Method for preparing a monolithic nanoporous silicate sol-gel material

Patent metadata

Field	Value
Publication number	US-11897776-B2
Application number	US-201917282536-A
Country	US
Kind code	B2
Filing date	Oct 4, 2019
Priority date	Oct 5, 2018
Publication date	Feb 13, 2024
Grant date	Feb 13, 2024

Abstract

A method for preparing a monolithic nanoporous silicate sol-gel material for modulating the pore size distribution for one single starting composition without the addition of a structuring agent. The method includes the following steps: a) synthesising a gel from at least one organosilylated precursor, the synthesis being carried out in an aqueous medium, optionally including an organic solvent and without a structuring agent, and b) drying the gel obtained in step a) at a temperature between 10° C. and 70° C., preferably between 15° C. and 55° C. and more preferably between 20° C. and 40° C., in a gas flow in a drying chamber to obtain a monolithic nanoporous silicate sol-gel material and a residual relative humidity in the drying chamber of between 0.1 and 20%, preferably between 0.5 and 10% and more preferably about 5%.

First claim

The invention claimed is:

1. A process for preparing monolithic nanoporous silicate sol-gel material, said process comprising the following steps:
a) synthesizing a gel from at least one organosilyl precursor, the synthesis being carried out in aqueous medium optionally comprising an organic solvent and without structuring agent,
b) drying the gel obtained in step a) at a temperature of between 10° C. and 70° C., in a stream of gas in a drying chamber until a monolithic nanoporous silicate sol-gel material is obtained and the residual relative humidity in the drying chamber is between 0.1% and 20%.

2. The process as claimed in claim 1 , wherein the drying step b) is carried out at a temperature of between 15° C. and 55° C.

3. The process as claimed in claim 1 , wherein the drying step b) is carried out at a temperature of between 20° C. and 40° C.

4. The process as claimed in claim 1 , wherein the residual relative humidity in the drying chamber in step b) is between 0.5% and 10%.

5. The process as claimed in claim 1 , wherein the residual relative humidity in the drying chamber in step b) is about 5%.

6. The process as claimed in claim 1 , wherein the synthesis is carried out without acidic or basic catalyst.

7. The process as claimed in claim 1 , wherein the at least one organosilyl precursor is selected from tetramethoxysilane, tetraethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, a fluoroalkyltrimethoxysilane, a fluoroalkyltriethoxysilane, a chloroalkyltrimethoxysilane, a chloroalkyltriethoxysilane, an alkyltrimethoxysilane, an alkyltriethoxysilane, an aminopropyltriethoxysilane, an aminopropyltrimethoxysilane and mixtures thereof.

8. The process as claimed in claim 1 , wherein the organic solvent is a C 1 to C 6 aliphatic alcohol.

9. The process as claimed in claim 1 , wherein the organic solvent is methanol or ethanol.

10. The process as claimed in claim 1 , wherein the organic solvent is methanol.

11. The process as claimed in claim 1 , wherein the drying step is carried out in a stream of dry gas.

12. The process as claimed in claim 1 , wherein the drying step comprises applying a stream of wet gas, said wet gas having a relative humidity of 30% to 80%.

13. The process as claimed in claim 6 , wherein the drying step is carried out in stages, each stage comprising decreasing the relative humidity in the chamber to a predefined level of relative humidity.

14. The process as claimed in claim 1 , wherein the drying step is carried out at a temperature of between 15° C. and 25° C.

15. The process as claimed in claim 1 , wherein the drying step is carried out at a temperature of about 20° C.

16. The process as claimed in claim 1 , wherein the drying step is carried out at a temperature of between 30° C. and 50° C.

17. The process as claimed in claim 1 , wherein the drying step is carried out at a temperature of about 40° C.

Assignees

• Commissariat Energie Atomique
• Centre National De La Rech Scientifique—Cnrs—

Inventors

• Tran Clarisse
• Tran-Thi Thu-Hoa
• Crunaire Sabine
• Wojkiewicz Jean-Luc

Classifications

• C01B33/155 Primary

  Preparation of hydroorganogels or organogels · CPC title

• B01J20/103

  comprising silica · CPC title

• B01J20/28047

  Gels · CPC title

• C01B33/158

  Purification; Drying; Dehydrating · CPC title

• C01B33/163 Primary

  by hydrolysis of organosilicon compounds, e.g. ethyl orthosilicate · CPC title