IP Library Granted Patent US 7,431,903
Granted Patent B2
US 7,431,903 · App. 10/494,176 · Granted Oct 7, 2008

Tubular titanium oxide particles and process for preparing same

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Quick Facts
Patent No.
US 7,431,903
App. No.
10/494,176
Granted
Oct 7, 2008
Kind
B2
Abstract

The process for preparing tubular titanium oxide particles comprises subjecting a water dispersion sol, which is obtained by dispersing (i) titanium oxide particles and/or (ii) titanium oxide type composite oxide particles comprising titanium oxide and an oxide other than titanium oxide in water, said particles having an average particle diameter of 2 to 100 nm, to hydrothermal treatment in the presence of an alkali metal hydroxide. After the hydrothermal treatment, reduction treatment (including nitriding treatment) may be carried out. The tubular titanium oxide particles obtained in this process are useful as catalysts, catalyst carriers, adsorbents, photocatalysts, decorative materials, optical materials and photoelectric conversion materials. Especially when the particles are used for semiconductor films for photovoltaic cells or photocatalysts, prominently excellent effects are exhibited.

Claims (28)

1. A process for preparing tubular crystalline titanium oxide-containing particles, comprising:

(a) preparing titanium oxide particles from peroxotitanic acid; and

(b) subjecting a water dispersion sol, which is obtained by dispersing (i) the titanium oxide particles and/or (ii) titanium oxide type composite oxide particles comprising the titanium oxide particles and oxide particles other than titanium oxide in water, said particles having an average particle diameter of 2 to 100 nm, to hydrothermal treatment in the presence of an alkali metal hydroxide to form tubular crystalline titanium oxide-containing particles.

2. The process for preparing tubular crystalline titanium oxide-containing particles as claimed in claim 1 , wherein reduction treatment is carried out after the hydrothermal treatment.

3. The process for preparing tubular crystalline titanium oxide-containing particles as claimed in claim 2 , wherein the reduction treatment comprises nitriding treatment.

4. The process for preparing tubular crystalline titanium oxide-containing particles as claimed in claim 1 , wherein the hydrothermal treatment is carried out in the presence of aramonium hydroxide and/or an organic base together with the alkali metal hydroxide.

5. The process for preparing tubular crystalline titanium oxide-containing particles as claimed in claim 1 , wherein the oxide other than titanium oxide is an oxide of one or more elements selected from Group Ia, Group Ib, Group IIa, Group IIb, Group IIIa, Group IIIb, Group IVa, Group IVb, Group Va, Group Vb, Group VIa, Group VIb, Group VIIa and Group VIII of the periodic table.

6. The process for preparing tubular crystalline titanium oxide-containing particles as claimed in claim 5 , wherein the oxide other than titanium oxide is one or more oxides selected from SiO 2 , ZrO 2 , ZnO, Al 2 O 3 , CeO 2 , Y 2 O 3 , Nd 2 O 3 , WO 3 , Fe 2 O 3 and Sb 2 O 5 .

7. Tubular crystalline titanium oxide-containing particles obtained by the process of claim 6 and having a sodium content of not more than 0.1% by weight in terms of Na 2 O.

8. Tubular crystalline titanium oxide-containing particles obtained by the process of claim 5 and having a sodium content of not more than 0.1% by weight in terms of Na 2 O.

9. Tubular crystalline titanium oxide-containing particles obtained by the process of claim 1 and having a sodium content of not more than 0.1% by weight in terms of Na 2 O.

10. Tubular crystalline titanium oxide-containing particles obtained by the process of claim 1 and having a sodium content of not more than 0.1% by weight in terms of Na 2 O.

11. A process for preparing tubular crystalline titanium oxide-containing particles, comprising:

(a) preparing titanium oxide particles from peroxotitanic acid; and

(b) subjecting a water dispersion of the titanium oxide particles and/or titanium oxide type composite oxide particles comprising the titanium oxide particles and oxide particles other than titanium oxide, said titanium oxide particles and/or composite oxide particles having an average particle diameter of 2 to 100 nm, to hydrothermal treatment in the presence of an alkali metal hydroxide, and

then subjecting the water dispersion to reduction treatment to form tubular crystalline titanium oxide-containing particles.

12. The process for preparing tubular crystalline titanium oxide-containing particles as claimed in claim 11 , wherein the reduction treatment comprises nitriding treatment.

13. The process for preparing tubular crystalline titanium oxide-containing particles as claimed in claim 11 , wherein ammonium hydroxide and/or one or more organic bases are allowed to be present together with the alkali metal hydroxide.

14. The process for preparing tubular crystalline titanium oxide-containing particles as claimed in claim 11 , wherein the oxide other than titanium oxide is an oxide of one or more elements selected from Group Ia, Group Ib, Group IIa, Group IIb, Group IIIa, Group IIIb, Group IVa, Group IVb, Group Va, Group Vb, Group VIa, Group VIb, Group VIIa and Group VIII of the periodic table.

15. Tubular crystalline titanium oxide-containing particles obtained by the process of claim 11 and having a sodium content of not more than 0.1% by weight in terms of Na 2 O.

16. Tubular crystalline titanium oxide-containing particles represented by the following compositional formula (1):

Ti a M b O x N y   (1)

wherein a and b are numbers satisfying the conditions of a+b=1 and b=0˜0.2, x and y are numbers satisfying the conditions of 1≦x+y<2, 1≦x<2 and 0≦y<0.2, and M is an element other than Ti, and

containing crystalline titanium oxide as a main component, wherein the crystalline titanium oxide is obtained by a process of preparing titanium oxide particles from peroxotitanic acid.

17. The tubular crystalline titanium oxide-containing particles as claimed in claim 16 , having an outer diameter (D out ) of 5 to 40 nm, an inner diameter (D in ) of 4 to 20 nm, a tube thickness of 0.5 to 10 nm, a length (L) of 50 to 1000 nm and a length (L)/outer diameter (D out ) ratio (L/D out ) of 10 to 200.

18. The tubular crystalline titanium oxide-containing particles as claimed in claim 17 , wherein the element M other than titanium is one or more elements selected from Group Ia, Group Ib, Group IIa, Group IIb, group IIIa, Group IIIb, Group IVa, Group IVb, Group Va, Group Vb, Group VIa, Group VIb, Group VIIa and Group VIII of the periodic table.

19. The tubular crystalline titanium oxide-containing particles as claimed in claim 16 , wherein the element M other than titanium is one or more elements selected from Group Ia, Group Ib, Group IIa, Group IIb, Group IIIa, Group IIIb, Group IVa, Group IVb, Group Va, Group Vb, Group VIa, Group VIb, Group VIIa and Group VIII of the periodic table.

20. The tubular crystalline titanium oxide-containing particles as claimed in claim 19 , wherein the element M other than titanium is one or more elements selected from Si, Zr, Zn, Al, Ce, Y, Nd, W, Fe and Sb.

Assignments (2)
CHANGE OF NAME Recorded Feb 27, 2009
From: CATALYSTS & CHEMICALS INDUSTRIES CO., LTD.
To: JGC CATALYSTS AND CHEMICALS LTD.
Reel/Frame 022320/0084 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 29, 2004
From: KOYANAGI, TSUGUO; SHIRONO, KATSUHIRO; TANAKA, ATSUSHI; KOMATSU, MICHIO
To: CATALYSTS & CHEMICALS INDUSTRIES CO. LTD.
Reel/Frame 015656/0304 →