# US 2016/0258153 A1 · Process for the Production of an Aerogel Material

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- Number: US 2016/0258153 A1
- Document ID: US20160258153A1
- Status: Published application
- Kind: A1
- Application number: 14/908,601
- Filed: 2014-07-28
- Published: 2016-09-08
- Earliest claimed: 2013-08-02
- Assignees: Empa EidgenöSsische MaterialprüFungs- Und Forschungsanstalt
- Applicants: Empa EidgenöSsische MaterialprüFungs-Und Forschungsanstalt
- Inventors: Matthias KOEBEL; Shanyu ZHAO; Samuel BRUNNER; Caroline SIMMEN
- Web page: https://patentgrep.com/patent/US20160258153A1

## CPC

- E04B 1/78: Heat insulating elements {(E04B1/7662 takes precedence)}
- C01B 33/145: Preparation of hydroorganosols, organosols or dispersions in an organic medium
- C01B 33/155: Preparation of hydroorganogels or organogels
- C01B 33/1585: {Dehydration into aerogels}
- E04B: GENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS (border constructions of opening in walls, floors or ceilings E06B1/00; {electromagnetic shielding H05K9/0001})
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}

## Abstract

A process for the production of an aerogel material comprises the following steps: a) preparation of a silicon oxide sol in an alcoholic solvent mixture; b) triggering of the gelation of the sol by adding base, whereby a gel is formed, and optionally aging of the gel; c) hydrophobicization of the optionally aged gel; d) removal of the solvent mixture by subcritical drying, whereby the aerogel material is formed. The silicon oxide sol formed in step a) comprises at least one acid-catalytically activatable hydrophobicization agent, wherein the volume fraction of the hydrophobicization agent in the sol is 5 to 60%. The hydrophobicization in step c) is induced as a result of release or addition of at least one hydrophobicization catalyst acting in combination with the hydrophobicization agent.

## Claims

### Claim 1

A process for the production of an aerogel material, comprising the following steps:
a) preparation of a silicon oxide sol in an alcoholic solvent mixture;
b) triggering of the gelation of the sol by adding base, whereby a gel is formed, and optionally aging of the gel;
c) hydrophobicization of the optionally aged gel;
d) removal of the solvent mixture by subcritical drying, whereby the aerogel material is formed;
characterized in that the silicon oxide sol formed in step a) comprises at least one acid-catalytically activatable hydrophobicization agent, where the volume fraction of the hydrophobicization agent in the sol is 5 to 60%, and that the hydrophobicization in step c) is induced as a result of release or addition of at least one hydrophobicization catalyst acting in combination with the hydrophobicization agent.

### Claim 2 (depends on 1)

The process according to claim 1, wherein the catalytically activatable hydrophobicization agent is hexamethyldisiloxane (HMDSO).

### Claim 3 (depends on 1)

The process according to claim 1, wherein the volume fraction of the hydrophobicization agent in the sol is 20 to 50%, in particular 25% to 40% and more particularly 34% to 38%.

### Claim 4 (depends on 1)

The process according to claim 1, wherein the hydrophobicization catalyst is formed by a radical decomposition reaction in situ in the gel.

### Claim 5 (depends on 1)

The process according to claim 1, wherein the hydrophobicization catalyst is released by slow-release agents in the gel and optionally by thermal activation.

### Claim 6 (depends on 1)

The process according to claim 1, wherein the hydrophobicization catalyst is gaseous HCl.

### Claim 7 (depends on 1)

The process according to claim 1, wherein the hydrophobicization catalyst is trimethylchlorosilane (TMCS) and/or HCl in an alcoholic solution.

### Claim 8 (depends on 1)

The process according to claim 1, wherein the sol further comprises at least one functional silane.

### Claim 9 (depends on 1)

The process according to claim 1, wherein the sol further comprises at least one polymerizable monomer.

### Claim 10 (depends on 1)

The process according to claim 1, wherein the step c) and optionally an initial phase of step d) are performed at overpressure.

### Claim 11 (depends on 1)

The process according to claim 1, wherein the step d) is performed at reduced pressure.

### Claim 12 (depends on 1)

The process according to claim 1, wherein the sol is added to a fiber-based matrix after initiation of gelation.

### Claim 13 (depends on 1)

The process according to claim 1, wherein at least the steps b) and c) are performed in a continuous process.

### Claim 14 (depends on 1)

Insulant panel, formed from an aerogel material produced according to claim 1.

### Claim 15

A precursor product for producing an aerogel material, comprising a silicon oxide sol and/or a silicon oxide gel in an alcoholic solvent mixture and at least one acid-catalytically activatable hydrophobicization agent.

### Claim 16 (depends on 2)

The process according to claim 2, wherein the volume fraction of the hydrophobicization agent in the sol is 20 to 50%, in particular 25% to 40% and more particularly 34% to 38%.

### Claim 17 (depends on 2)

The process according to claim 2, wherein the hydrophobicization catalyst is formed by a radical decomposition reaction in situ in the gel.

### Claim 18 (depends on 3)

The process according to claim 3, wherein the hydrophobicization catalyst is formed by a radical decomposition reaction in situ in the gel.

### Claim 19 (depends on 2)

The process according to claim 2, wherein hydrophobicization catalyst is released by slow-release agents in the gel and optionally by thermal activation.

### Claim 20 (depends on 3)

The process according to claim 3, wherein the hydrophobicization catalyst is released by slow-release agents in the gel and optionally by thermal activation.
