# US 8,147,918 B2 · Water-dilutable sol-gel composition > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 8,147,918 B2 - Document ID: US8147918B2 - Status: Granted - Kind: B2 - Application number: 12/159,785 - Filed: 2006-12-06 - Published: 2009-01-22 - Granted: 2012-04-03 - Earliest claimed: 2006-01-26 - Assignees: Evonik Degussa GmbH - Inventors: Burkhard Standke; Christian Wassmer; Peter Jenkner - Web page: https://patentgrep.com/patent/US8147918B2 ## CPC - C09D 4/00: Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond {; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16} - C09D 5/08: Anti-corrosive paints - C09D 183/14: in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms (C09D183/10 takes precedence) - C23C 2222/20: Use of solutions containing silanes - Y10T 428/31663: As siloxane, silicone or silane - C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D) - C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04) - Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION ## Abstract The present invention provides a sol-gel composition which is dilutable with water in any proportion and is based on the reaction of at least the following components: (i) a glycidyloxypropylalkoxysilane, (ii) an aqueous silica sol having a solids content of >1% by weight, (iii) an organic acid as hydrolysis catalyst, and (iv) n-propyl zirconate, butyl titanate or titanium acetylacetonate as crosslinker, starting from a mass ratio of the solids mass of component (ii) to component (i) 0.75, a process for preparing it and its use, in particular as a sol-gel composition for corrosion control coatings, a corresponding corrosion control coat or primer coat, and articles equipped with such a coating. ## Claims ### Claim 1 A water-dilutable sol-gel composition based on the reaction of at least the following components: (i) a glycidyloxypropylalkoxysilane, (ii) an aqueous silica sol having a solids content of >1% by weight, (iii) an organic acid as hydrolysis catalyst, and (iv) n-propyl zirconate as crosslinker, starting from a mass ratio of the solids mass of component (ii) to component (i) of 0.30 to 0.50. ### Claim 2 (depends on 1) The composition according to claim 1, wherein component (i) is selected from the group consisting of 3-glycidyloxypropyltrimethoxysilane, 3-glycidyloxypropyltriethoxysilane, 3-glycidyloxypropylmethyldimethoxysilane, 3-glycidyloxypropylmethyldiethoxysilane and mixtures thereof. ### Claim 3 (depends on 1) The composition according to claim 1, wherein colloidally disperse silica sol having a solids content of >20% to 50% by weight is component (ii). ### Claim 4 (depends on 1) The composition according to claim 1, wherein said organic acid is selected the group consisting of acetic acid, propionic acid and maleic acid. ### Claim 5 (depends on 1) The composition according to claim 1, wherein a content of component (iv) is 0.5% to 8% by weight, based on the composition. ### Claim 6 (depends on 1) The composition according to claim 1, which is further based on at least one tetraalkoxysilane, at least one alkylsilane or at least one phenyltrialkoxysilane as component (v). ### Claim 7 (depends on 1) The composition according to claim 1, having a pH of 6 to 9. ### Claim 8 (depends on 1) The composition according to claim 1, which is further based on at least one component (vi) selected from the group consisting of phosphoric acid, phosphates, polyacids, heteropolyacids, salts of polyacids, salts of heteropolyacids, flow control assistants, wetting agents, surfactants, aqueous dispersions of organic binders, nanoparticles, aminoalkylsilanes, aminoalkylsiloxanes, aqueous solutions of aminoalkylsilanes and aqueous solutions of aminoalkylsiloxanes. ### Claim 9 (depends on 1) The composition according to claim 1, wherein said sol particles have an average diameter of 40 to 200 nm. ### Claim 10 (depends on 1) The composition according to claim 1, having a solids content of >0.5% to <60% by weight, based on the total composition. ### Claim 11 (depends on 1) The composition according to claim 1, having a hydrolysis alcohol content of <5% by weight, based on the total composition. ### Claim 12 (depends on 1) The composition according to claim 1, having a 1 methoxypropan-2 ol content of ≦10% by weight, based on the total composition. ### Claim 13 (depends on 1) The composition according to claim 1, having a water content of around 99.5% to 30% by weight, based on the total composition. ### Claim 14 (depends on 1) The composition according to claim 1, further comprising at least one surfactant. ### Claim 15 (depends on 1) The composition according to claim 1, which is further based on a hydrophobicizing or oleophobicizing hydrosil system in a weight ratio of the hydrophobicizing or oleophobicizing hydrosil system to the composition of 1:0.01 to 0.01:1, the hydrosil system employed comprising <80% by weight of said siloxanes as active substance. ### Claim 16 (depends on 1) A process for preparing a sol-gel composition according to claim 1, comprising: initially introducing component (i), subsequently metering in component (iii) with effective commixing, then adding component (iv), thereafter adding component (ii), and causing reaction to take place, the reaction being carried out with the addition of at least one diluent, and starting from a mass ratio of the solids mass of component (ii) to component (i) of 0.30 to 0.50. ### Claim 17 (depends on 16) The process according to claim 16, wherein water, methanol, ethanol or 1 methoxy-propan-2 of is used as diluent. ### Claim 18 (depends on 16) The process according to claim 16, further comprising adding one or more components (v) which are introduced initially together with component (i). ### Claim 19 (depends on 16) The process according to claim 16, wherein the reaction is carried out at a temperature of 0 to 35° C. for a period of 1 to 60 minutes and the product mixture is allowed to afterreact at a temperature of 35 to 85° C. for 10 minutes to 4 hours. ### Claim 20 (depends on 16) The process according to claim 16, wherein a hydrolysis alcohol formed in the reaction, methanol, ethanol and/or n-propanol are/is removed from the system and, optionally, the amount of alcohol removed is replaced by a corresponding amount of water. ### Claim 21 (depends on 16) The process according to claim 16, further comprising adding at least one component (vi) to the product mixture. ### Claim 22 (depends on 16) The process according to claim 16, wherein the pH of the reaction mixture or product mixture is adjusted to a value of 6 to 9. ### Claim 23 (depends on 16) The process according to claim 16, wherein the product mixture is diluted with water. ### Claim 24 (depends on 16) A sol-gel composition obtainable according to claim 16. ### Claim 25 (depends on 1) A method of coating a substrate surface, comprising: coating said surface with a sol-gel composition according to claim 1. ### Claim 26 (depends on 25) The method according to claim 25, comprising applying the sol-gel composition to the substrate, to obtain a coated substrate, and subjecting said coated substrate to thermal curing. ### Claim 27 (depends on 25) The method according to claim 25, wherein said substrate is selected from the group consisting of, paper, cardboard, wood, chipboard, plastic, coating films, stone, ceramic, metal and metal alloys. ### Claim 28 (depends on 25) The method according to claim 25, wherein said substrate is selected from the group consisting of a metal or a metal alloy, and the coating on said substrate is a corrosion control coating. ### Claim 29 (depends on 25) The method according to claim 25, wherein said coating is an adhesion-promoting coating. ### Claim 30 (depends on 25) A coating obtainable by the method according to claim 25. ### Claim 31 (depends on 25) The method according to claim 25, wherein said coating has a thickness of 0.1 to 10 μm. ### Claim 32 (depends on 30) An article, comprising: a coating according to claim 30.