Method of preparing metal oxide-silica composite aerogel and metal oxide-silica composite aerogel prepared by using the same

Patent metadata

Field	Value
Publication number	US-10526207-B2
Application number	US-201615577742-A
Country	US
Kind code	B2
Filing date	Jun 1, 2016
Priority date	Jun 1, 2015
Publication date	Jan 7, 2020
Grant date	Jan 7, 2020

Abstract

Provided are a method of preparing a metal oxide-silica composite aerogel, which includes preparing metal oxide-silica composite precipitates by adding a metal salt solution to a silicate solution and performing a reaction, and drying the metal oxide-silica composite precipitates by irradiation with infrared rays in a wavelength range of 2 μm to 8 μm, and a metal oxide-silica composite aerogel having excellent physical properties, such as low tap density and high specific surface area, as well as excellent pore properties prepared by the method.

First claim

The invention claimed is:

1. A method of preparing a metal oxide-silica composite aerogel, the method comprising:
preparing metal oxide-silica composite precipitates by adding a metal salt solution to a silicate solution and performing a reaction; and
drying the metal oxide-silica composite precipitates by irradiation with infrared rays having a wavelength in a range of 2 μm to 8 μm in an apparatus equipped with a middle range infrared ray (MIR) lamp that generates the infrared rays at an intensity such that a temperature within the apparatus is in a range of 130−300° C.

2. The method of claim 1 , wherein the drying is performed by irradiation with infrared rays in a wavelength range in which the infrared rays resonate with a water molecule or a hydroxy group in a solvent used during preparation of the silicate solution and the metal salt solution.

3. The method of claim 1 , wherein the drying is performed by irradiation with infrared rays in a wavelength range of 2 μm to 4 μm.

4. The method of claim 1 , further comprising performing an additional drying process at a temperature in a range of 130° C. to 300° C., after the drying by the infrared irradiation.

5. The method of claim 1 , wherein the silicate solution is prepared by dissolving water glass at a concentration of 0.125 M to 3.0 M.

6. The method of claim 1 , wherein the metal salt solution has a metal ion concentration of 0.125 M to 3.0 M.

7. The method of claim 1 , wherein the metal salt comprises chloride including at least one metal selected from the group consisting of alkali metals, alkaline earth metals, lanthanides, actinides, transition metals, and Group 13 (IIIA) metals.

8. The method of claim 1 , wherein the metal salt comprises one selected from the group consisting of MgCl 2 and CaCl 2 ), or a mixture thereof.

9. The method of claim 1 , wherein the metal salt comprises MgCl 2 and CaCl 2 ) in amounts such that a molar ratio of magnesium ions to calcium ions is in a range of 1:2 to 2:1.

10. The method of claim 1 , wherein the reaction of the silicate solution with the metal salt solution is performed in a pH range of 3 to 9.5.

11. The method of claim 1 , wherein the reaction is performed in a pH range of 5 or more to less than 7.5 by further adding an acid catalyst during the reaction of the silicate solution with the metal salt solution.

12. The method of claim 11 , wherein the acid catalyst is hydrochloric acid.

13. The method of claim 1 , further comprising washing the metal oxide-silica composite precipitates using a washing solvent before the drying,
wherein the washing solvent comprises one selected from the group consisting of water, an alcohol-based compound, a hydrocarbon-based compound, and a ketone-based compound, or a mixture of two or more thereof.

14. The method of claim 13 , wherein the washing solvent comprises the alcohol-based compound.

15. A metal oxide-silica composite aerogel prepared by the method of claim 1 .

16. The metal oxide-silica composite aerogel of claim 15 , wherein the metal oxide-silica composite aerogel has an average particle diameter (D 50 ) of 7 μm to 15 μm, a tap density of 0.055 g/ml or less, and a Brunauer-Emmett-Teller (BET) specific surface area of 450 m 2 /g or more.

Assignees

• Lg Chemical Ltd

Inventors

• Kim Jong Hun
• Choi Jae Hoon
• Lee Je Kyun

Classifications

• B01J13/0091 Primary

  Preparation of aerogels, e.g. xerogels · CPC title

• C01B13/363

  Mixtures of oxides or hydroxides by precipitation · CPC title

• C01B13/185

  Preparing mixtures of oxides · CPC title

• C01P2006/11

  Powder tap density · CPC title

• C01P2006/12

  Surface area · CPC title