Polyimide aerogels, carbon aerogels, and metal carbide aerogels and methods of making same
First Claim
1. A process for producing polyimide aerogels comprising:
- contacting a diamine monomer and an aromatic dianhydride monomer in a solvent under conditions conducive to formation of a poly(amic acid);
contacting the poly(amic acid) in a first solvent with a dehydrating agent to form a polyimide gel by imidization; and
drying the polyimide gel in the presence of supercritical CO2 to afford an polyimide aerogel.
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Accused Products
Abstract
A preparation process of polyimide aerogels that composed of aromatic dianhydrides and aromatic diamines or a combined aromatic and aliphatic diamines is described. Also descried is a process to produce carbon aerogels derived from polyimide aerogel composed of a rigid aromatic diamine and an aromatic dianhydride. Finally, the processes to produce carbon aerogels or xerogel-aerogel hybrid, both of which impregnated with highly dispersed transition metal clusters, and metal carbide aerogels, deriving from the polyimide aerogels composed of a rigid aromatic diamine and an aromatic dianhydride, are described. The polyimide aerogels and the polyimide aerogel derivatives consist of interconnecting mesopores with average pore size at 10 to 30 nm and a mono-dispersed pore size distribution. The gel density could be as low as 0.008 g/cc and accessible surface area as high as 1300 m2/g.
133 Citations
111 Claims
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1. A process for producing polyimide aerogels comprising:
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contacting a diamine monomer and an aromatic dianhydride monomer in a solvent under conditions conducive to formation of a poly(amic acid);
contacting the poly(amic acid) in a first solvent with a dehydrating agent to form a polyimide gel by imidization; and
drying the polyimide gel in the presence of supercritical CO2 to afford an polyimide aerogel. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 55)
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12. A process of producing carbon aerogels comprising the steps of
providing a polyimide aerogel; - and
pyrolyzing the polyimide aerogel under in an inert atmosphere to form a carbon aerogel. - View Dependent Claims (65)
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13. A process of producing a carbon aerogel comprising the steps of
contacting a diamine monomer and an aromatic dianhydride monomer in a solvent under conditions conducive to formation of a poly(amic acid); -
contacting the poly(amic acid) in a solvent with a dehydrating agent to form a polyimide by imidization;
drying the polyimide gel in the presence of supercritical CO2 to afford an polyimide aerogel; and
pyrolyzing the polyimide aerogel under in an inert atmosphere to form a carbon aerogel. - View Dependent Claims (14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24)
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25. A process for producing carbon aerogels impregnated with dispersed metal particles comprising:
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contacting a diamine monomer and an aromatic dianhydride monomer in a solvent under conditions conducive to formation of a poly(amic acid);
dissolving a soluble metal ion salt and the poly(amic acid) in a solvent;
contacting the solution of poly(amic acid) and soluble metal ion salt with a dehydrating agent to form a polyimide gel by imidization of the poly(amic acid);
drying the polyimide gel in the presence of supercritical CO2 to afford an polyimide aerogel; and
pyrolyzing the derived aerogel under protection of an inert atmosphere to form the carbon aerogel having highly dispersed transition metal particles. - View Dependent Claims (28, 29, 35, 36, 37, 38, 80, 90)
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26. A process for producing carbon xerogel-aerogel hybrid impregnated with highly dispersed metal particles, the process comprising the steps of:
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contacting a diamine monomer and an aromatic dianhydride monomer in a solvent under conditions conducive to formation of a poly(amic acid);
dissolving a soluble metal salt and the poly(amic acid) in a solvent;
contacting the solution of poly(amic acid) and soluble metal ion salt with a dehydrating agent to form a polyimide gel by imidization of the poly(amic acid);
precipitating at least a portion of the soluble metal salt onto the polyimide gel;
drying the polyimide gel in the presence of supercritical CO2 to afford an polyimide aerogel; and
pyrolyzing the derived aerogel under protection of an inert atmosphere to form the carbon xerogel-aerogel having highly dispersed transition metal particles. - View Dependent Claims (103)
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27. A process for producing a metal carbide aerogel, a metal carbide-carbon aerogel or carbon aerogel impregnated with highly dispersed metal particles, the process comprising the steps of:
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contacting a diamine monomer and an aromatic dianhydride monomer in a solvent under conditions conducive to formation of a poly(amic acid);
preparing a solution of a soluble metal ion salt, an epoxide compound and the poly(amic acid) in a solvent such that a molar ratio of epoxide compound to the metal ion is between about 1 to about 8;
contacting the solution of poly(amic acid), an epoxide compound and soluble metal ion salt with a dehydrating agent to form a polyimide gel by imidization of the poly(amic acid);
drying the polyimide gel in the presence of supercritical CO2 to afford an polyimide aerogel; and
pyrolyzing the derived aerogel under protection of an inert atmosphere to form the aerogel having highly dispersed transition metal particles. - View Dependent Claims (30, 31, 32, 33, 34, 94, 95, 96, 97, 98, 99, 100, 101, 102, 105, 107, 109)
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- 53. A polyimide aerogel comprising at least one polyimide polymer.
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66. A carbon aerogel prepared by pyrolysis of a polyimide aerogel under an inert atmosphere at a temperature of between about 500°
- C. to about 1600°
C.
- C. to about 1600°
- 67. A carbon aerogel comprising carbon and nitrogen wherein the carbon aerogel comprises at least 0.01% nitrogen by weight.
- 81. A composite metal-carbon aerogel comprising nitrogen doped carbon aerogel domains, metal carbide domains, or a combination thereof.
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104. An article of manufacture comprising at least one aerogel selected from polyimide aerogels, carbon aerogels comprising carbon and nitrogen, metal carbide aerogels, hybrid carbon-metal carbide aerogels, each of which may have metal particles dispersed in the pores of the aerogel.
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106. An electrode composed of at least one aerogel selected from carbon aerogels comprising carbon and nitrogen, metal carbide aerogels, hybrid carbon-metal carbide aerogels, each of which may have metal particles dispersed in the pores of the aerogel.
- 108. An electrochemical cell comprising one or more electrodes composed of at least one aerogel selected from carbon aerogels comprising carbon and nitrogen, metal carbide aerogels, hybrid carbon-metal carbide aerogels, each of which may have metal particles dispersed in the pores of the aerogel.
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111. A supported metal catalyst comprising a carbon, metal carbide, or a composite carbon-metal carbide aerogel having metal particles dispersed therein or a metal carbide aerogel.
Specification