METHODS FOR PREPARING CARBON MATERIALS
The present application is directed to compositions and methods of preparing carbon materials. The carbon materials prepared according to compositions and methods described herein comprise enhanced electrochemical properties and find utility in any number of electrical devices, for example, as electrode material in ultracapacitors.
1 . A method comprising:
a) combining a solvent, a catalyst, a first monomer and a second monomer to yield a reaction mixture;
b) increasing the temperature of the reaction mixture at a holding ramp rate and holding the reaction mixture at a holding temperature sufficient to co-polymerize the first and second monomer to yield a polymer composition; and
c) optionally heating the polymer composition at a curing temperature, thereby forming a cured polymer composition comprising the solvent and a polymer formed from co-polymerizing the first and second monomer, wherein the solvent concentration in the cured polymer composition is at least 5 wt %, based on total weight of the cured polymer composition.
2 . The method of claim 1 , wherein the method further comprises pyrolyzing the cured polymer composition at a pyrolysis temperature thereby substantially removing the solvent and pyrolyzing the polymer to yield a carbon material.
3 - 10 . (canceled)
11 . A method comprising:
a) combining a solvent, a catalyst, a first monomer and a second monomer to yield a reaction mixture, and maintaining the reaction mixture at a reaction temperature for a reaction time;
b) increasing the temperature of the reaction mixture at a holding ramp rate and holding the reaction mixture at a holding temperature sufficient to co-polymerize the first and second monomer to yield a polymer composition; and
c) optionally heating the polymer composition up to a curing temperature, thereby forming a cured polymer composition comprising the solvent and a polymer formed from co-polymerizing the first and second monomer.
12 - 18 . (canceled)
19 . A method comprising:
a) combining a solvent, a catalyst, a first monomer and a second monomer to yield a reaction mixture;
b) increasing the temperature of the reaction mixture at a holding ramp rate and holding the reaction mixture for a holding time at a holding temperature sufficient to co-polymerize the first and second monomer to yield a polymer composition;
c) optionally heating the polymer composition at a curing temperature, thereby forming a cured polymer composition comprising the solvent and a polymer formed from co-polymerizing the first and second monomer.
20 - 27 . (canceled)
28 . A method comprising:
a) combining a solvent, a catalyst, a first monomer and a second monomer to yield a reaction mixture;
b) optionally holding the reaction mixture at a holding temperature sufficient to co-polymerize the first and second monomer to yield a polymer composition; and
c) heating the polymer composition by increasing an initial temperature at a curing ramp rate of at least 0.5° C./hour up to a curing temperature, thereby forming a cured polymer composition comprising the solvent and a polymer formed from co-polymerizing the first and second monomer.
29 - 30 . (canceled)
31 . A method comprising:
a) combining a solvent, a catalyst, a first monomer and a second monomer to yield a reaction mixture;
b) transferring the reaction mixture to a reaction vessel having a volume greater than 10 L and a surface area to volume aspect ratio greater than about 3 m 2 /m 3 ;
c) increasing the temperature of the reaction mixture at a holding ramp rate and holding the reaction mixture for a holding time at a holding temperature sufficient to co-polymerize the first and second monomer to yield a polymer composition; and
d) optionally heating the polymer composition at a curing temperature, thereby forming a cured polymer composition comprising the solvent and a polymer formed from co-polymerizing the first and second monomer.
32 - 50 . (canceled)
51 . The method of claim 1 , wherein the first monomer is a phenolic compound.
52 - 56 . (canceled)
57 . The method of claim 1 , wherein the second monomer is formaldehyde.
58 - 59 . (canceled)
60 . The method of claim 1 , wherein the solvent comprises water and a miscible acid.
61 . (canceled)
62 . The method of claim 1 , wherein the curing temperature ranges from about 70° C. to about 200° C.
63 - 83 . (canceled)
84 . The method of claim 2 , wherein the carbon material comprises a total pore volume of at least 0.01 cc/g.
85 - 88 . (canceled)
89 . The method of claim 2 , wherein the carbon material comprises a BET specific surface area of at least 5 m 2 /g.
90 - 93 . (canceled)
94 . The method of claim 2 , wherein the carbon material comprises a BET specific surface area of at least 1500 m 2 /g.
95 . The method of claim 2 , wherein the carbon materials have a pore structure comprising micropores, mesopores and a total pore volume, and wherein from 40% to 90% of the total pore volume resides in micropores, from 10% to 60% of the total pore volume resides in mesopores and less than 10% of the total pore volume resides in pores greater than 20 nm.
96 . The method of claim 2 , wherein the carbon materials comprise a total impurity content of less than 500 ppm of elements having atomic numbers ranging from 11 to 92 as measured by total reflection x-ray fluorescence.
97 - 99 . (canceled)
100 . The method of claim 1 , wherein the polymer comprises a total pore volume of at least 0.01 cc/g.
101 - 104 . (canceled)
105 . The method of claim 1 , wherein the polymer comprises a BET specific surface area of at least 5 m 2 /g.
106 - 112 . (canceled)
113 . The method of claim 1 , wherein the polymer has a pore structure comprising micropores, mesopores and a total pore volume, and wherein from 40% to 90% of the total pore volume resides in micropores, from 10% to 60% of the total pore volume resides in mesopores and less than 10% of the total pore volume resides in pores greater than 20 nm.
114 . The method of claim 1 , wherein the polymer comprises a total impurity content of less than 500 ppm of elements having atomic numbers ranging from 11 to 92 as measured by total reflection x-ray fluorescence.
115 . (canceled)
116 . The method of claim 1 , wherein the polymer comprises a total pore volume of at least 0.30 cc/g.
117 - 118 . (canceled)
119 . The method of claim 2 , wherein the pyrolysis temperature is greater than about 250° C.
120 - 122 . (canceled)
123 . A cured polymer composition, wherein the polymer is prepared according to claim 1 .
124 . A polymer composition comprising:
a solvent concentration greater than about 10 wt. % of the polymer composition; and
a polymer having a relative pore integrity greater than 0.4.
125 - 158 . (canceled)