Novel methods for sol-gel polymerization in absence of solvent and creation of tunable carbon structure from same

Patent metadata

Field	Value
Publication number	US-2020148886-A1
Application number	US-202016745197-A
Country	US
Kind code	A1
Filing date	Jan 16, 2020
Priority date	Mar 14, 2014
Publication date	May 14, 2020
Grant date	—

Abstract

The present application is directed to methods for solvent-free preparation of polymers and their subsequent processing into activated carbon materials. These methods unexpectedly demonstrate ability to tune pore structure in the polymer gel and carbon produced there from, while also providing distinct advantages over the current art.

First claim

1 - 31 . (canceled)

32 . A method for preparing a carbon material, comprising:
a. preparing a mixture by physically blending polymer precursors, wherein the mixture comprises less than 10% solvent by weight, and the polymer precursors comprise monomers; b. aging the mixture at a temperature for a time sufficient for the polymer precursors to react with each other and form a polymer; and c. pyrolyzing the polymer in an inert atmosphere.

33 . The method of claim 32 , wherein the inert atmosphere comprises nitrogen gas.

34 . The method of claim 32 , wherein the temperature ranges from 500 to 2400° C.

35 . The method of claim 32 , wherein the polymer precursors comprise hexamethylenetetramine and bisphenol A.

36 . The method of claim 35 , wherein the hexamethylenetetramine and bisphenol A are present at a mole ratio between 0.05:1 and 5:1, respectively.

37 . The method of claim 32 , wherein the pyrolyzing is performed in a rotary kiln, a microwave kiln, a pusher-type kiln, an elevator kiln, or a fluid bed reactor.

38 . The method of claim 32 , further comprising activating the pyrolyzed polymer in an atmosphere comprising carbon dioxide, carbon monoxide, steam, oxygen or combinations thereof.

39 . The method of claim 38 , wherein the activating is performed at a temperature ranging from 800 to 1300° C.

40 . The method of claim 38 , wherein the polymer precursors comprise hexamethylenetetramine and bisphenol A.

41 . The method of claim 40 , wherein the hexamethylenetetramine and bisphenol A are present at a mole ratio between 0.05:1 and 5:1, respectively.

42 . The method of claim 38 , wherein the activating is performed in a rotary kiln, a microwave kiln, a pusher-type kiln, an elevator kiln, or a fluid bed reactor.

43 . A method for preparing a carbon material, comprising:
a. preparing a mixture by physically blending polymer precursors, wherein the mixture comprises less than 10% solvent by weight, and the polymer precursors comprise monomers; and b. heating the mixture at temperatures ranging from 500 to 2400° C. in an inert atmosphere comprising nitrogen gas.

44 . The method of claim 43 , wherein the polymer precursors comprise hexamethylenetetramine and bisphenol A.

45 . The method of claim 44 , wherein the hexamethylenetetramine and bisphenol A are present at a mole ratio between 0.05:1 and 5:1, respectively.

46 . The method of claim 43 , wherein the heating is performed in a rotary kiln, a microwave kiln, a pusher-type kiln, an elevator kiln, or a fluid bed reactor.

47 . A method for preparing a carbon material, comprising:
a. preparing a mixture by physically blending polymer precursors, wherein the mixture comprises less than 10% solvent by weight, and the polymer precursors comprise monomers; and b. heating the mixture at temperatures ranging from 800 to 1300° C. in an atmosphere comprising carbon dioxide, carbon monoxide, steam, oxygen or combinations thereof.

48 . The method of claim 47 , wherein the polymer precursors comprise hexamethylenetetramine and bisphenol A.

49 . The method of claim 48 , wherein the hexamethylenetetramine and bisphenol A are present at a mole ratio between 0.05:1 and 5:1, respectively.

50 . The method of claim 47 , wherein the heating is performed in a rotary kiln, a microwave kiln, a pusher-type kiln, an elevator kiln, or a fluid bed reactor.

Assignees

• Group14 Technologies Inc

Inventors

• Costantino Henry R
• Chang Alan Tzu-Yang
• Kron Benjamin E
• Sakshaug Avery J
• Thompkins Leah A
• Feaver Aaron M

Classifications

• C08G8/22

  Resorcinol · CPC title

• H01M4/625

  Carbon or graphite · CPC title

• C01P2006/17

  Pore diameter distribution · CPC title

• C08L61/34

  Condensation polymers of aldehydes or ketones with monomers covered by at least two of the groups C08L61/04, C08L61/18 and C08L61/20 · CPC title

• C08L79/04

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