Hydrophobic aerogel materials

Patent metadata

Field	Value
Publication number	US-9868843-B2
Application number	US-201514873753-A
Country	US
Kind code	B2
Filing date	Oct 2, 2015
Priority date	Oct 3, 2014
Publication date	Jan 16, 2018
Grant date	Jan 16, 2018

Abstract

The present disclosure provides an aerogel composition which is durable and easy to handle, which has favorable performance in aqueous environments, and which also has favorable combustion and self-heating properties. Also provided is a method of preparing an aerogel composition which is durable and easy to handle, which has favorable performance in aqueous environments, and which has favorable combustion and self-heating properties. Further provided is a method of improving the hydrophobicity, the liquid water uptake, the heat of combustion, or the onset of thermal decomposition temperature of an aerogel composition.

First claim

What is claimed:

1. A method comprising:
a) Providing a precursor solution comprising silica gel precursor materials and a solvent;
b) Combining the precursor solution with a reinforcement material;
c) Allowing the silica gel precursor materials in the precursor solution to transition into a gel composition to form a reinforced, silica-based gel composition;
d) Extracting at least a portion of the solvent from the reinforced, silica-based gel composition to obtain a reinforced, silica-based aerogel composition; and
e) Exposing the reinforced, silica-based aerogel composition to heat treatment in a reduced oxygen atmosphere, wherein the heat treatment includes exposure to one or more temperatures between 500° C. and 700° C., and wherein the total duration of heat treatment in reduced oxygen atmosphere of the reinforced, silica-based aerogel composition is between 1 minute and 30 minutes;
wherein the method further comprises incorporating at least one hydrophobic-bound silicon into the reinforced, silica-based aerogel composition prior to step e).

2. The method of claim 1 , wherein the reinforcement material comprises a sheet of fiber reinforcement material.

3. The method of claim 1 , wherein the heat treatment in a reduced oxygen atmosphere of the reinforced, silica-based aerogel composition does not include exposure to a temperature above 700° C. for more than 1 minute.

4. The method of claim 1 , wherein the reduced oxygen atmosphere comprises 0.1% to 5% oxygen by volume.

5. The method of claim 1 , wherein the reinforced, silica-based aerogel composition has a hydrophobic organic content between 1 wt % and 12 wt % before the heat treatment and after the heat treatment.

6. The method of claim 1 , wherein the reinforced, silica-based aerogel composition comprises hydrophobic organic material before the heat treatment, and wherein at least 50% of the hydrophobic organic material in the reinforced, silica-based aerogel composition before the heat treatment comprises aliphatic hydrophobic groups.

7. The method of claim 1 , wherein the hydrophobic-bound silicon is incorporated into the reinforced, silica-based aerogel composition by including in the precursor solution at least one silica gel precursor material having at least one hydrophobic group.

8. The method of claim 1 , wherein the at least one hydrophobic-bound silicon is incorporated into the reinforced, silica-based aerogel composition by exposing the reinforced, silica-based gel or the reinforced, silica-based aerogel composition to a hydrophobizing agent.

9. A method comprising exposing a reinforced, silica-based aerogel composition comprising at least one hydrophobic-bound silicon to heat treatment in a reduced oxygen atmosphere, wherein the heat treatment includes exposure to one or more temperatures between 500° C. and 700° C., and wherein the total duration of the heat treatment in a reduced oxygen atmosphere of the reinforced, silica-based aerogel composition is between 1 minute and 30 minutes.

10. The method of claim 9 , wherein the reinforced, silica-based aerogel composition comprises a sheet of fiber reinforcement material.

11. The method of claim 9 , wherein the heat treatment in a reduced oxygen atmosphere of the reinforced, silica-based aerogel composition does not include exposure to a temperature above 700° C. for more than 1 minute.

12. The method of claim 9 , wherein the reduced oxygen atmosphere comprises 0.1% to 5% oxygen by volume.

13. The method of claim 9 , wherein the reinforced, silica-based aerogel composition has a hydrophobic organic content between 1 wt % and 12 wt % before the heat treatment and after the heat treatment.

