# US 11,897,771 B2 · Method of graphene exfoliation and/or stabilization and composition prepared therefrom > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 11,897,771 B2 - Document ID: US11897771B2 - Status: Granted - Kind: B2 - Application number: 17/741,696 - Filed: 2022-05-11 - Published: 2022-08-25 - Granted: 2024-02-13 - Earliest claimed: 2020-12-01 - Assignees: Turtle Wax, Inc. - Applicants: Turtle Wax, Inc. - Inventors: Michael A. Schultz - Web page: https://patentgrep.com/patent/US11897771B2 ## CPC - C01B 32/19: by exfoliation - C09G 1/06: Other polishing compositions - C01B 32/194: After-treatment - B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites - B82Y 40/00: Manufacture or treatment of nanostructures - C01B 2204/04: Specific amount of layers or specific thickness - C01B 2204/32: Size or surface area - C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer - C01P 2006/12: Surface area - C09D 5/00: Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced {(electrically insulating plastics, resins or waxes H01B3/30)}; Filling pastes - C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C} - C09G: POLISHING COMPOSITIONS (French polish C09F11/00); SKI WAXES - B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES - C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS - 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) ## Abstract The present disclosure provides a method of graphene exfoliation and/or stabilization. Both graphene and silica are mixed in an organic solvent to form a liquid precursor, which is then directed through an orifice formed by a metal cylinder and a flat metal plate. The metal cylinder is pressed against the flat metal plate by a high pressure. The high shear between the metal cylinder and the flat metal plate breaks down the thick layers of graphene to thin layers, which are stably dispersed in the gel formed by the silica. ## Claims ### Claim 1 A composition comprising graphene dispersed in a gel formed by silica, the composition prepared by a method comprising: providing a liquid precursor comprising both the graphene and the silica mixed in an organic solvent; and directing the liquid precursor through an orifice comprising a metal cylinder and a flat metal plate, wherein the metal cylinder is pressed against the flat metal plate, and the liquid precursor is directed through an opening on the flat metal plate to a position between the metal cylinder and the flat metal plate, wherein the composition has a viscosity of about 200,000 to about 600,000 centistokes. ### Claim 2 (depends on 1) The composition of claim 1, wherein at least 90% of the graphene has up to 10 layers. ### Claim 3 (depends on 1) The composition of claim 1, wherein the metal cylinder is pressed against the flat metal plate by a pressure of about 1500-6000 psi. ### Claim 4 (depends on 1) The composition of claim 1, wherein the liquid precursor is directed through the orifice by a pump. ### Claim 5 (depends on 1) The composition of claim 1, wherein the silica comprises fumed silica. ### Claim 6 (depends on 1) The composition of claim 1, wherein the organic solvent comprises a nonpolar petroleum distillate selected from the group consisting of light petroleum distillates (LPD) of C4-C9; medium petroleum distillates (MPD) of Cs-Cn, heavy petroleum distillates (HPD) of Cs-Cn, and mixtures thereof. ### Claim 7 (depends on 1) The composition of claim 1, wherein the organic solvent comprises a nonpolar organic oil with a carbon chain length of about 20 to about 50. ### Claim 8 (depends on 1) The composition of claim 1, wherein the gel formed by the silica comprises a three-dimensional structure. ### Claim 9 (depends on 1) The composition of claim 1, wherein the liquid precursor comprises the graphene with a first number of layers, and the composition comprises the graphene with a second number of layers, and the second number is less than the first number. ### Claim 10 (depends on 9) The composition of claim 9, wherein the first number is greater than 10, and the second number is 10 or less. ### Claim 11 (depends on 1) The composition of claim 1, wherein the liquid precursor comprises about 0.1 wt % to 20 wt % of the silica. ### Claim 12 (depends on 1) The composition of claim 1, wherein the liquid precursor comprises about 0.05 wt % to about 50 wt % of the graphene. ### Claim 13 (depends on 1) The composition of claim 1, wherein the graphene in the liquid precursor comprises graphene particles having an average thickness of about 6-8 nm and a typical surface area of about 120 to 150 m2/g. ### Claim 14 (depends on 1) The composition of claim 1, wherein the graphene in the liquid precursor comprises particles having an average particle diameter of about 5-25 microns. ### Claim 15 An automotive wax composition comprising a composition comprising graphene dispersed in a gel formed by silica, the composition prepared by a method comprising: providing a liquid precursor comprising both the graphene and the silica mixed in an organic solvent; and directing the liquid precursor through an orifice comprising a metal cylinder and a flat metal plate, wherein the metal cylinder is pressed against the flat metal plate, and the liquid precursor is directed through an opening on the flat metal plate to a position between the metal cylinder and the flat metal plate. ### Claim 16 (depends on 15) The automotive wax composition of claim 15 comprising at least one of anionic surfactants, cationic surfactants, non-ionic surfactants, amphoteric surfactants, non-10 mc emulsifiers, UV absorbers, mineral oil, butyl cellosolve, fragrances, colorants, preservatives, thickening agents, abrasive polishing agents, neutralizing agents, or stabilizing agents.