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WO2009082989A1 - Method for production of photocatalytically active titanium oxide for uv and visible region o light spectrum - Google Patents

Method for production of photocatalytically active titanium oxide for uv and visible region o light spectrum Download PDF

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Publication number
WO2009082989A1
WO2009082989A1 PCT/CZ2008/000150 CZ2008000150W WO2009082989A1 WO 2009082989 A1 WO2009082989 A1 WO 2009082989A1 CZ 2008000150 W CZ2008000150 W CZ 2008000150W WO 2009082989 A1 WO2009082989 A1 WO 2009082989A1
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WO
WIPO (PCT)
Prior art keywords
titanium oxide
production
visible region
photocatalytically active
production according
Prior art date
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Ceased
Application number
PCT/CZ2008/000150
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French (fr)
Inventor
Vaclav Stengl
Zbynek Cerny
Jana Bludska
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Institute of Inorganic Chemistry CAS
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Institute of Inorganic Chemistry CAS
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Filing date
Publication date
Application filed by Institute of Inorganic Chemistry CAS filed Critical Institute of Inorganic Chemistry CAS
Publication of WO2009082989A1 publication Critical patent/WO2009082989A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/20—Vanadium, niobium or tantalum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/031—Precipitation
    • B01J37/033—Using Hydrolysis
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • C01P2002/54—Solid solutions containing elements as dopants one element only

Definitions

  • the patent regards the method for production of photocatalytically active titanium oxide for the UV and visible region of light spectrum.
  • titanium oxide At the moment, the most common photocatalyzer is titanium oxide. After UV radiation illumination, a hole-electron pair originates on the surface and the consequence of this excitation is the origination of highly reactive OH radicals, which are able to break down organic compounds into the final products of mineralization - water and carbon dioxide.
  • Commercially available titanium oxide for photocatalysis is currently produced by hydrolysis of TiCl 4 . This process is very demanding in terms of cost and technical process. For applications of photocatalysis, cheap forms of titanium oxide have to be found, which, by means of dopants, increase photo-activity in the UV region or move photo-activity in the visible region of the light spectrum.
  • the aim of this patent is a simple method for production of price-available photocatalytically active titanium oxide; the principle of this method for production is that, in a water environment, titanyl sulphate (TiOSO 4 ) is hydrolyzed by thioacetamide or urea at a temperature of 40 - 100 °C and the acquired product dries at temperatures up to 120 °C. The dried product is further annealed at temperatures up to 1000 °C in oxygen atmosphere or air. Titanyl sulphate can be also hydrolyzed by hexamethyltetr amine.
  • TiOSO 4 titanyl oxide
  • a 5-liter beaker with 3 liters of distilled water acidified with concentrated sulphuric acid.
  • the solution was diluted to a total volume of 4 liters and 100 g of thioacetamide was added.
  • the solution was boiled under continuous stirring and maintained at this temperature for 6 hours.
  • the product was decanted by water, filtered and dried at 120 °C.
  • the acquired product was annealed in a furnace in an oxygen atmosphere at 700 °C.
  • the acquired product is a white, very fine, loose powder; according to X- ray powder diffraction, it is anatase modification of titanium oxide, active in the UV region.
  • TiOSO 4 titanyl oxide
  • the acquired product was annealed in a furnace in an oxygen atmosphere at 500 0 C.
  • the acquired product is a white, very fine, loose powder; according to X-ray powder diffraction, it is anatase modification of titanium oxide doped with zinc oxide. Zinc oxide doping increases photo-activity in the UV region.
  • TiOSO 4 titanyl oxide
  • Ce 2 (SO 4 ) 3 cerium sulphate
  • the solution was diluted to a total volume of 4 liters and 100 g of thioacetamide was added.
  • the solution was boiled under continuous stirring and maintained at this temperature for 3 hours.
  • the acquired product was annealed in a furnace in an oxygen atmosphere at 500 °C.
  • the acquired product is a white, very fine, loose powder; according to X-ray powder diffraction, it is anatase modification of titanium oxide doped with cerium oxide. Cerium oxide doping moves the photo-activity to the visible region.
  • TiOSO 4 titanyl oxide
  • neodymium oxide neodymium oxide was dissolved in a 5-liter beaker with 3 liters of distilled water acidified with concentrated sulphuric acid.
  • 1 g of neodymium oxide was dissolved in a minimum quantity of diluted hydrochloric acid (1 :1) and added to the reaction solution.
  • the solution was diluted to a total volume of 4 liters and 100 g of thioacetamide was added.
  • the solution was boiled under continuous stirring and maintained at this temperature for 3 hours.
  • the product was decanted by water, filtered and dried at 120 °C.
  • the acquired product was annealed in a furnace in an oxygen atmosphere at 500 0 C.
  • the acquired product is a white, very fine, loose powder; according to X-ray powder diffraction, it is anatase modification of titanium oxide doped with neodymium oxide. Neodymium oxide doping moves the photo-activity to the visible region.
  • the method for production of photocatalytically active titanium oxide can be used for the production of pigments used in self-cleansing paints or as a refill for AC units for air-cleansing or for volume-cleansing of water.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The method for production of photocatalytically active titanium oxide consisting in hydrolyses of titanyl sulphate by thioacetamide, urea or hydroxymethylamine in a water environment at temperatures of 40 - 100°C and drying of the acquired product at temperatures up to 120°C; the dried product is annealed up to a temperature of l,000°C in an oxygen atmosphere. During hydrolysis, dopants with soluble salts of components selected from groups Sc, Zn, Y, Zr, Nb, Cd, Al, Ta and lanthanides can be used.

