Preparation of polymeric resins and carbon materials

Patent metadata

Field	Value
Publication number	US-9714172-B2
Application number	US-201314647322-A
Country	US
Kind code	B2
Filing date	Nov 26, 2013
Priority date	Nov 26, 2012
Publication date	Jul 25, 2017
Grant date	Jul 25, 2017

Abstract

Methods for making carbon materials are provided. In at least one specific embodiment, the method can include combining one or more polymer precursors with one or more liquids to produce a mixture. The mixture can be an emulsion, dispersion, or a suspension. The liquid can include hexane, pentane, cyclopentane, benzene, toluene, o-xylene, m-xylene, p-xylene, diethyl ether, ethylmethylketone, dichloromethane, tetrahydrofuran, mineral oils, paraffin oils, vegetable derived oils, or any mixture thereof. The method can also include aging the mixture at a temperature and time sufficient for the polymer precursor to react and form polymer gel particles having a volume average particle size (Dv,50) of the polymer particles in gel form greater than or equal to 1 mm. The method can also include heating the polymer gel particles to produce a carbon material.

First claim

We claim:

1. A method for making a carbon material, comprising:
combining one or more polymer precursors with one or more liquids to produce a mixture, wherein the mixture is an emulsion, a dispersion, or a suspension, and wherein the liquid comprises hexane, pentane, cyclopentane, benzene, toluene, o-xylene, m-xylene, p-xylene, diethyl ether, ethylmethylketone, dichloromethane, tetrahydrofuran, a mineral oil, a paraffin oil, a vegetable derived oil, or any mixture thereof;
aging the mixture at a temperature and time sufficient for the polymer precursor to react and form polymer gel particles having a volume average particle size (Dv,50) of greater than or equal to 1 mm; and
heating the polymer gel particles to produce a carbon material.

2. The method according to claim 1 , wherein heating the polymer gel particles comprises pyrolyzing the polymer gel particles in an inert atmosphere at a temperature of about 500° C. to about 2,400° C. to produce the carbon material.

3. The method of claim 1 , wherein the carbon material has a total pore volume of about 1 cm 3 /g to about 7 cm 3 /g.

4. The method of claim 1 , wherein the carbon material comprises activated carbon.

5. The method of claim 1 , wherein the carbon material has a specific surface area of about 100 m 2 /g to about 3,000 m 2 /g.

6. The method of claim 1 , wherein the carbon material has a particle size distribution such that (Dv,90−Dv,10)/Dv,50 is less than 3, wherein the Dv,10, Dv,50, and Dv,90 are the particle sizes at 10%, 50%, and 90% of the particle size distribution by volume, respectively.

7. The method of claim 1 , wherein the polymer gel particles having the volume average particle size (Dv,50) of greater than or equal to 1 mm are made without milling, grinding, or other physical means of particle sizing.

8. The method of claim 1 , wherein:
the polymer gel particles having the volume average particle size (Dv,50) of greater than or equal to 1 mm are made without milling, grinding, or other physical means of particle sizing,
the carbon material has a total pore volume of about 1 cm 3 /g to about 7 cm 3 /g,
at least 50% of the total pore volume resides in pores having a diameter of about 50 Å to about 5,000 Å,
the carbon material has a specific surface area of about 100 m 2 /g to about 3,000 m 2 /g, and
the carbon material has a particle size distribution such that (Dv,90−Dv,10)/Dv,50 is less than 3, wherein the Dv,10, Dv,50, and Dv,90 are the particle sizes at 10%, 50%, and 90% of the particle size distribution by volume, respectively.

9. The method of claim 1 , further comprising combining an electrochemical modifier with the one or more polymer precursors, the one or more liquids, or the mixture, wherein the electrochemical modifier comprises nitrogen or silicon.

10. The method of claim 1 , further comprising combining an acid and a basic catalyst with the one or more polymer precursors and the one or more liquids to produce the mixture, wherein the acid comprises acetic acid, oxalic acid, or a mixture thereof, and wherein the basic catalyst comprises ammonium carbonate, ammonium bicarbonate, ammonium acetate, ammonium hydroxide, or any mixture thereof.

