Method of producing precursor fiber for carbon fiber and carbon fiber

Patent metadata

Field	Value
Publication number	US-11932971-B2
Application number	US-201917287510-A
Country	US
Kind code	B2
Filing date	Oct 24, 2019
Priority date	Oct 29, 2018
Publication date	Mar 19, 2024
Grant date	Mar 19, 2024

Abstract

A method of producing a precursor fiber for carbon fiber includes extruding a polyacrylonitrile copolymer solution from a spinneret into the air, immersing it in a coagulation bath liquid stored in a coagulation bath, redirecting traveling of the coagulating fiber bundle by a first guide immersed in the coagulation bath disposed below the spinneret, and pulling it out of the coagulation bath liquid into the air to prepare a coagulated fiber bundle, which is then subjected to at least a washing step in water, stretching step, oil agent applying step, and drying step, wherein the depth-directional coagulation bath immersion length, which means a distance between the starting point of the immersion of the spinning dope solution in the coagulation bath liquid and the first guide immersed in the coagulation bath where traveling of the coagulating fiber bundle is redirected, is 3 to 40 cm.

First claim

The invention claimed is:

1. A method of producing a precursor fiber for carbon fiber comprising:
extruding a spinning dope solution comprising a polyacrylonitrile copolymer solution from a spinneret into the air,
immersing the spinning dope solution in a coagulation bath liquid stored in a coagulation bath to obtain a coagulating fiber bundle,
redirecting traveling of the coagulating fiber bundle by a first guide immersed in the coagulation bath disposed below the spinneret, and
pulling the coagulating fiber bundle out of the coagulation bath liquid into the air to prepare a coagulated fiber bundle, which is then subjected to at least a washing step in water, stretching step, oil agent applying step, and drying step,
wherein a depth-directional coagulation bath immersion length, which means a distance between a starting point of the immersion of the spinning dope solution in the coagulation bath liquid and the first guide immersed in the coagulation bath where traveling of the coagulating fiber bundle is redirected, is 3 to 40 cm,
wherein the coagulating fiber bundle redirected by the first guide immersed in the coagulation bath is redirected again at least by a second guide immersed in the coagulation bath, the second guide being immersed in the coagulation bath and located in the coagulation solution below a straight line running from an exit point where the coagulating fiber bundle is pulled out into the air to the first guide immersed in the coagulation bath,
wherein a redirection angle (B) of the coagulating fiber bundle on the first guide immersed in the coagulation bath is 90° to 150°.

2. The method as set forth in claim 1 , wherein the coagulation bath immersion length, which is a sum of the depth-directional coagulation bath immersion length and an oblique-directional coagulation bath immersion length, is 10 to 500 cm, the oblique-directional coagulation bath immersion length being a distance between the first guide immersed in the coagulation bath where traveling of the coagulating fiber bundle is redirected and the exit point where it is pulled out into the air.

3. The method as set forth in claim 1 , wherein the first oblique-directional coagulation bath immersion length is 10 to 300 cm, the first oblique-directional coagulation bath immersion length being a distance between the first guide immersed in the coagulation bath where the coagulating fiber bundle is redirected and the second guide immersed in the coagulation bath where it is redirected again.

4. The method as set forth in claim 1 , wherein an angle (A), the angle between the straight line running from the spinneret hole located outermost in a take-up direction to the redirection point of the coagulating fiber bundle on the first guide immersed in the coagulation bath and the straight line perpendicular to the spinneret face, is 6.5° to 45°.

5. The method as set forth in claim 1 , wherein a length of the spinneret in the take-up direction is 5 to 20 cm.

6. The method as set forth in claim 1 , wherein the spinneret has 500 to 24,000 holes.

7. The method as set forth in claim 1 , wherein a take-up speed for the spinning dope solution is 10 m/min or more.

8. The method as set forth in claim 1 , wherein the coagulation bath liquid has a viscosity of 2 to 100 mPa·s.

9. The method as set forth in claim 1 , wherein the coagulation bath liquid is a liquid mixture of water and at least one solvent selected from the group consisting of dimethyl sulfoxide, dimethyl formamide, and dimethyl acetamide and has a solvent concentration of 25 to 85 mass %.

10. A method of producing carbon fiber comprising steps in which a precursor fiber for carbon fiber prepared by the method as set forth in claim 1 is subjected to stabilization treatment in an oxidizing atmosphere at a temperature of 200° C. to 300° C., preliminary carbonization treatment in an inert atmosphere at a temperature of 500° C. to 1,200° C., and then carbonization treatment in an inert atmosphere at a temperature of 1,200° C. to 3,000° C.

Assignees

• Toray Industries

Inventors

• Horinouchi Ayanobu
• Watanabe Fumitaka
• Okishima Yuuki

Classifications

• D01F9/22 Primary

  from polyacrylonitriles · CPC title

• D01F6/18

  from polymers of unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide · CPC title

• D01F9/328

  for manufacturing filaments from polyaddition, polycondensation, or polymerisation products · CPC title

• D01D5/06 Primary

  Wet spinning methods {(D01D5/0046 takes precedence)} · CPC title