Description

Method for production of photocatalytically active titanium oxide for UV and visible region of light spectrum
Technical field
The patent regards the method for production of photocatalytically active titanium oxide for the UV and visible region of light spectrum.
Background art
At the moment, the most common photocatalyzer is titanium oxide. After UV radiation illumination, a hole-electron pair originates on the surface and the consequence of this excitation is the origination of highly reactive OH radicals, which are able to break down organic compounds into the final products of mineralization - water and carbon dioxide. Commercially available titanium oxide for photocatalysis is currently produced by hydrolysis of TiCl4. This process is very demanding in terms of cost and technical process. For applications of photocatalysis, cheap forms of titanium oxide have to be found, which, by means of dopants, increase photo-activity in the UV region or move photo-activity in the visible region of the light spectrum.
Disclosure of the invention
The aim of this patent is a simple method for production of price-available photocatalytically active titanium oxide; the principle of this method for production is that, in a water environment, titanyl sulphate (TiOSO4) is hydrolyzed by thioacetamide or urea at a temperature of 40 - 100 °C and the acquired product dries at temperatures up to 120 °C. The dried product is further annealed at temperatures up to 1000 °C in oxygen atmosphere or air. Titanyl sulphate can be also hydrolyzed by hexamethyltetr amine.
The method with use of dopants during hydrolysis can be used. As dopants, soluble salts of scandium, zinc, yttrium, zirconium, niobium, tantalum, cadmium, aluminum or lanthanides can be used. Examples
The patent is further explained by means of examples for its realization.
Example 1
100 g of titanyl oxide (TiOSO4) was dissolved in a 5-liter beaker with 3 liters of distilled water acidified with concentrated sulphuric acid. The solution was diluted to a total volume of 4 liters and 100 g of thioacetamide was added. The solution was boiled under continuous stirring and maintained at this temperature for 6 hours. Afterward, the product was decanted by water, filtered and dried at 120 °C. The acquired product was annealed in a furnace in an oxygen atmosphere at 700 °C. The acquired product is a white, very fine, loose powder; according to X- ray powder diffraction, it is anatase modification of titanium oxide, active in the UV region.
Example 2
100 g of titanyl oxide (TiOSO4) was dissolved in a 5-liter beaker with 3 liters of distilled water acidified with concentrated sulphuric acid. The solution was diluted to a total volume of 4 liters and 100 g of thioacetamide was added. The solution was boiled under continuous stirring and maintained at this temperature for 3 hours. Furthermore, 200 g of urea was added to the reaction mixture and the reaction solution was maintained at boiling temperature until a weak alkaline reaction (pH = 7 - 7.5). Afterward, the product was decanted by water, filtered and dried at 120 °C. The acquired product was annealed in a furnace in an oxygen atmosphere at 600 °C. The acquired product is a white, very fine, loose powder; according to X-ray powder diffraction, it is anatase modification of titanium oxide, active in the UV region.
Example 3
100 g of titanyl oxide (TiOSO4) and 20 g of zinc sulphate (ZnSO4) were dissolved in a 5- liter beaker with 3 liters of distilled water acidified with concentrated sulphuric acid. The solution was diluted to a total volume of 4 liters and 100 g of thioacetamide was added. The solution was boiled under continuous stirring and maintained at this temperature for 3 hours. Furthermore, 200 g of urea was added to the reaction mixture and the reaction solution was maintained at boiling temperature until weak alkaline reaction (pH = 7 - 7.5). Afterward, the product was decanted by water, filtered and dried at 120 0C. The acquired product was annealed in a furnace in an oxygen atmosphere at 500 0C. The acquired product is a white, very fine, loose powder; according to X-ray powder diffraction, it is anatase modification of titanium oxide doped with zinc oxide. Zinc oxide doping increases photo-activity in the UV region.
Example 4
100 g of titanyl oxide (TiOSO4) and 1 g of cerium sulphate (Ce2(SO4)3. were dissolved in a 5 -liter beaker with 3 liters of distilled water acidified with concentrated sulphuric acid. The solution was diluted to a total volume of 4 liters and 100 g of thioacetamide was added. The solution was boiled under continuous stirring and maintained at this temperature for 3 hours. Furthermore, 200 g of urea was added to the reaction mixture and the reaction solution was maintained at boiling temperature until weak alkaline reaction (pH = 7 - 7.5). Afterward, the product was decanted by water, filtered and dried at 120 °C. The acquired product was annealed in a furnace in an oxygen atmosphere at 500 °C. The acquired product is a white, very fine, loose powder; according to X-ray powder diffraction, it is anatase modification of titanium oxide doped with cerium oxide. Cerium oxide doping moves the photo-activity to the visible region.
Example 5
100 g of titanyl oxide (TiOSO4) and 1 g of neodymium oxide was dissolved in a 5-liter beaker with 3 liters of distilled water acidified with concentrated sulphuric acid. 1 g of neodymium oxide was dissolved in a minimum quantity of diluted hydrochloric acid (1 :1) and added to the reaction solution. The solution was diluted to a total volume of 4 liters and 100 g of thioacetamide was added. The solution was boiled under continuous stirring and maintained at this temperature for 3 hours. Furthermore, 200 g of urea was added to the reaction mixture and the reaction solution was maintained at boiling temperature until weak alkaline reaction (pH = 7 - 7.5). Afterward, the product was decanted by water, filtered and dried at 120 °C. The acquired product was annealed in a furnace in an oxygen atmosphere at 500 0C. The acquired product is a white, very fine, loose powder; according to X-ray powder diffraction, it is anatase modification of titanium oxide doped with neodymium oxide. Neodymium oxide doping moves the photo-activity to the visible region. Industrial applicability
The method for production of photocatalytically active titanium oxide, according to the patent, can be used for the production of pigments used in self-cleansing paints or as a refill for AC units for air-cleansing or for volume-cleansing of water.

