IP Library › Granted Patent US 10,940,670
Granted Patent B2
US 10,940,670 · App. 15/570,568 · Granted Mar 9, 2021

Aerogel composite and method for preparing same

Inventor: Hyun-Chol Kim (Seoul, KR)
Assignee: SKC CO., LTD.
B32B5/28B29C70/305B32B5/24B32B37/02B32B38/08B32B38/10B32B38/162B32B38/164B32B43/006C01B33/1585B32B2038/0056B32B2307/304
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Quick Facts
Patent No.
US 10,940,670
App. No.
15/570,568
Granted
Mar 9, 2021
Kind
B2
Abstract

A method of preparing an aerogel composite, which includes a wetting pretreatment step for suppressing the generation of air bubbles in a fibrous material such as a mat, and a step of impregnating the fibrous material with a precursor by injecting the precursor in a vessel under a reduced pressure. The method provides a high quality, high insulation aerogel-impregnated composite without air bubbles.

Claims (50)

1. A method of preparing an aerogel composite, the method comprising:

wetting a fibrous material including at least one of inorganic fibers and organic fibers;

winding the wetted fibrous material with a separator in a roll form or laminating the wetted fibrous material with the separator in a planar form;

charging the fibrous material into a vessel;

preparing a gel-fiber composite by injecting a precursor into the vessel and gelating the precursor while removing residual air bubbles under vacuum;

taking out the gel-fiber composite from the vessel and removing the separator;

solvent substituting and organically surface-modifying the gel-fiber composite; and

atmospheric pressure drying the organically surface-modified gel-fiber composite,

wherein the organic surface modification is performed by using a mixture of silane and alkoxysilane as a treatment agent,

wherein a mixing ratio by weight of the silane to the alkoxysilane is in a range of 1:0.01 to 1:0.3, and

wherein the treatment agent for the organic surface modification further includes an opacifying agent selected from the group consisting of Al 2 O 3 , Fe 2 O 3 , TiO 2 , Carbon, graphite, SiC, a boron compound, and a mixture thereof.

2. The method of claim 1 , wherein the inorganic fibers comprise at least one selected from the group consisting of glass fibers, glass wool, rock wool, ceramic wool, and boron fibers; and

the organic fibers comprise at least one selected from the group consisting of nylon, aramid fibers, carbon fibers, polypropylene fibers, polyethylene fibers, polyester fibers, polyurethane fibers, acrylic fibers, polyvinyl chloride acetate fibers, rayon fibers, regenerated fibers, and waste fibers.

3. The method of claim 1 , wherein the wetting is performed by using at least one wetting agent selected from:

(i) at least one acid selected from the group consisting of sulfuric acid, nitric acid, hydrochloric acid, acetic acid, and hydrofluoric acid in a pH range of 1 to 5;

(ii) at least one water-soluble solvent selected from the group consisting of C1-C4 alcohol, acetone, ethylene glycol, glycol ethers, dimethylformamide (DMF), and tetrahydrofuran (THF); and

(iii) at least one surfactant selected from the group consisting of sodium fatty acid, sodium alkylbenzenesulfonic acid, linear alkylbenzene sulfonate (LAS), polyacrylamide, polyoxyethylene alkylamine, dialkyldimethyl ammonium salt, alkylbenzylmethyl ammonium salt, polyoxyethylene alkyl ether, fatty acid sorbitan ester, fatty acid diethanolamine, alkylmonoglyceryl ether, alkyl sulfobetaine, and alkyl carboxybetaine.

4. The method of claim 1 , wherein the separator is formed by treating a material, which is selected from the group consisting of stainless steel, a rubber membrane, a magnesium sheet, an aluminum sheet, polyvinyl chloride (PVC), polyethylene (PE), polyester, polypropylene (PP), polystyrene (PS), nylon, and a mixture material thereof, to allow a fluid to penetrate and permeate thereinto.

5. The method of claim 1 , wherein the precursor is a sol of sodium silicate, potassium silicate, or lithium silicate in a pH range of 3 to 7, or is tetraethoxysilane hydrolyzed by an acid catalyst.

6. A method of preparing an aerogel composite, the method comprising:

providing a fibrous material including at least one of inorganic fibers and organic fibers;

wetting the fibrous material;

charging the wetted fibrous material into a vessel;

impregnating the fibrous material with a precursor by injecting the precursor into the vessel after reducing a pressure in the vessel;

preparing a gel-fiber composite by gelation of the precursor;

substituting a solvent included in a gel of the gel-fiber composite and organically modifying an inner surface of the gel; and

atmospheric pressure drying the gel-fiber composite,

wherein the organic modification of inner surface of the gel is performed by using a mixture of silane and alkoxysilane as a treatment agent,

wherein a mixing ratio by weight of the silane to the alkoxysilane is in a range of 1:0.01 to 1:0.3, and

wherein the treatment agent for the organic surface modification further includes an opacifying agent selected from the group consisting of Al 2 O 3 , Fe 2 O 3 , TiO 2 , Carbon, graphite, SiC, a boron compound, and a mixture thereof.

7. The method of claim 6 , wherein a separator is inserted into the wetted fibrous material before the wetted fibrous material is charged into the vessel, and

the separator is removed after the gel-fiber composite is prepared.

8. The method of claim 7 , wherein the separator is wound with the wetted fibrous material in a roll form.

9. The method of claim 7 , wherein the separator and the wetted fibrous material are alternately stacked.

10. The method of claim 6 , wherein the solvent comprises water.

11. The method of claim 10 , wherein, before the fibrous material is impregnated with the precursor, a pressure in the vessel is reduced to a range of 0.001 Torr to 10 Torr.

12. The method of claim 6 , further comprising reducing a pressure in the vessel after the fibrous material is impregnated with the precursor.

13. The method of claim 12 , wherein, after the fibrous material is impregnated with the precursor, the pressure in the vessel is reduced to a range of 0.001 Torr to 10 Torr.

14. An aerogel composite comprising:

a fibrous material including at least one of inorganic fibers and organic fibers; and

an aerogel disposed in the fibrous material,

wherein, in a cutting surface of the aerogel composite, the number of pores having a diameter of 10 μm to 5 mm in an area of 1,500 mm 2 is 10 or less,

wherein, after the sol of the sodium silicate, potassium silicate, or lithium silicate is impregnated into the fibrous material under vacuum and gelated, the aerogel is prepared by solvent substitution and organic modification of an inner surface of the gel, and

wherein the organic modification of an inner surface of the gel is performed by using a mixture of silane and alkoxysilane as a treatment agent,

wherein a mixing ratio by weight of the silane to the alkoxysilane is in a range of 1:0.01 to 1:0.3, and

wherein the treatment agent for the organic surface modification further includes an opacifying agent selected from the group consisting of Al 2 O 3 , Fe 2 O 3 , TiO 2 , Carbon, graphite, SiC, a boron compound, and a mixture thereof.

15. The aerogel composite of claim 14 , wherein the aerogel is formed from a sol of sodium silicate, potassium silicate, or lithium silicate.

16. The aerogel composite of claim 14 , wherein the number of the pores is 5 or less.

17. The aerogel composite of claim 14 , wherein the number of the pores is 3 or less.

18. The aerogel composite of claim 14 , wherein the number of the pores is 2 or less.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 6, 2017
From: KIM, HYUN-CHOL
To: SKC CO., LTD.
Reel/Frame 044043/0453 →
Priority Claims (1)
KR 10-2016-0014993 · Feb 5, 2016 · national
Continuity (1)
Related Publication 20180326700A1 · Nov 15, 2018
Cited By (2)
US 12,552,673 US 12,595,181