Process for the manufacture of a precursor yarn

Patent metadata

Field	Value
Publication number	US-12234577-B2
Application number	US-201615766457-A
Country	US
Kind code	B2
Filing date	Oct 6, 2016
Priority date	Oct 8, 2015
Publication date	Feb 25, 2025
Grant date	Feb 25, 2025

Abstract

The present invention relates to a method for manufacturing precursor yarn comprising lignin, which may be further processed into intermediate carbon fibers and finally also carbon fibers. It also relates to carbon fibers and uses of said fibers. Said method involves applying a water-free spin finish.

First claim

The invention claimed is:

1. A method for manufacturing a precursor yarn comprising lignin, comprising:
a) providing cellulose and/or a cellulose derivative,
b) providing lignin and/or a lignin derivative,
c) dissolution of the cellulose and/or the cellulose derivative and the lignin and/or the lignin derivative in a solvent followed by subsequent mixing thus providing a dope consisting essentially of the cellulose and/or the cellulose derivative and the lignin and/or the lignin derivative and the solvent,
d) performing a spinning of the dope to a precursor material,
e) applying a water-free spin finish on said precursor material, and
f) drying of said precursor material, thus providing a precursor yarn comprising lignin,
wherein the water-free spin finish in step e) consists essentially of at least one organic solvent with a boiling point lower than that of water, and one or more anti-static agents or one or more anti-friction agents or both, wherein the at least one organic solvent consists essentially of one or more aprotic polar solvent selected from ketoalkyl or ketoalkoxy compounds and has the structure shown below,

and wherein
R1=H, CH 3 , O-(CH 2 ) n -CH 3 ; n=0-3,
R2=H, CH 3 , O-(CH 2 ) n -CH 3 ; n=0-3, and
optionally one or more protic polar solvent, and wherein the water-free spin finish is applied on said precursor material before drying of said precursor material.

2. A method according to claim 1 wherein the spinning in step d) is performed through a solution spinning or wet-spinning.

3. A method according to claim 1 wherein the application in step e) is performed by using a bath, oiler stone or dip roller or a combination thereof.

4. A method according to claim 1 wherein the one or more aprotic polar solvent has a dipole moment in the range of from 5×10 −30 Cm to 10×10 −30 Cm.

5. A method according to claim 1 wherein the water-free spin finish contains the one or more anti-static agents.

6. A method according to claim 1 wherein the water-free spin finish additionally is mixed with a water-containing spin finish within the range of from 1:10 to 10:1.

7. A method according to claim 1 wherein the temperature which is applied during the drying step f) does not exceed 150° C.

8. A method according to claim 1 wherein the spinning in step d) is performed through air-gap spinning or dry jet-wet spinning.

9. A method according to claim 1 wherein the water-free spin finish contains the one or more anti-friction agents.

10. A method according to claim 1 wherein the water-free spin finish additionally is mixed with a water-containing spin finish within the range of from 1:5 to 5:1.

11. A method according to claim 1 wherein the water-free spin finish additionally is mixed with a water-containing spin finish within the range of 1:1.

12. A method for manufacturing a precursor yarn comprising lignin, comprising:
a) providing cellulose and/or a cellulose derivative,
b) providing lignin and/or a lignin derivative,
c) dissolution of the cellulose and/or the cellulose derivative and the lignin and/or the lignin derivative in a solvent followed by subsequent mixing thus providing a dope consisting essentially of the cellulose and/or the cellulose derivative and the lignin and/or the lignin derivative and the solvent,
d) performing a spinning of the dope to a precursor material,
e) applying a water-free spin finish on said precursor material,
f) drying of said precursor material, thus providing a precursor yarn comprising lignin, and
g) performing a stabilization on the precursor yarn to produce a stabilized carbon fibre,
wherein the water-free spin finish in step e) consists essentially of at least one organic solvent with a boiling point lower than that of water, and one or more anti-static agentsor one or more anti-friction agents or both, wherein the at least one organic solvent consists essentially of an aprotic polar solvent selected from ketoalkyl or ketoalkoxy compounds and has the structure shown below,

and wherein
R 1 =H, CH 3 , O-(CH 2 ) n -CH 3 ; n=0-3,
R 2 =H, CH 3 , O-(CH 2 ) n -CH 3 ; n=0-3, and
wherein the water-free spin finish is applied on said precursor material before drying of said precursor material.

13. A method according to claim 12 wherein the stabilization is performed at a temperature from about 100 to about 450° C., wherein the stabilization is done at a residence time of from 10 to 180 minutes.

14. A method according to claim 12 further comprising:
h) performing a stretch-pre-carbonization on the stabilized carbon fiber to produce a highly oriented intermediate carbon fiber.

15. The method according to claim 14 wherein the stretch-pre-carbonization is realized by stretching the stabilized fiber up to 10-fold at a temperature below 1300° C.

16. The method according to claim 14 wherein the stretch-pre-carbonization is realized by stretching the stabilized fiber up to 10-fold at a temperature below 1100° C.

17. The method according to claim 14 wherein the stretch-pre-carbonization is realized by stretching the stabilized fiber up to 10-fold at a temperature below 1000° C.

18. A method according to claim 14 further comprising the following steps:
i) performing a carbonization step on the intermediate carbon fiber, thus providing a carbon fiber.

19. A method according to claim 12 further comprising:
i) performing a carbonization step on the stabilized carbon fibre, thus providing a carbon fiber.

20. A method according to claim 19 wherein the carbonization is performed at a temperature from 900 to 2000° C., in an inert gas.

21. A method according to claim 19 wherein the carbonization is performed at a temperature from 1200 to 1800°° C. in an inert gas.

22. A method according to claim 12 wherein the one or more aprotic polar solvent has a dipole moment in the range of from 5×10 −30 Cm to 10×10 −30 Cm.

23. A method according to claim 12 wherein the stabilization is performed at a temperature from about 200 to about 300° C., wherein the stabilization is done at a residence time of from 10 to 180 minutes.

24. A method according to claim 12 wherein the stabilization is performed at a temperature from about 220 to about 280° C. wherein the stabilization is done at a residence time of from 10 to 180 minutes.

25. A method according to claim 12 wherein the stabilization is performed at a temperature from about 100 to about 450° C., wherein the stabilization is done at a residence time of from 20 to 80 minutes.

26. A method according to claim 12 wherein the stabilization is performed at a temperature from about 200 to about 300° C., wherein the stabilization is done at a residence time of from 20 to 80 minutes.

27. A method according to claim 12 wherein the stabilization is performed at a temperature from about 220 to about 280° C. wherein the stabilization is done at a residence time of from 20 to 80 minutes.

Assignees

• Stora Enso Oyj

Inventors

• Garoff Niklas
• Protz Robert
• Erdmann Jens
• Ganster Johannes
• Lehmann Andre

Classifications

• D01F9/22

  from polyacrylonitriles · CPC title

• C08L1/02

  Cellulose; Modified cellulose · CPC title

• D01F9/16

  from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate (D01F9/18 takes precedence) · CPC title

• D01F11/00

  Chemical after-treatment of artificial filaments or the like during manufacture · 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