IP Library Granted Patent US 9,790,346
Granted Patent B2
US 9,790,346 · App. 14/889,395 · Granted Oct 17, 2017

Methods for recovering carbon fiber from carbon-fiber-reinforced polymer (CFRP) composites

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Quick Facts
Patent No.
US 9,790,346
App. No.
14/889,395
Granted
Oct 17, 2017
Kind
B2
Abstract

Method for recovering carbon fibers from carbon fiber reinforced polymer composites is provided. The recovered carbon fibers can be separable and can be substantially free of thermosetting resins. Compositions comprising said recovered carbon fibers are also provided.

Claims (34)

1. A method of recovering carbon fibers from fiber-reinforced composite, the method comprising:

providing the fiber-reinforced composite comprising the carbon fibers and a thermosetting resin;

contacting the fiber-reinforced composite with a first organic solvent including an alcohol to form carbon fiber bundles from the fiber-reinforced composite;

after contacting the fiber-reinforced composite with the first organic solvent, contacting the carbon fiber bundles with an acid solution to form acid-treated carbon fibers; and

contacting the acid-treated carbon fibers with a second organic solvent.

2. The method of claim 1 , wherein the thermosetting resin comprises an epoxy resin or a phenol resin.

3. The method of claim 1 , wherein the alcohol of the first organic solvent includes benzyl alcohol.

4. The method of claim 1 , wherein the second organic solvent includes an alcohol.

5. The method of claim 4 , wherein the second organic solvent includes benzyl alcohol.

6. The method of claim 1 , wherein contacting the fiber-reinforced composite with the first organic solvent comprises heating the fiber-reinforced composite and the first organic solvent to a temperature of about 50° C. to about 200° C.

7. The method of claim 1 , wherein contacting the acid-treated carbon fibers with the second organic solvent comprises heating the acid-treated carbon fibers and the second organic solvent to a temperature of about 50° C. to about 200° C.

8. The method of claim 1 , wherein the acid solution comprises nitric acid.

9. The method of claim 1 , wherein contacting the carbon fiber bundles with the acid solution comprises heating the carbon fiber bundles and the acid solution to a temperature of at least about 40° C.

10. The method of claim 1 , further comprising isolating the carbon fibers from the second organic solvent.

11. The method of claim 10 , wherein the carbon fibers, after isolating from the second organic solvent, are separable and substantially free of the thermosetting resin.

12. A method of recovering carbon fibers from fiber-reinforced composite, the method comprising:

providing the fiber-reinforced composite comprising the carbon fibers and a thermosetting resin;

contacting the fiber-reinforced composite with a first organic solvent to form carbon fiber bundles from the fiber-reinforced composite;

combining the carbon fiber bundles with a second organic solvent to form a mixture;

heating the mixture under solvothermal conditions; and

isolating the carbon fibers from the mixture.

13. The method of claim 12 , wherein the thermosetting resin comprises an epoxy resin or a phenol resin.

14. The method of claim 12 , wherein the first organic solvent comprises one or more of chloroform, dichloromethane, tetrahydrofuran, meta-xylene, N,N-dimethylformamide, carbon tetrachloride, benzene, or toluene.

15. The method of claim 12 , wherein the second organic solvent comprises one or more of an alcohol, chloroform, dichloromethane, tetrahydrofuran, meta-xylene, N,N-dimethylformamide, carbon tetrachloride, benzene, or toluene.

16. The method of claim 12 , wherein the first organic solvent includes dichloromethane and the second organic solvent includes benzyl alcohol.

17. The method of claim 12 , wherein the first organic solvent includes chloroform and the second organic solvent includes propanol.

18. The method of claim 12 , wherein heating the mixture under solvothermal conditions occurs in a sealed chamber.

19. The method of claim 12 , wherein heating the mixture under solvothermal conditions comprises heating the mixture to a temperature of about 150° C to about 250° C.

20. The method of claim 12 , wherein the carbon fibers, after isolating from the mixture, are separable and substantially free of the thermosetting resin.

21. A composition comprising:

a non-acidic organic solvent solution, wherein the non-acidic organic solvent comprises one or more of chloroform, dichloromethane, tetrahydrofuran, meta-xylene, N,N-dimethylformamide, carbon tetrachloride, benzene, or toluene;

recycled carbon fibers dispersed in the non-acidic organic solvent; and

a thermosetting resin at least partially dissolved in the non-acidic organic solvent.

22. The composition of claim 21 , wherein the thermosetting resin comprises an epoxy resin or a phenol resin.

Assignments (4)
RELEASE OF SECURITY INTEREST IN PATENTS, RECORDED ON JANUARY 29, 2019 AT REEL 048373 FRAME 0217 Recorded Sep 22, 2025
From: CRESTLINE DIRECT FINANCE, L.P., AS COLLATERAL AGENT
To: EMPIRE TECHNOLOGY DEVELOPMENT LLC
Reel/Frame 072936/0464 →
RELEASE OF SECURITY INTEREST Recorded Jul 31, 2019
From: CRESTLINE DIRECT FINANCE, L.P.
To: EMPIRE TECHNOLOGY DEVELOPMENT LLC
Reel/Frame 049924/0794 →
SECURITY INTEREST Recorded Jan 29, 2019
From: EMPIRE TECHNOLOGY DEVELOPMENT LLC
To: CRESTLINE DIRECT FINANCE, L.P.
Reel/Frame 048373/0217 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 5, 2015
From: ZHAO, CHONGJUN; SHITIAN, MUZI; MA, WEIFENG; QIAN, XIUZHEN; ZHANG, JINCHAO; CHEN, XIN
To: EAST CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
Reel/Frame 036973/0723 →