Preparation method for graphene oxide fiber, and fiber obtained thereby

Patent metadata

Field	Value
Publication number	US-12312707-B2
Application number	US-202017607762-A
Country	US
Kind code	B2
Filing date	Apr 30, 2020
Priority date	Apr 30, 2019
Publication date	May 27, 2025
Grant date	May 27, 2025

Abstract

Disclosed in the present invention are a preparation method for a graphene oxide fiber, and fiber obtained thereby. A polyelectrolyte is prepared into a spinning stock solution by means of a wet spinning method, graphene oxide is added in a coagulation tank to serve as a coagulation bath, the spinning stock solution is injected into the coagulation bath, a diffusion reaction is carried out, and winding, washing and drying are carried out to obtain the graphene oxide fiber; the preparation method has the advantages that equipment is simple, the costs are low, the spinnability is good, and the method is suitable for large-scale production; moreover, the prepared fiber has multiple layers of fiber walls; the fiber has good tensile strength and a super-high specific surface area and is widely applied to the fields of catalysis, adsorption, flexible sensors, thermal preservation and insulation materials and tissue engineering.

First claim

The invention claimed is:

1. A preparation method for graphene oxide fiber, wherein the method comprises the following steps:
step 1: adding polyelectrolyte into water to obtain spinning stock solution wherein the polyelectrolyte is chitosan oligosaccharide, the molecular weight of the polyelectrolyte is 2000-10000 Da;
step 2: adding graphene oxide into water, optionally stirring and/or ultrasonic processing, to obtain coagulation bath;
step 3: injecting the spinning stock solution obtained in step 1 into the coagulation bath obtained in step 2, and winding, washing and drying to obtain the graphene oxide fiber.

2. The preparation method of claim 1 , wherein in step 1, the molecular weight of the polyelectrolyte is 2000-6000 Da.

3. The preparation method of claim 1 , wherein in step 1, the mass percentage concentration of the polyelectrolyte in the spinning stock solution is 5-60%.

4. The preparation method of claim 1 , wherein in step 1, the pH of the obtained spinning stock solution is adjusted to 2-6.

5. The preparation method of claim 3 , wherein in step 1, the mass percentage concentration of the polyelectrolyte in the spinning stock solution is 5-40%.

6. The preparation method of claim 3 , wherein in step 1, the mass percentage concentration of the polyelectrolyte in the spinning stock solution is 5-20%.

7. The preparation method of claim 1 , wherein in step 2, the mass percentage concentration of the graphene oxide in the coagulation bath is 0.2-1%.

8. The preparation method of claim 7 , wherein in step 2, the mass percentage concentration of the graphene oxide in the coagulation bath is 0.2-0.5%.

9. The preparation method of claim 4 , wherein in step 1, the pH of the obtained spinning stock solution is adjusted to 3.5-5.

10. The preparation method of claim 1 , wherein in step 3, after the fiber is obtained, it is optionally immersed in a multivalent cationic salt solution.

11. The preparation method of claim 10 , wherein the concentration of the multivalent cationic salt solution is 1-10%.

12. The preparation method of claim 11 , wherein the concentration of the multivalent cationic salt solution is 3-8%.

13. The preparation method of claim 11 , wherein the concentration of the multivalent cationic salt solution is 5%.

14. A graphene oxide fiber, obtained by the preparation method of claim 1 , wherein the graphene oxide fiber has a hollow structure and has a single-layer fiber wall, or multi-layer fiber wall where an aperture of each fiber wall gradually increases from inside to outside, showing a gradient structure; wherein the graphene oxide fiber comprises a polyelectrolyte wherein the polyelectrolyte is a chitosan oligosaccharide and the molecular weight of the polyelectrolyte is 2000-10000 Da.

15. The graphene oxide fiber of claim 14 , wherein the fiber wall of the graphene oxide fiber is multi-layered.

16. The graphene oxide fiber of claim 14 , wherein the graphene oxide and the polyelectrolyte in the graphene oxide fiber are electrostatically bound together.

17. An article, wherein the article comprises or is made of the graphene oxide fiber of claim 14 .

Assignees

• Univ Qingdao

Inventors

• Sui Kunyan
• Xia Yanzhi
• Pan Na
• Lin Min
• Fan Wenxin
• Cui Huilin
• Li Yuyu

Classifications

• D10B2101/12

  Carbon; Pitch · CPC title

• D01D1/02 Primary

  Preparation of spinning solutions · CPC title

• D01F9/00

  Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments · CPC title

• D01F1/10

  Other agents for modifying properties · CPC title

• D01D5/06 Primary

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