Method of preparing metal containing compounds using hydrodynamic cavitation

• US 6,589,501 B2
• Filed: 01/15/2002
• Issued: 07/08/2003
• Est. Priority Date: 10/25/1999
• Status: Expired due to Term

• Current Assignee: Arisdyne Systems Incorporated, Worcester Polytechnic Institute
• Original Assignee: Five Peaks Technology LLC, Worcester Polytechnic Institute
• Inventors: Find, Josef, Moser, William R., Krausz, Ivo M., Emerson, Sean Christian, Kozyuk, Oleg V.
• Primary Examiner(s): Langel, Wayne A.
• Application Number:
  US10/047,452
• Publication Number:
  US 20020193254A1
• Time in Patent Office: 539 Days
• Field of Search: 423/592, 423/593, 423/594, 423/595, 423/598, 423/604, 423/606, 423/607, 423/610, 423/611, 423/622, 423/632, 423/636, 423/639, 423/659
• US Class Current: 423/659
• CPC Class Codes: B01J 19/008 Processes for carrying out reactions under cavitation conditions
• CPC Class Codes: B01J 37/031 Precipitation
• CPC Class Codes: B22F 2202/01 Use of vibrations
• CPC Class Codes: B22F 2999/00 Aspects linked to processes or compositions used in powder metallurgy
• CPC Class Codes: B22F 9/30 with decomposition of metal compounds, e.g. by pyrolysis
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01B 13/363 Mixtures of oxides or hydroxides by precipitation
• CPC Class Codes: C01G 23/053 Producing by wet processes, e.g. hydrolysing titanium salts
• CPC Class Codes: C01G 39/00 Compounds of molybdenum
• CPC Class Codes: C01G 49/0054 containing one rare earth metal, yttrium or scandium
• CPC Class Codes: C01G 51/00 Compounds of cobalt
• CPC Class Codes: C01G 53/00 Compounds of nickel
• CPC Class Codes: C01P 2002/34 perovskite-type (ABO3)
• CPC Class Codes: C01P 2002/60 Compounds characterised by their crystallite size
• CPC Class Codes: C01P 2002/72 by d-values or two theta-values, e.g. as X-ray diagram
• CPC Class Codes: C01P 2004/64 Nanometer sized, i.e. from 1-100 nanometer
• CPC Class Codes: C01P 2006/82 water content

Abstract

A process for the preparation of nanostructured materials in high phase purities using cavitation is disclosed. The method comprises mixing a metal containing solution with a precipitating agent and passing the mixture into a cavitation chamber. The chamber consists of a first element to produce cavitation bubbles, and a second element that creates a pressure zone sufficient to collapse the bubbles. The process is useful for the preparation of mixed metal oxide catalysts and materials for piezoelectrics and superconductors.

Claims

1. A process for the preparation of nanostructured materials in high phase purities comprising:

a) mixing a metal containing solution with a precipitating agent to form a mixed solution that precipitates a product;

b) passing the mixed solution at elevated pressure into a cavitation chamber to create cavitation thereby forming a cavitated precipitated product, said cavitation chamber includes;

i) means for creating a cavitation zone, and

ii) means for controlling said cavitation zone by providing adjustable back pressure within said cavitation zone;

c) removing the cavitated precipitated product and the mixed solution from the cavitation chamber; and

d) separating the cavitated precipitated product from the mixed solution.

2. The process of claim 1, wherein at least some precipitation of the mixed solution occurs in step (b).

3. The process of claim 1, wherein both high shear and at least some in situ calcination of the mixed solution occur in the cavitation chamber.

4. The process of claim 1, wherein said means for creating said cavitation zone includes a first element internally situated within a flow-through channel having a flow area wherein said first element produces a local constriction of the flow area, said cavitation zone is formed immediately after said first element.

5. The process of claim 1, wherein said cavitation chamber further comprises means for creating a second cavitation zone to produce a multi-stage process.

6. The process of claim 5, wherein said means for creating said second cavitation zone includes a second element internally situated within said flow-through channel having a second flow area downstream of said first element wherein said second element produces a second local constriction of the second flow area, said second cavitation zone is formed immediately after said second element.

7. The process of claim 6, wherein said means for controlling said cavitation zone is varying the distance between the first and second element to provide adjustable back pressure within said cavitation zone.

8. The process of claim 6, wherein said means for controlling said cavitation zone is the second local constriction produced downstream of said first element thereby providing adjustable back pressure within said cavitation zone.

9. The process of claim 6, wherein said cavitation chamber further comprises means for controlling said second cavitation zone to produce a multi-stage process.

10. The process of claim 9, wherein said means for controlling said second cavitation zone includes a third element internally situated within said flow-through channel downstream of said second element to produce a third local constriction downstream of said second element thereby providing adjustable back pressure within said cavitation zone.

11. The process of claim 4, wherein said means for controlling said cavitation zone includes a second element internally situated within said flow-through channel downstream of said first element to produce a second local constriction thereby providing adjustable back pressure within said cavitation zone.

12. The process of claim 11, wherein said means for controlling said cavitation zone creates an elevated pressure zone between said cavitation zone and said second local constriction.

13. The process of claim 11, wherein said second element is a control valve.

14. A process for the preparation of nanostructured materials in high phase purities comprising:

a) mixing a metal containing solution with a precipitating agent to form a mixed solution that precipitates a product;

b) passing the mixed solution at elevated pressure and at a velocity into a cavitation chamber to create cavitation thereby forming a cavitated precipitated product, said cavitation chamber includes;

i) means for creating a cavitation zone, and

ii) means for controlling said cavitation zone by providing back pressure within said cavitation zone;

c) removing the cavitated precipitated product and the mixed solution from the cavitation chamber; and

d) separating the cavitated precipitated product from the mixed solution.

15. The process of claim 14, wherein at least some precipitation of the mixed solution occurs in step (b).

16. The process of claim 14, wherein both high shear and at least some in situ calcination of the mixed solution occur in the cavitation chamber.

17. The process of claim 14, wherein said means for creating said cavitation zone includes a first element internally situated within a flow-through channel having a flow area wherein said first element produces a local constriction of the flow area, said cavitation zone is formed immediately after said first element.

18. The process of claim 14, wherein the velocity of the mixed solution passing into the cavitation chamber is at a velocity sufficient to create cavitation bubbles to form downstream of the first element.

19. The process of claim 17, wherein said means for controlling includes a second element internally situated within said flow-through channel downstream of said first element to produce a second local constriction thereby providing back pressure within said cavitation zone to create an elevated pressure zone between said cavitation zone and said second local constriction.

20. The process of claim 19, wherein the cavitation bubbles are formed in said cavitation zone and the cavitation bubbles collapse in the elevated pressure zone.

21. The process of claim 20, wherein the second element provides adjustable back pressure within said cavitation zone to control said elevated pressure zone.

22. The process of claim 21, wherein the second element is a control valve.

23. The process of claim 14, further comprising a second cavitation chamber situated in series with said cavitation chamber.