Method for making high purity metal oxide particles and materials made thereof

Patent metadata

Field	Value
Publication number	US-9249028-B2
Application number	US-201213560516-A
Country	US
Kind code	B2
Filing date	Jul 27, 2012
Priority date	Feb 8, 2010
Publication date	Feb 2, 2016
Grant date	Feb 2, 2016

Abstract

The present invention is directed to a method of making metal oxide and mixed metal oxide particles. The method includes treating a mixture formed from a metal source, such as metal alkoxide, a surfactant, and a first alcohol in an aqueous media at a very high metal oxide yield. The mixture is reacted using a catalyst to form metal oxide particles having a desired particle size in said mixture. By washing the particles with an aprotic solvent, the residual carbon content of the particles can be significantly reduced. The method is particularly suitable for forming silica particles. The metal oxide particles can then be heat treated to form synthetic fused metal oxides such as, for example, synthetic fused silica.

First claim

What is claimed is:

1. A method for producing porous metal oxide, metal hydroxide, metal carbonate, sulfate or metal oxalate particles, the method comprising:
forming metal oxide, hydroxide, carbonate, sulfate, or oxolate particles from an alkoxide or organometallic material wherein the method of forming the particles comprises;
(i) mixing a first solution comprising an organometaloxo oligomer with a second solution comprising, water, a surfactant, and an alcohol to form a first mixture;
(ii) adding a phase enhancer to the first mixture to form a second mixture;
(iii) adding a catalyst to the second mixture to form the metal particles; and
(iv) removing residual organic materials in the particles by treating the particles with water, at least one aprotic solvent, or a combination thereof via stripping, washing, or a combination thereof.

2. The method of claim 1 , wherein removing residual organic materials in the particles comprises treating the particles from step (iii) with an aprotic solvent.

3. The method of claim 2 , wherein subsequent to formation of the particles in step (iii) and prior to and/or after treating the particles in step (iv), the method further comprises heating the particles at about 20° C. to about 110° C. and stripping organic material from the particles under pressures of from −13 psig to +0.5 psig with or without gas sparging.

4. The method of claim 2 comprising heating the particles for a first period of time prior to the treating operation (iv), and subsequently stripping organic material from the particles by adding water to the system and heating the particles to between 20° C. and 110° C. sufficient to facilitate the removal of organic material from the particles.

5. The method of claim 2 , wherein treating with the aprotic solvent comprises:
(a) rinsing the particles with the aprotic solvent to remove organic material from the particles;
(b) decanting the aprotic solvent carrying the organic material; and
(c) repeating (a) and (b) until the particles have a desired level of hydrocarbon material.

6. The method of claim 5 comprising washing the particles with water between successive rinsings with the aprotic solvent.

7. The method of claim 2 , wherein treating the particles with the aprotic solvent comprises adding water and the aprotic solvent to the particles, and heating the particles to remove a majority of the residual organic material, a majority of the aprotic solvent, and at least a portion of the water.

8. The method of claim 7 , wherein treating the particles with the solution of water and the aprotic solvent and heating the particles are each performed two or more times until a desired residual hydrocarbon level is obtained.

9. The method of claim 1 , wherein the aprotic solvent is chosen from acetone, dimethyl ether, dichloromethane, tetrahydrofuran, dimethylformamide, acetonitrile, dimethyl sulfoxide, ethyl acetate, or a combination of two or more thereof.

10. The method of claim 1 , where removing residual organic materials in the particles comprises treating the particles from step (iii) with water.

11. The method of claim 2 , wherein subsequent to treating the particles with the aprotic solvent, or as part of the process, one or more of the solutions formed during the process are regularly decanted in order to remove surfactants and higher alcohols from the solution.

12. The method of claim 1 comprising treating the particles with the aprotic solvent at a temperature of from about 20 to about 110° C.

13. The method of claim 1 comprising treating the particles with an aprotic solvent two or more times.

14. The method of claim 2 further comprising curing the particles prior to treating with the aprotic solvent, wherein curing comprises ageing the particles, heating the particles, or heating and ageing the particles.

15. The method of claim 2 further comprising:
(v) thermally treating the particles to calcine and/or densify the particles.

16. The method of claim 1 comprising densifying the particles with or without a prior calcining treatment.

17. The method of claim 1 , wherein the organometaloxo oligomer comprises a metal chosen from Si, Ti, Fe, Al, Zr, Nb, Y, Mg, Mn, Co, Ni, Cu, V, Ce, alkaline metals, alkaline earth metals, rare earth metals, or a combination of two or more thereof.

18. The method of claim 1 , wherein the organometaloxo oligomer is a polyalkoxysiloxane, and the first solution is prepared by at least partially hydrolyzing a silicon alkoxide to form a polyalkoxysiloxane; and
the first mixture is formed by combining the polyalkoxysiloxane with water, a first surfactant, a first alcohol, and a second catalyst.

19. The method of claim 18 , wherein the first second catalyst can be an acid or a base.

20. The method of claim 18 , wherein the water to polyalkoxysiloxane molar ratio is from about 0.25 to about 4.

21. The method of claim 18 , wherein the first catalyst can be a base catalyst chosen from an organic base, an inorganic base, or a combination of two or more thereof.

22. The method of claim 21 , wherein the first catalyst comprises ammonia hydroxide.

23. The method of claim 18 , wherein the polyalkoxysiloxane comprises from about 4 to about 20 Si—O units.

24. The method of claim 1 further comprising recycling the organic material that has been collected by stripping, decanting, washing with or without additional purification, separating the organic material, and supplying the organic material back into a metal alkoxide generation or particle formation generation operation.

25. The method of claim 2 wherein subsequent to treatment of the metal oxide particles with the aprotic solvent, the aprotic solvent is separated from the particles and recycled for a subsequent washing operation.

26. A method for producing high purity porous metal oxide, metal hydroxide, or carbonate particles with a surface area between 150-1200 m 2 /g and/or a metal impurity of about 50 ppb or less for each metal impurity, the method comprising forming metal oxide, hydroxide, carbonate, sulfate, or oxolate particles from an alkoxide or organometallic material wherein the method of forming the particles comprises, mixing a first solution comprising an organometaloxo oligomer with a second solution comprising, water, a surfactant, and an alcohol to form a first mixture, adding a phase enhancer to the first mixture to form a second mixture, adding a catalyst to the second mixture to form the metal particles, and removing residual organic materials, including alcohols generated from the alkoxides, in the particles by treating the particles via stripping, washing, or a combination thereof, the treating of the particles using water, at least one aprotic solvent, or combinations thereof.

Assignees

• Devera Antonio L
• Panchula Martin
• Momentive Performance Mat Inc

Inventors

• Devera Antonio L
• Panchula Martin

Classifications

• C01B33/18

  Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof (preparation of aerogels by dehydrating gels C01B33/158; treatment to enhance the pigmenting or filling properties C09C) · CPC title

• C01B33/12 Primary

  Silica; Hydrates thereof, e.g. lepidoic silicic acid · CPC title

• Y10T428/2982

  Particulate matter [e.g., sphere, flake, etc.] · CPC title

• C01P2004/61

  Micrometer sized, i.e. from 1-100 micrometer · CPC title

• C01P2004/03

  obtained by SEM · CPC title