optionally as a mixture with nonionic emulsifiers having an HLB value of less than 12, (C) at least one cationd.c surfactant selected from (CI) compounds of the formula (III) and (C2) compounds of the formula (IV) where the radicals and indices have the meaning stated in claim 1, (D) water and optionally (E) further ccmponents, the preparation thereof and the use thereof, in particular for the hydrophobing impregnation and mass hydrophobing of mineral and organic building materials. 36

Full Text	Aqueous dispersions of organosllicona compounds The invention relates to aqueous dispersions of organosllicona compounds, the preparation thereof and the use thereof, in particular for the hydrophobing impregnation and mass hydrophotaing of mineral and organic building materials. Silanes and slogans have long been used for the production of structures, for example solutions of silanes in organic solvents, as described, for example, in DE-A 1069057. For cost reasons, but rot least also because of the health hazards, during handling of organic solvents and the associated environmental pollution, working with organic solvents is disadvantageous. Aqueous formulations based on alkylalkoxysilanes and -slogans are known. EP-A 234 024 describes silanes emulsions comprising nonionic emulsifiers, which have an HLB value of from 4 to 15. According to EP-A. 340 816 the stability of these compositions is improved by the addition of buffer salts. EP-A 631 999 describes aqueous formulations based on alkylalkoxysilanes, which contain cationic emulsifiers. According to WO-A 199516752 and EP-A 907 622, amine soaps are said to be suitable in particular for the preparation of silane/siloxane emulsions. WO-A 199522580 describes a series of further cationic emulsifiers in silane/siloxane emulsions. According to EP-A 1 147 072, the stability of silane/siloxane emulsions is particularly good when ionic emulsifiers are used in combination with nonionogenic emulsifiers which have an HLB value of less than 11. Nevertheless, the aqueous structure preservatives prepared according to the prior art do not always have the desired stability and efficiency. The invention relates to aqueous dispersions containing (A) at least one crcanosilicon compound selected from (Al) silanes of the formula (I) , in which R may be identical or different and are monovalent, SiC-bonded, optionally substituted hydrocarbon radicals having at least 4 carbon atoms, R1 may be identical or different and are monovalent, optionally substituted hydrocarbon radicals, R2 may be identical or different and are monovalent, SiC-bonded, optionally substituted hydrocarbon radicals having 1 to 3 carbon atoms, a is 1, 2 or 3 and b is 0, 1 or 2, with the proviso that the sum of a and b is 1, 2 or 3, and/or the partial hydrolysis products thereof, and (A2) silicates containing units of the formula (II) , in which R3 may be identical or different and is a hydrogen atom or a monovalent, SiC-bcnded, optionally substituted hydrocarbon radical, R4 may be identical or different and is a hydrogen atom or a monovalent, optionally substituted hydrocarbon radical, c is 0, 1, 2 or 3 and d is 0, 1, 2 or 3, with the proviso that the sum of c and d is less than or equal to 3, 3 (B) at least one nonionic emulsifier having an HLB value greater than or equal to 12, preferably greater than or ec'ual to 14, optionally as a mixture with nonionic emulsifiers having an HLB value o£ less than 12, (C) at least one cationic surfactant selected from (CI) compounds cf the formula R^R'(4-e)N' X' (III) and (C2) compounds of the formula (IV), in which R5 are optionally substituted hydrocarbon radicals, R6 may be identical or different and are optionally substituted aliphatic hydrocarbon radicals having at least 10 carbon atoms or optionally substituted aromatic hydrocarbon radicals having at least 6 carbon atoms, R7 are optionally substituted aliphatic hydrocarbon radicals having at least 10 carbon atoms or optionally substituted aromatic hydrocarbon radicals having at least 6 carbon atoms, R8 are optionally substituted hydrocarbon radicals, R9 may be identical or different and are optionally substituted hydrocarbon radicals, e is 2 or 3 an3 X" is a monovalent organic or inorganic anion, 4 (D) water and optionally (E) further components. Examples of the radical R are 1-n-butyl, 2-n-butyl, isobutyl, tert-butyl, n-pentyl, isopentyl, neopentyl and tert-pentyl radical; hexyl radicals, such as the n-hexyl radical; heptyl radicals, such as the n-heptyl radical; octyl radicals, such as the n-octyl radical, and isooctyl radicals, such as the 2,2,4-trimethylpentyl radical; nonyl radicals, such as the n-nonyl radical; decyl radicals, such as the n-decyl radical; dodecyl radicals, such as the n-dodecyl radical; octadecyl radicals, such as the n-octadecyl radical; cycloalkyl radicals, such as the cyclopentyl, cyclohexyl, cycloheptyl and methyleyelohexyl radicals; aryl radicals, such as the phenyl, naphthyl, anthryl and phenanthryl radical; alkaryl radicals, such as o-, m- and p-tolyl radicals; xylyl radicals and ethylphenyl radicals; and aralkyl radicals, such as the benzyl radical and the a- and the P-phenylethyl radical. Examples of substituted radicals R are aminoethylaminopropyl, glycidyloxypropyl and methacroylpropyl radical. Radicals R are preferably hydrocarbon radicals having at least 4 carbon atoms, particularly preferably hydrocarbon radicals having 6 to IS carbon atoms, in particular hexyl and octyl radicals, very particularly preferably the n-hexyl radical, n-octyl radical and isooctyl radical, such as the 2,2,4-trimethylpentyl radical. Examples of the radical R1 are the radicals stated below for R^. 5 Radicals R1 are prsferably c-ptionally substituted alkyl radicals having 1 to 4 carkon atoms, particularly preferably the rriethyl, ethyl, n-butyl, 2-metho>:yethyl and isopropyl radical, in particular the ethyl radical. Radicals R' are pra:fer£ibly alkyl radicals having 1 to 3 carbon atoms, such as methyl, ethyl, n-propyl and isopropyl radicals, particularly preferably the methyl radical. The value of a is preferably 1. The value of b is preferably 0 or 1. Examples of silanes (Al) are isobutyltriethoxysilane, hexyl-triethoxysilane, hexylmethyldiethoxysilane, n-octyltrimethoxy-silane, n-octyltriethoxysilane, n-octyltributoxysilane, isooctyltriethDxysilane, n-decyltriethoxysilane, dodecyImethyldimethoxysi1ane, hexadecyltrimethoxysilane, octadecylmethyldimethoxysilane, octadecylmethyldiethoxysilane and octadecyltriethoxysilane and aminoethylaminopropyl-triethox'/silane, glycidoxypropyltrimethoxysilane and methacroylpropyltrietho>r/-silane. Silane (Al) is preferably n-hexyltriethoxysilane, n-octyltriethoxysilane and isooctyltriethoxysilane, n-octyltriethoxysilane and isooctyltriethoxysilane being particularly preferred. If (Al) are partial hydrolysis products, those having 2 to 10 Si atoms are preferred. Partial hydrolysis products form when some of the radicals OR1 in the silanes of the formula (I) are eliminated by reaction with water or steam and OH groups bonded to silicon f rom These in turn can condense with elimination of 6 water to give silcxe.ne bonds, resulting in oligomers which may also con-cain OH croups i.n addition to groups OR1 Partial hydrolysis pro:iucts of silanes of the formula (I) may also be present as -an impur:.ty i.n the silane of the formula (I) . Examples of ra:licals R^ are alkyl radicals, such as the methyl, ethyl, n-propyl, isopropyl, 1-n-butyl, 2-n-butyl, isobutyl, tert-butyl, n-pentyl, isopentyl, neopentyl and tert-pentyl radical; hexyl radicals, such as the n-hexyl radical; heptyl radicals, such as the n-heptyl radicals; octyl radicals, such as the n-octyl radical, and isooctyl radicals, such as the 2,2,4-trimethylpentyl radical; nonyl radicals, such as the n-nonyl radical; decyl radicals, such as the n-decyl radical; dodecyl radicals, such as the n-dodecyl radical; octadecyl radicals, such as the n-octadecyl radical; cycloalkyl radicals, such as the cyalcpentyl, cyclohexyl and cycloheptyl radical and methyleyelohexyl radicals; alkenyl radicals, such as the vinyl, 1-propenyl and 2-propenyl radical; aryl radicals, such as the phenyl, naphthyl, anthryl and phenanthryl radical; alkaryl radicals, such as the o-, m- and p-tolyl radicals; xylyl radicals and ethylphenyl radicals; and aralkyl radicals, such as the benzyl radical and the a- and the p-phenylethyl radical. Examples of substituted radicals R^ are the trifluoropropyl radical, the amincpropyl radical, the aminoethylaminopropyl radical, the glycidyloxypropyl radical and the mercaptopropyl radical. R3 are preferably hydrocarbon radicals optionally substituted by oxygen- and nitrogen-containing functional groups and having 1 to 18 carbon atoms, particularly preferably alkyl radicals having 1 to 18 carbon atoms or aromatic hydrocarbon radicals having 6 to 9 carkon atoms, very particularly preferably 7 methyl, ri-hexyl, r-hepfyl, n-octyl, isooctyl, n-dodecyl. phenyl and ethylphenyl radicals;, in particular the methyl radical. Examples of the radical R4are the radicals stated for Radicals R3 are preferably a hydrogen atom or optionally substituted alkyl radicals having 1 to 4 carbon atoms, particularly preferably a hydrogen atom or the methyl, ethyl, n-butyl,, isopropyl and 2-methoxyethyl radicals, in particular a hydrogen atom or irethyl or ethyl radicals. In formula (II), c is preferably 1, 2 or 3. The value of d is preferably 0 or 1. Siloxanes (A2) used according to the invention are any desired silicone oils, silicone resins and oligomeric siloxanes known to date, which contain units of the formula (II). The siloxanes (A2) used according to the invention preferably contain no further units apart from the units of the formula (II) . Examples of (A2) are organopolysiloxanes, such as organopolysiloxanes v;hich contain alkoxy groups and can be prepared by reacting methyltrichlorosilane and optionally other alkyltrichlorosilanes or phenyltrichlorosilane with ethanol in water and correspond to empirical formulae such as CH3Si(OCH2CH3)o.801.i or C6H5Si (OCH2CH3) 0.7O1.2; these oligomeric siloxanes have a viscosity of less than 500 mPa.s, preferably less than 100 mPa.s, in particular less than 50 mPa.s, at 2 5°C; 8 oligomeric silDxeres which are obtainable by hydrolysis/condensation fron methyltriethoxysilane and isooctyl-rietnDxysi-.ane and correspond, for example, to the formula ( [Mesi:)3,: ] o :-,-o.5 :iOSi03/2] 0.02-0.2 [EtOi/2] 0.3-0.6)x (Me is methy]., 10 is isccctyl and Et is ethyl) and have a weight average molar ::iass of 1()00-10 000 g/mol ; silicone resins in which c :.s 1 in at least 70% of the units of the formula (II) and c is 2 in the other units of the formula (II), preferably silicone resins in which c is 1 in at least 80% of the units cf the formula (II), in particular 90% of the units of the formula (II); these resins have a viscosity of more than 1000 mPa.s, preferably more than 5000 mPa.s, in particular more than 10 000 mPa.s, at 25°C and a content of from 1 to 6% b/ weight of alkoxy groups and from 0.2 to 1% by weight of hydrDxyl groups; and polydimethylsiloxanes having a viscosity of from 30 to 1 000 000 mPa.3 at 25°C, which may contain hydroxyl groups and/or aminoalkyl groups. These siloxanes (A2) are preferably silicone resins, mixtures of highly viscous silicone resins with low-viscosity oligomers or silicone oils being particularly preferred. These mixtures have a viscosity cf preferably from 100 to 100 000 mPa.s, in particular from 100 0 to 10 000 mPa.s, at 25°C. Component (A) is preferably (Al) or a mixture of (Al) and (A2), particularly preferably (Al). If component (A) is a mixture of (Al) and (A2), the proportion of (Al) in the mixture is preferably from 2 0 to 96% by weight, in particular frcrr. 50 to 80% by weight, based in each case on 9 the sun of (Al) arid (A2) . The dispersiors according to the invention contain component (A) in amounts of, preferably, from 5 to 70% by weight, particularly preferably fron 30 to 65% by weight, based in each case on the total formulation. Examples of tha ncnionogenic emulsifiers (B) used according to the invention are sorbitan fatty acid esters, ethoxylated sorbitan fatty acid esters, ethoxylated fatty acids, ethoxylated linear or branched alcohols having 10 to 20 carbon atoms, ethoxylatec, alkylphenols, pent aery thrityl fatty acid esters, glyceryl esters and alkylpolyglycosides. The nonionogenic emulsifiers (B) are preferably sorbitan fatty acid esters, ethoxylated sorbitan fatty acid esters, ethoxylated fatty acids, ethoxylated linear or branched alcohols having 10 to 2 0 carbon atoms and ethoxylated triglycerides. Preferably, the dispersions according to the invention contain no ethoxrylated alkylphenols since it is known that these are not environmentally compatible. The component (B) used according to the invention may be only one nonionogenic emulsifier having an HLB value of greater than or equal to 12, particularly greater than or equal to 14, or a mixture of a plurality of nonionogenic emulsifiers, with the proviso that at least one emulsifier has an HLB value greater than or equal to 12, in particular greater than or equal to 14. Mixtures of nonionogenic emullsifiers, of which at least one emulsifier has an HLB value greater than or equal to 12, are 10 preferably used aS component (B) . The proportion of emulsifiers having an HLB value greater than or equal to 12 in the emulsifier mixture (B; is preferably at least 30% by weight. The HLB value is an expression of the equilibrium between hydrophilic cin;l hydrophobic groups of an emulsifier. The definition of the HLB value and methods for determining it are generally known and are described, for example, in Journal of Colloid and Interface Science 298 (2006) 441-450 and the literature cited there. Examples of the ncnionogenic emulsifiers (B) used according to the invention and having an HLB value greater than or equal to 12 are (HLB values according to manufacturer, POE is polyoxyeuhylena): 11 Examples of nonionogenic emulsifiers which can additionally be used and have an HLB value The dispersions according to the invention contain component (B) in amounts of, preferably, from 1.0 to 10% by weight, particularly preferably frora 1.5 to 3% by weight, based in each case on zha total formulation. Examples of radicals R^ and R^ are, in each case independently of one another, the examples stated for radical R^. Radicals R" are preferably alkyl radicals having 1 to 4 carbon atoms, particularly preferably the methyl radical. Examples of hydrocarbon radicals R^ and R'^ are, in each case independently