Method for producing core-shell hybrid materials

Patent metadata

Field	Value
Publication number	US-11318442-B2
Application number	US-201816476166-A
Country	US
Kind code	B2
Filing date	Jan 8, 2018
Priority date	Jan 6, 2017
Publication date	May 3, 2022
Grant date	May 3, 2022

Abstract

A method for producing a core-shell hybrid material made of an activated carbon core surrounded by a mesoporous silica sol-gel shell, the method including the formation of a mesoporous silica sol-gel shell around activated carbon particles. Also, the core-shell hybrid material formed by the method, and its use as a filtering material in filtering systems.

First claim

The invention claimed is:

1. A method for preparing a core-shell hybrid material consisting of an active carbon core surrounded by a shell of a mesoporous sol-gel silica material, said method comprising the formation of a mesoporous sol-gel silica shell around active carbon particles.

2. The method as claimed in claim 1 , wherein the mesoporous sol-gel silica shell is formed from at least one organosilicon precursor chosen from tetramethoxysilane (TMOS), tetraethoxysilane (TEOS), phenyltrimethoxysilane (PhTMOS), phenyltriethoxysilane (PhTEOS), (2-phenylethyl)triethoxysilane, 3 aminopropyltriethoxysilane (APTES), (3-glycidyloxypropyl)trimethoxysilane (GPTMOS), (3-glycidyloxypropyl)triethoxysilane (GPTES), N-(2-aminoethyl)-3-(trimethoxysilyl)propylamine (NH2-TMOS), N (trimethoxysilylpropyl)ethylenediamine triacetate, acetoxyethyltrimethoxysilane (AETMS), ureidopropyltriethoxysilane (UPTS), 3-(4-semicarbazidyl)propyltriethoxysilane (SCPTS) and mixtures thereof.

3. The method as claimed in claim 1 , wherein the organosilicon precursor is tetramethoxysilane or tetraethoxysilane.

4. The method as claimed in claim 1 , wherein the organosilicon precursor is a mixture of tetramethoxysilane and of a functionalized organosilicon precursor, advantageously chosen from phenyltrimethoxysilane (PhTMOS), phenyltriethoxysilane (PhTEOS), (2-phenylethyl)triethoxysilane, 3-aminopropyltriethoxysilane (APTES), (3 glycidyloxypropyl)trimethoxysilane (GPTMOS), (3-glycidyloxypropyl)triethoxysilane (GPTES), N-(2-aminoethyl)-3-(trimethoxysilyl)propylamine (NH2-TMOS), N (trimethoxysilylpropyl)ethylenediamine triacetate, acetoxyethyltrimethoxysilane (AETMS), ureidopropyltriethoxysilane (UPTS), 3-(4-semicarbazidyl)propyltriethoxysilane (SCPTS) and mixtures thereof.

5. The method as claimed in claim 1 , wherein the formation of the mesoporous sol-gel silica shell around active carbon particles comprises:
a) the formation of a sol-gel nanoparticle shell around active carbon in a basic aqueous solution starting from at least one organosilicon precursor, the aqueous solution containing aqueous ammonia (NH4OH) and a surfactant,
b) the recovery of the active carbon surrounded by the sol-gel material shell prepared in step a),
c) the elimination of any surfactant residues from the active carbon surrounded by the sol-gel material shell so as to free the pores of the sol-gel material formed in step a),

and wherein, in step a), a basic aqueous solution containing aqueous ammonia, the surfactant and the active carbon is first provided, then the at least one organosilicon precursor is added, this precursor being solubilized in an organic solvent.

6. The method as claimed in claim 1 , wherein the organic solvent is chosen from C1 to C4 linear aliphatic alcohols.

7. The method as claimed in claim 1 , wherein the organic solvent is ethanol.

8. The method as claimed in claim 1 , wherein the active carbon is in powder form.

9. The method as claimed in claim 1 , wherein the surfactant is an ionic surfactant.

10. The method as claimed in claim 1 , wherein the surfactant is cetyltrimethylammonium bromide.

11. The method as claimed in claim 1 , wherein the step of formation of the sol-gel silica nanoparticle shell comprises the preparation of a sol of a mixture of at least one organosilicon precursor in an aqueous solution containing an organic solvent, followed by the coating of the active carbon with this sol.

12. The method as claimed in claim 1 , wherein the active carbon is in the form of rods of millimetric size and the coating of said active carbon is carried out by dipping the rods in the sol then removing them from the sol or by pouring the sol over the rods through a sieve.

13. The method as claimed in claim 1 , wherein the active carbon is in powder form and the coating is carried out by adding the active carbon powder to the sol, then the mixture obtained is poured into molds.

Assignees

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

Inventors

• Tran-Thi Thu-Hoa
• Theron Christophe
• Bamogo William
• Nguyen Trung-Hieu

Classifications

• C02F1/283

  using coal, charred products, or inorganic mixtures containing them · CPC title

• C02F1/288

  using composite sorbents, e.g. coated, impregnated, multi-layered · CPC title

• B01J20/3225

  involving a post-treatment of the coated or impregnated product · CPC title

• B01J20/28047

  Gels · CPC title

• B01J20/28023

  Fibres or filaments (fibres or filaments in the form of membranes B01J20/28038; B01J20/28007 takes precedence) · CPC title