Improved emulsion and suspension polymerization processes, and improved electrochemical performance for carbon derived from same

Patent metadata

Field	Value
Publication number	US-2016039970-A1
Application number	US-201414775792-A
Country	US
Kind code	A1
Filing date	Mar 13, 2014
Priority date	Mar 13, 2013
Publication date	Feb 11, 2016
Grant date	—

Abstract

The present application is directed to methods for preparation of polymer particles in gel form and carbon materials made therefrom. 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. The methods herein can also be employed generally to improve emulsion and/or suspension polymerization processes by improved control of diffusion of acidic and basic species between the polymer and secondary phases.

First claim

1 . A method for making polymer particles in gel form via an emulsion or suspension process, the method comprising preparing a reactant mixture comprising a monomer component containing one or more phenolic compounds and one or more crosslinking compounds, and a carrier fluid, wherein:
the carrier fluid contains less than 50 wt % cyclohexane, based on the total weight of the carrier fluid, the monomer component polymerizes to form the polymer particles in gel form, the carrier fluid comprises an acid, a base, a catalyst, or a combination thereof, at a concentration for each species of at least 50% of the saturation limit, and a volume average particle size (Dv,50) of the polymer particles in gel form is greater than or equal to 1 mm.

2 . A method for making polymer particles in gel form via an emulsion or suspension process, the method comprising preparing a reactant mixture comprising a monomer component containing one or more phenolic compounds and one or more crosslinking compounds, and a carrier fluid, wherein:
the monomer component polymerizes to form the polymer particles in gel form, the carrier fluid is free of or contains a surfactant at a concentration less than the critical micelle concentration, the carrier fluid comprises an acid, a base, a catalyst, or a combination thereof, at a concentration for each species of at least 50% of the saturation limit, and a volume average particle size (Dv,50) of the polymer particles in gel form is greater than or equal to 1 mm.

3 - 5 . (canceled)

6 . The method of claim 1 , wherein the carrier fluid comprises one or more vegetable oils, one or more mineral oils, one or more chlorinated hydrocarbons, one or more paraffinic oils, or any mixture thereof.

7 - 13 . (canceled)

14 . The method of claim 1 , wherein the one or more phenolic compounds and the one or more crosslinking compounds are prepolymerized with one another to form a prepolymer prior to making the polymer particles in gel form via the emulsion or suspension process.

15 . The method of claim 1 , wherein the reaction mixture further comprises 0.01 wt % to 20 wt % of a non-ionic surfactant having a molecular weight of from about 100 Daltons to about 2,000 Daltons.

16 . The method of claim 1 , further comprising heating the polymer particles in gel form in an inert atmosphere at a temperature of from about 500° C. to about 2,400° C. to produce pyrolyzed particles.

17 - 24 . (canceled)

25 . The method of claim 1 , wherein the reactant mixture further comprises a nitrogen-containing electrochemical modifier.

26 . (canceled)

27 . (canceled)

28 . The method of claim 1 , further comprising:
heating the polymer particles in gel form in an inert atmosphere at a temperature of from 500° C. to 2,400° C. to produce pyrolyzed particles; and activating the pyrolyzed particles in an atmosphere comprising carbon dioxide, carbon monoxide, steam, oxygen, or any mixture thereof at a temperature of from 500° C. to 1,300° C. to produce activated particles.

29 . The method of claim 28 , wherein the activated particles have a total pore volume of greater than 0.5 cm 3 /g and a gerameter (GM) of greater than or equal to 24.

30 . The method of claim 2 , wherein the carrier fluid comprises one or more vegetable oils, one or more mineral oils, one or more chlorinated hydrocarbons, one or more paraffinic oils, or any mixture thereof.

31 . The method of claim 2 , wherein the one or more phenolic compounds and the one or more crosslinking compounds are prepolymerized with one another to form a prepolymer prior to making the polymer particles in gel form via the emulsion or suspension process.

32 - 38 . (canceled)

39 . A suspension or emulsion polymerization process, comprising an aqueous polymer phase and an oil secondary phase, wherein a pHabs of the aqueous polymer phase and an oil secondary phase are within 1 pHabs unit of each other.

40 . The suspension or emulsion polymerization process of claim 39 , wherein the pHabs of the aqueous polymer phase and the oil secondary phase are within 0.5 pHabs units of each other.

41 . The suspension or emulsion polymerization process of claim 39 , wherein the pHabs of the aqueous polymer phase and the oil secondary phase are within 0.1 pHabs units of each other.

42 . The suspension or emulsion polymerization process of claim 39 , wherein the pHabs of the aqueous polymer phase is at least 0.1 pHabs units greater than the pHabs of the oil secondary phase.

43 . The suspension or emulsion polymerization process of claim 39 , wherein the pHabs of the aqueous polymer phase is at least 0.5 pHabs units greater than the pHabs of the oil secondary phase.

44 . A suspension or emulsion polymerization process, comprising an aqueous polymer phase and an oil secondary phase, wherein a pHabs of the aqueous polymer phase is at least 1 pHabs unit greater than a pHabs of the oil secondary phase.

45 . The suspension or emulsion polymerization process of claim 39 , wherein the pHabs of the aqueous polymer phase is at least 0.1 pHabs units lower than the pHabs of the oil secondary phase.

46 . The suspension or emulsion polymerization process of claim 39 , wherein the pHabs of the aqueous polymer phase is at least 0.5 pHabs units lower than the pHabs of the oil secondary phase.

47 . A suspension or emulsion polymerization process, comprising an aqueous polymer phase and an oil secondary phase, wherein a pHabs of the aqueous polymer phase is at least 1 pHabs unit lower than a pHabs of the oil secondary phase.

Assignees

• Ludvik Joseph Frank
• Dong Xing
• Qureshi Shahid P
• Knazek Gerald
• Energ2 Technologies Inc
• Georgia Pacific Chemicals Llc

Inventors

• Kron Benjamin E
• Geramita Katharine
• Costantino Henry R
• Ludvik Joseph Frank
• Dong Xing
• Qureshi Shahid P
• Knazek Gerald A

Classifications

• C01B32/312

  Preparation · CPC title

• C01P2006/16

  Pore diameter · CPC title

• C01B32/336

  characterised by gaseous activating agents · CPC title

• C01P2006/14

  Pore volume · CPC title

• C01B32/05

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