of one another, decyl radicals, such as the n-decyl radical; dcdecyl radicals, such as the n-dodecyl radical; hexadecyl radicals, heptadecyl radicals, octadecyl radicals, such as -he n-DCtadecyl radical; aryl radicals, such as the 13 phenyl, naphtrL/i, £i.rthryl and phenanthryl radical; alkaryl radiccils, siich as o--, m- and p-tolyl radicals; xylyl radicals and ethylphenyl radi-cals;; and aralkyl radicals, such as the benzyl radical and the a- and the p-phenylethyl radical. Examples of su'ostituted hyd^rocarbon radicals R^ and R' are, in each case independently of one another, lauramidoethyl radicals, palHiitair.idoethyl radicals and stearamidoethyl radicals. Radicals R'" are preferably linear alkyl radicals having 12 to 22 carbon atoms or aromatic radicals, particularly preferably aromatic hydro:;arbon radicals, in particular the benzyl radical. Radicals R' are preferably linear alkyl radicals having 12 to 22 carbon atoms, in particular the lauryl, palmityl, oleyl or stearyl radical. Examples of radicals R^ aore the examples stated for radicals R^, R^ and RRadicals R^ are preferably optionally substituted alkyl radicals having 1 to 22 carbon atoms, particularly preferably the methyl, lauryl, palmityl, oleyl, stearyl, lauramidoethyl, palmitamidoethyl and stearamidoethyl radical. Radicals R^ are preferably alkyl radicals having 1 to 4 carbon atoms, particularly preferably the methyl radical. Examples of anion X' and halide ions, such as the chloride, bromide and iodide :.on, hydrogensulfate ions, alkylsulfate ions, such as the meth-ji'lsulfate ion, and dialkylphosphate 14 ions . An anion X" is preferably a chloride, bromide, iodide or methylsulfate anion, particularly preferably a chloride or methylsulfate anion, Examples of tha component (Cl) used according to the invention are all ;<:no :ju5ternary amiaonium compounds which carry at least one substituted or unsubstituted hydrocarbon radical having lecist ic carbon atoms such as> dodecyldimethylairoT.onium chloride, tetradecyltrimethylammonium bromide, stearyltrimethylamraonium chloride, distearyldimethylainraonium chloride, cetyltrimethylammonium chloride, behenyltrimethylarnmonium bromide, dodecylbenzyldimethylammonium chloride and benzyl-trimethylaininoniurr. chloride. Components (Cl) are preferably aryl- or alkyltrimethylammonium salts, such as stearyltrimethylammonium chloride and cetyltrimethylaminium chloride, particularly preferably benzyltrialkylamir.cnium salts, in particular trimethylbenzyl-ammonium chloride and trimethylbenzylammonium methosulfate. Examples of the componejnt (C2) used according to the invention are all kno^,^7n quaternar-^^' imidazolinium compounds which carry at least one substituted or unsubstituted hydrocarbon radical having at least 10 carbon atoms, such as l-methyl-2-stearyl-3-stearylamidoethylimidazolinium methosulfate, l-methyl-2-norstearyl-3-stearylamidoethylimidazolinium methosulfate, 1-methyl-2-oleyl-3-cleylamidoethylimidazolinium methosulfate, 1-methyl-2-stearyl-3-meth)limidazolinium methosulfate, 1-methyl-2-behenyl-3-methyliraidazolinium methosulfate and l-methyl-2-dodecyl-3-methyliir.idazolinium methosulfate. 15 Componenr. (C2) is preferabl]-l-methyl-2-stearyl-3-stearyl-araidoethylini:.dazolinum. methosulfate, 1-methyl-2-norst€5aryl-3-sceeryL amidoethylimidazolinium methosulf ate and 1-methyl-2-oleyl -3 -cleylaniidoethylimidazolinium methosulfate . Components (C) used according to the invention are preferably benzyltrimethylairrr.or.-ium compounds or quaternary imidazolinium compounds, q-aaternary imidazolinium compounds being particularly preferred. The dispersions according to the invention contain component (C) in amounts of, preferably, from 0.1 to 5% by weight, particularly preferably from 0.3 to 1.5% by weight, based in each case on the total amount of the dispersion. In the case of dispersions according to the invention, the weight ratio of component (B) to component (C) is preferably from 0.5 to 10, in particular from 2 to 5. The water (D) used according to the invention may be any desired type of v;ater, such as, for example, natural waters, such as, for example, rainwater, groundwater, spring water, river water and seawater, chemical waters, such as, for example, demineralized v/ater or distilled or (multiply) redistilled v/ater, waters for medicinal or pharmaceutical purposes, such as, for example, purified water (Aqua purificata; Pharm.. Eur. 3), Aqua deionisata, Aqua destillata. Aqua bidestillata. Aqua ad injectionam or Aqua conservata, drinking water according to the German drinking water regulation and mineral waters. The water (D) used according to the invention is preferably water having a ccnductivity of less than 10 uS/cm, in 16 particular less than 2 uS/cn. The dispersions according to the invention contain component (D) in amounts of, preferabLy, from 20 to 9 5% by weight, particularly ;pc:eferabiy fron 40 to 60% by weight, based in each case on che total araount; of dispersion. The further co:Tipcnents (E) optionally used according to the invention may be all additives which have also been used to date in aq-ueous dispersions, such as, for example, thickeners, organosilicon comrpounds which differ from (Al) and (A2), catalysts, substances for adjusting the pH, buffer substances, fillers, fragrances, dyes, antifreezes, such as glycols and glycol ether, and preservatives. Examples of optionally used thickeners (E) are polyacrylic acid, polyacrylates, cellulose ethers, such as carboxymethylcellulose ctnd hydroxyethylcellulose, natural gums, such as xanthan gum, and polyurethanes. Examples of optionally used organosilicon compounds (E) are silanes which contain no hydrocarbon groups having at least 4 carbon atoms, such as, for example, tetraethoxysilane, trimethylmethoxysilane, aminopropyltriethoxysilane and aminopropyIme tby1dime thoxys i1ane. Examples of substances for adjusting the pH are, in addition to aminosilanes, also amines, such as, for example, monoethanolamine, or alkali metal hydroxides. If required for ensuring the constancy of the pH over a relatively long period, buffer systems, such as salts of acetic acid, salts of phosphoric acia, salts of citric acid, in each case in combination with the free acid, may also be used, depending on the desired pE. 17 The dispersior-D accordirig to the invention may contain silicon dioxide (silicic acr.ds) , titanium dioxide or aluminum oxide havincf a BET sarface area of, preferably, from 20 to 1000 m2/g, a part:.cle siz:2 cf, preferably, less than 10 and an agglomerate si?,e cf, preferably, less than 100 ]im as fillers (E) . The optionally used fillers (E) are particularly preferably silicic acids, in particular those having a BET surface area of from 50 to 800 m2/g. These silicic acids may be pyrogenic or precipitated silicic acids. In particular, pretreated silicic acids, such as, fcr example, commercially available completely or partly hydrophcbed silicic acids, can be used as fillers (E). Examples of commercially available hydrophobic silicic acids which can be used according to the invention are pyrogenic, treated silicic acid having a BET surface area of 12 0 m2/g and a carbon content of 0.8% by weight (available under the name HDK® HI5 from Wacker Chemie AG, Germany) , a pyrogenic treated silicic acid having a BET surface area of 140 m2/g and a carbon content of 2.8% by weight (available under the nanie HDK® H2000 from Wacker Chemie AG, Germany) and a precipitated silicic acid treated with polydimethylsiloxane and having a BET surface area of 90 m2/g (available under the name "Sipernat DlO" from Degassa AG, Germany). The dispersions according to the invention are preferably free of water-immiscible solvents or contain water-immiscible solvents in amounts of not more than 1% by weight, based on the total amount of dispersion. In the context of the present invention, "water-immiscible solvents" are to be understood as meaning all solvents which are soluble in arr.cunts of not more than 1 g/1 in water at 20°C and a pressure of 101.325 kPa. 18 In particular, these water-:.mir.iscible solvents have a vapor pressure of 0,1. kFa or higher at 20°C. Examples of such water-immiscible solvents are benzene, toluene, xyler.e, hexane, cyclohexane and paraffinic hydrcoarbon mixtures. The dispersions according to the invention are preferably those containing (A) organosilicon compound (Al), optionally as a mixture with (A2), (B) mixtures of ncnionocfenic emulsifiers, of which at least one emulsifier has an. HLB value greater than or equal to 12, (C) cationic surfactant of the formulae (III) and/or (IV), (D) water and optionally (E) further co:npcner.ts . The dispersions according to the invention are particularly preferably those containing (-A) from 10 to 6C% by weight of (Al) and from 0 to 20% by weight of (A2), (B) from 1.0 to 10% by v/eight of mixtures of nonionogenic emulsifiers, of which at least one emulsifier has an HLB value greater than or equal to 12, (C) from 0.1 to 5% by weight of cationic surfactant of the formulae (III) and/or (IV), (D) water and optionally (E) further co:npcnents. In particular, the dispersions according to the invention contain no further components over and above the components 19 (A) , (B) , (C) , (C) a,nd (E) . The preparaticci cf the aqaeous dispersions according to the invention is effected 'by processes known per se. Usually, the preparation is effected hy sirrple stirring of all constituents at temperatures cf prefe^rabiy from 1 to 50°C and optionally subsequent horaDgeriization, for example using jet dispersers, rotor-stator hDmcgenizers at peripheral speeds of preferably from 5 to 40 m/s, colloid mills or high-pressure homogenizers at homogenization pressures of preferably from 50 to 2000 bar. The invention furtherraoi-e relates to a process for the preparation of the dispersions according to the invention by mixing the components (h), (B), (C), (D) and optionally (E). In a preferred eirtodiment of the process according to the invention, the ccirponent (B; , at part of the component (D) and optionally component (C) are initially introduced, the component (A) is incorporated using a rotor-stator homogenizer, the remaining amount of component (D), optionally component (E) and, unless also alz-eady initially introduced at the beginning, componenr (C) are incorporated with homogenization. This is preferably followed by homogenization using a high-pressure homogenizer at frcm 50 to 2000 bar, in particular at from 100 to 500 bar. Homogenization techniques, including high-pressure homogenizers, are generally known. In this context, reference may be made, for example, to Chemie Ingenieur Technik, 74(7), 901-909 2002. In the process according to the invention, it is possible - if desired - to use the components (Al) and/or {A2) and optionally 20 (E) in the :from cf dispersions or solutions and to mix then with the rerriciiMing components. The dispersions according to the invention are preferably milky, white to fceice liquids. The dispersion^ eccordirig to the invention have a pH of preferably from 5 to 9, in particular from 6 to 8. The dispersions according to the invention have a proportion of nonvolatile compounds (for example determined according to ASTM D 5095) of preferably from 10 to 80% by weight, particularly preferably from 20 to 70% by weight. The dispersions according to the invention have a volume-average particle size preferably from 0.1 to 10 urn, in particular from 0.3 to 1.5 pm. The dispersity of the dispersions according to the invention is in the range of preferably from 0.5 to 5, particularly preferably from 1.5 to 1. This value is calculated from (D90 D10)/D50, where Dx is the particle size at which x% of the volume of the internal phase are present in particles of less than or equal to this particle size. The dispersions according to the invention have a viscosity of, preferably, less than 10 000 mPa.s, in particular less than 1000 mPa.s, measured in each case at 25°C. The dispersions according to the invention have the advantage that they have a very long shelf-life. The dispersions according to the invention have the advantage 21 that they can be prepared economically. The dispersions sccording to the invention have the advantage that they are sin.ple to handle. The dispersions according to the invention have the advantage that they can oe easily diluted and have a very long shelf-life even in dilute from The process for the preparation of the dispersions according to the invention has the advantage that it can be carried out in a simple manner. The dispersions according to the invention have the advantage that they develop a very good and stable impregnating effect and very good .penetration behavior on different substrates . The aqueous dispersions according to the invention can be used for all purposes for which dispersions based on organosilicon compounds have also been used to date. They are, for example, outstandingly suitable as preservatives for structures, in particular for hydrophobing various mineral or organic substrates. The manner in which such dispersions are used is known to the person skilled in the art. The present invention furthermore relates to a process for the treatment of substrates, wherein the substrates are brought into contact with the dispersions according to the invention. Examples of substrates which can be treated with the dispersions according to the invention are mineral substances, such as masonry, mortar, brick, limestone, marble, sand-lime brick, sandstone, granite, porphyry, concrete and cellular 22 concrete, and :)rcan;.c substances, such as wood, paper, board, textiles and mannade and natzural fibers . In the process according to the invention, the dispersions generally penetrate into the capillaries of the substrate and dry there. In the process according to the invention, mineral substrates and wood-base materials are preferably used. The treatment according to the invention preferably comprises impregnation, coating, priming and injection, particularly preferably impregnation, in particular the substrate being brought into contact with the dispersion and the dispersion penetrating partly or completely into the substrate. The impregncition accordi.ng to the invention preferably comprises hydrophobing impregnation and can be effected both as impregnation of the surface and as injection or as mass hydrophobing. The water absorption of the substrate is drastically reduced by the hydrophobing according to the invention, which reduces the thermal conductivity but also prevents the destruction of the building materials by the