PREPARATION OF POLYMERIC RESINS AND CARBON MATERIALS

• US 20170152340A1
• Filed: 06/30/2016
• Published: 06/01/2017
• Est. Priority Date: 02/09/2012
• Status: Active Grant

• Current Assignee: Group14 Technologies Inc.
• Original Assignee: BASF SE
• Inventors: Geramita, Katharine, Costantino, Henry R., Feaver, Aaron M., Thompkins, Leah A., Chang, Alan Tzu-Yang, Sakshaug, Avery, Kron, Benjamin E.
• Granted Patent: US 11,401,363 B2
• Time in Patent Office: Days
• CPC Class Codes: C01B 32/05 Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
• CPC Class Codes: C01B 32/30 Active carbon
• CPC Class Codes: C01B 32/336 characterised by gaseous activating agents
• CPC Class Codes: C08G 8/22 Resorcinol
• CPC Class Codes: H01G 11/34 characterised by carbonisation or activation of carbon
• CPC Class Codes: H01G 11/44 Raw materials therefor, e.g. resins or coal
• CPC Class Codes: H01M 10/0525 Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
• CPC Class Codes: H01M 10/054 Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
• CPC Class Codes: H01M 10/06 Lead-acid accumulators semi-lead accumulators H01M10/20
• CPC Class Codes: H01M 12/06 with one metallic and one gaseous electrode
• CPC Class Codes: H01M 12/08 composed of a half-cell of a fuel-cell type and a half-cell of the secondary-cell type
• CPC Class Codes: H01M 4/133 Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
• CPC Class Codes: H01M 4/14 Electrodes for lead-acid accumulators
• CPC Class Codes: H01M 4/36 Selection of substances as active materials, active masses, active liquids
• CPC Class Codes: H01M 4/587 for inserting or intercalating light metals
• CPC Class Codes: H01M 4/625 Carbon or graphite
• CPC Class Codes: H01M 4/96 Carbon-based electrodes
• CPC Class Codes: Y02E 60/10 Energy storage using batteries
• CPC Class Codes: Y02E 60/13 Energy storage using capacitors

Abstract

The present application is directed to methods for preparation of carbon materials. The carbon materials comprise enhanced electrochemical properties and find utility in any number of electrical devices, for example, as electrode material in ultracapacitors or batteries.

Claims

1. A method for making polymer particles in gel form via an emulsion or suspension process, the method comprising:

a) preparing a reactant mixture comprising a monomer component comprising one or more phenolic compounds, one or more crosslinking compounds, and a carrier fluid; and

b) polymerizing the one or more phenolic compounds with the one or more crosslinking compounds,

wherein the carrier fluid comprises a surfactant in a concentration equal to or greater than the critical micelle concentration and the volume average particle size (Dv,50) of the polymer particles is less than or equal to 1 mm.

4. The method according to claim 1, wherein the Dv,50 of the polymer particles is less than or equal to 0.5 mm.

5. The method according to claim 1, wherein the Dv,50 of the polymer particles is less than or equal to 0.1 mm.

8. The method according to claim 1, wherein the carrier fluid comprises one or more vegetable oils, one or more minerals oils having from about 15 to about 40 carbon atoms, one or more chlorinated hydrocarbons, one or more paraffinic oils, or any combination thereof.

9. The method according to claim 1, wherein the monomer component is an aqueous mixture comprising the one or more phenolic compounds and one or more catalysts.

10. The method according to claim 9, wherein the one or more catalysts comprises an organic acid.

11. The method according to claim 9, wherein the one or more catalysts comprises a volatile basic salt.

12. The method according to claim 9, wherein the one or more catalysts comprises a volatile basic salt and comprises an organic acid.

13. The method according to claim 11, wherein the volatile basic salt is ammonium carbonate, ammonium bicarbonate, ammonium acetate, or ammonium hydroxide, or a combination thereof.

14. The method according to claim 11, wherein the organic acid is acetic acid, formic acid, propionic acid, maleic acid, oxalic acid, uric acid, lactic acid, or a combination thereof.

15. The method according to claim 9, wherein the one or more catalysts contains a total of less than 500 ppm moieties comprising arsenic, antimony, bismuth, or ions thereof, or a halogen.

16. The method according to claim 9, wherein a molar ratio of the one or more phenolic compounds to the one or more catalysts ranges from about 5 to about 400.

17. The method according to claim 9, wherein a molar ratio of the one or more phenolic compounds to the one or more catalysts ranges from about 5 to about 50.

18. The method according to claim 1, wherein the polymer particles in gel form are made via the suspension process, the reactant mixture is a suspension and the method further comprises agitation of the suspension with a mixer.

19. The method according to claim 1, further comprising separating the polymer particles from the carrier fluid to provide separated polymer particles in gel form.

20. The method according to claim 1, further comprising heating the reactant mixture to a temperature ranging from about 30°

C. to about 100°

C.

2. A method for making polymer particles in gel form via an emulsion or suspension process, the method comprising:

a) preparing a reactant mixture comprising a monomer component comprising one or more phenolic compounds, one or more crosslinking compounds, and a carrier fluid; and

b) polymerizing the one or more phenolic compounds with the one or more crosslinking compounds,

wherein the carrier fluid comprises 50 wt % or more of cyclohexane, based on the total weight of the carrier fluid, and the volume average particle size (Dv,50) of the polymer particles is less than or equal to 1 mm.

3. A method for making polymer particles in gel form via an emulsion or suspension process, the method comprising:

a) preparing a reactant mixture comprising a monomer component comprising one or more phenolic compounds, one or more crosslinking compounds, and a carrier fluid; and

b) polymerizing the one or more phenolic compounds with the one or more crosslinking compounds,

wherein the carrier fluid comprises 50 wt % or more of cyclohexane, based on the total weight of the carrier fluid, and the volume average particle size (Dv,50) of the polymer particles is greater than or equal to 1 mm.

6. The method according to claim 3, wherein the Dv,50 of the polymer particles is less than or equal to 2 mm.

7. The method according to claim 3, wherein the Dv,50 of the polymer greater than or equal to 4 mm.

21-54. -54. (canceled)