Method for one-step synthesis, cross-linking and drying of aerogels

Patent metadata

Field	Value
Publication number	US-10414894-B2
Application number	US-201515500376-A
Country	US
Kind code	B2
Filing date	Jul 31, 2015
Priority date	Jul 31, 2014
Publication date	Sep 17, 2019
Grant date	Sep 17, 2019

Abstract

A method of synthesizing aerogels and cross-linked aerogels in a single step and in a single pot without requiring any solvent exchange is described. Porous matrices are synthesized through a modification of hydrolysis condensation of alkoxides in which addition of water is minimized. The reaction occurs in an ethanol-water azeotrope mixture; the water in the azeotrope slowly hydrolyzes the alkoxide. Additionally, after gelation, the porous matrix is dried in supercritical ethanol rather than liquid CO2, which allows for elimination of solvent exchange steps. These modifications allow for the preparation of aerogel monoliths in any size in one step and in one pot and much faster than conventional procedures. In addition, the method provides for custom aerogel parts with large dimensions, as well as high volume fabrication of aerogels. The custom aerogel parts may be used in a variety of thermal insulation applications.

First claim

The invention claimed is:

1. A method for producing an aerogel, comprising:
providing a first solution comprising an alkoxide;
providing a second solution comprising a catalyst;
mixing the first and second solutions to provide a gelation mixture;
wherein the mixing of the first and second solutions results in formation of a wet gel as a result of hydrolysis of the alkoxide and polymerization of the hydrolyzed alkoxide; and
after gelation, drying the wet gel in an organic solvent and water azeotrope mixture heated at supercritical temperature and pressure to form an aerogel, wherein the drying is performed with the wet gel outside of any mold.

2. The method of claim 1 , wherein the organic solvent is ethanol.

3. The method of claim 1 , wherein the method includes no solvent exchange step.

4. The method of claim 1 , wherein the wet gel is not dried in liquid or supercritical CO 2 .

5. The method of claim 1 , wherein the alkoxide is tetraethyl orthosilicate (TEOS) or tetramethyl orthosilicate (TMOS).

6. The method of claim 1 , wherein the catalyst is an acid, a metal salt or a base.

7. The method of claim 1 , wherein the first solution further comprises a first acrylic monomer and the second solution further comprises a second acrylic monomer, wherein the first acrylic monomer is hexanedioldiacryate or acrylated dipentaerthritol and wherein the second acrylic monomer is hexanedioldiacrylate or acrylated dipentaerthritol.

8. The method of claim 7 wherein the first solution or second solution further comprises a photoinitiator.

9. The method of claim 8 , wherein photopolymerization is induced by exposure of the gel to a source of visible light at an intensity sufficient to cause photopolymerization.

10. The method of claim 1 , wherein the alkoxide is present in an amount ranging from about 0.1% v/v to 50% v/v based on total volume of the gelation mixture.

11. The method of claim 1 , wherein the gelation mixture comprises an amine present in an amount ranging from about 0.1% v/v to 20% v/v based on total volume of the gelation mixture.

12. The method of claim 1 , wherein the gelation mixture comprises a supercritical organic solvent present in an amount ranging from about 20% v/v to 90% v/v based on total volume of the gelation mixture, and wherein the organic solvent is chosen from one or more of ethanol, methanol, butanol, propanol, acetone, or dimethylsulfoxide.

13. The method of claim 1 , wherein the first solution further comprises a first monomer and the second solution further comprises a second monomer.

14. The method of claim 13 , wherein the first monomer and/or second monomer are capable of being polymerized by free radical initiation, photoinitiation, and/or thermal initiation.

15. The method of claim 1 , wherein the first solution and second solution comprise an ethanol-water azeotrope mixture.

16. The method of claim 2 , wherein the first solution and second solution comprise an ethanol-water azeotrope mixture.

Assignees

• Univ Virginia Commonwealth

Inventors

• Bertino Massimo

Classifications

• C08J2201/022

  premixing or pre-blending a part of the components of a foamable composition, e.g. premixing the polyol with the blowing agent, surfactant and catalyst and only adding the isocyanate at the time of foaming · CPC title

• C08J2201/0522

  the liquid phase being organic · CPC title

• C08J9/286 Primary

  the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers · CPC title

• C01B33/1585

  Dehydration into aerogels · CPC title

• B01J13/0091

  Preparation of aerogels, e.g. xerogels · CPC title