Method of preparing metal oxide-silica composite aerogel and metal oxide-silica composite aerogel prepared thereby

Patent metadata

Field	Value
Publication number	US-10792650-B2
Application number	US-201615533936-A
Country	US
Kind code	B2
Filing date	Oct 19, 2016
Priority date	Oct 22, 2015
Publication date	Oct 6, 2020
Grant date	Oct 6, 2020

Abstract

The present invention relates to a method of preparing an ultra-light metal oxide-silica composite aerogel having high specific surface area and high pore volume and a metal oxide-silica composite aerogel prepared thereby. The preparation method according to the present invention may not only have good economic efficiency because production costs are relatively reduced in comparison to the related art, but may also effectively prevent the collapse of a pore structure by suppressing a shrinkage phenomenon during drying, and thus, a metal oxide-silica composite aerogel having ultra-light properties as well as high porosity characteristics, such as high specific surface area and high pore volume, may be prepared.

First claim

The invention claimed is:

1. A method of preparing a metal oxide-silica composite aerogel, the method comprising steps of:
(1) adding a metal ion solution having a concentration of metal ions in a range of 0.125 M to 1.0 M and comprising a first acid catalyst to a first water glass solution having a concentration of water glass in a range of 0.125 M to 1.0 M and performing a primary reaction to prepare a metal oxide-silica composite agglomerate;
(2) adding a second water glass solution having a concentration of water glass in a range of 0.5 M to 3.0 M to the agglomerate and a second acid catalyst and performing a secondary reaction to prepare a metal oxide-silica composite wet gel; and
(3) drying the metal oxide-silica composite wet gel,
wherein the second water glass solution of step (2) is added in an amount of 5 vol % to 500 vol % based on 100 vol % of the first water glass solution.

2. The method of claim 1 , wherein the metal ion solution is a binary metal ion solution including calcium ions (Ca 2+ ) and magnesium ions (Mg 2+ ).

3. The method of claim 2 , wherein a molar ratio of the calcium ion (Ca 2+ ) to the magnesium ion (Mg 2+ ) in the metal ion solution is in a range of 1:0.3 to 1:3.0.

4. The method of claim 1 , wherein the metal ion solution is added so that a volume ratio of the first water glass solution to the metal ion solution is in a range of 5:1 to 1:5.

5. The method of claim 1 , wherein the primary reaction of step (1) is performed in a pH range of 4 to 7, and
wherein the secondary reaction is performed in a pH range of 4 to 6.

6. The method of claim 1 , wherein the second water glass solution of step (2) is added in an amount of 20 vol % to 200 vol % based on 100 vol % of the first water glass solution.

7. The method of claim 1 , wherein the second water glass solution and the second acid catalyst of step (2) are sequentially added,
wherein the second acid catalyst is added in an amount such that a pH value after the addition of the second acid catalyst is reduced by 40% to 65% of a pH value before the addition of the second acid catalyst.

8. The method of claim 1 , further comprising adding a third water glass solution and a third acid catalyst and performing a tertiary reaction after step (2),
wherein the third water glass solution is added so that a total amount of the third water glass solution and the second water glass solution is in a range of 20 vol % to 200 vol % based on 100 vol % of the first water glass solution,
wherein a water glass concentration in the third water glass solution is in a range of 0.5 M to 3.0 M.

9. The method of claim 8 , wherein the third water glass solution and the third acid catalyst are sequentially added,
wherein third acid catalyst is added in an amount such that a pH value after the addition of the third acid catalyst is reduced by 40% to 65% of a pH value before the addition of the third acid catalyst.

10. The method of claim 1 , wherein the drying of step (3) is performed by atmospheric pressure drying at a temperature of 100° C. to 190° C. for 1 hour to 4 hours.

Assignees

• Lg Chemical Ltd

Inventors

• Kim Jong Hun
• Jeon Hyun Woo
• Lee Je Kyun

Classifications

• C01B33/158 Primary

  Purification; Drying; Dehydrating · CPC title

• B01J31/02

  containing organic compounds or metal hydrides · CPC title

• C01B33/1585 Primary

  Dehydration into aerogels · CPC title

• C01P2006/16

  Pore diameter · CPC title

• C01P2006/14

  Pore volume · CPC title