Preparation of polymeric resins and carbon materials

Patent metadata

Field	Value
Publication number	US-10654722-B2
Application number	US-201715649546-A
Country	US
Kind code	B2
Filing date	Jul 13, 2017
Priority date	Nov 26, 2012
Publication date	May 19, 2020
Grant date	May 19, 2020

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. Carbon particles comprising a mean particle diameter of at least 1 mm and a span of 3 or less, wherein the span is equal to (Dv,90−Dv,10)/Dv,50, wherein the Dv,10, the Dv,50, and the Dv,90 are the volume particle sizes measured at 10%, 50% and 90%, respectively, of the particle size distribution, wherein greater than 75% of the carbon particles have a spherical geometry as determined by optical microscopy and image analysis, and wherein the carbon particles have a total specific surface area of about 1,500 m 2 /g to 1,900 m 2 /g.

2. The carbon particles of claim 1 , wherein greater than 90% of the carbon particles have a spherical geometry as determined by optical microscopy and image analysis.

3. The carbon particles of claim 1 , wherein the carbon particles have a total pore volume of about 0.5 cm 3 /g up to 0.8 cm 3 /g.

4. The carbon particles of claim 1 , wherein the span is from about 1 to 3.

5. The carbon particles of claim 1 , wherein the span is 1.5 or less.

6. The carbon particles of claim 1 , wherein the mean particle diameter is 2.3 mm to about 10 mm.

7. The carbon particles of claim 1 , wherein the mean particle diameter is greater than 2 mm to about 10 mm.

8. The carbon particles of claim 1 , wherein the mean particle diameter is at least 1 mm to about 4 mm.

9. The carbon particles of claim 1 , wherein the carbon particles have a total ash content of 0.1 wt % or less.

10. The carbon particles of claim 1 , wherein the mean particle diameter is at least 1 mm to about 4 mm, wherein the span is 2 or less, and wherein greater than 95% of the carbon particles have a spherical geometry as determined by optical microscopy and image analysis.

11. The carbon particles of claim 1 , wherein the carbon particles contain less than 500 ppm of all elements having an atomic number of 11 to 92, as measured by proton induced x-ray emission.

12. 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 comprising carbon particles, wherein:
the carbon particles comprise a mean particle diameter of at least 1 mm and a span of 3 or less, wherein the span is equal to (Dv,90−Dv,10)/Dv,50, wherein the Dv,10, the Dv,50, and the Dv,90 are the volume particle sizes measured at 10%, 50% and 90%, respectively, of the particle size distribution,
greater than 75% of the carbon particles have a spherical geometry as determined by optical microscopy and image analysis, and
the carbon particles have a total specific surface area of about 1,500 m 2 /g to 1,900 m 2 /g.

13. The method of claim 12 , wherein the mean particle diameter is greater than 2 mm to about 10 mm.

14. A carbon material comprising carbon particles having a mean particle diameter of at least 1 mm to about 4 mm and a span of 3 or less, wherein the span is equal to (Dv,90−Dv,10)/Dv,50, wherein the Dv,10, the Dv,50, and the Dv,90 are the volume particle sizes measured at 10%, 50% and 90%, respectively, of the particle size distribution, wherein:
greater than 90% of the carbon particles have a spherical geometry as determined by optical microscopy and image analysis,
the carbon particles have a total pore volume of about 0.1 cm 3 /g to about 3 cm 3 /g, and
the carbon particles have a total specific surface area of about 1,500 m 2 /g to 1,900 m 2 /g.

15. The carbon material of claim 14 , wherein the mean particle diameter is greater than 2 mm to about 10 mm.

16. The carbon material of claim 14 , wherein the total specific surface area is about 1,700 m 2 /g to 1,900 m 2 /g.

17. The carbon material of claim 14 , wherein a pore structure of the carbon particles comprises about 20% up to 47% of mesopores.

18. The carbon material of claim 14 , wherein a pore structure of the carbon particles comprises at least 50% up to 90% of micropores.

19. The carbon material of claim 14 , wherein the total pore volume is about 0.5 cm 3 /g up to 0.8 cm 3 /g.

20. The carbon particles of claim 14 , wherein the carbon particles have a total ash content of 0.1 wt % or less.

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

• H01G11/04

  Hybrid capacitors · CPC title

• C01B32/318

  characterised by the starting materials · CPC title

• C01B32/312

  Preparation · CPC title

• C01B32/05

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

• H01G11/38

  Carbon pastes or blends; Binders or additives therein · CPC title