influence of freezing and thawing cycles or salt or, in the case of wood-based materials, by rotting or fungal attack. Thus, not only is the value of the material thus treated preserved but, for example, lower energy consumption for heating and air conditioning is also ensured. For the imprecnatior. applications according to the invention, the dispersions according to the invention are added to the surface of the sukstrate by customary distribution methods known to date, such as, for example, by brushing, spraying, 23 knife coating, rolling, pouring, spreading with a trowel, immersion and roll coati.ng. For masonry treatment, it is necessary for the preparations to penetrate far into the masonry. Low-visccsaty dispersions are therefore preferred for the masonry treatment The property of penetrating into the masonry may be be meterial property or the penetration is artificially pron.cted by transporting the dispersions into the masoni-y with elevated pi'essure. The dispersions according to the invention can also be used in combinations with organic dispersions and pigments for formulating coating materials, in order to impart hydrophobic properties to these coating materials. This application can also be effected in combination with fluoroorganic polymer dispersions, for example if an oil- and dirt-repellent effect is also desired in addit:ion to water-repellent effect, for example to prevent damage to the structure by graffiti. In the process according to the invention, the dispersion according to the invention can be applied in concentrated form or in a forra dilated with water, depending on substrate and the intended effect. If the application according to the invention is effected in dilute form, the content of component (A) in the dispersion used is then preferably from 2 to 3 5% by weight, in particular from 5 to 20% by weight. The process for the treatment of substrates has the advantage that it is efficient and economical and that the substrates are protected in the long term from the influence of water. In the follov;i:.ig examples, all data relating to parts and percentages are based on weight, unless stated otherwise. Unless s-ated otherwise, the following examples are carried out at a pressure of the ambient atmosphere, i.e. at about 24 1000 hPa, and at: rcom temperature, i.e. about 20°C,, or a temperature which is established on combining the reactants at room temperature withoat. additional heating or cooling. Example 1 45 parts of is ooctyltrieithoxysilane (available under the name SILRES® 3S 1701. from Wacker Chemie AG, Munich, Germany) are mixed with 1 part of ethoxylated sorbitan laurate (HLB = 16.7) and 1 part of sortitan laurate (HLB =8.6) using an Ultra-Turrax® (HCA^'-Werke GmbH &: Co. KG, Staufen, Germany). Thereafter, 52.3 parts of ilemineralized water (conductivity In order to test the quality and stability, the following tests were carried out en the emulsion: particle size measurement (D[4,3] = volume-mean particle size) using a Malvern Kastersizer (Malvern Instruments GmbH, Herrenberg, Germany; measuring principle: Frauenhofer diffraction). Stability on centrifuging (Ih at 4000 revolutions per min, which corresponds to a load with 2500 times the force of gravity) , visual assessment of water or oil deposits and of the creaming of the eirulsion. Stability on storage at'elevated temperature in a closed vessel 25 for 14 d at ;JC-'C, vi^sual assessment of water and oil deposits and of the creaning of t:he emulsion and determination of the molar fractior. of alkYltrialkcxysilane, based on the sum of the silicon in the silanes find siloxanes in comparison with the fraction befora the storage at elevated temperature, by quantitative ■'Si--1MR analysis ,. The results cire shourn in table 1. Example 2 The procedure Sescribed in example 1 is repeated, except that 0.75 pari: of an ethoxylated isotridecyl alcohol having 5 ethylene glycol groups iHLB = 11.2), 0.75 part of an ethox^^la-ced castor oil having 200 ethylene glycol groups (HLB = 18.1) and 0.5 part of l-methyl-2-norstearyl-3-stearic acid amidoethylimidazclir-ium methosulfate/propylene glycol 3:1 (available under the name Rewoquat® W 75 PG from Tego Service GmbH, Essen, Germany) are used as emulsifiers. The results are shown in table 1. Con^euratl-ve example 1 The procedure described in example 1 is repeated, except that no hexadecyltrimethylammonium chloride is used. The results are shovMn in table 1. Comparative example 2 The procedure described in example 1 is repeated, except that, instead of the ncnionogenic emiulsifers, exclusively 2 parts of hexadecyltrimsthylcirttmonium chloride are used as an emulsifier. 26 The results are shown in table 1. Comparative example 3 The procedure fiescr:.bed in example 1 is repeated, except that, instead of the ncnionog€;nic emulsifiers, 2 parts of l-miethyl-2-norsteciryl-3 --s r.eeri.c acid anidoethylimidazolinium methosulfate/pcopvlene glycol 3:1 are used as an emulsifier. The results are shoMnn in table 1. Comparative example 4 The procedure described in example 1 is repeated, except that 2 parts of oleic acid and 0.5 part of monoethanolamine are used as an emulsifisr. The results are shown in table 1. Comparative example 5 The procedure described in example 1 is repeated, except that 1 part of hexadecyltrimethylaromonium chloride and 1 part of sorbitan laurate (HLB =8.6) are used as an emulsifier. The results are shoum in table 1. Example 3 15 parts of the isooctyltriethoxysilane used in example 1 and 10 parts of octadecylmethyldimethoxysilane are mixed with 5 parts of an oligomeric alkoxysiloxane of the empirical formula CHjSi (OCH2CH;.) o.8Oi.1 and with 7 parts of a methylsilicone resin having a glass transition temperature of 45°C, an average molar mass of about 10 000 g/mol and a content of ethoxy groups of 2.8% by weight (available under the name SILRES® BS1321 from Wacker Chemie AG, Munich, Germany), 0.25 part of 27 aminoeithyltrierthoxysilane and 2 parts of a hydrophobized silicic acid (aveilable under the name HDK® H 2000 from Wacker Chemie AG, Munich, (Germany) ,. The mixture thus obtained is processed with 1.2 parts: of an ethoxylated isotridecyl alcohol having 16 ethylene glycol groups (HLB =15.5), 0.5 part of 1-methyl--2-no3rstaaryl-3-st;ear;-C acid amidoethyliirddazoliniua: methosulfate and 55 part.s of water using an Ultra-Turrax to give cin emulsion. 4 part:s of a 50% strength aqueous emulsion of a polydimethylsilcxane containing amino groups and having a viscosity of 5 00 n.Pa.s and an amine number of 0.15 meq/g (available under the name SIILRES® BS 13 06 from Wacker Chemie AG, Munich, Germany; are; also added to this emulsion. The emulsion is homogenized using a high pressure homogenizer (APV 2000, Invensys APV Unna) at 200 bar. The results ara shown in table 1, Example 4 25 parts of the isoocty].triethoxysilane used in example 1 are mixed with 5 parts of an oligomeric alkoxysiloxane of the empirical fonrula CK3Si (OCH2CH3)and with 7 parts of methylsilicone resin, which consists of 90 mol% of units of the formula (II), in which c is 1, and 10% of units of the formula (II), in which c is 2, having a weight average molar mass of 6700 g/mol and a content of ethoxy groups of 3.1% by weight and of hydroxy groups of 0.57% by weight, 0.25 part of aminoethylaminoprcpyltriethoxysilane and 2 parts of a hydrophobized silicic acid (available under the name HDK® H 2000 from Wacker Chemie A3, Munich, Germany). The mixture thus obtained is processed with 0.6 part of an ethoxylated isotridecyl alcohcl havi.ng 5 ethylene glycol groups (HLB = 11.2), 0.6 part of an ethoxylated castor oil having 200 ethy¬lene glycol groups (HLB = 18.1), 0.5 part of 28 benzyltrimetnylannoriam chloride and 55 parts of water using an Ultra-Turrax to give an emulsion. 4 parts of a 5 0% strength. aqueous emalsiDn cf a polydi-methylsiloxane containing amino groups and havLnc; a viscosity of 500 mPa.s and an amine number of 0.15 meq/g (available under the name SILRES® BS 1306 from Wacker Chemie AG, MUNISH. ch, Gerrmany) are also added to this emulsion. The emulsion i.s homogenized using a high-pressure homogenizer (APV 2000, ]:nvensys APV Unna) at 2 00 bar. The results ara shouod in table 1. Exeunple 5 The dispersions according to the invention are used for impregnating munstar disks. For the production of the mortar disks, 2700 g of standard sand (available from Normensand GmbH, 592 69 Beckurn near Munster, Germany) , 9 00 g of white cement PZ 450 Z (available from Dyckerhoff Zementwerke AG, D-65203 Wiesbaden, Germany) and 4 50 g of tapwater were mixed. The 29 mixture is \'J.:\e:.:\ pcured into plastic rings (diameter 8.5 cm, height 2 cm), which are present on a plastic film. For compaction and removal C)f a;-r inclusions, a spatula is inserted frequcently iat:) the material and the supernatant of the concrete mix is ther, removed using the spatula. The samples are covered with a film and cleaned at the edges. The test specimens must be stored for at least 3 months under standard climatic conditions (23C, 50% relative humidity) before being used. Immediately before use, the top of the samples is sandblasted for removing the sintered cement layer. Prior to impregnation, the nortar disks thus obtained are immersed for 2 minutes in demineralized water and, after packing in film, are stored for 12 hours at room temperature. Thereafter, thay are stored without packing for 2 hours under standard clime.tic conditions (23/50) and are impregnated after determining the initial weight (Wl). This is done by a procedure in wnich the test specimens are immersed for 1 minute in the respective dispersion according to the invention (excess liquid level about 5 cm). The dispersions according to examples 1 and 2 are used in concentrated form and the dispersions according to examples 3 and 4 diluted in weight ratio 1:4 with water for the impregnation. Weighing (W2) is now effected again, and the absorption of impregnating agent is determ.ined from the difference (W2 - Wl). For development of the hydrophobic effect, the samples are stored for 14 3ays under standard climatic conditions (23/50). The test specimens are now weighed again (W5) and placed for 24 hours in demineralized water (excess water level 5 cm) . The water absorption is determined by weighings (W6). The percentage water absorption is calculated according to (W6 -W5)/W5 X 100, The results and a blind test without dispersion 30 Patent, claims! 1. An aqueous lispersion containing (A) at least one crcanosiilicon compound selected from (Al) silanes of then formula (I) , in which R may be identical or different and are monovalent, SiC-bonded, optionallY substituted hydrocarbon radicals having at least 4 carbon acorns, R1 may be identical or different and are monovalent, optionally substituted hyarccarbon radicals, R2 may be identical or different and are monovalent, SiC-bonded, optionally substituted hydrocarbon radicals having 1 to 3 carbon a-oms, a is 1, 2 or 3 and b is 0, 1 or 2, with the proviso that the sum of a and b is 1, 2 or 3, and/or the partial hydrolysis products thereof, and (A2) siloxanes containing units of the formula (II) , in which R3 may be identical or different and is a hydrogen atom or a monovalent, SiC-bcnded, optionally substituted hydrocarbon radical, R4 may be identical or different and is a hydrogen atom or a monovalent,, optionally substituted hydrocarbon radical, c is 0, 1, 2 or 3 and d is 0, 1, 2 or 3, with the proviso that the sum of c and d is less than or equal to 3, 32 (B) at least one enulsifier having an HLB value greaten: than or equal to 12, optionally as a mixture with nonioriic emulsifiers having an HLB value of less than 12, (C) at least o:ie cationj.c surfactant selected from (Cl) compouncLD of 1:l:.e l;ormula R^'eR'(4-e)n' X" (III) and (C2) compounds of the formula (IV) , in which R5 are optionally substituted hydrocarbon radicals, R6 may be identical or different and are optionally substituted aliphatic hydrocarbon reidicals having at least 10 carbon atoms or optionally substituted aromtatic hydrocarbon radicals having at least 6 carbon atoms, R7 are optionally substituted aliphatic hydrocarbon radicals having at least 10 carbon atoms or optionally substituted aromatic hydrocarbon raclicals having at least 6 carbon atoms, R8 are optionally substituted hydrocarbon radicals, R9 may be identical or different and are optionally substituted hydrocarbon radicals, e is 2 or 3 and X" is a monovalent organic or inorganic anion, (D) water 33 and optionally (E) further components . 2. The aqueous dispersion as claimed in claim 1, wherein components (A) is or a mixture of (Al) and {A2). 3. The aqueous dispersion as claimed in claim 1 or 2, wherein component (B) is at least one nonionic emulsifier having an HLB value greater than or equaal to 14, optionally as a mixture with nonionic einulsifiers having an HLB value of less than 12. 4. The aqueous dispersion as claimed in one or more of claims 1 to 3, wherein mixtures of nonionic emulsifiers, of which at least one emulsifier has an HLB value greater than or equal to 12, are used as component (B). 5. The aqueous dispersion as claimed in one or more of claims 1 to 4, wherein component (C) is a benzyltrimethylammonium compound or a quaternary imidazolinium compound. 6. The aqueous dispersion as claimed in one or more of claims 1 to 5,which is an aqueous dispersion containing (A) organosilision compound (Al), optionally as a mixture with (A2), (B) mixtures of ncnionic emulsifiers, of which at least one emulsifier has an HLB value greater than or equal to 12, (C) cationic sarfactant of the formulae (III) and/or (IV), (D) water and optionally (E) further components 7. The aqueous dispersion as claimed in one or more of claims 1 to 6, which is an aqueous dispersion containing 34 (A) from 10 to 6C% by weight of (Al) and from 0 to 20% by- weight of (A2), (B) from 1.0 to 10% by weight of mixtures of nonionogenic emulsifiers, of which at: least one emulsifier has an HLB value greater than or ecual to 12, (C) from 0.1 to) 5% by weight of cationic surfactant of the formulae (III) arc/or (]:V), (D) Welter and optionally (E) further components. 8. A process for the preparation of the dispersions as claimed in one or more of claims! 1 to 7 by mixing the components (A) , (B) , (C) , (D) and optionally (E) . 9. A process fDr the treatment of substrates, wherein the substrates are brought into contact with the dispersions as claimed in one or more of claims 1 to 7. 10. The process as claimed in claim 9, wherein the substrates to be treated are mineral substrates and wood-based materials.

