Gelled composition for an organic monolithic gel, uses thereof and process for preparing same

Patent metadata

Field	Value
Publication number	US-10363536-B2
Application number	US-201415120723-A
Country	US
Kind code	B2
Filing date	Mar 4, 2014
Priority date	Mar 4, 2014
Publication date	Jul 30, 2019
Grant date	Jul 30, 2019

Abstract

This composition is such that said polyhydroxybenzenes comprise several said unsubstituted polyhydroxybenzenes R and R′ and in that the composition comprises a water-soluble cationic polyelectrolyte P.

First claim

The invention claimed is:

1. A gelled carbon-based composition forming an organic polymeric monolithic gel which is capable of forming an aerogel by drying and a porous carbon monolith by pyrolysis of said aerogel,
wherein the composition comprises a resin derived at least partly from:
a first unsubstituted polyhydroxybenzene,
a premix comprising at least a second unsubstituted polyhydroxybenzene and at least one substituted polyhydroxybenzene substituted with one or more alkyl groups, and
formaldehyde(s),

wherein the composition comprises a water-soluble cationic polyelectrolyte.

2. The gelled composition as claimed in claim 1 , characterized in that the composition has a heat conductivity of less than or equal to 40 mW·m −1 ·K −1 .

3. The gelled composition as claimed in claim 1 , characterized in that the composition comprises a product of a mixing reaction, in an aqueous solvent:
of said first unsubstituted polyhydroxybenzene, and
of said premix comprising:
in minor amount by mass, said second unsubstituted polyhydroxybenzene, which is identical to or different from said first unsubstituted polyhydroxybenzene, and
in major amount by mass, said at least one substituted polyhydroxybenzene.

4. The gelled composition as claimed in claim 1 , characterized in that the composition is derived from said premix in equal or major amount by moles relative to said first unsubstituted polyhydroxybenzene, the [premix/(first unsubstituted polyhydroxybenzene+premix)] mole ratio in the composition being greater than or equal to 0.5 and less than 1.

5. The gelled composition as claimed in claim 4 , characterized in that said premix comprises, in a mass fraction of less than 10%, said second unsubstituted polyhydroxybenzene, and, in a mass fraction of greater than 80%, at least two said substituted polyhydroxybenzenes.

6. The gelled composition as claimed in claim 3 , characterized in that said first and second unsubstituted polyhydroxybenzenes are each a resorcinol, and in that the composition comprises at least two said substituted polyhydroxybenzenes comprising in major amount by mass methyl resorcinols and in minor amount by mass dimethyl resorcinols and an ethyl resorcinol.

7. The gelled composition as claimed in claim 6 , characterized in that said methyl resorcinols comprise in major amount by mass 5-methyl resorcinol and in minor amount by mass 4-methyl resorcinol and 2-methyl resorcinol, in that said dimethyl resorcinols comprise 2,5-dimethyl resorcinol and 4,5-dimethyl resorcinol, and in that said ethyl resorcinol is 5-ethyl resorcinol.

8. The gelled composition as claimed in claim 1 , characterized in that the composition has for said aerogel a density of less than or equal to 0.20 and a compression strength, defined for compression of a plate formed from said aerogel with a thickness equal to 9 mm along 50% of said thickness, which is greater than or equal to 0.15 MPa, or even 2 MPa.

9. The gelled composition as claimed in claim 1 , characterized in that it comprises the product of a polymerization reaction in an aqueous solvent of said polyhydroxybenzenes and formaldehyde(s), in the presence of said cationic polyelectrolyte dissolved in the solvent and of an acid catalyst, the product of the polymerization reaction comprising said cationic polyelectrolyte in a mass fraction of between 0.2% and 2%.

10. The gelled composition as claimed in claim 1 , characterized in that said water-soluble cationic polyelectrolyte is an organic polymer chosen from the group consisting of quaternary ammonium salts, poly(vinylpyridinium chloride), poly(ethyleneimine), poly(vinylpyridine), poly(allylamine hydrochloride), poly(trimethylammonium ethylmethacrylate chloride), poly(acrylamide-co-dimethylammonium chloride), and mixtures thereof.

11. The gelled composition as claimed in claim 10 , characterized in that said water-soluble cationic polyelectrolyte is a salt comprising units derived from a quaternary ammonium.

12. The gelled composition as claimed in claim 4 , characterized in that the [premix/(first unsubstituted polyhydroxybenzene+premix)] mole ratio in the composition is of between 0.6 and 0.8.

13. The gelled composition as claimed in claim 11 , characterized in that said water-soluble cationic polyelectrolyte is poly(diallyldimethylammonium chloride) or poly(diallyldimethylammonium bromide).

Assignees

• Hutchinson

Inventors

• Dufour Bruno
• Dorie Hugo
• Sonntag Philippe

Classifications

• C08J2361/12

  with polyhydric phenols · CPC title

• C08J3/075

  Macromolecular gels · CPC title

• E04B1/78

  Heat insulating elements {(E04B1/7662 takes precedence)} · CPC title

• C08G8/22

  Resorcinol · CPC title

• C01B32/05

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