IP Library Granted Patent US 12,173,165
Granted Patent B2
US 12,173,165 · App. 18/297,478 · Granted Dec 24, 2024

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

Inventors: Henry R. Costantino (Woodinville, WA); Alan Tzu-Yang Chang (Renton, WA); Benjamin E. Kron (Seattle, WA); Avery J. Sakshaug (Snohomish, WA); Leah A. Thompkins (Seattle, WA); Aaron M. Feaver (Seattle, WA)
Assignee: Group14 Technologies, Inc.
C09C1/48C01B32/05C08F2/02C08G8/22C08G14/08C08G69/44C08G73/0638C08G73/065C08L61/34C08L77/12C08L79/04H01G11/24H01G11/34H01M4/587H01M10/06H01M12/08C01P2002/82C01P2006/12C01P2006/14C01P2006/17C01P2006/40C08L2201/54H01M4/625H01M10/052Y02E60/10Y02E60/13
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Quick Facts
Patent No.
US 12,173,165
App. No.
18/297,478
Granted
Dec 24, 2024
Kind
B2
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.

Claims (25)

1. A method for preparing a polymer, the method comprising physical blending of a solvent-free mixture of solid particles comprising solid polymer precursors by one of ball milling, jet milling, Fritsch milling or planetary milling, and aging the solvent-free mixture at a temperature and for a time sufficient for the one or more polymer precursors to react with each other and form a polymer gel, and wherein the solvent-free mixture comprises less than 1% solvent by weight.

2. The method of claim 1 , wherein the solvent-free mixture comprises less than 0.1% solvent by weight.

3. The method of claim 1 , wherein the temperature is at or above the glass transition temperature of one or more species of polymer precursor particles.

4. The method of claim 1 , wherein the temperature is at or above the melting temperature of one or more species of polymer precursor particles.

5. The method of claim 1 , wherein the temperature is at or above 30 C below the melting temperature of one or more species of polymer precursor particles.

6. The method of claim 1 , wherein the polymer precursors are selected from an amine-containing compound, an alcohol-containing compound and a carbonyl-containing compound.

7. The method of claim 1 , wherein the polymer precursors are selected from an alcohol, a phenol compound, a polyalcohol, a sugar, an alkyl amine, an aromatic amine, an aldehyde, a ketone, a carboxylic acid, an ester, melamine, a urea, an acid halide and an isocyanate.

8. The method of claim 7 , wherein the phenolic compound is phenol, resorcinol, naphthol, bisphenol A, or any combination thereof.

9. The method of claim 7 , wherein the sugar is fructose, sucrose, glucose, or any combination thereof.

10. The method of claim 7 , wherein the carboxylic acid is acetic acid, formic acid, oxalic acid, lactic acid, citric acid, cyanuric acid, or any combination thereof.

11. The method of claim 1 , wherein the polymer precursors further comprise hexamethylenetetramine.

12. The method of claim 11 , wherein the polymer precursors comprise hexamethylenetetramine and bisphenol A present at a mole ratio between 0.05:1 to 5:1.

13. The method of claim 1 , further comprising pyrolyzing the solvent free polymer gel particles in an inert atmosphere at temperatures ranging from 500° C. to 2400° C. to obtain pyrolyzed porous carbon.

14. The method of claim 13 , further comprising activating the porous carbon to obtain activated porous carbon by a method comprising contacting the pyrolyzed polymer gel particles with an atmosphere comprising carbon dioxide, carbon monoxide, steam, oxygen or combinations thereof at a temperature may ranging from 800° C. to 1300° C.

15. A carbon having a maximum theoretical capacitance of greater than 26 F/cm 3 ,

wherein:

the carbon is formed from a mixture comprising hexamethylenetetramine and bisphenol A, such that a mole ratio of the hexamethylenetetramine to the bisphenol A ranges from 1.63:1 to 5:1;

a pore structure of the carbon comprises at least 97.8% micropores;

nitrogen content of the carbon is 1-8%;

BET surface area of carbon ranges from about 1,500 m 2 /g to about 2,000 m 2 /g; and

the capacitance is measured at a current density of 0.5 Amp/g employing an electrolyte comprising tetraethylammonium tetrafluoroborate in acetonitrile.

16. The carbon of claim 15 , wherein the maximum theoretical capacitance of greater than 27 F/cm 3 .

17. The carbon of claim 15 , wherein the maximum theoretical capacitance of greater than 28 F/cm 3 .

18. The carbon of claim 15 , wherein the maximum theoretical capacitance of greater than 29 F/cm 3 .

19. An electrode comprising a carbon material according to claim 15 .

Assignments (1)
SECURITY INTEREST Recorded Jul 1, 2026
From: GROUP14 TECHNOLOGIES, INC.
To: NOMURA STRATEGIC VENTURES FUND 1, LP
Reel/Frame 075876/0771 →
Continuity (4)
Continuation 16893186 · Jun 4, 2020
Continuation 16745197 · Jan 16, 2020
Continuation 15125920
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