Full Text

Aqueous dispersions of organosllicona compounds
The invention relates to aqueous dispersions of organosllicona compounds, the preparation thereof and the use thereof, in particular for the hydrophobing impregnation and mass hydrophotaing of mineral and organic building materials.
Silanes and slogans have long been used for the production of structures, for example solutions of silanes in organic solvents, as described, for example, in DE-A 1069057. For cost reasons, but rot least also because of the health hazards, during handling of organic solvents and the associated environmental pollution, working with organic solvents is disadvantageous.
Aqueous formulations based on alkylalkoxysilanes and -slogans are known. EP-A 234 024 describes silanes emulsions comprising nonionic emulsifiers, which have an HLB value of from 4 to 15. According to EP-A. 340 816 the stability of these compositions is improved by the addition of buffer salts. EP-A 631 999 describes aqueous formulations based on alkylalkoxysilanes, which contain cationic emulsifiers. According to WO-A 199516752 and EP-A 907 622, amine soaps are said to be suitable in particular for the preparation of silane/siloxane emulsions. WO-A 199522580 describes a series of further cationic emulsifiers in silane/siloxane emulsions. According to EP-A 1 147 072, the stability of silane/siloxane emulsions is particularly good when ionic emulsifiers are used in combination with nonionogenic emulsifiers which have an HLB value of less than 11.
Nevertheless, the aqueous structure preservatives prepared according to the prior art do not always have the desired stability and efficiency.

