# US 11,896,956 B2 · Process for producing composite material > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 11,896,956 B2 - Document ID: US11896956B2 - Status: Granted - Kind: B2 - Application number: 16/966,144 - Filed: 2019-01-30 - Published: 2022-06-09 - Granted: 2024-02-13 - Earliest claimed: 2018-01-30 - Assignees: Anaphite Limited - Applicants: Anaphite Limited - Inventors: Samuel Burrow; Alexander Hewitt; Elena Mogort-Valls - Web page: https://patentgrep.com/patent/US11896956B2 ## CPC - B01J 21/063: {Titanium; Oxides or hydroxides thereof} - B01J 21/18: Carbon - B01J 31/06: containing polymers {(organometallic polymers B01J31/123; polymer-bound organometallic complexes B01J31/165; coordination polymers B01J31/1691)} - B01J 35/39: Photocatalytic properties - B01J 35/40: characterised by dimensions, e.g. grain size (in a colloidal state B01J35/23; crystallite size B01J35/77) - B01J 35/45: Nanoparticles - B01J 37/0072: {Preparation of particles, e.g. dispersion of droplets in an oil bath} - B01J 37/009: {Preparation by separation, e.g. by filtration, decantation, screening} - B01J 37/031: {Precipitation} - B01J 37/035: {Precipitation on carriers} - B01J 37/04: Mixing {(B01J37/0009, B01J37/0018 take precedence)} - B01J 37/06: Washing {(B01J37/0009, B01J37/0018 take precedence)} - C01B 32/19: by exfoliation - C01B 32/192: starting from graphitic oxides - C01B 32/194: After-treatment - C01B 32/225: Expansion; Exfoliation - C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram - C01P 2002/82: by IR- or Raman-data - C01P 2002/84: by UV- or VIS- data - C01P 2002/85: by XPS, EDX or EDAX data - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS - C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C} - C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS ## Abstract A process is disclosed comprising, providing a source of graphene, providing a particulate material, dispersing a mixture of the source of graphene and the particulate material in a first dispersion fluid to form a dispersion mixture, and providing a source of a base in the first dispersion fluid, thereby causing the source of graphene and particulate material in the dispersion mixture to interact forming a composite. The particulate material is preferably titanium dioxide comprising anatase and/or rutile which provides an effective photocatalytic composite. Also disclosed is apparatus to remove pollutants from fluids using the photocatalytically active material. ## Claims ### Claim 1 A process for producing a composite, the process comprising: a) providing a first dispersion fluid comprising a source of graphene selected from graphene and partially oxidised graphene, wherein the partially oxidized graphene includes oxygen in an amount of up to 10% by weight; b) providing a particulate material, which is a polymeric material selected from meta-aramid, para-aramid, polycarbonate, poly(methyl methacrylate) (PMMA), nylon, polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), polyaryletherketone, polypropylene carbonate, polyester, polylactic acid, polyurethane, polyvinyl alcohol, polyvinyl acetate and polyvinyl ester; c) dispersing the particulate material in the first dispersion fluid comprising the graphene or the partially oxidised graphene, to form a dispersion mixture, and d) providing a base in the dispersion mixture, thereby causing the graphene and the particulate material in the dispersion mixture to interact forming the composite. ### Claim 2 (depends on 1) The process according to claim 1, wherein the source of graphene is graphene. ### Claim 3 (depends on 1) The process as claimed in claim 1, wherein the particulate material comprises a polymeric material selected from one or more of PMMA, PTFE, PVDF, polyaryletherketone, polypropylene carbonate, polyester, polylactic acid, polyurethane, polyvinyl alcohol, polyvinyl acetate and polyvinyl ester. ### Claim 4 (depends on 1) The process as claimed in claim 1, wherein the process is performed in the absence of a surfactant. ### Claim 5 (depends on 1) The process as claimed in claim 1, further comprising homogenising the dispersion mixture. ### Claim 6 (depends on 1) The process as claimed in claim 1, further comprising homogenising the source of graphene in a graphene dispersion fluid. ### Claim 7 (depends on 1) The process as claimed in claim 1, further comprising homogenising the particulate material in a material dispersion fluid. ### Claim 8 (depends on 1) The process as claimed in claim 1, further comprising sonicating the dispersion mixture. ### Claim 9 (depends on 1) The process as claimed in claim 1, further comprising sonicating the source of graphene in a graphene dispersion fluid. ### Claim 10 (depends on 1) The process as claimed in claim 1, further comprising sonicating the particulate material in a material dispersion fluid. ### Claim 11 (depends on 1) The process as claimed in claim 1, wherein the graphene and the particulate material are mixed in a ratio of 3 to 500 parts by weight of the particulate material to 1 part by weight of the source of graphene. ### Claim 12 (depends on 1) The process as claimed in claim 1, wherein the composite has an I(D)/I(G) ratio at a laser excitation of 532 nm wavelength and 2.33 eV, of less than 0.75. ### Claim 13 (depends on 1) The process as claimed in claim 1, wherein the base comprises a source of a Brønsted base and/or a source of a Lewis base. ### Claim 14 (depends on 13) The process as claimed in claim 13, wherein the base comprises a source of hydroxide ions. ### Claim 15 (depends on 14) The process as claimed in claim 14, wherein the source of hydroxide ions comprises an ion exchange resin, ammonia solution or an alkali solution. ### Claim 16 (depends on 13) The process as claimed in claim 13, wherein the base comprises a ketone. ### Claim 17 (depends on 16) The process as claimed in claim 16, wherein the first dispersion fluid comprises acetone. ### Claim 18 (depends on 17) The process as claimed in claim 17, wherein the first dispersion fluid comprises a mixture of acetone and water with a weight ratio of acetone to water of 0.5:1 to 6:1. ### Claim 19 (depends on 1) The process as claimed in claim 1, further comprising providing a surfactant in the first dispersion fluid. ### Claim 20 (depends on 1) The process as claimed in claim 1, wherein the first dispersion fluid comprises one or more of dimethylsulfoxide, acetone, water, tetrahydrofuran, Chloroform, N-methyl-2-pyrrolidone, dimethylformamide, dimethylacetamide, gamma-butyrolactone, 1,3-dimethyl-2-imidazolidinone, benzyl benzoate, N-vinylpyrrolidone, N-dodecyl-2-pyrrolidone, n-propanol, isopropanol, and N-octyl-2-pyrrolidone. ### Claim 21 (depends on 1) The process as claimed in claim 1, wherein the source of graphene comprises graphene flakes. ### Claim 22 (depends on 21) The process as claimed in claim 21, wherein the source of graphene comprises graphite flakes and the process further comprises providing a graphite dispersion of graphite flakes in a graphene dispersion fluid and homogenising the graphite dispersion, thereby forming a dispersion comprising graphene. ### Claim 23 (depends on 1) The process as claimed in claim 1, wherein the particulate material has a particle size in a range 5 nm to 1 μm. ### Claim 24 (depends on 1) The process as claimed in claim 1, further comprising recovering the composite, and optionally recovering the first dispersion fluid. ### Claim 25 (depends on 1) The process as claimed in claim 1, wherein the process is conducted at a temperature in a range of from 0° C. to 260° C.