Purification of carbon nanotubes based on the chemistry of fenton's reagent
The present invention is directed to methods of purifying carbon nanotubes (CNTs). In general, such methods comprise the following steps: (a) preparing an aqueous slurry of impure CNT material; (b) establishing a source of Fe 2+ ions in the slurry to provide a catalytic slurry; (c) adding hydrogen peroxide to the catalytic slurry to provide an oxidative slurry, wherein the Fe 2+ ions catalyze the production of hydroxyl radicals; and (d) utilizing the hydroxyl radicals in the oxidative slurry to purify the CNT material and provide purified CNTs.
1. A method comprising the steps of:
a) preparing an aqueous slurry of impure carbon nanotube (CNT) material, wherein the impure CNT material comprises Fe impurities and CNTs;
b) adding a non-oxidizing mineral acid to the aqueous slurry to adjust and maintain pH of said aqueous slurry between about 1 and about 3, thereby providing an acidic slurry;
c) adding hydrogen peroxide to the acidic slurry to form an oxidative slurry, wherein at least some of the Fe impurities are converted into Fe 2+ , and wherein Fe 2+ present in the oxidative slurry catalyzes a production of hydroxyl radicals; and
d) utilizing the hydroxyl radicals to purify the CNT material and provide purified CNTs.
2. The method of claim 1 , wherein the CNTs in the impure CNT material are selected from the group consisting of single-wall carbon nanotubes, double-wall carbon nanotubes, multi-wall carbon nanotubes, and combinations thereof.
3. The method of claim 1 , further comprising seeding the aqueous slurry with catalytic Fe 2+ by adding an iron salt.
4. The method of claim 1 , further comprising stirring the oxidative slurry to facilitate purification.
5. The method of claim 1 , further comprising a step of allowing phase separation to occur such that the purified CNTs are separated from other oxidative slurry components.
6. The method of claim 5 , further comprising a step of decanting to additionally separate the purified CNTs from other oxidative slurry components.
7. The method of claim 1 , further comprising a repetition of at least one of the steps of which the method is comprised.
8. The method of claim 1 , wherein the non-oxidizing mineral acid is hydrochloric acid.
9. A method comprising the steps of:
a) preparing an aqueous slurry of impure carbon nanotube (CNT) material, wherein the impure CNT material comprises CNTs;
b) establishing a source of Fe 2+ ions in the aqueous slurry to provide a catalytic slurry;
c) adding a non-oxidizing mineral acid to the catalytic slurry to provide an acidic slurry;
d) adding hydrogen peroxide to the acidic slurry to provide an oxidative slurry with a pH between about 1 and about 3, wherein the Fe 2+ ions catalyze a production of hydroxyl radicals; and
e) utilizing the hydroxyl radicals in the oxidative slurry to purify the CNT material and provide purified CNTs.
10. The method of claim 9 , wherein the CNTs in the impure CNT material are selected from the group consisting of single-wall carbon nanotubes, double-wall carbon nanotubes, multi-wall carbon nanotubes, and combinations thereof.
11. The method of claim 9 , wherein the source of Fe 2+ ions in the aqueous slurry is established by adding an iron salt.
12. The method of claim 9 , further comprising stirring the oxidative slurry to facilitate purification.
13. The method of claim 9 , further comprising a step of allowing phase separation to occur such that the purified CNTs are separated from other oxidative slurry components.
14. The method of claim 13 , further comprising a step of decanting to additionally separate the purified CNTs from other oxidative slurry components.
15. The method of claim 9 , further comprising a repetition of at least one of the steps of which the method is comprised.
16. The method of claim 9 , wherein the non-oxidizing mineral acid is hydrochloric acid.
17. A method comprising the steps of:
a) preparing an aqueous slurry of impure carbon nanotube (CNT) material, wherein the impure CNT material comprises small-diameter carbon nanotubes;
b) establishing a source of Fe 2+ ions in the aqueous slurry to provide a catalytic slurry;
c) adding a non-oxidizing mineral acid to the catalytic slurry to provide an acidic slurry;
d) adding hydrogen peroxide to the acidic slurry to provide an oxidative slurry with a pH between about 1 and about 3, wherein the Fe 2+ ions catalyze a production of hydroxyl radicals; and
e) utilizing the hydroxyl radicals in the oxidative slurry to purify the CNT material and provide purified CNTs.
18. The method of claim 17 , wherein the source of Fe 2+ ions in the aqueous slurry is established by adding an iron salt.
19. The method of claim 17 , further comprising stirring the oxidative slurry to facilitate purification.
20. The method of claim 17 , further comprising a step of allowing phase separation to occur such that the purified CNTs are separated from other oxidative slurry components.
21. The method of claim 20 , further comprising a step of decanting to additionally separate the purified CNTs from other oxidative slurry components.
22. The method of claim 17 , further comprising a repetition of at least one of the steps of which the method is comprised.
23. The method of claim 17 , wherein the non-oxidizing mineral acid is hydrochloric acid.
24. A method comprising the steps of:
a) preparing an aqueous slurry of impure carbon nanotube (CNT) material, wherein the impure CNT material comprises CNTs;
b) establishing a source of metal ions in the aqueous slurry to provide a catalytic slurry;
c) adding a non-oxidizing mineral acid to the catalytic slurry to provide an acidic slurry;
d) adding hydrogen peroxide to the acidic slurry to provide an oxidative slurry with a pH between about 1 and about 3, wherein the metal ions catalyze a production of hydroxyl radicals; and
e) utilizing the hydroxyl radicals in the oxidative slurry to purify the CNT material and provide purified CNTs.
25. The method of claim 24 , wherein the metal ions are selected from the group consisting of Cu(I), Ti(III), Cr(II), Co(II), Mn(III), and combinations thereof.
26. The method of claim 24 , wherein the non-oxidizing mineral acid is hydrochloric acid.