The invention relates to aqueous dispersions containing (A) at least one crcanosilicon compound selected from (Al) silanes of the formula
(I) ,
in which
R may be identical or different and are monovalent, SiC-bonded,
optionally substituted hydrocarbon radicals having at least 4
carbon atoms,
R1 may be identical or different and are monovalent, optionally
substituted hydrocarbon radicals,
R2 may be identical or different and are monovalent, SiC-bonded,
optionally substituted hydrocarbon radicals having 1 to 3
carbon atoms,
a is 1, 2 or 3 and
b is 0, 1 or 2, with the proviso that the sum of a and b is 1,
2 or 3,
and/or the partial hydrolysis products thereof, and
(A2) silicates containing units of the formula
(II) ,
in which
R3 may be identical or different and is a hydrogen atom or a
monovalent, SiC-bcnded, optionally substituted hydrocarbon
radical,
R4 may be identical or different and is a hydrogen atom or a
monovalent, optionally substituted hydrocarbon radical,
c is 0, 1, 2 or 3 and
d is 0, 1, 2 or 3, with the proviso that
the sum of c and d is less than or equal to 3,
3

(B) at least one nonionic emulsifier having an HLB value greater than or equal to 12, preferably greater than or ec'ual to 14, optionally as a mixture with nonionic emulsifiers having an HLB value o£ less than 12,
(C) at least one cationic surfactant selected from (CI) compounds cf the formula
R^R'(4-e)N' X' (III)
and
(C2) compounds of the formula
(IV),
in which
R5 are optionally substituted hydrocarbon radicals,
R6 may be identical or different and are optionally substituted
aliphatic hydrocarbon radicals having at least 10 carbon atoms
or optionally substituted aromatic hydrocarbon radicals having
at least 6 carbon atoms,
R7 are optionally substituted aliphatic hydrocarbon radicals
having at least 10 carbon atoms or optionally substituted
aromatic hydrocarbon radicals having at least 6 carbon atoms,
R8 are optionally substituted hydrocarbon radicals,
R9 may be identical or different and are optionally substituted
hydrocarbon radicals,
e is 2 or 3 an3
X" is a monovalent organic or inorganic anion,
4

(D) water
and optionally
(E) further components.
Examples of the radical R are 1-n-butyl, 2-n-butyl, isobutyl, tert-butyl, n-pentyl, isopentyl, neopentyl and tert-pentyl radical; hexyl radicals, such as the n-hexyl radical; heptyl radicals, such as the n-heptyl radical; octyl radicals, such as the n-octyl radical, and isooctyl radicals, such as the 2,2,4-trimethylpentyl radical; nonyl radicals, such as the n-nonyl radical; decyl radicals, such as the n-decyl radical; dodecyl radicals, such as the n-dodecyl radical; octadecyl radicals, such as the n-octadecyl radical; cycloalkyl radicals, such as the cyclopentyl, cyclohexyl, cycloheptyl and methyleyelohexyl radicals; aryl radicals, such as the phenyl, naphthyl, anthryl and phenanthryl radical; alkaryl radicals, such as o-, m- and p-tolyl radicals; xylyl radicals and ethylphenyl radicals; and aralkyl radicals, such as the benzyl radical and the a- and the P-phenylethyl radical.
Examples of substituted radicals R are aminoethylaminopropyl, glycidyloxypropyl and methacroylpropyl radical.
Radicals R are preferably hydrocarbon radicals having at least 4 carbon atoms, particularly preferably hydrocarbon radicals having 6 to IS carbon atoms, in particular hexyl and octyl radicals, very particularly preferably the n-hexyl radical, n-octyl radical and isooctyl radical, such as the 2,2,4-trimethylpentyl radical.
Examples of the radical R1 are the radicals stated below for R^.
5

Radicals R1 are prsferably c-ptionally substituted alkyl radicals having 1 to 4 carkon atoms, particularly preferably the rriethyl, ethyl, n-butyl, 2-metho>:yethyl and isopropyl radical, in particular the ethyl radical.
Radicals R' are pra:fer£ibly alkyl radicals having 1 to 3 carbon atoms, such as methyl, ethyl, n-propyl and isopropyl radicals, particularly preferably the methyl radical.
The value of a is preferably 1.
The value of b is preferably 0 or 1.
Examples of silanes (Al) are isobutyltriethoxysilane, hexyl-triethoxysilane, hexylmethyldiethoxysilane, n-octyltrimethoxy-silane, n-octyltriethoxysilane, n-octyltributoxysilane, isooctyltriethDxysilane, n-decyltriethoxysilane, dodecyImethyldimethoxysi1ane, hexadecyltrimethoxysilane, octadecylmethyldimethoxysilane, octadecylmethyldiethoxysilane and octadecyltriethoxysilane and aminoethylaminopropyl-triethox'/silane, glycidoxypropyltrimethoxysilane and methacroylpropyltrietho>r/-silane.
Silane (Al) is preferably n-hexyltriethoxysilane, n-octyltriethoxysilane and isooctyltriethoxysilane, n-octyltriethoxysilane and isooctyltriethoxysilane being particularly preferred.
If (Al) are partial hydrolysis products, those having 2 to 10 Si atoms are preferred. Partial hydrolysis products form when some of the radicals OR1 in the silanes of the formula (I) are eliminated by reaction with water or steam and OH groups bonded to silicon f rom These in turn can condense with elimination of
6

water to give silcxe.ne bonds, resulting in oligomers which may also con-cain OH croups i.n addition to groups OR1 Partial hydrolysis pro:iucts of silanes of the formula (I) may also be present as -an impur:.ty i.n the silane of the formula (I) .
Examples of ra:licals R^ are alkyl radicals, such as the methyl, ethyl, n-propyl, isopropyl, 1-n-butyl, 2-n-butyl, isobutyl, tert-butyl, n-pentyl, isopentyl, neopentyl and tert-pentyl radical; hexyl radicals, such as the n-hexyl radical; heptyl radicals, such as the n-heptyl radicals; octyl radicals, such as the n-octyl radical, and isooctyl radicals, such as the 2,2,4-trimethylpentyl radical; nonyl radicals, such as the n-nonyl radical; decyl radicals, such as the n-decyl radical; dodecyl radicals, such as the n-dodecyl radical; octadecyl radicals, such as the n-octadecyl radical; cycloalkyl radicals, such as the cyalcpentyl, cyclohexyl and cycloheptyl radical and methyleyelohexyl radicals; alkenyl radicals, such as the vinyl, 1-propenyl and 2-propenyl radical; aryl radicals, such as the phenyl, naphthyl, anthryl and phenanthryl radical; alkaryl radicals, such as the o-, m- and p-tolyl radicals; xylyl radicals and ethylphenyl radicals; and aralkyl radicals, such as the benzyl radical and the a- and the p-phenylethyl radical.
Examples of substituted radicals R^ are the trifluoropropyl
radical, the amincpropyl radical, the aminoethylaminopropyl
radical, the glycidyloxypropyl radical and the mercaptopropyl
radical.
R3 are preferably hydrocarbon radicals optionally substituted by oxygen- and nitrogen-containing functional groups and having 1 to 18 carbon atoms, particularly preferably alkyl radicals having 1 to 18 carbon atoms or aromatic hydrocarbon radicals having 6 to 9 carkon atoms, very particularly preferably
7

methyl, ri-hexyl, r-hepfyl, n-octyl, isooctyl, n-dodecyl. phenyl and ethylphenyl radicals;, in particular the methyl radical.
Examples of the radical R4are the radicals stated for
Radicals R3 are preferably a hydrogen atom or optionally substituted alkyl radicals having 1 to 4 carbon atoms, particularly preferably a hydrogen atom or the methyl, ethyl, n-butyl,, isopropyl and 2-methoxyethyl radicals, in particular a hydrogen atom or irethyl or ethyl radicals.
In formula (II), c is preferably 1, 2 or 3.
The value of d is preferably 0 or 1.
Siloxanes (A2) used according to the invention are any desired silicone oils, silicone resins and oligomeric siloxanes known to date, which contain units of the formula (II).
The siloxanes (A2) used according to the invention preferably contain no further units apart from the units of the formula (II) .
Examples of (A2) are organopolysiloxanes, such as
organopolysiloxanes v;hich contain alkoxy groups and can be prepared by reacting methyltrichlorosilane and optionally other alkyltrichlorosilanes or phenyltrichlorosilane with ethanol in water and correspond to empirical formulae such as CH3Si(OCH2CH3)o.801.i or C6H5Si (OCH2CH3) 0.7O1.2; these oligomeric siloxanes have a viscosity of less than 500 mPa.s, preferably less than 100 mPa.s, in particular less than 50 mPa.s, at 2 5°C;
8

oligomeric silDxeres which are obtainable by hydrolysis/condensation fron methyltriethoxysilane and isooctyl-rietnDxysi-.ane and correspond, for example, to the formula ( [Mesi:)3,: ] o :-,-o.5 :iOSi03/2] 0.02-0.2 [EtOi/2] 0.3-0.6)x (Me is methy]., 10 is isccctyl and Et is ethyl) and have a weight average molar ::iass of 1()00-10 000 g/mol ;
silicone resins in which c :.s 1 in at least 70% of the units of the formula (II) and c is 2 in the other units of the formula (II), preferably silicone resins in which c is 1 in at least 80% of the units cf the formula (II), in particular 90% of the units of the formula (II); these resins have a viscosity of more than 1000 mPa.s, preferably more than 5000 mPa.s, in particular more than 10 000 mPa.s, at 25°C and a content of from 1 to 6% b/ weight of alkoxy groups and from 0.2 to 1% by weight of hydrDxyl groups; and
polydimethylsiloxanes having a viscosity of from 30 to
1 000 000 mPa.3 at 25°C, which may contain hydroxyl groups
and/or aminoalkyl groups.
These siloxanes (A2) are preferably silicone resins, mixtures of highly viscous silicone resins with low-viscosity oligomers or silicone oils being particularly preferred. These mixtures have a viscosity cf preferably from 100 to 100 000 mPa.s, in particular from 100 0 to 10 000 mPa.s, at 25°C.
Component (A) is preferably (Al) or a mixture of (Al) and (A2), particularly preferably (Al).
If component (A) is a mixture of (Al) and (A2), the proportion of (Al) in the mixture is preferably from 2 0 to 96% by weight, in particular frcrr. 50 to 80% by weight, based in each case on
9

