A method is provided for making mesoporous resin. It comprises: (a) providing a nucleophilic component which comprises a phenolic compound or a phenol condensation prepolymer optionally with one or more modifying reagents selected from hydroquinone, resorcinol, urea, aromatic amin
A method is provided for making mesoporous resin. It comprises: (a) providing a nucleophilic component which comprises a phenolic compound or a phenol condensation prepolymer optionally with one or more modifying reagents selected from hydroquinone, resorcinol, urea, aromatic amines and heteroaromatic amines; (b) dissolving the nucleophilic component in a pore former selected from the group consisting of a diol, a diol ether, a cyclic ester, a substituted cyclic ester, a substituted linear amide, a substituted cyclic amide, an amino alcohol and a mixture of any of the above with water, together with at least one electrophilic cross-linking agent selected from the group consisting of formaldehyde, paraformaldehyde, furfural and hexamethylene tetramine; and (c) condensing the nucleophilic component and the electrophilic cross-linking agent in the presence of the pore former to form a porous resin. The resin may be formed in situ by pouring the partially cross-linked resin into hot oil. Mesoporous resin beads are obtained which can be carbonized into mesoporous carbon beads.
대표청구항▼
The invention claimed is: 1. A method of making mesoporous carbon, the method comprising: (a) providing a nucleophilic component which comprises a phenolic compound or a phenol condensation prepolymer optionally with one or more modifying reagents selected from hydroquinone, resorcinol, urea, aroma
The invention claimed is: 1. A method of making mesoporous carbon, the method comprising: (a) providing a nucleophilic component which comprises a phenolic compound or a phenol condensation prepolymer optionally with one or more modifying reagents selected from hydroquinone, resorcinol, urea, aromatic amines and heteroaromatic amines; (b) dissolving the nucleophilic component in a pore former selected from the group consisting of a diol, a diol ether, a cyclic ester, a substituted cyclic ester, a substituted linear amide, a substituted cyclic amide, an amino alcohol and a mixture of any of the above with water, together with at least one electrophilic cross-linking agent selected from the group consisting of formaldehyde, paraformaldehyde, furfural and hexamethylene tetramine; (c) condensing the nucleophilic component and the electrophilic cross-linking agent in the presence of the pore former to form a porous resin; (d) comminuting the porous resin; and (e) carbonising the comminuted porous resin to form mesoporous carbon by treatment in an inert atmosphere at 600° C. to 800° C. with a heating rate up to 10° C. per minute of treatment time. 2. The method of claim 1, wherein the nucleophilic component is a phenol-formaldehyde novolac. 3. The method of claim 1, wherein the modifying reagent is aniline, melamine or hydroxymethylated melamine. 4. The method of claim 1, further comprising incorporating dispersed heteroatoms into the porous resin. 5. The method of claim 4, comprising incorporating metal heteroatoms into the resin by dissolving a metal salt in the pore former. 6. The method of claim 4, comprising incorporating non-metal heteroatoms into the resin by adding an organic precursor containing the heteroatoms to the pore former. 7. The method of claim 1, wherein the pore former is ethylene glycol. 8. The method of claim 1, wherein the pore former is selected from the group consisting of 1,4-butylene glycol, diethylene glycol, triethylene glycol, γ-butyrolactone, propylene carbonate, dimethylformamide, N-methyl-2-pyrrolidone and monoethanolamine. 9. The method of claim 1, wherein at least 120 parts by weight of the pore former are used to dissolve 100 parts by weight of the nucleophilic component. 10. The method of claim 1, wherein there is dissolved in the pore former as electrophilic cross linking agent hexamethylene tetramine at a concentration of at least 9 parts by weight per 100 parts by weight of the nucleophilic component. 11. The method of claim 1, wherein the nucleophilic component which is a phenol-formaldehyde novolac and the electrophilic cross-linking agent which is hexamine are dissolved in the pore former which is ethylene glycol by smoothly increasing the temperature to 100-105° C. and the temperature is gradually raised to 150-160° C. to complete cross-linking of the resin. 12. The method of claim 1, wherein the particle size of the porous resin formed in step (e) is between 1 and 1000 μm. 13. The method of claim 1, wherein the pore former is removed from the porous resin by washing said resin with water. 14. The method of claim 11, wherein the pore former is removed from the porous resin by vacuum distillation at a temperature below 100° C. 15. The method of claim 1, wherein the porous resin is carbonized in an atmosphere selected from the group consisting of carbon dioxide, nitrogen and argon. 16. The method of claim 1, further comprising activating the porous carbon by heating it at high temperature in the presence of carbon dioxide, steam or a mixture thereof. 17. The method of claim 1, further comprising activating the porous carbon by heating it in carbon dioxide at above 800° C. 18. The method of claim 1, further comprising activating the porous carbon by heating it in air at above 400° C. 19. The method of claim 1, in which the mesoporous carbon contains macropores, mesopores of pore size between 2 and 50 nm and micropores with a mean pore size less than 2 nm.
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