Process for the preparation of solid state materials and said materials

• US 5,466,646 A
• Filed: 08/18/1992
• Issued: 11/14/1995
• Est. Priority Date: 08/18/1992
• Status: Expired due to Fees

• Current Assignee: Worcester Polytechnic Institute
• Original Assignee: Worcester Polytechnic Institute
• Inventors: Moser, William R.
• Primary Examiner(s): PAL, ASOKKUMAR
• Application Number:
  US07/931,766
• Time in Patent Office: 1,183 Days
• Field of Search: 502/5, 502/60, 502/234, 502/235, 502/236, 502/523
• US Class Current: 502/60
• CPC Class Codes: B01J 37/031 Precipitation
• CPC Class Codes: Y10S 502/523 Miscellaneous specific techniques of general applicability

Abstract

A process for the preparation of solid state materials such as catalysts, electrolytes, piezo electric materials and superconductors is disclosed. The process produces materials with high phase purity. Novel solid state materials having high phase purity are also disclosed.

Claims

1. A process for producing solid state materials having a phase purity greater than about 99% and less than 1% in discrete separate phase compounds comprising (1) mixing together a metal containing solution and a second solution containing a precipitating agent to form a mixed solution, (2) pressurizing the mixed solution to a pressure in the range from about 1,000 to about 50,000 psig, (3) passing the mixed solution into a fluidizing apparatus wherein high shear forces act on the mixed solution, (4) depressurizing the mixed solution so as to cause cavitation, and (5) separating a solid state material from the cavitated mixed solution.

3. The process of claim 1, wherein the metal containing solution and the precipitating agent containing solution are mixed prior to passage into the fluidizing apparatus.

4. The process of claim 1, wherein an additional solution material containing a solid support is added along with the metal containing solution and the precipitating agent containing solution to form the mixed solution.

5. The process of claim 1, wherein the mixed solution is recycled through the fluidizer apparatus.

6. The process of claim 1, wherein the precipitating agent solution is gradually added to the mixed solution as it recycled.

7. The process of claim 1, wherein the metal containing solution is gradually added to the mixed solution as it is recycled.

8. The process of claim 1, wherein the metal containing solution and the precipitating agent solution are mixed together as they enter the pressurizing pump.

9. The process of claim 1, wherein the metal containing solution is a metal salt solution.

10. The process of claim 1, wherein the salt is selected from any of a nitrate, an acetate, chloride, sulfate or bromide.

11. The process of claim 1, wherein the solid state material is a metal catalyst.

13. The process of claim 1, wherein the metal containing solution and the precipitating agent solution are mixed together in a separate vessel.

14. The process of claim 13, wherein the metal containing solution contains a source of silica and the so formed mixed solution is a zeolite gel.

15. The process of claim 14, wherein the zeolite gel is formed in an autoclave.

16. The process of claim 15, wherein the autoclave is pressurized.

17. The process of claim 15, wherein the zeolite gel is recycled between the autoclave and the fluidizer apparatus.

18. The process of claim 1, wherein the precipitating agent solution contains a source of silica and the mixed solution forms as a zeolite gel as the two solutions are mixed together.

19. The process of claim 18, wherein the precipitating agent containing solution is gradually added to the mixed solution which is being recycled through the fluidizer apparatus.

2. The process of claim 2, wherein the pressure is of from about 12,000 to 25,000 psig.

12. The process of claim 12, wherein the metal catalyst comprises a mixture of metals.

20. A process for producing a metal-containing crystalline product comprising:

(1) subjecting a metal-containing solution to high pressure at a pressure in the range from about 1,000 to about 50,000 psig and high shear force in the presence of a precipitating agent, (2) depressurizing the resulting solution; and

(3) transferring the depressurized solution to a crystallization vessel to affect hydrothermal synthesis of a metal-containing crystalline product.

21. A process of claim 20, wherein (1) mixing a metal-containing solution is with a precipitating agent;

(2) pressurizing the mixed solution;

(3) passing the mixed solution into a fluidizing apparatus, wherein high shear forces act on the mixed solution;

(4) depressurizing the mixed solution;

(5) transferring the depressurized solution into a high pressure autoclave under hydrothermal synthesis conditions, whereby at least a portion of the metal-containing solution is converted into a metal-containing crystalline product; and

(6) cooling the mixture and separating the metal containing crystalline product from the remaining solution by liquid-solid preparation.

22. The process of claim 21, wherein the metal-containing solution is a zeolite gel and the hydrothermal synthesis is carried out at a temperature from about 60°

C. to about 170°

C. under a pressure ranging from about 14 psia to about 800 psia from about 4 hours to about 170 hours.