the sun of (Al) arid (A2) .
The dispersiors according to the invention contain component (A) in amounts of, preferably, from 5 to 70% by weight, particularly preferably fron 30 to 65% by weight, based in each case on the total formulation.
Examples of tha ncnionogenic emulsifiers (B) used according to the invention are sorbitan fatty acid esters, ethoxylated sorbitan fatty acid esters, ethoxylated fatty acids, ethoxylated linear or branched alcohols having 10 to 20 carbon atoms, ethoxylatec, alkylphenols, pent aery thrityl fatty acid esters, glyceryl esters and alkylpolyglycosides.
The nonionogenic emulsifiers (B) are preferably sorbitan fatty acid esters, ethoxylated sorbitan fatty acid esters, ethoxylated fatty acids, ethoxylated linear or branched alcohols having 10 to 2 0 carbon atoms and ethoxylated triglycerides.
Preferably, the dispersions according to the invention contain no ethoxrylated alkylphenols since it is known that these are not environmentally compatible.
The component (B) used according to the invention may be only one nonionogenic emulsifier having an HLB value of greater than or equal to 12, particularly greater than or equal to 14, or a mixture of a plurality of nonionogenic emulsifiers, with the proviso that at least one emulsifier has an HLB value greater than or equal to 12, in particular greater than or equal to 14.
Mixtures of nonionogenic emullsifiers, of which at least one emulsifier has an HLB value greater than or equal to 12, are
10

preferably used aS component (B) . The proportion of emulsifiers having an HLB value greater than or equal to 12 in the emulsifier mixture (B; is preferably at least 30% by weight.
The HLB value is an expression of the equilibrium between hydrophilic cin;l hydrophobic groups of an emulsifier. The definition of the HLB value and methods for determining it are generally known and are described, for example, in Journal of Colloid and Interface Science 298 (2006) 441-450 and the literature cited there.
Examples of the ncnionogenic emulsifiers (B) used according to the invention and having an HLB value greater than or equal to 12 are (HLB values according to manufacturer, POE is polyoxyeuhylena):
11

Examples of nonionogenic emulsifiers which can additionally be used and have an HLB value

The dispersions according to the invention contain component (B) in amounts of, preferably, from 1.0 to 10% by weight, particularly preferably frora 1.5 to 3% by weight, based in each case on zha total formulation.
Examples of radicals R^ and R^ are, in each case independently of one another, the examples stated for radical R^.
Radicals R" are preferably alkyl radicals having 1 to 4 carbon atoms, particularly preferably the methyl radical.
Examples of hydrocarbon radicals R^ and R'^ are, in each case independently of one another, decyl radicals, such as the n-decyl radical; dcdecyl radicals, such as the n-dodecyl radical; hexadecyl radicals, heptadecyl radicals, octadecyl radicals, such as -he n-DCtadecyl radical; aryl radicals, such as the
13

phenyl, naphtrL/i, £i.rthryl and phenanthryl radical; alkaryl radiccils, siich as o--, m- and p-tolyl radicals; xylyl radicals and ethylphenyl radi-cals;; and aralkyl radicals, such as the benzyl radical and the a- and the p-phenylethyl radical.
Examples of su'ostituted hyd^rocarbon radicals R^ and R' are, in each case independently of one another, lauramidoethyl radicals, palHiitair.idoethyl radicals and stearamidoethyl radicals.
Radicals R'" are preferably linear alkyl radicals having 12 to 22 carbon atoms or aromatic radicals, particularly preferably aromatic hydro:;arbon radicals, in particular the benzyl radical.
Radicals R' are preferably linear alkyl radicals having 12 to 22 carbon atoms, in particular the lauryl, palmityl, oleyl or stearyl radical.
Examples of radicals R^ aore the examples stated for radicals R^, R^ and RRadicals R^ are preferably optionally substituted alkyl radicals having 1 to 22 carbon atoms, particularly preferably the methyl, lauryl, palmityl, oleyl, stearyl, lauramidoethyl, palmitamidoethyl and stearamidoethyl radical.
Radicals R^ are preferably alkyl radicals having 1 to 4 carbon atoms, particularly preferably the methyl radical.
Examples of anion X' and halide ions, such as the chloride, bromide and iodide :.on, hydrogensulfate ions, alkylsulfate ions, such as the meth-ji'lsulfate ion, and dialkylphosphate
14

ions .
An anion X" is preferably a chloride, bromide, iodide or methylsulfate anion, particularly preferably a chloride or methylsulfate anion,
Examples of tha component (Cl) used according to the invention are all ;<:no :ju5ternary amiaonium compounds which carry at least one substituted or unsubstituted hydrocarbon radical having lecist ic carbon atoms such as> dodecyldimethylairoT.onium chloride, tetradecyltrimethylammonium bromide, stearyltrimethylamraonium chloride, distearyldimethylainraonium chloride, cetyltrimethylammonium chloride, behenyltrimethylarnmonium bromide, dodecylbenzyldimethylammonium chloride and benzyl-trimethylaininoniurr. chloride.
Components (Cl) are preferably aryl- or alkyltrimethylammonium salts, such as stearyltrimethylammonium chloride and cetyltrimethylaminium chloride, particularly preferably benzyltrialkylamir.cnium salts, in particular trimethylbenzyl-ammonium chloride and trimethylbenzylammonium methosulfate.
Examples of the componejnt (C2) used according to the invention are all kno^,^7n quaternar-^^' imidazolinium compounds which carry at least one substituted or unsubstituted hydrocarbon radical having at least 10 carbon atoms, such as l-methyl-2-stearyl-3-stearylamidoethylimidazolinium methosulfate, l-methyl-2-norstearyl-3-stearylamidoethylimidazolinium methosulfate, 1-methyl-2-oleyl-3-cleylamidoethylimidazolinium methosulfate, 1-methyl-2-stearyl-3-meth)limidazolinium methosulfate, 1-methyl-2-behenyl-3-methyliraidazolinium methosulfate and l-methyl-2-dodecyl-3-methyliir.idazolinium methosulfate.
15

Componenr. (C2) is preferabl]-l-methyl-2-stearyl-3-stearyl-araidoethylini:.dazolinum. methosulfate, 1-methyl-2-norst€5aryl-3-sceeryL amidoethylimidazolinium methosulf ate and 1-methyl-2-oleyl -3 -cleylaniidoethylimidazolinium methosulfate .
Components (C) used according to the invention are preferably benzyltrimethylairrr.or.-ium compounds or quaternary imidazolinium compounds, q-aaternary imidazolinium compounds being particularly preferred.
The dispersions according to the invention contain component (C) in amounts of, preferably, from 0.1 to 5% by weight, particularly preferably from 0.3 to 1.5% by weight, based in each case on the total amount of the dispersion.
In the case of dispersions according to the invention, the weight ratio of component (B) to component (C) is preferably from 0.5 to 10, in particular from 2 to 5.
The water (D) used according to the invention may be any desired type of v;ater, such as, for example, natural waters, such as, for example, rainwater, groundwater, spring water, river water and seawater, chemical waters, such as, for example, demineralized v/ater or distilled or (multiply) redistilled v/ater, waters for medicinal or pharmaceutical purposes, such as, for example, purified water (Aqua purificata; Pharm.. Eur. 3), Aqua deionisata, Aqua destillata. Aqua bidestillata. Aqua ad injectionam or Aqua conservata, drinking water according to the German drinking water regulation and mineral waters.
The water (D) used according to the invention is preferably water having a ccnductivity of less than 10 uS/cm, in
16

particular less than 2 uS/cn.
The dispersions according to the invention contain component (D) in amounts of, preferabLy, from 20 to 9 5% by weight, particularly ;pc:eferabiy fron 40 to 60% by weight, based in each case on che total araount; of dispersion.
The further co:Tipcnents (E) optionally used according to the invention may be all additives which have also been used to date in aq-ueous dispersions, such as, for example, thickeners, organosilicon comrpounds which differ from (Al) and (A2), catalysts, substances for adjusting the pH, buffer substances, fillers, fragrances, dyes, antifreezes, such as glycols and glycol ether, and preservatives.
Examples of optionally used thickeners (E) are polyacrylic acid, polyacrylates, cellulose ethers, such as
carboxymethylcellulose ctnd hydroxyethylcellulose, natural gums, such as xanthan gum, and polyurethanes.
Examples of optionally used organosilicon compounds (E) are silanes which contain no hydrocarbon groups having at least 4 carbon atoms, such as, for example, tetraethoxysilane, trimethylmethoxysilane, aminopropyltriethoxysilane and aminopropyIme tby1dime thoxys i1ane.
Examples of substances for adjusting the pH are, in addition to aminosilanes, also amines, such as, for example, monoethanolamine, or alkali metal hydroxides. If required for ensuring the constancy of the pH over a relatively long period, buffer systems, such as salts of acetic acid, salts of phosphoric acia, salts of citric acid, in each case in combination with the free acid, may also be used, depending on the desired pE.
17

The dispersior-D accordirig to the invention may contain silicon dioxide (silicic acr.ds) , titanium dioxide or aluminum oxide havincf a BET sarface area of, preferably, from 20 to 1000 m2/g, a part:.cle siz:2 cf, preferably, less than 10 and an agglomerate si?,e cf, preferably, less than 100 ]im as fillers (E) .
The optionally used fillers (E) are particularly preferably silicic acids, in particular those having a BET surface area of from 50 to 800 m2/g. These silicic acids may be pyrogenic or precipitated silicic acids. In particular, pretreated silicic acids, such as, fcr example, commercially available completely or partly hydrophcbed silicic acids, can be used as fillers (E). Examples of commercially available hydrophobic silicic acids which can be used according to the invention are pyrogenic, treated silicic acid having a BET surface area of 12 0 m2/g and a carbon content of 0.8% by weight (available under the name HDK® HI5 from Wacker Chemie AG, Germany) , a pyrogenic treated silicic acid having a BET surface area of 140 m2/g and a carbon content of 2.8% by weight (available under the nanie HDK® H2000 from Wacker Chemie AG, Germany) and a precipitated silicic acid treated with polydimethylsiloxane and having a BET surface area of 90 m2/g (available under the name "Sipernat DlO" from Degassa AG, Germany).
The dispersions according to the invention are preferably free of water-immiscible solvents or contain water-immiscible solvents in amounts of not more than 1% by weight, based on the total amount of dispersion.
In the context of the present invention, "water-immiscible solvents" are to be understood as meaning all solvents which are soluble in arr.cunts of not more than 1 g/1 in water at 20°C and a pressure of 101.325 kPa.
18

