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

Patent metadata

Field	Value
Publication number	US-10556800-B2
Application number	US-201615743643-A
Country	US
Kind code	B2
Filing date	Dec 8, 2016
Priority date	Dec 9, 2015
Publication date	Feb 11, 2020
Grant date	Feb 11, 2020

Abstract

The present invention relates to a method of preparing a metal oxide-silica composite aerogel containing a high ratio of a metal oxide and a metal oxide-silica composite aerogel prepared thereby. The method of preparing a metal oxide-silica composite aerogel according to the present invention may adjust a metal oxide ratio to a high level while easily forming a uniform network structure by performing a primary reaction under an acidic condition and a secondary reaction under a basic condition, and thus, since the prepared metal oxide-silica composite aerogel may contain a high ratio of the metal oxide, mechanical properties may not only be excellent, but high specific surface area and low tap density characteristics may also be exhibited.

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 to a water glass solution and performing a primary reaction to prepare a metal oxide-silica composite agglomerate;
(2) adding a base catalyst to the agglomerate 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 primary reaction is performed under a condition in which pH<7.07, and
the secondary reaction is performed under a condition in which pH>7.07,
wherein the primary reaction and the secondary reaction are performed under a condition satisfying Equation 1:
4≤ X−Y< 6  [Equation 1]

wherein, in Equation 1, X is the pH in the secondary reaction, and Y is the pH in the primary reaction.

2. The method of claim 1 , wherein a concentration of water glass in the water glass solution is in a range of 0.125 M to 3.0 M.

3. The method of claim 1 , wherein a concentration of metal ions in the metal ion solution is in a range of 0.125 M to 3.0 M.

4. 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+ ).

5. The method of claim 4 , 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.

6. The method of claim 1 , wherein the metal ion solution comprises an acid catalyst.

7. The method of claim 6 , wherein the acid catalyst comprises at least one selected from the group consisting of hydrochloric acid, nitric acid, acetic acid, sulfuric acid, and hydrofluoric acid.

8. The method of claim 1 , wherein the metal ion solution is added so that a molar ratio of silicon in the water glass solution to metal ions in the metal ion solution is in a range of 1:0.3 to 1:2.5.

9. The method of claim 1 , wherein the primary reaction is performed in a pH range of 4 to 7.

10. The method of claim 1 , wherein the secondary reaction is performed in a pH range of 8.5 to 10.

11. The method of claim 1 , wherein the pH of the secondary reaction is adjusted by the base catalyst.

12. The method of claim 1 , wherein the base catalyst comprises at least one selected from the group consisting of sodium hydroxide, ammonia, and potassium hydroxide.

13. 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.

14. A metal oxide-silica composite aerogel prepared by the method of claim 1 , wherein the metal oxide comprises calcium oxide (CaO) and magnesium oxide (MgO).

15. The metal oxide-silica composite aerogel of claim 14 , wherein a molar ratio of silicon (Si) in the aerogel to metallic elements is in a range of 1:0.2 to 1:2.0.

16. The metal oxide-silica composite aerogel of claim 14 , wherein the aerogel comprises 15 wt % to 60 wt % of the metal oxide.

17. The metal oxide-silica composite aerogel of claim 14 , wherein the aerogel has a specific surface area of greater than 150 m 2 /g and equal to or less than 500 m 2 /g.

18. The metal oxide-silica composite aerogel of claim 14 , wherein the aerogel has a tap density of 0.07 g/ml to 0.30 g/ml.

Assignees

• Lg Chemical Ltd

Inventors

• Kim Jong Hun
• Lee Je Kyun

Classifications

• C01B33/1585 Primary

  Dehydration into aerogels · CPC title

• C01F5/02

  Magnesia · CPC title

• C01P2006/11

  Powder tap density · CPC title

• C01F11/02

  Oxides or hydroxides (production of lime C04B2/00) · CPC title

• B01J31/0209

  Esters of carboxylic or carbonic acids · CPC title