14. The method of claim 9 , wherein the reinforced, silica-based aerogel composition comprises hydrophobic organic material before the heat treatment, and wherein at least 50% of the hydrophobic organic material in the reinforced, silica-based aerogel composition before the heat treatment comprises aliphatic hydrophobic groups.

15. The method of claim 9 , wherein the reinforced, silica-based aerogel composition after the heat treatment has a lower liquid water uptake percentage relative to the reinforced, silica-based aerogel composition before the heat treatment.

16. The method of claim 9 , wherein the reinforced, silica-based aerogel composition after the heat treatment has a lower heat of combustion relative to the first reinforced, silica-based aerogel composition before the heat treatment.

17. The method of claim 9 , wherein the reinforced, silica-based aerogel composition after the heat treatment has a higher onset of thermal decomposition temperature relative to the reinforced, silica-based aerogel composition before the heat treatment.

18. A reinforced, silica-based aerogel composition produced by the method of claim 11 .

19. The reinforced, silica-based aerogel composition of claim 18 , wherein the reinforced, silica-based aerogel composition has the following properties:
i) liquid water uptake of 40 wt % or less;
ii) onset of thermal decomposition of hydrophobic organic materials of 500° C. or higher.

20. The reinforced, silica-based aerogel composition of claim 19 , wherein the reinforced, silica-based aerogel composition has the following properties:
iii) heat of combustion of less than 717 cal/g; and iv) thermal conductivity of 40 mW/M*K or less.

21. The reinforced, silica-based aerogel composition of claim 19 , wherein the hydrophobic organic content in the reinforced, silica-based aerogel composition is between 1 wt % and 12 wt %.

22. The reinforced, silica-based aerogel composition of claim 19 , wherein the reinforced, silica-based aerogel composition has a ratio of T 1-2 :T 3 of between 0.01 and 0.4.

23. A reinforced aerogel composition comprising a silica-based framework; wherein the reinforced aerogel composition has the following properties:
i) liquid water uptake of 40 wt % or less;
ii) onset of thermal decomposition of hydrophobic organic materials of 515° C. or higher;
iii) heat of combustion of less than 717 cal/g; and
iv) thermal conductivity of 40 mW/M*K or less.

24. The reinforced aerogel composition of claim 23 , wherein the reinforced aerogel composition has the following properties:
ii) onset of thermal decomposition of hydrophobic organic materials between 515° C. and 635° C.;
iii) heat of combustion between 265 cal/g and 717 cal/g; and
iv) thermal conductivity between 15 mW/M*K and 40 mW/M*K.

25. The reinforced aerogel composition of claim 24 , wherein the reinforced aerogel composition comprises a sheet of fiber reinforcement material.

26. The reinforced aerogel composition of claim 24 , wherein the reinforced aerogel composition has a density of 0.40 g/cm3 or less.

27. The reinforced aerogel composition of claim 24 , wherein the reinforced aerogel composition has a thermal conductivity between 15 mW/M*K and 30 mW/M*K.

28. The reinforced aerogel composition of claim 24 , wherein the reinforced aerogel composition has a heat of combustion of less than 600 cal/g.

29. The reinforced aerogel composition of claim 24 , wherein the reinforced aerogel composition has a heat of combustion of 550 cal/g or less.

30. The reinforced aerogel composition of claim 24 , wherein the reinforced aerogel composition has a heat of combustion of 500 cal/g or less.

31. The re

Assignees

• Aspen Aerogels Inc
• Aspen Aerogels Inc

Inventors

• Evans Owen Richard
• Dekrafft Kathryn Elizabeth
• Zafiropoulos Nicholas Anthony
• Dong Wenting
• Mihalcik David J
• Gould George L
• Melnikova Irene

Classifications

• C01B33/159

  Coating or hydrophobisation · CPC title

• C08K2003/2262

  of manganese · CPC title

• C08K3/22

  of metals · CPC title

• C01B33/1585 Primary

  Dehydration into aerogels · CPC title

• C08K2003/2241

  Titanium dioxide · CPC title