Silica materials and methods of making thereof

Patent metadata

Field	Value
Publication number	US-11512002-B2
Application number	US-201916388725-A
Country	US
Kind code	B2
Filing date	Apr 18, 2019
Priority date	Apr 18, 2018
Publication date	Nov 29, 2022
Grant date	Nov 29, 2022

Abstract

Disclosed herein are methods for the preparation of porous metal oxide materials, including metal oxide xerogels and metal oxide aerogels. Methods for preparing porous metal oxide materials can comprise (i) reacting a metal alkoxide with water in the presence of a catalyst system to form a partially hydrolyzed sol, (ii) contacting the partially hydrolyzed sol with a base catalyst and a non-aqueous solvent to form a precursor gel; and (iii) drying the precursor gel to form the porous metal oxide material. The catalyst system employed in step (i) comprises a combination of a weak acid and a strong acid.

First claim

What is claimed is:

1. A method for preparing a porous metal oxide material comprising:
(i) reacting a metal alkoxide with water in the presence of a catalyst system to form a partially hydrolyzed sol, wherein the catalyst system comprises a strong acid and a weak acid;
(ii) contacting the partially hydrolyzed sol with a base catalyst and an alcohol to form a precursor gel; and
(iii) drying the precursor gel to form the porous metal oxide material;
wherein the weak acid and the strong acid are present in a molar ratio of weak acid:strong acid of from 1:1 to 200:1.

2. The method of claim 1 , wherein the weak acid and the strong acid are present in a molar ratio of weak acid:strong acid of from 4:1 to 70:1.

3. The method of claim 1 , wherein the weak acid comprises acetic acid.

4. The method of claim 1 , wherein the strong acid comprises nitric acid, sulfuric acid, or a combination thereof.

5. The method of claim 1 , wherein the metal alkoxide comprises a silicon alkoxide.

6. The method of claim 5 , wherein the silicon alkoxide is selected from the group consisting of tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, tetrabutoxysilane, and combinations thereof.

7. The method of claim 5 , wherein the partially hydrolyzed sol comprises at least 10 wt % silica, based on the total weight of the partially hydrolyzed sol.

8. The method of claim 1 , wherein the water and the metal alkoxide are present in a molar ratio of water:metal alkoxide of from 2:1 to 5:1.

9. The method of claim 1 , wherein step (i) comprises reacting the metal alkoxide with the water in the presence of the catalyst system at a temperature of 50° C. or less.

10. The method of claim 9 , wherein step (i) comprises reacting the metal alkoxide with the water in the presence of the catalyst system at room temperature.

11. The method of claim 1 , wherein the base comprises ammonium hydroxide.

12. The method of claim 1 , wherein the alcohol comprises methanol, ethanol, propanol, butanol, or any combination thereof.

13. The method of claim 1 , wherein step (ii) comprises contacting the partially hydrolyzed sol with the base catalyst and the alcohol for a period of less than three hours at room temperature.

14. The method of claim 1 , wherein the method further comprises aging the precursor gel.

15. The method of claim 1 , wherein the method further comprises rinsing the precursor gel.

16. The method of claim 1 , wherein the precursor gel comprises a film, a polymeric gel, or a colloidal gel.

17. The method of claim 1 , wherein drying the precursor gel comprises supercritically drying the precursor gel.

18. The method of claim 17 , wherein the method further comprises calcining the supercritically dried precursor.

19. The method of claim 1 , wherein the porous metal oxide material comprises a metal oxide aerogel.

Assignees

• Univ Virginia Patent Foundation

Inventors

• Sonn Jong Ho
• Norris Pamela M

Classifications

• C01B33/1585

  Dehydration into aerogels · CPC title

• B01J21/08

  Silica · CPC title

• B01J31/0209

  Esters of carboxylic or carbonic acids · CPC title

• C01B33/155 Primary

  Preparation of hydroorganogels or organogels · CPC title

• C01P2006/14

  Pore volume · CPC title