High-density microporous carbon and method for preparing same

Patent metadata

Field	Value
Publication number	US-2019127528-A1
Application number	US-201716094282-A
Country	US
Kind code	A1
Filing date	Apr 14, 2017
Priority date	Apr 18, 2016
Publication date	May 2, 2019
Grant date	—

Abstract

A gelled aqueous polymer composition made from a resin produced by polycondensation of at least: a polyhydroxybenzene R, preferably resorcinol, hexamethylenetetramine HMTA, an anionic polyelectrolyte PA, preferably phytic acid. An aerogel obtained by drying these microparticles, and porous carbon microspheres obtained from the gel microparticles by pyrolysis. A method for producing a polymerised aqueous gel, an aerogel and porous carbon microspheres. Electrodes and electrochemical cell prepared from the porous carbon particles.

First claim

1 - 20 . (canceled)

21 . A gelled aqueous polymeric composition based on a resin resulting from the polycondensation of at least the following monomers:
a polyhydroxybenzene R, hexamethylenetetramine HMTA, an anionic polyelectrolyte AP with a molar mass of less than or equal to 2000 g/mol.

22 . The composition as claimed in claim 21 , wherein the polyhydroxybenzene R is resorcinol.

23 . The composition as claimed in claim 21 , in which the anionic polyelectrolyte comprises nitrogen atoms or phosphorus atoms.

24 . The composition as claimed in claim 23 , in which the anionic polyelectrolyte is phytic acid HPhy.

25 . The composition as claimed in claim 21 in which the anionic polyelectrolyte comprises several carboxylic acid functional groups.

26 . The composition as claimed in claim 25 , in which the anionic polyelectrolyte is chosen from: citric acid, oxalic acid, fumaric acid, maleic acid, succinic acid, ethylenediaminetetraacetic acid, polyacrylic acids or polymethacrylic acids.

27 . The composition as claimed in claim 21 , which is in the form of gel microparticles in an aqueous medium.

28 . The composition as claimed in claim 21 , in which the monomers comprise at least one cationic polyelectrolyte.

29 . The composition as claimed in claim 21 , in which the AP/HMTA molar ratio is from 0.010 to 0.150.

30 . The composition as claimed in claim 21 , in which the ratio by weight R/W of the polyhydroxybenzene, to the aqueous medium conforms to:
0.01 ≤R/W≤ 2.

31 . The composition as claimed in claim 21 , in which the ratio by weight HMTA/W of the hexamethylenetetramine to the aqueous medium conforms to:
0.01≤HMTA/ W≤ 1.

32 . The composition as claimed in claim 21 , in which the molar ratio R/HMTA of the polyhydroxybenzene, to the HMTA conforms to:
2 ≤R /HMTA≤4.

33 . A process for the manufacture of a gelled aqueous polymeric composition as claimed in claim 21 , this process comprising the following stages:
a) the mixing in an aqueous solvent of the polyhydroxybenzene(s) R and of the hexamethylenetetramine HMTA, so as to form a polycondensate, b) the introduction into the product of stage a) of the anionic polyelectrolyte AP, c) the heating of the mixture of stage b).

34 . The process as claimed in claim 33 , in which:
stage a) is carried out at a temperature ranging from 40 to 80° C., stage c) is carried out at a temperature ranging from 70 to 100° C.

35 . The process as claimed in claim 33 , in which stage b) comprises the addition of the anionic polyelectrolyte, in the form of an aqueous solution in several goes to the product of stage a).

36 . The process as claimed in claim 33 , which comprises a stage of addition of a cationic polyelectrolyte between stages b) and c).

37 . The process as claimed in claim 33 , which comprises a stage of dilution with water of the composition of stage b).

38 . The process as claimed in claim 33 , wherein the polyhydroxybenzene R is resorcinol.

39 . The process as claimed in claim 33 which additionally comprises a stage of drying in an oven to prepare an aerogel.

40 . The process as claimed in claim 39 which additionally comprises at least one pyrolysis stage to prepare a porous carbon.

Assignees

• Hutchinson

Inventors

• Astafyeva Ksenia
• Dufour Bruno
• Stalmach Sara-Lyne
• Sonntag Philippe

Classifications

• H01G11/24

  characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor · CPC title

• C08K5/524

  Esters of phosphorous acids, e.g. of H3PO3 · CPC title

• C01P2006/12

  Surface area · CPC title

• C08J2379/04

  Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors · CPC title

• C08J9/286

  the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers · CPC title