In particular, these water-:.mir.iscible solvents have a vapor pressure of 0,1. kFa or higher at 20°C.
Examples of such water-immiscible solvents are benzene, toluene, xyler.e, hexane, cyclohexane and paraffinic hydrcoarbon mixtures.
The dispersions according to the invention are preferably those containing
(A) organosilicon compound (Al), optionally as a mixture with (A2),
(B) mixtures of ncnionocfenic emulsifiers, of which at least one emulsifier has an. HLB value greater than or equal to 12,
(C) cationic surfactant of the formulae (III) and/or (IV),
(D) water and optionally
(E) further co:npcner.ts .
The dispersions according to the invention are particularly preferably those containing
(-A) from 10 to 6C% by weight of (Al) and from 0 to 20% by weight of (A2),
(B) from 1.0 to 10% by v/eight of mixtures of nonionogenic emulsifiers, of which at least one emulsifier has an HLB value greater than or equal to 12,
(C) from 0.1 to 5% by weight of cationic surfactant of the formulae (III) and/or (IV),
(D) water and optionally
(E) further co:npcnents.
In particular, the dispersions according to the invention contain no further components over and above the components
19

(A) , (B) , (C) , (C) a,nd (E) .
The preparaticci cf the aqaeous dispersions according to the invention is effected 'by processes known per se. Usually, the preparation is effected hy sirrple stirring of all constituents at temperatures cf prefe^rabiy from 1 to 50°C and optionally subsequent horaDgeriization, for example using jet dispersers, rotor-stator hDmcgenizers at peripheral speeds of preferably from 5 to 40 m/s, colloid mills or high-pressure homogenizers at homogenization pressures of preferably from 50 to 2000 bar.
The invention furtherraoi-e relates to a process for the preparation of the dispersions according to the invention by mixing the components (h), (B), (C), (D) and optionally (E).
In a preferred eirtodiment of the process according to the invention, the ccirponent (B; , at part of the component (D) and optionally component (C) are initially introduced, the component (A) is incorporated using a rotor-stator homogenizer, the remaining amount of component (D), optionally component (E) and, unless also alz-eady initially introduced at the beginning, componenr (C) are incorporated with homogenization. This is preferably followed by homogenization using a high-pressure homogenizer at frcm 50 to 2000 bar, in particular at from 100 to 500 bar.
Homogenization techniques, including high-pressure homogenizers, are generally known. In this context, reference may be made, for example, to Chemie Ingenieur Technik, 74(7), 901-909 2002.
In the process according to the invention, it is possible - if desired - to use the components (Al) and/or {A2) and optionally
20

(E) in the :from cf dispersions or solutions and to mix then with the rerriciiMing components.
The dispersions according to the invention are preferably milky, white to fceice liquids.
The dispersion^ eccordirig to the invention have a pH of preferably from 5 to 9, in particular from 6 to 8.
The dispersions according to the invention have a proportion of nonvolatile compounds (for example determined according to ASTM D 5095) of preferably from 10 to 80% by weight, particularly preferably from 20 to 70% by weight.
The dispersions according to the invention have a volume-average particle size preferably from 0.1 to 10 urn, in particular from 0.3 to 1.5 pm.
The dispersity of the dispersions according to the invention is in the range of preferably from 0.5 to 5, particularly preferably from 1.5 to 1. This value is calculated from (D90 D10)/D50, where Dx is the particle size at which x% of the volume of the internal phase are present in particles of less than or equal to this particle size.
The dispersions according to the invention have a viscosity of, preferably, less than 10 000 mPa.s, in particular less than 1000 mPa.s, measured in each case at 25°C.
The dispersions according to the invention have the advantage that they have a very long shelf-life.
The dispersions according to the invention have the advantage
21

that they can be prepared economically.
The dispersions sccording to the invention have the advantage that they are sin.ple to handle.
The dispersions according to the invention have the advantage that they can oe easily diluted and have a very long shelf-life even in dilute from
The process for the preparation of the dispersions according to the invention has the advantage that it can be carried out in a simple manner.
The dispersions according to the invention have the advantage that they develop a very good and stable impregnating effect and very good .penetration behavior on different substrates .
The aqueous dispersions according to the invention can be used for all purposes for which dispersions based on organosilicon compounds have also been used to date. They are, for example, outstandingly suitable as preservatives for structures, in particular for hydrophobing various mineral or organic substrates. The manner in which such dispersions are used is known to the person skilled in the art.
The present invention furthermore relates to a process for the treatment of substrates, wherein the substrates are brought into contact with the dispersions according to the invention.
Examples of substrates which can be treated with the dispersions according to the invention are mineral substances, such as masonry, mortar, brick, limestone, marble, sand-lime brick, sandstone, granite, porphyry, concrete and cellular
22

concrete, and :)rcan;.c substances, such as wood, paper, board, textiles and mannade and natzural fibers .
In the process according to the invention, the dispersions generally penetrate into the capillaries of the substrate and dry there.
In the process according to the invention, mineral substrates and wood-base materials are preferably used.
The treatment according to the invention preferably comprises impregnation, coating, priming and injection, particularly preferably impregnation, in particular the substrate being brought into contact with the dispersion and the dispersion penetrating partly or completely into the substrate.
The impregncition accordi.ng to the invention preferably comprises hydrophobing impregnation and can be effected both as impregnation of the surface and as injection or as mass hydrophobing.
The water absorption of the substrate is drastically reduced by the hydrophobing according to the invention, which reduces the thermal conductivity but also prevents the destruction of the building materials by the influence of freezing and thawing cycles or salt or, in the case of wood-based materials, by rotting or fungal attack. Thus, not only is the value of the material thus treated preserved but, for example, lower energy consumption for heating and air conditioning is also ensured.
For the imprecnatior. applications according to the invention, the dispersions according to the invention are added to the surface of the sukstrate by customary distribution methods known to date, such as, for example, by brushing, spraying,
23

knife coating, rolling, pouring, spreading with a trowel, immersion and roll coati.ng. For masonry treatment, it is necessary for the preparations to penetrate far into the masonry. Low-visccsaty dispersions are therefore preferred for the masonry treatment The property of penetrating into the masonry may be be meterial property or the penetration is artificially pron.cted by transporting the dispersions into the masoni-y with elevated pi'essure.
The dispersions according to the invention can also be used in combinations with organic dispersions and pigments for formulating coating materials, in order to impart hydrophobic properties to these coating materials. This application can also be effected in combination with fluoroorganic polymer dispersions, for example if an oil- and dirt-repellent effect is also desired in addit:ion to water-repellent effect, for example to prevent damage to the structure by graffiti.
In the process according to the invention, the dispersion according to the invention can be applied in concentrated form or in a forra dilated with water, depending on substrate and the intended effect. If the application according to the invention is effected in dilute form, the content of component (A) in the dispersion used is then preferably from 2 to 3 5% by weight, in particular from 5 to 20% by weight.
The process for the treatment of substrates has the advantage that it is efficient and economical and that the substrates are protected in the long term from the influence of water.
In the follov;i:.ig examples, all data relating to parts and percentages are based on weight, unless stated otherwise. Unless s-ated otherwise, the following examples are carried out at a pressure of the ambient atmosphere, i.e. at about
24

1000 hPa, and at: rcom temperature, i.e. about 20°C,, or a temperature which is established on combining the reactants at room temperature withoat. additional heating or cooling.
Example 1
45 parts of is ooctyltrieithoxysilane (available under the name SILRES® 3S 1701. from Wacker Chemie AG, Munich, Germany) are mixed with 1 part of ethoxylated sorbitan laurate (HLB = 16.7) and 1 part of sortitan laurate (HLB =8.6) using an Ultra-Turrax® (HCA^'-Werke GmbH &: Co. KG, Staufen, Germany). Thereafter, 52.3 parts of ilemineralized water (conductivity In order to test the quality and stability, the following tests were carried out en the emulsion:
particle size measurement (D[4,3] = volume-mean particle size) using a Malvern Kastersizer (Malvern Instruments GmbH, Herrenberg, Germany; measuring principle: Frauenhofer diffraction).
Stability on centrifuging (Ih at 4000 revolutions per min, which corresponds to a load with 2500 times the force of gravity) , visual assessment of water or oil deposits and of the creaming of the eirulsion. Stability on storage at'elevated temperature in a closed vessel
25

for 14 d at ;JC-'C, vi^sual assessment of water and oil deposits and of the creaning of t:he emulsion and determination of the molar fractior. of alkYltrialkcxysilane, based on the sum of the silicon in the silanes find siloxanes in comparison with the fraction befora the storage at elevated temperature, by quantitative ■'Si--1MR analysis ,.
The results cire shourn in table 1.
Example 2
The procedure Sescribed in example 1 is repeated, except that 0.75 pari: of an ethoxylated isotridecyl alcohol having 5 ethylene glycol groups iHLB = 11.2), 0.75 part of an ethox^^la-ced castor oil having 200 ethylene glycol groups (HLB = 18.1) and 0.5 part of l-methyl-2-norstearyl-3-stearic acid amidoethylimidazclir-ium methosulfate/propylene glycol 3:1 (available under the name Rewoquat® W 75 PG from Tego Service GmbH, Essen, Germany) are used as emulsifiers.
The results are shown in table 1.
Con^euratl-ve example 1
The procedure described in example 1 is repeated, except that no hexadecyltrimethylammonium chloride is used.
The results are shovMn in table 1.
Comparative example 2
The procedure described in example 1 is repeated, except that, instead of the ncnionogenic emiulsifers, exclusively 2 parts of hexadecyltrimsthylcirttmonium chloride are used as an emulsifier.
26

