Doped, pyrogenically prepared oxides

• US 6,613,300 B2
• Filed: 08/09/2001
• Issued: 09/02/2003
• Est. Priority Date: 12/05/1996
• Status: Expired due to Term

• Current Assignee: Evonik Operations GmbH (Rag-Stiftung)
• Original Assignee: Degussa AG (Rag-Stiftung)
• Inventors: Golchert, Rainer, Janzon, Karlheinz, Mangold, Helmut, Katusic, Stipan
• Primary Examiner(s): MARCANTONI, PAUL D
• Application Number:
  US09/924,594
• Publication Number:
  US 20020035950A1
• Time in Patent Office: 754 Days
• Field of Search: 423/335, 423/337, 423/592.1, 423/610, 423/608, 423/618, 423/625, 423/606, 423/278, 501/133
• US Class Current: 423/278
• CPC Class Codes: A61K 8/25 Silicon; Compounds thereof
• CPC Class Codes: A61Q 1/02 Preparations containing skin colorants, e.g. pigments preparations in powder form A61Q1/12
• CPC Class Codes: B01J 12/02 for obtaining at least one reaction product which, at normal temperature, is in the solid state
• CPC Class Codes: B01J 19/26 Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
• CPC Class Codes: B01J 2219/00094 Jackets
• CPC Class Codes: B01J 2219/00108 involving reactant vapours
• CPC Class Codes: B01J 2219/00119 Heat exchange inside a feeding nozzle or nozzle reactor
• CPC Class Codes: B01J 2219/00121 by direct heating or cooling
• CPC Class Codes: B01J 2219/1946 conical
• CPC Class Codes: B01J 37/0054 Drying of aerosols
• CPC Class Codes: B01J 37/0238 via the gaseous phase-sublimation
• CPC Class Codes: B01J 37/105 Hydropyrolysis
• CPC Class Codes: B01J 37/343 of ultrasonic wave energy
• CPC Class Codes: C01B 13/24 in the presence of hot combustion gases
• CPC Class Codes: C01B 33/181 by a dry process
• CPC Class Codes: C01G 23/07 Producing by vapour phase processes, e.g. halide oxidation
• CPC Class Codes: C01P 2002/54 one element only
• CPC Class Codes: C01P 2004/03 obtained by SEM
• CPC Class Codes: C01P 2004/50 Agglomerated particles
• CPC Class Codes: C01P 2004/62 Submicrometer sized, i.e. from 0.1-1 micrometer
• CPC Class Codes: C01P 2006/12 : Surface area
• CPC Class Codes: C08K 3/22 : of metals
• CPC Class Codes: C08L 21/00 : Compositions of unspecified rubbers
• CPC Class Codes: C09C 1/00 : Treatment of specific inorganic materials other than fibrous fillers tenebrescent materials C09K9/00; luminescent materials C09K11/00; Preparation of carbon black
• CPC Class Codes: C09C 1/30 : Silicic acid

Abstract

Doped, pyrogenically prepared oxides of metals and/or non-metals which are doped with one or more doping components in an amount of 0.00001 to 20 wt. %. The doping component may be a metal and/or non-metal or an oxide and/or a salt of a metal and/or a non-metal. The BET surface area of the doped oxide may be between 5 and 600 m²/g. The doped pyrogenically prepared oxides of metals and/or non-metals are prepared by adding an aerosol which contains an aqueous solution of a metal and/or non-metal to the gas mixture during the flame hydrolysis of vaporizable compounds of metals and/or non-metals.

Claims

1. A doped, pyrogenic oxide of at least one of a metal, a non-metal and a metalloid, produced by a process comprising:

providing an aerosol comprised of,

at least one of a solution and a suspension of a substance to be doped selected from the group consisting of a metal salt, a non-metal salt, a metalloid salt, and mixtures thereof, and

at least one of a solution and a suspension of a doping substance selected from the group consisting of a metal salt, a non-metal salt, a metalloid salt, and mixtures thereof;

mixing the aerosol with a combustible gas stream to create a combustible gas stream mixture;

reacting the gas stream mixture in a flame; and

separating the resulting doped, pyrogenic oxide from the gas stream mixture.

2. The doped, pyrogenic oxide according to claim 1, wherein the substance to be doped comprises at least one member selected from the group consisting of aluminum, niobium, titanium, tungsten, zirconium, germanium, boron and silicon.

3. The doped, pyrogenic oxide according to claim 1, wherein the doping substance comprises at least one of a transition metal and a noble metal.

4. The doped, pyrogenic oxide according to claim 1, wherein the resulting doped, pyrogenic oxide comprises at least one member selected from the group consisting of SiO₂, TiO₂, Al₂O₃, B₂O₃, ZrO₂, GeO₂, WO₃, and Nb₂O₅.

5. The doped, pyrogenic oxide according to claim 1, wherein the at least one of a solution and a suspension of a substance to be doped comprises SiCl₄, and wherein the at least one of a solution and a suspension of a doping substance comprises cerium (III) chloride.

6. The doped, pyrogenic oxide according to claim 1, wherein the process by which the oxide is produced comprises a further step of treating the resulting doped, pyrogenic oxide with air at an elevated temperature containing water vapor.

7. The doped, pyrogenic oxide according to claim 1, wherein the at least one of a solution and a suspension of a doping substance comprises a 5% aqueous cerium (III) chloride solution.

8. The doped, pyrogenic oxide according to claim 1, wherein the at least one of a solution and a suspension of a doping substance comprises a 0.5% aqueous potassium chloride solution.

9. The doped, pyrogenic oxide according to claim 1, wherein the resulting doped, pyrogenic oxide is doped with at least one doping component in an amount of from 0.00001 to 20% by weight.

10. The doped, pyrogenic oxide according to claim 1, wherein the resulting doped, pyrogenic oxide has a BET surface area of from 5 to 600 m²/g.

11. The doped, pyrogenic oxide according to claim 1, wherein the doping component comprise at least one member selected from cerium, a cerium salt, and an oxide of cerium.

12. The doped, pyrogenic oxide according to claim 1, wherein the doping component comrpises at least one member selected from a noble metal, a noble metal salt and a noble metal oxide.

13. The doped, pyrogenic oxide according to claim 1, wherein the doping component comprises at least one member selected from a transition series element, a transition series element salt and a transition series oxide.

14. The doped, pyrogenic oxide according to claim 1, wherein the providing an aerosol is via nebulization.

15. The doped, pyrogenic oxide according to claim 1, wherein the nebulization is ultrasonic nebulization.

16. The doped, pyrogenic oxide according to claim 1, wherein the doping component comprises at least one of potassium, a potassium salt, and an oxide of potassium.

17. The doped, pyrogenic oxide according to claim 1, wherein an amount of the doping substance is from 1 to 10,000 ppm of the resulting doped, pyrogenic oxide.

18. A method of improving a thickening effect in unsaturated polyester resins, comprising adding to such resins the doped, pyrogenic oxide according to claim 5.