Gelled aqueous polymer composition, pyrolysed carbonated composition produced therefrom for a supercapacitor electrode, and methods for the production thereof

Patent metadata

Field	Value
Publication number	US-10629388-B2
Application number	US-201515316775-A
Country	US
Kind code	B2
Filing date	Jun 10, 2015
Priority date	Jun 11, 2014
Publication date	Apr 21, 2020
Grant date	Apr 21, 2020

Abstract

The invention relates to a gelled aqueous polymer composition for forming, by means of drying then pyrolysis, a monolithic porous carbon, to a pyrolysed carbonated composition produced by the drying, followed by the pyrolysis, of said gelled composition, to a porous carbon electrode for a supercapacitor comprising said pyrolysed composition, and to methods for producing said respectively gelled and pyrolysed compositions. A gelled composition according to the invention, produced from the polycondensation of polyhydroxybenzene(s) and hexymethylenetetramine, is such that the hexymethylenetetramine comprised therein represents a mass fraction of between 7% and 15% inclusive. Said gelled composition is produced by a) polycondensation in an aqueous solvent of the polyhydroxybenzene(s) and hexymethylenetetramine, followed by b) gelling by heating of said polycondensate.

First claim

The invention claimed is:

1. A gelled aqueous polymer composition capable of forming, by drying and then pyrolysis, a monolithic porous carbon, the composition comprising the product of a polycondensation reaction in an aqueous solvent W of polyhydroxybenzene(s) R and hexamethylenetetramine H,
wherein
the polycondensation reaction is performed with polyhydroxybenzene(s) R and hexamethylenetetramine H as sole monomers, without a catalyst and without formaldehyde, such that an H/(R+H+W) fraction by weight is from 7% to 15% inclusive.

2. The gelled composition of claim 1 , wherein the H/(R+H+W) fraction by weight is from 10% to 14% inclusive.

3. The gelled composition of claim 1 , wherein a R/H molar ratio of the polyhydroxybenzene(s) R and the hexamethylenetetramine H in the polycondensation reaction is from 2 to 4 inclusive.

4. The gelled composition of claim 1 , wherein a R/W ratio of the polyhydroxybenzene(s) R and the aqueous solvent W in the polycondensation reaction is from 0.07 to 1 inclusive.

5. The gelled composition of claim 1 , wherein the composition is devoid of any amphiphilic polymer, any hydrophobic compound, or any mixture thereof.

6. The gelled composition of claim 1 , wherein:
the aqueous solvent W is water and the polyhydroxybenzene(s) R is resorcinol.

7. A process for preparing the gelled composition of claim 1 , the process comprising:
a) performing a polycondensation reaction in an aqueous solvent W of polyhydroxybenzene(s) R and hexamethylenetetramine H in order to obtain a polycondensate in an aqueous medium; and then
b) a gelling by heating the polycondensate, in order to obtain the gelled composition;
wherein
the polycondensation reaction is performed with polyhydroxybenzene(s) R and hexamethylenetetramine H as sole monomers, without a catalyst and without formaldehyde, such that an H/(R+H+W) fraction by weight is from 7% to 15% inclusive.

8. The process of claim 7 , comprising:
a1) dissolving the polyhydroxybenzene(s) R in a first portion of the aqueous solvent W, in order to obtain a first aqueous solution;
a2) dissolving by heating the hexamethylenetetramine H in a second portion of the aqueous solvent, in order to obtain a second aqueous solution; and
a3) contacting the first aqueous solution with the second aqueous solution, until a third homogeneous aqueous solution comprising the polycondensate is obtained.

9. A gelled aqueous polymer composition capable of forming, by drying and then pyrolysis, a monolithic porous carbon, wherein the composition consists of the product of a polycondensation reaction in an aqueous solvent W of polyhydroxybenzene(s) R and hexamethylenetetramine H,
wherein the polycondensation reaction is performed with polyhydroxybenzene(s) R and hexamethylenetetramine H as sole monomers, without a catalyst and without formaldehyde, such that an H/(R+H+W) fraction by weight is from 7% to 15% inclusive.

Assignees

• Hutchinson

Inventors

• Dorie Hugo
• Ayme-Perrot David
• Sonntag Philippe
• Dufour Bruno

Classifications

• C01P2006/12

  Surface area · CPC title

• H01G11/32

  Carbon-based · CPC title

• C01B32/05

  Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30 · CPC title

• C01P2006/16

  Pore diameter · CPC title

• Y02E60/13

  Energy storage using capacitors · CPC title