METHOD FOR PURIFYING MULTI-WALLED CARBON NANOTUBES

• US 20150093322A1
• Filed: 04/26/2013
• Published: 04/02/2015
• Est. Priority Date: 04/27/2012
• Status: Abandoned Application

• Current Assignee: Showa Denko KK (Resonac Holdings Corp.)
• Original Assignee: Showa Denko KK (Resonac Holdings Corp.)
• Inventors: Yamamoto, Ryuji, Nakamura, Takeshi
• Application Number:
  US14/396,539
• Publication Number:
  US 20150093322A1
• Time in Patent Office: Days
• US Class Current: 423/447.2
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: B82Y 40/00 Manufacture or treatment of nanostructures
• CPC Class Codes: C01B 2202/06 Multi-walled nanotubes
• CPC Class Codes: C01B 2202/22 Electronic properties
• CPC Class Codes: C01B 2202/24 Thermal properties
• CPC Class Codes: C01B 2202/30 Purity
• CPC Class Codes: C01B 32/162 characterised by catalysts
• CPC Class Codes: C01B 32/17 Purification
• CPC Class Codes: H01M 10/052 Li-accumulators
• CPC Class Codes: H01M 4/625 Carbon or graphite
• CPC Class Codes: Y02E 60/10 Energy storage using batteries

Abstract

A method comprising adding a multi-walled carbon nanotube synthesized by the vapor phase process to a nitric acid aqueous solution of not lower than 0.2 mol/L so as to dissolve a catalyst metal present in the multi-walled carbon nanotube, performing solid-liquid separation to isolate solid matter, and subjecting the isolated solid matter to heat treatment at a temperature higher than 150° C. gives a purified multi-walled carbon nanotube in which the amount of a metallic element left in the multi-walled carbon nanotube originating the catalyst metal is not smaller than 1000 ppm and not larger than 8000 ppm determined by ICP optical emission spectrometry and the amount of an anion left in the multi-walled carbon nanotube originating in the acid is smaller than 20 ppm determined by ion chromatography analysis.

Claims

1. A method for purifying a multi-walled carbon nanotube, the method comprising:

adding a multi-walled carbon nanotube synthesized by a vapor phase process to a nitric acid aqueous solution of not lower than 0.2 mol/L so as to dissolve a catalyst metal present in the multi-walled carbon nanotube,

performing solid-liquid separation to isolate solid matter, and

subjecting the solid matter to heat treatment at a temperature higher than 150°

C.

2. The purification method according to claim 1, further comprising adding the solid matter resulting from solid-liquid separation to pure water and performing another round of solid-liquid separation to isolate solid matter.

3. The purification method according to claim 2, wherein the process of adding the solid matter resulting from solid-liquid separation to pure water and then performing another round of solid-liquid separation to isolate solid matter is repeated until the pH of the liquid resulting from solid-liquid separation reaches not lower than 1.5 and not higher than 6.0.

4. The purification method according to claim 1, wherein the amount of the multi-walled carbon nanotube added to the nitric acid aqueous solution is not smaller than 0.1% by mass and not larger than 5% by mass in terms of a solid content concentration.

5. The purification method according to claim 1, wherein the heat treatment is performed in an air atmosphere at a temperature not lower than 200°

C. and lower than 350°

C.

6. The purification method according to claim 1, wherein the dissolution of the catalyst metal present in the multi-walled carbon nanotube into the nitric acid aqueous solution is performed under atmospheric pressure.

7. The purification method according to claim 1, further comprising, prior to the dissolution of the catalyst metal present in the multi-walled carbon nanotube into the nitric acid aqueous solution, grinding the multi-walled carbon nanotube.

8. A purified multi-walled carbon nanotube synthesized by a vapor phase process and then washed with an acid, wherein the amount of a metallic element left in the multi-walled carbon nanotube originating in a catalyst metal is not smaller than 1000 ppm and not larger than 8000 ppm determined by ICP optical emission spectrometry and the amount of an anion left in the multi-walled carbon nanotube originating in the acid is smaller than 20 ppm determined by ion chromatography analysis.

9. The purified multi-walled carbon nanotube according to claim 8, wherein the surface layer of the multi-walled carbon nanotube is covered with amorphous carbon.

10. An electrode for a battery, the electrode comprising the purified multi-walled carbon nanotube according to claim 8.

11. A method for producing a purified multi-walled carbon nanotube, the method comprising

a step of preparing a multi-walled carbon nanotube by a supported catalyst method,

a step of adding the prepared multi-walled carbon nanotube to a nitric acid aqueous solution of not lower than 0.2 mol/L,

a step of performing solid-liquid separation to isolate the acid-treated multi-walled carbon nanotube, and

a step of subjecting the isolated multi-walled carbon nanotube to heat treatment at a temperature higher than 150°

C.