Method of preparing hydrophobic silica aerogel and hydrophobic silica aerogel prepared thereby

Patent metadata

Field	Value
Publication number	US-10294111-B2
Application number	US-201615527663-A
Country	US
Kind code	B2
Filing date	Nov 4, 2016
Priority date	Nov 27, 2015
Publication date	May 21, 2019
Grant date	May 21, 2019

Abstract

The present invention relates to a method of preparing a high hydrophobic silica aerogel having a low tap density and a hydrophobic silica aerogel prepared thereby. The method of preparing a hydrophobic silica aerogel according to the present invention may have good productivity and economic efficiency, because preparation time is reduced by simultaneously performing surface modification and solvent substitution in a single step, and may control a degree of hydrophobicity of the prepared silica aerogel by controlling a surface modification reaction by including a step of adding ammonium hydroxide. Thus, a hydrophobic silica aerogel having excellent physical properties, such as tap density and specific surface area, as well as high hydrophobicity obtained by controlling the degree of hydrophobicity may be prepared.

First claim

The invention claimed is:

1. A method of preparing a hydrophobic silica aerogel, the method comprising steps of:
(1) adding a water glass solution and an acid catalyst to a reactor and performing a reaction to prepare a silica wet gel;
(2) adding an inorganic acid and a surface modifier solution to the silica wet gel and performing a surface modification reaction comprising adding ammonium hydroxide after an entire amount of the surface modifier solution is added to prepare a hydrophobic silica wet gel; and
(3) drying the hydrophobic silica wet.

2. The method of claim 1 , wherein the water glass solution contains 1 wt % to 11 wt % of silicon dioxide (SiO 2 ).

3. The method of claim 1 , wherein the acid catalyst is used present in a molar ratio of 0.2 to 1.5 based on water glass in the water glass solution.

4. The method of claim 1 , wherein aging is performed after the reaction of step 1, and
wherein the aging is performed by maintaining at a temperature of 50° C. to 90° C. for 1 hour to 10 hours.

5. The method of claim 1 , wherein the silica wet gel is milled before adding the inorganic acid in step 2.

6. The method of claim 1 , wherein the surface modifier solution is prepared by adding a surface modifier to a non-polar organic solvent and mixing together, and
a concentration of the surface modifier in the surface modifier solution is in a range of 0.1 M to 4 M.

7. The method of claim 6 , wherein the surface modifier comprises at least one selected from the group consisting of trimethylchlorosilane (TMCS), hexamethyldisilazane (HMDS), methyltrimethoxysilane, and trimethylethoxysilane, and
wherein the non-polar organic solvent comprises at least one selected from the group consisting of hexane, heptane, toluene, and xylene.

8. The method of claim 1 , wherein the surface modifier solution is added in an amount such that a molar ratio of a surface modifier to water glass in the water glass solution is in a range of 0.07 to 2.

9. The method of claim 1 , wherein the surface modifier solution is added when the inorganic acid is added to the silica wet gel and a temperature in the reactor reaches 25° C. to 95° C.

10. The method of claim 1 , wherein, after an entire amount of the surface modifier solution is added, the ammonium hydroxide is added when a pH in the reactor reaches 5 to 10.

11. The method of claim 1 , wherein the ammonium hydroxide is added in an amount such that a pH in the reactor after the addition of the ammonium hydroxide is increased by 5% to 57% in comparison to a pH in the reactor before the addition of the ammonium hydroxide.

12. The method of claim 1 , wherein the ammonium hydroxide is added in an amount such that a molar ratio of the ammonium hydroxide to a surface modifier in the surface modifier solution is in a range of 0.5 to 25.

13. The method of claim 1 , further comprising washing the hydrophobic silica wet gel before the drying of step (3), and
wherein the washing is performed by a dilution process or an exchange process using a non-polar solvent.

Assignees

• Lg Chemical Ltd

Inventors

• Kim Young Hun
• Oh Jin Hee
• Lee Je Kyun

Classifications

• C01B33/159 Primary

  Coating or hydrophobisation · CPC title

• C01B33/154 Primary

  by acidic treatment of aqueous silicate solutions · CPC title

• C09C1/3018

  Grinding · CPC title

• C09C1/3081

  Treatment with organo-silicon compounds · CPC title

• C01P2006/11

  Powder tap density · CPC title