Method for making carbon nanotubes
US-9206049-B2 · Dec 8, 2015 · US
US10010867B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10010867-B2 |
| Application number | US-201414485642-A |
| Country | US |
| Kind code | B2 |
| Filing date | Sep 12, 2014 |
| Priority date | Feb 27, 2009 |
| Publication date | Jul 3, 2018 |
| Grant date | Jul 3, 2018 |
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The invention is directed to a process for producing carbon nanofibers and/or carbon nanotubes, which process comprises pyrolyzing a particulate cellulosic and/or carbohydrate substrate that has been impregnated with a compound of an element or elements, the metal or alloy, respectively, of which is capable of forming carbides, in a substantially oxygen free, volatile silicon compound containing atmosphere, optionally in the presence of a carbon compound.
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The invention claimed is: 1. A process for producing carbon nano fibers and/or tubes, the process comprising: pyrolyzing a particulate cellulosic and/or carbohydrate substrate that has been impregnated with a metal compound or combination of metal compounds, which are capable of forming carbides, in the presence of volatile silicon compounds in a substantially oxygen free, inert stationary atmosphere, optionally in the presence of a carbon compound. 2. The process according to claim 1 , wherein the said substrate is selected from microcrystalline cellulose, sugar, or a mixture of sugar and microcrystalline cellulose, and soy meal. 3. The process according to claim 1 , wherein the substrate comprises carbonaceous bodies produced by a hydrothermal treatment of agricultural materials such as sugars, starch, soy meal, (hemi)cellulose; dehydrated products of the above compounds. 4. The process according to claim 1 , wherein the substrate is impregnated with a compound of nickel, cobalt, iron and/or molybdenum, followed by drying and pyrolyzing. 5. The process according to claim 1 , wherein the said substrate is pyrolysed in the presence of a silicon rubber compound. 6. The process according to claim 1 , wherein the said silicon compound is an alkyl siloxane. 7. The process according to claim 6 , wherein the said siloxane compound is a trimer of dimethyl siloxane. 8. A process according to claim 7 , wherein: the pyrolyzing is at a temperature between 500 and 1000° C. for a period between 5 min and 5 hours; and the atmosphere is substantially free of carbon compounds. 9. The process according to claim 1 , wherein the pyrolyzing is at a temperature between 500 and 1000° C. for a period between 5 min and 5 hours. 10. A process according to claim 9 , wherein: the substrate comprises carbonaceous bodies produced by a hydrothermal treatment of agricultural materials, such as, sugars, starch, soy meal, (hemi)cellulose, as well as dehydrated products of the above compounds, such as, furfural and 2-hydroxyfurfural; the substrate is impregnated with a compound of nickel, cobalt, iron and/or molybdenum, followed by drying and pyrolyzing; and the said substrate is pyrolyzed in the presence of a silicon rubber compound. 11. The process according to claim 1 , wherein the atmosphere is substantially free of carbon compounds. 12. The process according to claim 1 , wherein the atmosphere further contains at least one carbon compound selected from the group consisting of toluene, CO, CO/H 2 mixtures, CH 4 , C 2 H 4 , lower alkanes, alkylenes, alcohols, alkyns, and aromatic compounds.
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