Method of manufacturing silica aerogel

Patent metadata

Field	Value
Publication number	US-12570535-B2
Application number	US-202118016527-A
Country	US
Kind code	B2
Filing date	Jul 23, 2021
Priority date	Jul 24, 2020
Publication date	Mar 10, 2026
Grant date	Mar 10, 2026

Abstract

Provided is a method of manufacturing a silica aerogel, which includes: (1) manufacturing a hydrogel composite; (2) washing the manufactured hydrogel composite with a washing solvent; and (3) drying the washed hydrogel composite, wherein, impurities are removed from the hydrogel composite in Step (2), and the washing solvent is heated to a temperature equal to or higher than the boiling point (b.p.) of the washing solvent.

First claim

The invention claimed is:

1 . A method of manufacturing a silica aerogel, comprising:
(1) manufacturing a hydrogel composite; (2) washing the manufactured hydrogel composite with a washing solvent; and (3) drying the washed hydrogel composite, wherein impurities are removed from the hydrogel composite in Step (2), and the washing solvent is heated to a temperature higher than the boiling point (b.p.) of the washing solvent, wherein the washing solvent after being heated has a temperature of 110° C. to 200° C., and wherein the washing solvent is a mixture comprising ethanol and water.

2 . The method of claim 1 , wherein the washing solvent is a mixed phase of a gaseous phase and a liquid phase.

3 . The method of claim 1 , wherein the washing solvent comprises 85% by volume to 99% by volume of ethanol.

4 . The method of claim 1 , wherein the washing solvent after being heated has a temperature of 80° C. to 120° C.

5 . The method of claim 1 , wherein the impurities comprise one or more selected from the group consisting of residues derived from a base catalyst used during the manufacturing of the hydrogel composite, residues derived from a surface modifying agent, and silica fine particles.

6 . The method of claim 5 , wherein the base catalyst comprises one or more selected from the group consisting of sodium hydroxide, potassium hydroxide, ammonium hydroxide (NH 4 OH), tetramethylammonium hydroxide (TMAH), tetraethylammonium hydroxide (TEAH), tetrapropylammonium hydroxide (TPAH), tetrabutylammonium hydroxide (TBAH), methylamine, ethylamine, isopropylamine, monoisopropylamine, diethylamine, diisopropylamine, dibutylamine, trimethylamine, triethylamine, triisopropylamine, tributylamine, choline, monoethanolamine, diethanolamine, 2-aminoethanol, 2-(ethyl amino) ethanol, 2-(methylamino) ethanol, N-methyl diethanolamine, dimethylaminoethanol, diethylaminoethanol, nitrilotriethanol, 2-(2-aminoethoxy) ethanol, 1-amino-2-propanol, triethanolamine, monopropanolamine, and dibutanolamine.

7 . The method of claim 5 , wherein the surface modifying agent comprises a silazane-based compound.

8 . The method of claim 5 , wherein the silica fine particles are silica aerogel particles detached from the hydrogel composite during the washing in Step (2) as an impurity generated during the manufacturing of the hydrogel composite.

9 . The method of claim 5 , wherein the residues derived from the base catalyst and the residues derived from surface modifying agent comprise ammonia (NH 3 ), ammonium ions (NH 4 + ), and a mixture thereof.

10 . The method of claim 1 , wherein a flow rate of the washing solvent is in a range of 10 mL/m 2 /min to 800 mL/m 2 /min.

11 . The method of claim 1 , wherein a volume flow ratio of the hydrogel composite and the washing solvent in Step (2) is in a range of 1:1 to 1:9.

12 . The method of claim 1 , wherein Step (2) is performed for 30 minutes to 200 minutes.

13 . The method of claim 1 , wherein Step (3) is performed by supercritical drying, ambient drying, or a combination of both.

14 . The method of claim 1 , further comprising:
recovering the waste washing solvent in Step (2) to form a recovered waste washing solution; and purifying the recovered waste washing solution.

15 . The method of claim 14 , wherein the purifying of the recovered waste washing solvent comprises:
introducing the recovered waste washing solvent into a purification column to purify the waste washing solvent to yield a purified washing solution; and reusing the purified washing solvent as the washing solvent in Step (2).

Assignees

• Lg Chemical Ltd

Inventors

• Kim Young Hun
• Kang Tae Gyeong
• Shin Joon Ho
• Baek Se Won
• Oh Kyoung Shil
• Park Sang Woo
• Yoo Sung Jin

Classifications

• C01B33/152

  Preparation of hydrogels · CPC title

• C01B33/159

  Coating or hydrophobisation · CPC title

• C01B33/158

  Purification; Drying; Dehydrating · CPC title

• C01B33/1585 Primary

  Dehydration into aerogels · CPC title