Claims

C L A I M S
1. The method for production of photocatalytically active titanium oxide for the UV and the visible region of the light spectrum characte rize d in that titanyl sulphate (TiOSO4) is hydrolyzed in a water environment at a temperature of 40 - 100 0C and the acquired product is dried at temperatures up to 120 0C.
2. The method for production according to claim 1 characterize d in that titanyl sulphate is hydrolyzed by thioacetamide.
3. The method for production according to claim 1 characterized i n that titanyl sulphate is hydrolyzed by urea.
4. The method for production according to claim 1 characteri zed in that titanyl sulphate is hydrolyzed by hexamethyltetramine.
5. The method for production according to claims 2, 3 or 4 characterize d in that soluble salts of components from groups Sc, Zn, Y, Zr, Nb, Cd, Al, Ta and lanthanides are added during hydrolysis.
6. The method for production according to claims 2, 3, 4 or 5 characterized in that the dried product is annealed up to a temperature of 1000 °C in air or an oxygen atmosphere.
PCT/CZ2008/000150 2008-01-03 2008-12-15 Method for production of photocatalytically active titanium oxide for uv and visible region o light spectrum Ceased WO2009082989A1 (en)

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CZPV2008-4 2008-01-03
CZ20080004A CZ301406B6 (en) 2008-01-03 2008-01-03 Process for preparing photocatalytic active titanium dioxide for visible light spectrum range

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101984501A (en) * 2010-09-27 2011-03-09 彩虹集团公司 Preparation method of titanium dioxide composite sizing agent used by dye sensitized solar cell
RU2509727C2 (en) * 2011-12-30 2014-03-20 Учреждение Российской академии наук Институт химии твердого тела Уральского отделения РАН Method of producing nanopowder zirconium, yttrium and titanium composite oxide
CN108187651A (en) * 2017-12-28 2018-06-22 山东纳安环保科技有限公司 A kind of preparation method and application for carrying zinc nano-titanium dioxide
CN113042028A (en) * 2021-03-26 2021-06-29 福州大学 Preparation method of immobilized Y and Yb double-doped titanium dioxide porous film
US11753309B2 (en) 2018-08-30 2023-09-12 Tayca Corporation Titanyl sulfate hydrate powder, method for producing titanyl sulfate hydrate powder, method for producing aqueous titanyl sulfate solution, method of producing electrolyte solution, and method for producing redox flow battery

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EP1443023A1 (en) * 2003-01-31 2004-08-04 Sumitomo Chemical Company, Limited A method for producing titanium oxide

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JPH06293519A (en) * 1992-07-28 1994-10-21 Ishihara Sangyo Kaisha Ltd Production of titanium oxide particles and film
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EP1443023A1 (en) * 2003-01-31 2004-08-04 Sumitomo Chemical Company, Limited A method for producing titanium oxide

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101984501A (en) * 2010-09-27 2011-03-09 彩虹集团公司 Preparation method of titanium dioxide composite sizing agent used by dye sensitized solar cell
RU2509727C2 (en) * 2011-12-30 2014-03-20 Учреждение Российской академии наук Институт химии твердого тела Уральского отделения РАН Method of producing nanopowder zirconium, yttrium and titanium composite oxide
CN108187651A (en) * 2017-12-28 2018-06-22 山东纳安环保科技有限公司 A kind of preparation method and application for carrying zinc nano-titanium dioxide
US11753309B2 (en) 2018-08-30 2023-09-12 Tayca Corporation Titanyl sulfate hydrate powder, method for producing titanyl sulfate hydrate powder, method for producing aqueous titanyl sulfate solution, method of producing electrolyte solution, and method for producing redox flow battery
CN113042028A (en) * 2021-03-26 2021-06-29 福州大学 Preparation method of immobilized Y and Yb double-doped titanium dioxide porous film

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Publication number Publication date
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CZ20084A3 (en) 2009-07-15

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