Process for the manufacture of a shaped body

Patent metadata

Field	Value
Publication number	US-10968540-B2
Application number	US-201615766470-A
Country	US
Kind code	B2
Filing date	Oct 6, 2016
Priority date	Oct 8, 2015
Publication date	Apr 6, 2021
Grant date	Apr 6, 2021

Abstract

The present invention relates to a method for manufacturing a shaped body comprising lignin which may be further processed into intermediate carbon fibers and finally also carbon fibers. Uses of said fibers are also disclosed. The present invention addresses the problem of lignin leaching into a precipitation bath. The solution to this problem is a novel method for minimizing the loss of lignin through the addition of certain salts into the precipitation bath.

First claim

The invention claimed is:

1. A method for manufacturing a shaped body comprising lignin, comprising the following steps:
a) providing cellulose and/or a cellulose derivative,
b) providing lignin and/or a lignin derivative,
c) dissolution of said cellulose and/or a cellulose derivative, and lignin and/or a lignin derivative, followed by subsequent mixing thus providing a dope,
d) performing a shaping of the dope to a precursor material,
e) performing a coagulation of said precursor material in a bath containing a coagulation liquid, wherein the coagulation liquid comprises one or more salts, wherein said one or more salts have cations selected from the 1 st , 2 nd , or 3 rd main groups of the periodic table and
f) drying of said precursor material, thus providing a shaped body comprising lignin.

2. A method for manufacturing a shaped body comprising lignin according to claim 1 wherein said shaping in step d) involves a solvent extrusion step.

3. A method for manufacturing a shaped body comprising lignin according to claim 1 wherein said shaped body is a filament, non-woven fabric film or a membrane.

4. A method for manufacturing a shaped body comprising lignin according to claim 1 wherein a concentration of said cations is in a range of from 0.01 mmol/l up to 1000 mmol/l.

5. A method for manufacturing a shaped body comprising lignin according to claim 1 wherein the coagulation bath in step e) also contains one or more acids.

6. A method for manufacturing a shaped body comprising lignin according to claim 1 wherein the salts are washed out from the shaped body after the coagulation bath treatment in step e).

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

8. A method according to claim 1 comprising the following additional steps:
g) forming the shaped body comprising lignin in the form of a filament, and
h) performing a stabilization on the filament, thus providing a stabilized carbon fibre.

9. A method according to claim 8 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.

10. A method according to claim 8 comprising the following additional step:
i) performing a stretch-pre-carbonization, thus providing a highly oriented intermediate carbon fiber.

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

12. A method according to claim 8 comprising the following additional step:
j) performing a carbonization step on the stabilized carbon fiber, thus providing a carbon fiber.

13. A method according to claim 12 wherein the carbonization is performed at a temperature from 900 to 2000° C.

14. A method for manufacturing a shaped body comprising lignin according to claim 1 wherein said shaped body is a filament.

15. A method for manufacturing a shaped body comprising lignin according to claim 1 wherein said shaped body is a filament yarn.

16. A method for manufacturing a shaped body comprising lignin according to claim 1 wherein said one or more salts in step e) are cations are divalent cations, namely Ca 2+ and Mg 2+ .

17. A method for manufacturing a shaped body
comprising lignin according to claim 1 wherein the concentration of said cations is in the range of from 0.05 mmol/l to 1 mmol/l.

18. A method for manufacturing a shaped body comprising lignin according to claim 1 wherein the coagulation bath in step e) also contains one or more alkaline media.

19. A method according to claim 2 wherein the solvent extrusion in step d) is performed through air-gap spinning or dry jet-wet spinning.

20. A method according to claim 8 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.

21. A method according to claim 8 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.

22. A method according to claim 8 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.

23. A method according to claim 8 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.

24. A method according to claim 8 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.

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

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

27. A method according to claim 10 , further comprising the step:
j) performing a carbonization step on the highly oriented intermediate carbon fiber, thus providing a carbon fiber.

28. A method according to claim 12 wherein the carbonization is performed at a temperature from 1200 to 1800° C.

29. A method according to claim 12 wherein the carbonization is performed in an inert gas.

Assignees

• Stora Enso Oyj

Inventors

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

Classifications

• D01F9/16

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

• C08L97/00

  Compositions of lignin-containing materials (of polysaccharides C08L1/00 - C08L5/00) · 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

• D01F2/02

  from solutions of cellulose in acids, bases or salts · CPC title

• D01F9/17 Primary

  from lignin · CPC title