Hydrophobic silica wet gel and aerogel

Patent metadata

Field	Value
Publication number	US-2024359451-A1
Application number	US-202418636591-A
Country	US
Kind code	A1
Filing date	Apr 16, 2024
Priority date	Apr 20, 2023
Publication date	Oct 31, 2024
Grant date	—

Abstract

The invention provides hydrophobic silica wet gel, hydrophobic silica aerogel, and methods that can be used to form an enhanced hydrophobic silica aerogel sheet having an advantageous combination of properties. Some embodiments of the invention provide a hydrophobic silica aerogel having advantageous properties, such as desirable performance on visible transmission, haze, or both.

First claim

What is claimed is:

1 . A method of making a hydrophobic silica aerogel, comprising the steps of:
preparing a silica wet gel from a precursor material comprising a first alkoxysilane, solvent, catalyst and water, wherein the first alkoxysilane is selected from methyl silicate 51 and tetramethoxysilane; preparing a hydrophobic treatment solution from a second alkoxysilane and diluent, wherein the second alkoxysilane is selected from methyltrimethoxysilane and methyltriethoxysilane; exposing the silica wet gel to the hydrophobic treatment solution to form a hydrophobic silica wet gel; aging either the silica wet gel or the hydrophobic silica wet gel for an aging time period; subjecting the hydrophobic silica wet gel to solvent extraction with an extraction solvent for an extraction time period of less than 24 hours; and subjecting the hydrophobic silica wet gel to drying to form a hydrophobic silica aerogel.

2 . The method of claim 1 wherein the aging time period is at least 7 days (168 hours).

3 . The method of claim 1 wherein the step of aging comprises aging the silica wet gel or the hydrophobic silica wet gel at room temperature.

4 . The method of claim 1 wherein the step of aging comprises aging either the silica wet gel or the hydrophobic silica wet gel for an aging time period until structural changes of the silica wet gel or the hydrophobic silica wet gel no longer occur.

5 . The method of claim 1 wherein the method is devoid of using a surfactant.

6 . The method of claim 1 wherein the method is devoid of using a hydrophobic agent other than the hydrophobic treatment solution.

7 . The method of claim 1 wherein each of the solvent, the diluent and the extraction solvent is methanol.

8 . The method of claim 1 wherein the extraction time period is less than 20 hours.

9 . The method of claim 1 wherein the hydrophobic silica aerogel is formed having a water contact angle of at least 90°.

10 . The method of claim 1 wherein the step of subjecting the hydrophobic silica wet gel to drying forms the hydrophobic silica aerogel such that less than 1% solvent remains within the hydrophobic silica aerogel.

11 . The method of claim 1 wherein the step of subjecting the hydrophobic silica wet gel to drying forms the hydrophobic silica aerogel with a shrinkage value of 4% or less.

12 . The method of claim 1 wherein the step of subjecting the hydrophobic silica wet gel to drying forms the hydrophobic silica aerogel with a visible transmission of at least 97.8% and a haze value of 3% or less.

13 . A method of making a hydrophobic silica aerogel, comprising the steps of:
preparing a first solution by mixing a first alkoxysilane and solvent, wherein the first alkoxysilane is selected from methyl silicate 51 and tetramethoxysilane; preparing a second solution by mixing solvent, ammonium hydroxide and water; mixing the first solution and the second solution together; allowing components in the first solution and the second solution to react to form a silica wet gel; preparing a third solution by combining methyltrimethoxysilane and diluent; adding the third solution to the silica wet gel; allowing the third solution to react with the silica wet gel to form a hydrophobic silica wet gel; aging either the silica wet gel or the hydrophobic silica wet gel for an aging time period; subjecting the hydrophobic silica wet gel to solvent extraction with an extraction solvent; subjecting the hydrophobic silica wet gel to drying to form a hydrophobic silica aerogel; and wherein the method is devoid of using a surfactant.

14 . The method of claim 13 wherein the method is devoid of using a hydrophobic agent other than the third solution.

