Device for producing carbon nanotube fibers and method for producing carbon nanotube fibers using same

Patent metadata

Field	Value
Publication number	US-10774449-B2
Application number	US-201515514106-A
Country	US
Kind code	B2
Filing date	Oct 28, 2015
Priority date	Oct 28, 2014
Publication date	Sep 15, 2020
Grant date	Sep 15, 2020

Abstract

The present invention relates to an apparatus for producing a carbon nanotube fiber. The apparatus includes: a vertical reactor having a reaction zone; a concentric double-pipe inlet tube disposed on top of the reaction zone and consisting of an inner pipe through which a spinning feedstock including a spinning solution and a first gas is introduced into the reaction zone and an outer pipe defining a concentric annular portion surrounding the inner pipe and through which a second gas is introduced into the reaction zone; heating means for heating the reaction zone; and a discharge unit disposed under the bottom of the reaction zone to discharge a carbon nanotube fiber therethrough. The spinning feedstock entering the reaction zone through the inner pipe of the inlet tube is carbonized and graphitized while flowing from the top to the bottom of the reaction zone to form a carbon nanotube fiber consisting of a continuous sock (or aggregates) of carbon nanotubes. The second gas entering the reaction zone through the outer pipe of the inlet tube forms a gas curtain surrounding the circumference of the continuous sock of carbon nanotubes while flowing from the top to the bottom of the reaction zone. The gas curtain minimizes the contamination of the inner wall of the reactor and facilitates the discharge of the carbon nanotube fiber. Therefore, the apparatus of the present invention is suitable for the production of a carbon nanotube fiber in a continuous manner.

First claim

What is claimed is:

1. A method for producing a carbon nanotube fiber, with an apparatus comprising:
a vertical reactor having a reaction zone;
a concentric double-pipe inlet tube disposed on top of the reaction zone and consisting of an inner pipe through which a spinning feedstock comprising a spinning solution and a first gas is introduced into the reaction zone and an outer pipe defining a concentric annular portion surrounding the inner pipe and through which a second gas is introduced into the reaction zone;
a heating mechanism for heating the reaction zone; and
a discharge unit disposed under the bottom of the reaction zone to discharge a carbon nanotube fiber there through,
wherein the spinning feedstock entering the reaction zone through the inner pipe of the inlet tube is carbonized and graphitized while flowing from the top to the bottom of the reaction zone to form a carbon nanotube fiber consisting of a continuous sock of carbon nanotubes;
wherein the second gas entering the reaction zone through the outer pipe of the inlet tube forms a gas curtain surrounding the circumference of the continuous sock of carbon nanotubes while flowing from the top to the bottom of the reaction zone; and
wherein a sprayer is disposed at an opening through the inner pipe of the inlet tube and is in communication with the reaction zone and the spinning feedstock entering the inner pipe, and the sprayer is configured and arranged to spray the spinning solution in the reaction zone;
the method comprising the steps of;
introducing the second gas into the reaction zone through the outer pipe of the inlet tube to form a gas curtain in the reaction zone,
introducing the first gas into the reaction zone surrounded by the gas curtain through the inner pipe of the inlet tube,
allowing the spinning solution to react to form a continuous sock of carbon nanotubes while descending in an internal zone defined by the gas curtain, and
winding the continuous sock of carbon nanotubes under a bottom of the reactor to produce a carbon nanotube fiber.

2. The according to claim 1 , wherein the second gas entering from the outer pipe of the inlet tube forms a gas curtain along the inner wall of the reactor so that the continuous sock of carbon nanotubes or the carbon nanotube fiber formed in the reaction zone is physically prevented from approaching the inner wall of the reactor.

3. The method according to claim 1 , wherein the second gas entering from the gas inlet tube forms a gas curtain while flowing along the inner wall of the reactor so that a catalyst attached to the inner wall of the reactor is physically removed.

4. The method according to claim 1 , wherein an annular opening through which the outer pipe is in communication with the reaction zone is spaced apart from the inner pipe.

5. The method according to claim 4 , wherein the annular opening is separated from an opening, through which the inner pipe is in communication with the reaction zone, through an annular thermal insulator positioned between the inner pipe and the outer pipe.

6. The method according to claim 1 , wherein the reaction zone consists of a preheating zone and a heating zone and the spinning feedstock introduced into the reaction zone sequentially passes through the preheating zone and the heating zone.

7. The method according to claim 1 , wherein the apparatus further comprises a supply unit for supplying the spinning solution to the inner pipe of the inlet tube, a supply unit for supplying the first gas to the inner pipe of the inlet tube, and a supply unit for supplying the second gas to the outer pipe of the inlet tube.

8. The method according to claim 1 , wherein the first gas or the second gas is supplied at such a linear velocity that laminar flows are formed in the reaction zone.

9. The method according to claim 7 , wherein the first gas supply unit has a flow controller, by which the first gas is supplied at such a linear velocity that laminar flows are formed and the second gas supply unit has a flow controller, by which the second gas is supplied at such a linear velocity that laminar flows are formed.

10. The method according to claim 7 , wherein the mixing unit prepares the spinning solution as a catalyst or a catalyst precursor in a carbon source.

11. The method according to claim 1 , wherein each of the first gas and the second gas is an inert gas, a reducing gas or a mixed gas thereof.

12. The method according to claim 1 , wherein the apparatus further comprises a circulation line through which each of the first gas and the second gas released from the reactor reenters the reactor for reuse.

13. The method according to claim 1 , wherein the spinning solution is a catalyst or a catalyst precursor in a carbon source.

14. The method according to claim 1 , wherein the discharge unit comprises a winder, for winding and collecting the carbon nanotube fiber discharged from the bottom of the reactor.

15. The method according to claim 1 , wherein the discharge unit has an inlet through which an inert gas is fed to form an inert gas curtain surrounding the circumference of a continuous aggregate of the carbon nanotube fiber discharged from the reaction zone.

16. A carbon nanotube fiber produced using the method according to claim 1 .

17. The method according to claim 10 , wherein the carbon source is ethanol, methanol, propanol, acetone, xylene, chloroform, ethyl acetate, diethyl ether, polyethylene glycol, ethyl formate, mesitylene, tetrahydrofuran (THF), dimethylformamide (DMF), dichloromethane, hexane, benzene, carbon tetrachloride, or pentane.

18. The method according to claim 13 , wherein the carbon source is ethanol, methanol, propanol, acetone, xylene, chloroform, ethyl acetate, diethyl ether, polyethylene glycol, ethyl formate, mesitylene, tetrahydrofuran (THF), dimethylformamide (DMF), dichloromethane, hexane, benzene, carbon tetrachloride, or pentane.

19. The method according to claim 1 , wherein the sprayer comprises a nozzle, an atomizer or a shower head.

Assignees

• Lg Chemical Ltd

Inventors

• Yoon Ki Yong
• Lee Youngho
• Kim Ji Eun
• Choe Yongjin

Classifications

• D01F11/16

  by physicochemical methods · CPC title

• C01P2004/13

  Nanotubes · CPC title

• C01B32/164

  involving continuous processes · CPC title

• C01B2202/08

  Aligned nanotubes · CPC title

• D01F9/133 Primary

  Apparatus therefor · CPC title