# US 10,370,497 B2 · Method for producing a cross-linked siloxane network > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,370,497 B2 - Document ID: US10370497B2 - Status: Granted - Kind: B2 - Application number: 15/664,846 - Filed: 2017-07-31 - Published: 2018-03-01 - Granted: 2019-08-06 - Earliest claimed: 2016-08-23 - Assignees: Milliken & Company - Applicants: Milliken & Company - Inventors: Russell A. Stapleton - Web page: https://patentgrep.com/patent/US10370497B2 ## CPC - C08G 77/06: Preparatory processes - C08G 77/08: characterised by the catalysts used - C08G 77/26: nitrogen-containing groups - C08L 83/04: Polysiloxanes - C08G 77/045: {containing less than 25 silicon atoms} - C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS - C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06) ## Abstract A method for producing a cross-linked siloxane network comprises the steps of: (a) providing a first part comprising (i) a first siloxane compound comprising at least one cyclic siloxane moiety, (ii) an inorganic particulate material, and (iii) an aminosilane compound, (b) providing a second part, the second part comprising a hydroxide salt, (c) combining the first part and the second part to produce a reaction mixture, (d) heating the reaction mixture to a temperature sufficient for the hydroxide salt to open the ring of the cyclic siloxane moiety, and (e) maintaining the reaction mixture at an elevated temperature so that at least a portion of the opened cyclic siloxane moieties react to produce a cross-linked siloxane network. ## Claims ### Claim 1 A method for producing a cross-linked siloxane network, the method comprising the steps of: (a) providing a first part comprising (i) a first siloxane compound comprising at least two cyclic siloxane moieties, (ii) an inorganic particulate material, and (iii) an aminosilane compound, wherein, optionally, at least a portion of the aminosilane compound is disposed on the surface of the inorganic particulate material; (b) providing a second part, the second part comprising a hydroxide salt; (c) combining the first part and the second part to produce a reaction mixture; (d) heating the reaction mixture to a temperature sufficient for the hydroxide salt to open the ring of the cyclic siloxane moiety; and (e) maintaining the reaction mixture at an elevated temperature so that at least a portion of the opened cyclic siloxane moieties react to produce a cross-linked siloxane network. ### Claim 2 (depends on 1) The method of claim 1, wherein the first part further comprises a second siloxane compound, and the second siloxane compound comprises at least one cyclic siloxane moiety. ### Claim 3 (depends on 1) The method of claim 1, wherein the inorganic particulate material is a metal oxide. ### Claim 4 (depends on 3) The method of claim 3, wherein the inorganic particulate material is silica. ### Claim 5 (depends on 1) The method of claim 1, wherein the inorganic particulate material is present in the first part in an amount of about 0.5 wt. % to about 10 wt. % based on the total weight of the first part. ### Claim 6 (depends on 1) The method of claim 1, wherein at least a portion of the aminosilane compound is disposed on the surface of the inorganic particulate material. ### Claim 7 (depends on 1) The method of claim 1, wherein the aminosilane compound is an amino-functional alkoxysilane compound. ### Claim 8 (depends on 7) The method of claim 7, wherein the aminosilane compound conforms to the structure of Formula (C) wherein R101, R102, and R103 are independently selected from the group consisting of alkyl groups and alkoxy groups, provided at least one of R101, R102, and R103 is an alkoxy group, R104 is an alkanediyl group, and R105 is selected from the group consisting of hydrogen, —R106—NH2, and —R107—N(H)—R108—NH2, where R106, R107, and R108 are independently selected from the group consisting of alkanediyl groups. ### Claim 9 (depends on 8) The method of claim 8, wherein the aminosilane compound is selected from the group consisting of (3-aminopropyl)trimethoxysilane, (3-aminopropyl)-methyl-dimethoxysilane, (3-aminopropyl)-dimethyl-methoxysilane, (3-aminopropyl)triethoxysilane, (3-aminopropyl)-ethyl-diethoxysilane, (3-aminopropyl)-diethyl-ethoxysilane, and mixtures thereof. ### Claim 10 (depends on 1) The method of claim 1, wherein aminosilane compound is present in the first part in an amount of about 100 ppm or more, based on the total weight of the first part. ### Claim 11 (depends on 1) The method of claim 1, wherein the hydroxide salt comprises a cation selected from the group consisting of a lithium cation, a sodium cation, a potassium cation, ammonium cations, and phosphonium cations. ### Claim 12 (depends on 11) The method of claim 11, wherein the cation is selected from the group consisting of ammonium cations and phosphonium cations. ### Claim 13 (depends on 12) The method of claim 12, wherein the hydroxide salt is selected from the group consisting of tetramethylammonium hydroxide, tetrabutylammonium hydroxide, tetrabutylphosphonium hydroxide, and mixtures thereof. ### Claim 14 (depends on 13) The method of claim 13, wherein the hydroxide salt is tetrabutylphosphonium hydroxide. ### Claim 15 (depends on 1) The method of claim 1, wherein the reaction mixture is heated to a temperature of about 120° C. or more.