15 . The method of claim 13 wherein the aging time period is at least 7 days (168 hours).

16 . The method of claim 13 wherein the step of aging either the silica wet gel or the hydrophobic silica wet gel is performed at room temperature.

17 . The method of claim 13 wherein the step of aging comprises aging either the silica wet gel or the hydrophobic silica wet gel for an aging time period until structural changes of the silica wet gel or the hydrophobic silica wet gel no longer occur.

18 . The method of claim 13 wherein the step of subjecting the hydrophobic silica wet gel to solvent extraction is performed during an extraction time period of less than 24 hours.

19 . The method of claim 13 wherein each of the solvent, the diluent and the extraction solvent is methanol.

20 . The method of claim 13 wherein the step of subjecting the hydrophobic silica wet gel to drying forms the hydrophobic silica aerogel with a shrinkage value of 4% or less.

21 . The method of claim 13 wherein the step of subjecting the hydrophobic silica wet gel to drying forms the hydrophobic silica aerogel with less than 1% solvent remaining within the hydrophobic silica aerogel.

22 . The method of claim 13 wherein the hydrophobic silica aerogel is formed having a water contact angle of at least 90°.

23 . The method of claim 13 wherein the step of subjecting the hydrophobic silica wet gel to drying forms the hydrophobic silica aerogel with a visible transmission of at least 97.8% and a haze value of 3% or less.

24 . A method of making a hydrophobic silica aerogel, comprising the steps of:
preparing a first solution by mixing a first alkoxysilane and solvent, wherein the first alkoxysilane is selected from methyl silicate 51 and tetramethoxysilane; preparing a second solution by mixing ammonium hydroxide and water; mixing the first solution and the second solution together; allowing components in the first solution and the second solution to react to form a silica wet gel; aging the silica wet gel for an aging time period; preparing a third solution by mixing catalyst and solvent; preparing a fourth solution by mixing a second alkoxysilane, catalyst and diluent, wherein the second alkoxysilane is selected from methyltrimethoxysilane and methyltriethoxysilane; preparing a solvent exchange solution by mixing the third solution, the fourth solution and an extraction solvent; subjecting the silica wet gel to the solvent exchange solution for an extraction time period of less than 24 hours and allowing components in the solvent exchange solution to react with the silica wet gel to form a hydrophobic silica wet gel; and subjecting the hydrophobic silica wet gel to drying to form a hydrophobic silica aerogel; and wherein the method is devoid of using a surfactant.

25 . The method of claim 24 wherein the method is devoid of using a hydrophobic agent other than the second alkoxysilane in the solvent exchange solution.

26 . The method of claim 24 wherein the aging time period is at least 7 days (168 hours).

27 . The method of claim 24 wherein the step of aging the silica wet gel is performed at room temperature.

28 . The method of claim 24 wherein the step of aging comprises aging the silica wet gel for an aging time period until structural changes of the silica wet gel no longer occur.

29 . The method of claim 24 wherein the method is devoid of using a surfactant.

30 . The method of claim 24 wherein each of the solvent, the diluent and the extraction solvent is methanol.

31 . The method of claim 24 wherein the

Assignees

• Cardinal Cg Co

Inventors

• Chowdhury Reaz Ahmed
• Myli Kari B

Classifications

• E06B3/6715

  specially adapted for increased thermal insulation or for controlled passage of light (E06B3/66323 takes precedence; coating of glass pains C03C17/00; devices or arrangements for controlling the intensity, colour, phase, polarisation or direction of light G02F1/00) · CPC title

• E06B3/66328

  of rubber, plastics or similar materials (E06B3/66314, E06B3/66323 and E06B3/66342 take precedence; transparent materials E06B3/66333) · CPC title

• E06B3/66319

  of rubber, plastics or similar materials · CPC title

• E06B3/66314

  of tubular shape (E06B3/66323 and E06B3/66333 take precedence) · CPC title

• B32B2250/44

  Number of layers variable across the laminate · CPC title