Preparation method of hydrophobic silica aerogel

Patent metadata

Field	Value
Publication number	US-9862614-B2
Application number	US-201514650519-A
Country	US
Kind code	B2
Filing date	Feb 4, 2015
Priority date	Feb 6, 2014
Publication date	Jan 9, 2018
Grant date	Jan 9, 2018

Abstract

Provided is a method for preparing a hydrophobic silica aerogel by using a Soxhlet extraction, and a hydrophobic silica aerogel prepared by using the method. Since the preparation method according to the present invention may simultaneously perform washing and drying of a hydrophobic silica wet gel as well as solvent substitution and may remove an extraction solvent without an additional separation process, a hydrophobic silica aerogel having low tap density and high specific surface area may be easily prepared.

First claim

The invention claimed is:

1. A method for preparing a hydrophobic silica aerogel, the method comprising Soxhlet extracting a hydrophobic silica wet gel, wherein solvent substitution, washing, and drying are simultaneously performed on the hydrophobic silica wet gel during the Soxhlet extraction, and
wherein the Soxhlet extraction is performed at a reboiler temperature of 25° C. to 40° C., a condenser temperature of −20° C. to 10° C., and a pressure of 5 bar to 70 bar.

2. The method of claim 1 , wherein the hydrophobic silica wet gel is prepared by adding a surface modifier and an inorganic acid to a water glass solution and performing a reaction.

3. The method of claim 2 , wherein the surface modifier and the water glass solution are added in a volume ratio of 0.05:1 to 0.3:1; and
the water glass solution comprises silica in an amount of 0.1 wt % to 10 wt %.

4. The method of claim 2 , wherein the surface modifier comprises any one selected from the group consisting of a silane-based compound, a siloxane-based compound, a silanol-based compound, a silazane-based compound, and a hydrate thereof, or a mixture of two or more thereof.

5. The method of claim 2 , wherein the surface modifier comprises any one selected from the group consisting of hexaalkyldisilazane, tetraalkyldisilazane, and a hydrate thereof, or a mixture of two or more thereof.

6. The method of claim 2 , wherein the surface modifier comprises any one selected from the group consisting of hexamethyldisilazane, hydrated hexamethyldisilazane, and tetramethyldisilazane, or a mixture of two or more thereof.

7. The method of claim 2 , wherein the reaction is performed in a temperature range of 25° C. to 80° C.

8. The method of claim 2 , wherein the inorganic acid comprises any one selected from the group consisting of nitric acid, hydrochloric acid, acetic acid, sulfuric acid, and hydrofluoric acid, or a mixture of two or more thereof.

9. The method of claim 2 , further adding a non-polar organic solvent to the water glass solution.

10. The method of claim 9 , wherein the non-polar organic solvent comprises any one selected from the group consisting of hexane, heptane, toluene, and xylene, or a mixture of two or more thereof.

11. The method of claim 1 , wherein the hydrophobic silica wet gel is a hydrophobic silica lyogel or a hydrophobic silica hydrogel.

12. The method of claim 1 , wherein the Soxhlet extraction is performed by:
(A) supplying a hydrophobic silica wet gel into an extractor;
(B) performing an extraction by flowing an extraction solvent contained in a reboiler into the extractor including the hydrophobic silica wet gel through a condenser; and
(c) venting the extraction solvent which is obtained as a result of the extraction.

13. The method of claim 12 , wherein the extraction solvent is evaporated in the reboiler to be transferred to the condenser and is liquefied in the condenser to be transferred into the extractor.

14. The method of claim 12 , wherein the Soxhlet extraction is performed by circulating the extraction solvent in a sequence of the reboiler, the condenser, and the extractor.

15. The method of claim 1 , wherein the Soxhlet extraction is performed by using an extraction solvent that exists in a gas phase under conditions including a temperature of 20° C. to 40° C. and a pressure of 0.5 atm to 1.5 atm.

16. The method of claim 1 , wherein the Soxhlet extraction is performed by using an extraction solvent that has a vapor pressure of 100 kPa or more at 20° C.

17. The method of claim 1 , wherein the Soxhlet extraction is performed by using an extraction solvent that has a surface tension of 12 mN/m or less.

18. The method of claim 1 , wherein the Soxhlet extraction is performed by using carbon dioxide or dimethyl ether as an extraction solvent.

19. The method of claim 1 , wherein the Soxhlet extraction is performed in a pressure of 40 bar to 70 bar by using carbon dioxide as an extraction solvent.

20. The method of claim 1 , wherein the Soxhlet extraction is performed in a pressure of 5 bar to 20 bar by using dimethyl ether as an extraction solvent.

21. The method of claim 1 , wherein the Soxhlet extraction is performed by using a non-polar extraction solvent that has a surface tension of 0.1 mN/m to 12 mN/m.

22. The method of claim 1 , wherein the hydrophobic silica aerogel is a powder.

23. The method of claim 22 , wherein the hydrophobic silica aerogel powder has a specific surface area of 650 m 2 /g to 720m 2 /g.

24. The method of claim 22 , wherein the hydrophobic silica aerogel powder has a tap density of 0.09 g/ml to 0.24 g/ml.

25. The method of claim 22 , wherein the hydrophobic silica aerogel powder is composited with fibers to form a blanket.

Assignees

• Lg Chemical Ltd

Inventors

• Oh Kyoung Shil
• Oh Jin Hee
• Kim Ye Hon
• Cho Dong Hyun
• Kim Mi Ri
• Yu Sung Min
• Lee Je Kyun

Classifications

• C01B33/1585 Primary

  Dehydration into aerogels · CPC title

• C01B33/159

  Coating or hydrophobisation · CPC title

• C01P2006/11

  Powder tap density · CPC title

• C01B33/16

  Preparation of silica xerogels · CPC title

• C01P2006/12

  Surface area · CPC title