The results are shown in table 1.
Comparative example 3
The procedure fiescr:.bed in example 1 is repeated, except that, instead of the ncnionog€;nic emulsifiers, 2 parts of l-miethyl-2-norsteciryl-3 --s r.eeri.c acid anidoethylimidazolinium methosulfate/pcopvlene glycol 3:1 are used as an emulsifier.
The results are shoMnn in table 1.
Comparative example 4
The procedure described in example 1 is repeated, except that 2 parts of oleic acid and 0.5 part of monoethanolamine are used as an emulsifisr.
The results are shown in table 1.
Comparative example 5
The procedure described in example 1 is repeated, except that 1 part of hexadecyltrimethylaromonium chloride and 1 part of sorbitan laurate (HLB =8.6) are used as an emulsifier.
The results are shoum in table 1.
Example 3
15 parts of the isooctyltriethoxysilane used in example 1 and 10 parts of octadecylmethyldimethoxysilane are mixed with 5 parts of an oligomeric alkoxysiloxane of the empirical formula CHjSi (OCH2CH;.) o.8Oi.1 and with 7 parts of a methylsilicone resin having a glass transition temperature of 45°C, an average molar mass of about 10 000 g/mol and a content of ethoxy groups of 2.8% by weight (available under the name SILRES® BS1321 from Wacker Chemie AG, Munich, Germany), 0.25 part of
27

aminoeithyltrierthoxysilane and 2 parts of a hydrophobized silicic acid (aveilable under the name HDK® H 2000 from Wacker Chemie AG, Munich, (Germany) ,. The mixture thus obtained is processed with 1.2 parts: of an ethoxylated isotridecyl alcohol having 16 ethylene glycol groups (HLB =15.5), 0.5 part of 1-methyl--2-no3rstaaryl-3-st;ear;-C acid amidoethyliirddazoliniua: methosulfate and 55 part.s of water using an Ultra-Turrax to give cin emulsion. 4 part:s of a 50% strength aqueous emulsion of a polydimethylsilcxane containing amino groups and having a viscosity of 5 00 n.Pa.s and an amine number of 0.15 meq/g (available under the name SIILRES® BS 13 06 from Wacker Chemie AG, Munich, Germany; are; also added to this emulsion. The emulsion is homogenized using a high pressure homogenizer (APV 2000, Invensys APV Unna) at 200 bar.
The results ara shown in table 1,
Example 4
25 parts of the isoocty].triethoxysilane used in example 1 are mixed with 5 parts of an oligomeric alkoxysiloxane of the empirical fonrula CK3Si (OCH2CH3)and with 7 parts of methylsilicone resin, which consists of 90 mol% of units of the formula (II), in which c is 1, and 10% of units of the formula (II), in which c is 2, having a weight average molar mass of 6700 g/mol and a content of ethoxy groups of 3.1% by weight and of hydroxy groups of 0.57% by weight, 0.25 part of aminoethylaminoprcpyltriethoxysilane and 2 parts of a hydrophobized silicic acid (available under the name HDK® H 2000 from Wacker Chemie A3, Munich, Germany). The mixture thus obtained is processed with 0.6 part of an ethoxylated isotridecyl alcohcl havi.ng 5 ethylene glycol groups (HLB = 11.2), 0.6 part of an ethoxylated castor oil having 200 ethy¬lene glycol groups (HLB = 18.1), 0.5 part of
28

benzyltrimetnylannoriam chloride and 55 parts of water using an Ultra-Turrax to give an emulsion. 4 parts of a 5 0% strength. aqueous emalsiDn cf a polydi-methylsiloxane containing amino groups and havLnc; a viscosity of 500 mPa.s and an amine number of 0.15 meq/g (available under the name SILRES® BS 1306 from Wacker Chemie AG, MUNISH. ch, Gerrmany) are also added to this emulsion. The emulsion i.s homogenized using a high-pressure homogenizer (APV 2000, ]:nvensys APV Unna) at 2 00 bar.
The results ara shouod in table 1.

Exeunple 5
The dispersions according to the invention are used for impregnating munstar disks. For the production of the mortar disks, 2700 g of standard sand (available from Normensand GmbH, 592 69 Beckurn near Munster, Germany) , 9 00 g of white cement PZ 450 Z (available from Dyckerhoff Zementwerke AG, D-65203 Wiesbaden, Germany) and 4 50 g of tapwater were mixed. The
29

mixture is \'J.:\e:.:\ pcured into plastic rings (diameter 8.5 cm, height 2 cm), which are present on a plastic film. For compaction and removal C)f a;-r inclusions, a spatula is inserted frequcently iat:) the material and the supernatant of the concrete mix is ther, removed using the spatula. The samples are covered with a film and cleaned at the edges. The test specimens must be stored for at least 3 months under standard climatic conditions (23C, 50% relative humidity) before being used. Immediately before use, the top of the samples is sandblasted for removing the sintered cement layer.
Prior to impregnation, the nortar disks thus obtained are immersed for 2 minutes in demineralized water and, after packing in film, are stored for 12 hours at room temperature. Thereafter, thay are stored without packing for 2 hours under standard clime.tic conditions (23/50) and are impregnated after determining the initial weight (Wl). This is done by a procedure in wnich the test specimens are immersed for 1 minute in the respective dispersion according to the invention (excess liquid level about 5 cm). The dispersions according to examples 1 and 2 are used in concentrated form and the dispersions according to examples 3 and 4 diluted in weight ratio 1:4 with water for the impregnation. Weighing (W2) is now effected again, and the absorption of impregnating agent is determ.ined from the difference (W2 - Wl).
For development of the hydrophobic effect, the samples are stored for 14 3ays under standard climatic conditions (23/50). The test specimens are now weighed again (W5) and placed for 24 hours in demineralized water (excess water level 5 cm) . The water absorption is determined by weighings (W6). The percentage water absorption is calculated according to (W6 -W5)/W5 X 100, The results and a blind test without dispersion
30

Patent, claims!
1. An aqueous lispersion containing
(A) at least one crcanosiilicon compound selected from
(Al) silanes of then formula
(I) ,
in which
R may be identical or different and are monovalent, SiC-bonded,
optionallY substituted hydrocarbon radicals having at least 4
carbon acorns,
R1 may be identical or different and are monovalent, optionally
substituted hyarccarbon radicals,
R2 may be identical or different and are monovalent, SiC-bonded,
optionally substituted hydrocarbon radicals having 1 to 3
carbon a-oms,
a is 1, 2 or 3 and
b is 0, 1 or 2, with the proviso that the sum of a and b is 1,
2 or 3,
and/or the partial hydrolysis products thereof, and
(A2) siloxanes containing units of the formula
(II) ,
in which
R3 may be identical or different and is a hydrogen atom or a
monovalent, SiC-bcnded, optionally substituted hydrocarbon
radical,
R4 may be identical or different and is a hydrogen atom or a
monovalent,, optionally substituted hydrocarbon radical,
c is 0, 1, 2 or 3 and
d is 0, 1, 2 or 3, with the proviso that
the sum of c and d is less than or equal to 3,
32

(B) at least one enulsifier having an HLB value
greaten: than or equal to 12, optionally as a mixture with
nonioriic emulsifiers having an HLB value of less than 12,
(C) at least o:ie cationj.c surfactant selected from
(Cl) compouncLD of 1:l:.e l;ormula
R^'eR'(4-e)n' X" (III)
and
(C2) compounds of the formula
(IV) ,
in which
R5 are optionally substituted hydrocarbon radicals,
R6 may be identical or different and are optionally substituted
aliphatic hydrocarbon reidicals having at least 10 carbon atoms
or optionally substituted aromtatic hydrocarbon radicals having
at least 6 carbon atoms,
R7 are optionally substituted aliphatic hydrocarbon radicals
having at least 10 carbon atoms or optionally substituted
aromatic hydrocarbon raclicals having at least 6 carbon atoms,
R8 are optionally substituted hydrocarbon radicals,
R9 may be identical or different and are optionally substituted
hydrocarbon radicals,
e is 2 or 3 and
X" is a monovalent organic or inorganic anion,
(D) water
33

and optionally
(E) further components .
2. The aqueous dispersion as claimed in claim 1, wherein components (A) is or a mixture of (Al) and {A2).
3. The aqueous dispersion as claimed in claim 1 or 2, wherein component (B) is at least one nonionic emulsifier having an HLB value greater than or equaal to 14, optionally as a mixture with nonionic einulsifiers having an HLB value of less than 12.
4. The aqueous dispersion as claimed in one or more of claims 1 to 3, wherein mixtures of nonionic emulsifiers, of which at least one emulsifier has an HLB value greater than or equal to 12, are used as component (B).
5. The aqueous dispersion as claimed in one or more of claims 1 to 4, wherein component (C) is a benzyltrimethylammonium compound or a quaternary imidazolinium compound.
6. The aqueous dispersion as claimed in one or more of claims 1 to 5,which is an aqueous dispersion containing

(A) organosilision compound (Al), optionally as a mixture with (A2),
(B) mixtures of ncnionic emulsifiers, of which at least one emulsifier has an HLB value greater than or equal to 12,
(C) cationic sarfactant of the formulae (III) and/or (IV),
(D) water and optionally
(E) further components
7. The aqueous dispersion as claimed in one or more of claims 1
to 6, which is an aqueous dispersion containing
34

(A) from 10 to 6C% by weight of (Al) and from 0 to 20% by-
weight of (A2),
(B) from 1.0 to 10% by weight of mixtures of nonionogenic
emulsifiers, of which at: least one emulsifier has an HLB value
greater than or ecual to 12,
(C) from 0.1 to) 5% by weight of cationic surfactant of the
formulae (III) arc/or (]:V),
(D) Welter and
optionally
(E) further components.
8. A process for the preparation of the dispersions as claimed
in one or more of claims! 1 to 7 by mixing the components (A) ,
(B) , (C) , (D) and optionally (E) .
9. A process fDr the treatment of substrates, wherein the
substrates are brought into contact with the dispersions as
claimed in one or more of claims 1 to 7.
10. The process as claimed in claim 9, wherein the substrates
to be treated are mineral substrates and wood-based materials.

Documents:

2992-CHE-2008 CORRESPONDENCE OTHERS 18-07-2013.pdf

2992-CHE-2008 EXAMINATION REPORT REPLY RECEIVED. 03-12-2013.pdf

2992-CHE-2008 FORM-3 25-02-2013.pdf

2992-CHE-2008 AMENDED CLAIMS 03-12-2013.pdf

2992-CHE-2008 AMENDED PAGES OF SPECIFICATION 03-12-2013.pdf

2992-CHE-2008 CORRESPONDENCE OTHERS 25-02-2013.pdf

2992-CHE-2008 FORM-3 03-12-2013.pdf

2992-che-2008 abstract.pdf

2992-che-2008 claims.pdf

2992-che-2008 correspondence-others.pdf

2992-che-2008 description (complete).pdf

2992-che-2008 form-1.pdf

2992-che-2008 form-18.pdf

2992-che-2008 form-26.pdf

2992-che-2008 form-3.pdf

2992-che-2008 form-5.pdf

2992-che-2008 others.pdf

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Patent Number

258175

Indian Patent Application Number

2992/CHE/2008

PG Journal Number

50/2013

Publication Date

13-Dec-2013

Grant Date

12-Dec-2013

Date of Filing

28-Nov-2008

Name of Patentee

WACKER CHEMIE AG

Applicant Address

HANNS-SEIDEL-PLATZ 4, 81737 MUNCHEN

Inventors:

#	Inventor's Name	Inventor's Address
1	RAUTSCHEK, HOLGER	MUHLENBLICK 1, 01612 NUNCHRITZ
2	ACKERMANN, HARTMUT	ROBERT-KOCH-STR. 15B, 84489 BURGHAUSEN

PCT International Classification Number

C09D5/00; C09D5/00

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1	102007047907.9	2007-11-30	Germany