# US 8,541,337 B2 · Quaternary oxides and catalysts containing quaternary oxides

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- Number: US 8,541,337 B2
- Document ID: US8541337B2
- Status: Granted
- Kind: B2
- Application number: 12/978,255
- Filed: 2010-12-23
- Published: 2011-04-21
- Granted: 2013-09-24
- Earliest claimed: 2005-12-29
- Assignees: The Board of Trustees of the University of Illinois
- Applicants: Rong-Cai Xie; Jian-Ku Shang; Pinggui Wu
- Inventors: Rong-Cai Xie; Jian-Ku Shang; Pinggui Wu
- Web page: https://patentgrep.com/patent/US8541337B2

## CPC

- C01B 3/042: Decomposition of water (by electrolysis of water C25B1/04)
- A61L 2/084: Visible light
- A61L 9/205: {using a photocatalyst or photosensitiser}
- B01J 23/02: of the alkali- or alkaline earth metals or beryllium
- B01J 23/10: of rare earths
- B01J 23/44: Palladium
- B01J 23/50: Silver
- B01J 23/70: of the iron group metals or copper
- B01J 23/72: Copper
- B01J 27/24: Nitrogen compounds
- B01J 35/39: Photocatalytic properties
- B01J 37/0215: {Coating}
- B01J 37/0225: {of metal substrates}
- B01J 37/033: {Using Hydrolysis}
- B01J 37/10: in the presence of water, e.g. steam
- C01G 23/047: Titanium dioxide
- C01G 23/053: Producing by wet processes, e.g. hydrolysing titanium salts
- C03C 17/225: {Nitrides}
- C03C 17/256: {Coating containing TiO2}
- B01J 21/06: Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J 21/063: {Titanium; Oxides or hydroxides thereof}
- C01P 2002/52: containing elements as dopants
- C01P 2006/40: Electric properties
- C02F 2305/10: Photocatalysts
- C03C 2217/212: TiO2
- C03C 2217/24: Doped oxides
- C03C 2217/71: Photocatalytic coatings
- C03C 2218/116: by spin-coating, centrifugation
- Y02E 60/36: Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- 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)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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)
- C03C: CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C02F: TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE (separation in general B01D; special arrangements on waterborne vessels of installations for treating water, waste water or sewage, e.g. for producing fresh water, B63J; adding materials to water to prevent corrosion C23F; treating radioactively-contaminated liquids G21F9/04; regeneration of reactants for recirculation into processes, see the relevant places for the processes)
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

A quaternary oxide includes a dopant metal, a dopant nonmetal, titanium, and oxygen. The atomic ratio of titanium, oxygen and dopant nonmetal may be 1:0.5-1.99:0.01-1.5. Quaternary oxides may be used in catalytic compositions, in coatings for disinfecting surfaces and in coatings for self-cleaning surfaces. A method of making a quaternary oxide includes combining ingredients including a titanium source, a dopant nonmetal source, a dopant metal salt, and a polar organic solvent to form a reaction mixture; and heating the reaction mixture.

## Claims

### Claim 1

A method of making a catalytic composition, comprising:
combining ingredients to form a reaction mixture, the ingredients comprising a titanium source, a dopant nonmetal source comprising at least one nonmetal selected from the group consisting of boron, nitrogen, sulfur and fluorine, a metal salt different from the dopant nonmetal source and not including titanium, and a polar organic solvent; and
heating the reaction mixture to form a catalytic composition comprising titanium, the metal other than titanium, the dopant nonmetal, and oxygen.

### Claim 2 (depends on 1)

The method of claim 1, where the titanium source is selected from the group consisting of titanium(IV) halide, titanium(IV) alkoxide, titanium(IV) nitrate, and titanium(IV) oxysulfate.

### Claim 3 (depends on 1)

The method of claim 1, where the metal salt comprises an ion of a metal selected from the group consisting of calcium, cobalt, nickel, copper, gallium, strontium, yttrium, zirconium, palladium, silver, tin, lanthanum and platinum.

