Method of producing carbon fibers and carbon fiber composites from plant derived lignin and its blends

Patent metadata

Field	Value
Publication number	US-11512173-B2
Application number	US-201715799240-A
Country	US
Kind code	B2
Filing date	Oct 31, 2017
Priority date	Oct 31, 2016
Publication date	Nov 29, 2022
Grant date	Nov 29, 2022

Abstract

Carbon fiber composites containing lignin carbon fibers are described. The lignin carbon fibers can be derived from organosolv lignin obtained from single source lignocellulosic feedstocks or combinations of such feedstocks or lignin obtained via other pulping or extraction methods. Also described are methods of preparing the carbon fiber composites.

First claim

What is claimed is:

1. A carbon fiber reinforced polymer composite comprising:
a polymeric matrix material; and
a lignin carbon fiber embedded in the polymeric matrix material, wherein the lignin carbon fiber is substantially non-crystalline and free of surface defects and has a regular circular cross-section; wherein the lignin carbon fiber is prepared from non-chemically modified lignin isolated from a lignocellulosic feedstock material selected from a grass or a combination of a grass and a hardwood via an organosolv pulping process performed at a temperature of about 140° C. to about 170° C. and by a process comprising thermostabilizing a raw lignin fiber prepared from the non-chemically modified lignin by heating the raw lignin fiber from room temperature to about 250° C. at a rate of about 0.017° C. per minute to about 0.1° C. per minute; and wherein the lignin carbon fiber is free of a surface treatment or coating, and is free of a carbon from a non-lignin source; and further wherein an interfacial shear strength (IFSS) between the lignin carbon fiber and the polymeric matrix material is higher than the IFSS would be between a non-lignin carbon fiber and the same polymeric matrix material.

2. The composite of claim 1 , wherein the composite has a non-explosive failure mechanism.

3. The composite of claim 1 , wherein the lignin carbon fiber is prepared by carbonizing a melt-spun lignin fiber under an inert atmosphere at a temperature of about 1000° C.

4. The composite of claim 1 , wherein the polymeric matrix material comprises a thermoset polymer.

5. The composite of claim 4 , wherein the thermoset polymer is an epoxy.

6. The composite of claim 1 , wherein the lignocellulosic feedstock material is a grass.

7. The composite of claim 1 , wherein the polymeric matrix material comprises a thermoplastic polymer.

8. A method of preparing a carbon fiber reinforced polymer composite, the method comprising:
(a) providing a lignin carbon fiber, wherein the lignin carbon fiber is substantially non-crystalline and free of surface defects and has a regular circular cross-section; wherein the lignin carbon fiber is prepared from non-chemically modified lignin prepared from a lignocellulosic feedstock material selected from a grass or a combination of a grass and a hardwood via an organosolv pulping process performed at a temperature of about 140° C. to about 170° C. and by a process comprising thermostabilizing a raw lignin fiber prepared from the non-chemically modified lignin by heating the raw lignin fiber from room temperature to about 250° C. at a rate of about 0.017° C. per minute to about 0.1° C. per minute to provide a thermostabilized lignin fiber and carbonizing the thermostabilized lignin fiber to provide the lignin carbon fiber; and further wherein the lignin carbon fiber is free of a surface treatment or coating, and is free of a carbon from a non-lignin source; and
(b) embedding the lignin carbon fiber in the polymeric matrix material or a precursor thereof.

9. The method of claim 8 , wherein step (b) comprises placing the lignin carbon fiber in a mold; introducing a thermosetting or thermoplastic polymer resin into the mold, optionally wherein the polymer resin is an epoxy resin; and curing the polymer resin.

10. The method of claim 8 , wherein step (a) comprises:
(i) providing a lignocellulosic feedstock material selected from a grass and a combination of a grass and a hardwood;
(ii) treating the lignocellulosic feedstock material to provide an isolated lignin, wherein said treating comprises an organosolv pulping process performed at a temperature of about 140° C. to about 170° C.;
(iii) melt-spinning the isolated lignin to provide a lignin fiber;
(iv) thermostabilizing the lignin fiber by heating the lignin fiber from room temperature to about 250° C. at a rate of about 0.017° C. per minute to about 0.1° C. per minute to provide a thermostabilized lignin fiber; and
(v) carbonizing the thermostabilized lignin fiber, to provide a lignin carbon fiber.

11. The method of claim 10 , wherein the carbonizing of step (v) comprises heating the thermostabilized lignin fiber under an inert atmosphere from room temperature to about 1000° C. at a rate of about 10° C. per minute or less; and holding the temperature at about 1000° C. for a period of time.

12. The method of claim 10 , wherein the isolated lignin provided by step (ii) has a glass transition temperature (T g ) of between about 107° C. and about 135° C.

13. The method of claim 10 , wherein the isolated lignin provided by step (ii) has a purity of about 95% or more.

14. The method of claim 8 , wherein the lignin carbon fiber has a diameter of about 40 microns or less.

15. The method of claim 8 , wherein the lignin carbon fiber has a failure stress of about 250 MPa or more.

16. The method of claim 8 , wherein the composite has a tensile modulus of about 9 GPa and/or a failure stress of about 85 MPa.

17. A discontinuous fiber composite, wherein the discontinuous fiber composite comprises a polymeric matrix material and a plurality of short lignin carbon fibers embedded in the polymeric matrix material, wherein the lignin carbon fibers are prepared from non-chemically modified lignin prepared from a lignocellulosic feedstock material via an organosolv pulping process performed at a temperature of about 140° C. to about 170° C., wherein the lignocellulosic feedstock material is selected from a grass or a combination of a grass and a hardwood, and further wherein the lignin carbon fibers are prepared by a process comprising themostabilizing raw lignin fibers by heating the raw lignin carbon fibers from room temperature to about 250° C. a rate of about 0.017° C. per minute to about 0.1° C. per minute.

18. The discontinuous fiber composite of claim 17 , wherein the lignin carbon fibers are free of a surface treatment or coating.

Assignees

• Univ Tennessee Res Found
• Tennera Llc

Inventors

• Harper David Paul
• Hosseinaei Omid
• Penumadu Dayakar
• Meek Nathan Kieran
• Webb Daniel
• Mynes James
• Labbe Nicole
• Bozell Joseph John
• Rials Timothy G
• Young Stephen Andrew

Classifications

• C08K3/04

  Carbon · CPC title

• D01F9/17

  from lignin · CPC title

• C08J5/042 Primary

  with carbon fibres · CPC title

• C08J5/24

  Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs · CPC title

• C08J2363/00

  Characterised by the use of epoxy resins; Derivatives of epoxy resins · CPC title