# US 9,040,489 B2 · Nanocrystalline photocatalytic colloid, a method of producing it and its use > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 9,040,489 B2 - Document ID: US9040489B2 - Status: Granted - Kind: B2 - Application number: 13/148,192 - Filed: 2010-02-26 - Published: 2012-03-22 - Granted: 2015-05-26 - Earliest claimed: 2009-02-26 - Assignees: Jagiellonian University - Applicants: Przemyslaw Labuz; Wojciech Macyk; Grazyna Stochel; Piotr B. Heczko; Magdalena Strus; Justyna Derdzinska - Inventors: Przemyslaw Labuz; Wojciech Macyk; Grazyna Stochel; Piotr B. Heczko; Magdalena Strus; Justyna Derdzinska - Web page: https://patentgrep.com/patent/US9040489B2 ## CPC - B01J 35/39: Photocatalytic properties - A61L 2/18: Liquid substances - A61L 12/088: {Heavy metals} - B01J 21/063: {Titanium; Oxides or hydroxides thereof} - B01J 35/393: {Metal or metal oxide crystallite size} - B01J 35/45: Nanoparticles - B01J 37/0072: {Preparation of particles, e.g. dispersion of droplets in an oil bath} - C01G 23/047: Titanium dioxide - C09C 1/3669: {Treatment with low-molecular organic compounds} - A61L 2103/15: Laboratory, medical or dentistry appliances, e.g. catheters or sharps - B01J 35/23: in a colloidal state - B01J 2235/00: Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties - B01J 2235/30: Scanning electron microscopy; Transmission electron microscopy - C01P 2002/84: by UV- or VIS- data - C01P 2004/04: obtained by TEM, STEM, STM or AFM - C01P 2006/10: Solid density - C01P 2006/60: Optical properties, e.g. expressed in CIELAB-values - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS - A61L: METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES (preservation of bodies or disinfecting characterised by the agents employed A01N; preserving, e.g. sterilising, food or foodstuffs A23; preparations for medical, dental or toiletry purposes A61K) - C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20) - C09C: TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES (treatment of materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone C04B14/00, C04B18/00, C04B20/00); PREPARATION OF CARBON BLACK {; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS} - C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS ## Abstract The present invention relates to a nanocrystalline photocatalyst active upon visible light irradiation, with a high degree of dispersion, stable in the form of a transparent colloidal solution in an aqueous environment, containing nanocrystals of titanium dioxide (TiO2) surface-modified via direct chemisorption of organic compounds. The present invention in turn relates to a method of producing the material as well as its use as a photosterilizer, photobacteriocide, photomycocide, and/or photocatalyst, in particular for the sterilization of glass surfaces, transparent plastics and transparent materials, in particular contact lenses, medical catheters, glass and plastic conduits as well as other surfaces, whose sterilization is desirable and/or required. ## Claims ### Claim 1 A nanocrystalline photocatalyst active upon visible light irradiation in the form of a transparent colloidal solution, comprising: a. a dispersed phase containing nanoparticles of titanium dioxide TiO2 of a size less than 100 nm and surface-modified with an organic compound selected from the group consisting of: disodium salt of 4,5-dihydroxy-1,3-benzenedisulfonic acid, rutin and ascorbic acid, and b. a liquid dispersing medium, wherein the colloidal solution has a pH of about 7. ### Claim 2 (depends on 1) The nanocrystalline photocatalyst of claim 1, wherein the liquid dispersing medium is an aqueous solution. ### Claim 3 (depends on 1) The nanocrystalline photocatalyst of claim 1, wherein the nanoparticles of titanium dioxide are additionally conjugated with a molecule. ### Claim 4 (depends on 3) The nanocrystalline photocatalyst of claim 3, wherein the molecule is an antibody, peptide, biotin, or a vitamin. ### Claim 5 A nanocrystalline photocatalyst active upon visible light irradiation in the form of a transparent colloidal solution, comprising: a. a dispersed phase containing nanoparticles of titanium dioxide TiO2 of a size less than 100 nm and surface-modified with rutin, and b. a liquid dispersing medium, wherein said nanocrystalline photocatalyst exhibits stability in aqueous solutions at pH of about 7. ### Claim 6 (depends on 5) The nanocrystalline photocatalyst of claim 5, wherein the liquid dispersing medium is an aqueous solution. ### Claim 7 (depends on 5) The nanocrystalline photocatalyst of claim 5, wherein the nanoparticles of titanium dioxide are additionally conjugated with a molecule. ### Claim 8 (depends on 7) The nanocrystalline photocatalyst of claim 7, wherein the molecule is an antibody, peptide, biotin, or a vitamin. ### Claim 9 A method of producing a nanocrystalline photocatalyst active upon visible light irradiation in the form of a transparent colloidal solution, comprising: a. supplementing into a colloidal aqueous solution of TiO2 with an organic compound to form a sol, wherein the organic compound undergoes chemisorption on the surface of TiO2 and is selected from the group consisting of: disodium salt of 4,5-dihydroxy-1,3-benzenedisulfonic acid, rutin and ascorbic acid, b. bringing the pH of the resulting sol of step a) to about 7 and performing dialysis on the resulting sol against an aqueous solution to form a stable suspension of nanoparticles of titanium dioxide TiO2 of a size less than 100 nm. ### Claim 10 (depends on 9) The method of claim 9, wherein the chemisorption is performed in an acidic environment. ### Claim 11 (depends on 10) The method of claim 10, wherein the chemisorption is performed at pH of about 2.5. ### Claim 12 (depends on 10) The method of claim 10, wherein the chemisorption is performed in the presence of nitric acid. ### Claim 13 (depends on 10) The method of claim 10, wherein after the chemisorption is complete, the resulting colloidal solution is brought to pH of about 7 using an aqueous solution of a base. ### Claim 14 (depends on 9) The method of claim 9, wherein the chemisorption is performed in the presence of an alcohol. ### Claim 15 (depends on 14) The method of claim 14, wherein the alcohol is isopropanol. ### Claim 16 (depends on 9) The method of claim 9, wherein a colloidal solution of TiO2 is supplemented with the organic compound at a molar ratio of 1:1. ### Claim 17 (depends on 1) A method of producing a layer on a solid substrate, comprising coating the solid substrate with the nanocrystalline photocatalyst of claim 1. ### Claim 18 (depends on 17) The method of claim 17, wherein the solid substrate is glass, metal, plastics or paper. ### Claim 19 (depends on 1) A preparation comprising: the nanocrystalline photocatalyst of claim 1. ### Claim 20 (depends on 19) The preparation of claim 19, wherein the preparation is a photosterilizing, photobacteriocidal, photomycocidal, or photocatalytic preparation. ### Claim 21 (depends on 10) A method, comprising: applying the preparation of claim 10 on surfaces of glass and plastic elements. ### Claim 22 (depends on 21) The method of claim 21, wherein the preparation is applied on a contact lens, a medical catheter, or a glass or plastic conduit.