### Claim 4 (depends on 1)

The method of claim 1, where the heating comprises maintaining the reaction mixture at a temperature of from 50° C. to 250° C. for a period of at least 4 hours.

### Claim 5 (depends on 4)

The method of claim 4, where the combining comprises mixing the titanium source and the dopant nonmetal source with the polar organic solvent to form a first mixture, and adding the metal salt to the first mixture.

### Claim 6 (depends on 5)

The method of claim 5, further comprising adding water to the first mixture.

### Claim 7 (depends on 4)

The method of claim 4, further comprising removing a precipitate from the reaction mixture after the heating.

### Claim 8 (depends on 7)

The method of claim 7, further comprising calcining the precipitate.

### Claim 9 (depends on 1)

The method of claim 1, where the heating comprises maintaining the reaction mixture at a temperature of from 100° C. to 350° C. for a period of at least 4 hours.

### Claim 10 (depends on 9)

The method of claim 9, where the heating is performed in an autoclave.

### Claim 11 (depends on 9)

The method of claim 9, where the combining comprises:
mixing the polar organic solvent with the dopant nonmetal source to form a first mixture;
adding the titanium source to the first mixture to form a second mixture; and
adding the metal salt to the second mixture.

### Claim 12 (depends on 11)

The method of claim 11, further comprising adding water to the second mixture.

### Claim 13 (depends on 9)

The method of claim 9, further comprising removing a precipitate from the reaction mixture after the heating.

### Claim 14

A method of making a catalytic composition, the method comprising:
combining a titanium source and a dopant nonmetal source comprising at least one nonmetal selected from the group consisting of boron, nitrogen, sulfur and fluorine with a polar organic solvent to form a first mixture;
adding a metal salt different from the dopant nonmetal source and not including titanium to the first mixture to form a reaction mixture;
heating the reaction mixture at a temperature of from 50° C. to 250° C. for a period of at least 4 hours;
removing a precipitate from the reaction mixture; and
calcining the precipitate, thereby forming a catalytic composition comprising titanium, the metal other than titanium, the dopant nonmetal, and oxygen.

### Claim 15 (depends on 14)

The method of claim 14, further comprising adding water to the first mixture.

### Claim 16 (depends on 14)

The method of claim 14, where
the titanium source is selected from the group consisting of titanium(IV) halide, titanium(IV) alkoxide, titanium(IV) nitrate, and titanium(IV) oxysulfate; and
the metal salt comprises an ion of a metal selected from the group consisting of calcium, cobalt, nickel, copper, gallium, strontium, yttrium, zirconium, palladium, silver, tin, lanthanum and platinum.

### Claim 17

A method of making a catalytic composition, comprising:
combining a polar organic solvent with a dopant nonmetal source comprising at least one nonmetal selected from the group consisting of boron, nitrogen, sulfur and fluorine to form a first mixture;
adding a titanium source to the first mixture to form a second mixture;
adding a metal salt different from the dopant nonmetal source and not including titanium to the second mixture to form a reaction mixture; and
heating the reaction mixture in an autoclave at a temperature of from 100° C. to 350° C. for a period of at least 4 hours to form a catalytic composition comprising titanium, the metal other than titanium, the dopant nonmetal, and oxygen.

### Claim 18 (depends on 17)

The method of claim 17, further comprising adding water to the second mixture.

### Claim 19 (depends on 17)

The method of claim 17, where
the titanium source is selected from the group consisting of titanium(IV) halide, titanium(IV) alkoxide, titanium(IV) nitrate, and titanium(IV) oxysulfate; and
the metal salt comprises an ion of a metal selected from the group consisting of calcium, cobalt, nickel, copper, gallium, strontium, yttrium, zirconium, palladium, silver, tin, lanthanum and platinum.