11. A method for making a carbon material, comprising:
mixing a polymer precursor and a liquid to produce an emulsion, wherein a continuous phase of the emulsion comprises the liquid, and wherein the liquid comprises hexane, pentane, cyclopentane, benzene, toluene, o-xylene, m-xylene, p-xylene, diethyl ether, ethylmethylketone, dichloromethane, tetrahydrofuran, mineral oils, paraffin oils, vegetable derived oils, or any mixture thereof;
aging the mixture at a temperature and for a time sufficient for the polymer precursor to react and form polycondensation polymer gel particles having a volume average particle size (Dv,50) of greater than or equal to 1 mm; and
heating the polycondensation polymer gel particles to produce a carbon material.

12. The method of claim 11 , wherein the polymer precursor comprises an aldehyde and at least one compound selected from the group consisting of: an amine-containing compound, an alcohol-containing compound, and a carbonyl-containing compound.

13. The method of claim 11 , wherein the polymer precursor comprises formaldehyde and at least one compound selected from the group consisting of: phenol, resorcinol, and urea.

14. The method of claim 11 , wherein:
the polycondensation polymer gel particles having the volume average particle size (Dv,50) of greater than or equal to 1 mm are made without milling, grinding, or other physical means of particle sizing,
the carbon material has a total pore volume of about 1 cm 3 /g to about 7 cm 3 /g,
at least 50% of the total pore volume resides in pores having a diameter of about 50 Å to about 5,000 Å,
the carbon material has a specific surface area of about 100 m 2 /g to about 3,000 m 2 /g, and
the carbon material has a particle size distribution such that (Dv,90−Dv,10)/Dv,50 is less than 3, wherein the Dv,10, Dv,50, and Dv,90 are the particle sizes at 10%, 50%, and 90% of the particle size distribution by volume, respectively.

15. The method of claim 11 , further comprising mixing an electrochemical modifier with the polymer precursor and the liquid, wherein the electrochemical modifier comprises nitrogen or silicon.

16. The method of claim 11 , further comprising mixing an acid and a basic catalyst with the a polymer precursor and the liquid to produce the emulsion, wherein the acid comprises acetic acid, oxalic acid, or a mixture thereof, and wherein the basic catalyst comprises ammonium carbonate, ammonium bicarbonate, ammonium acetate, ammonium hydroxide, or any mixture thereof.

17. A method for preparing a carbon material, comprising:
mixing a surfactant, one or more polymer precursors, water, and an organic solvent to produce an emulsion or suspension, wherein a total weight of the surfactant and organic solvent contains less than 50 wt % cyclohexane;
aging the emulsion or suspension at a temperature and for a time sufficient for the one or more polymer precursors to react and form condensation polymer gel particles having a volume average particle size (Dv,50) greater than or equal to 1 mm; and
heating the condensation polymer gel particles to produce a carbon material.

18. The method of claim 17 , further comprising mixing an acid with the surfactant, the polymer precursor, water, and the organic solvent to produce the emulsion or suspension, wherein the acid comprises acetic acid, oxalic acid, or a mixture thereof, and wherein the polymer precursor comprises formaldehyde and at least one of phenol, resorcinol, and urea.

19. The method of claim 18 , further comprising mixing a basic catalyst with the surfactant, the polymer precursor, water, the organic solvent, and the acid to produce the emulsion or suspension, and wherein the basic catalyst comprises ammonium carbonate, ammonium bicarbonate, ammonium acetate, ammonium hydroxide, or any mixture thereof.

20. The method of claim 19 , wherein:
the condensation polymer gel particles having the volume average particle size (Dv,50) of greater than or equal to 1 mm are made without milling, grinding, or other physical means of particle sizing,
the carbon material has a total pore volume of about 1 cm 3 /g to about 7 cm 3 /g,
a specific surface area of about 100 m 2 /g to about 3,000 m 2 /g, and
a particle size distribution such that (Dv,90−Dv,10)/Dv,50 is less than 3, wherein the Dv,10, Dv,50, and Dv,90 are the particle sizes at 10%, 50%, and 90% of th

Assignees

• Georgia Pacific Chemicals Llc
• Energ2 Tech Inc

Inventors

• Geramita Katharine
• Kron Benjamin E
• Costantino Henry R
• Feaver Aaron M
• Sakshaug Avery
• Thompkins Leah A
• Chang Alan Tzu-Yang
• Dong Xing
• Qureshi Shahid P
• Hines John B
• Knazek Gerald A
• Ludvik Joseph Frank

Classifications

• C01B32/318

  characterised by the starting materials · CPC title

• H01G11/32

  Carbon-based · CPC title

• C01P2006/14

  Pore volume · CPC title

• C01B32/312

  Preparation · CPC title

• H01M4/587

  for inserting or intercalating light metals · CPC title