Method for recovering organic fibers from a composite material

Patent metadata

Field	Value
Publication number	US-10167374-B2
Application number	US-201414899420-A
Country	US
Kind code	B2
Filing date	Jun 19, 2014
Priority date	Jun 20, 2013
Publication date	Jan 1, 2019
Grant date	Jan 1, 2019

Abstract

The invention relates to a method for recovering organic fibers from a composite material comprising a polymer matrix and organic fibers, wherein the method comprises the following steps: providing a solution comprising a mixture of water and alcohol; placing the composite material inside a reactor; contacting the mixture and the composite material in order to perform a solvolysis reaction of the composite material; and recovering the organic fibers; wherein the pressure and the temperature in the reactor are adjusted such as to fall within the homogeneous sub-critical range of the phase diagram, within the super-critical range or near the critical point; and wherein the temperature is lower than the melting temperature of the organic fibers.

First claim

The invention claimed is:

1. A method for recovering organic fibers from a composite material comprising a polymer matrix and organic fibers, the method comprising the following steps:
providing a solution comprising a mixture of water and alcohol;
disposing the composite material inside a reactor;
placing the mixture in contact with said composite material in order to carry out a solvolysis reaction of said polymer matrix of said composite material;
recovering said organic fibers;
wherein said organic fibers are selected from aramid fibers, plant fibers and any mixture thereof;
wherein the pressure and temperature in said reactor are adjusted so as to fall within the homogeneous subcritical region of the phase diagram, within the supercritical region, or within 50° C. of the critical temperature and within 50 bar of the critical pressure;
wherein said temperature is below the degradation temperature of the organic fibers and is set to at most 300° C.; and
wherein said mixture of water and alcohol has a water/alcohol volume ratio of between 50:50 and 75:25.

2. The method according to claim 1 , wherein the temperature and/or pressure is supercritical.

3. The method according to claim 1 , wherein said aramid fibers are selected from the group consisting of metaaramid fibers, paraaramid fibers, para-aramid and meta-aramid copolymer fibers, and any mixture thereof.

4. The method according to claim 1 , wherein said plant fibers are selected from the group consisting of flax fibers, banana fibers, hemp fibers, nettle fibers, coconut fibers, henequen fibers, sisal fibers, jute fibers, ramie fibers, fibers from wheat straw or any other grain, wood fibers, and any mixture thereof.

5. The method according to claim 1 , wherein said polymer matrix is thermoset polymer or thermoplastic polymer.

6. The method according to claim 1 , wherein said mixture of water and alcohol has a water/alcohol volume ratio of between 50:50 and 70:30.

7. The method according to claim 1 , wherein said mixture and the composite material are placed in contact for 15 to 105 minutes.

8. The method according to claim 1 , wherein said mixture and the composite material are placed in contact by circulating a stream of said mixture through the reactor inside which said composite material is disposed.

9. The method according to claim 1 , further comprising the step consisting in reducing said composite material to granules before being placed in contact with said mixture.

10. The method according to claim 1 , further comprising the recovery of effluent produced by the solvolysis and discharged outside the reactor; and optionally the burning of the effluent to heat the reactor.

11. The method according to claim 1 , wherein the pressure and temperature in said reactor are adjusted so as to fall within the homogeneous subcritical region of the phase diagram.

12. The method according to claim 1 , wherein said organic fibers are flax fibers.

13. The method according to claim 1 , wherein said alcohol is selected from the group consisting of methanol, ethanol, n-propanol, isopropanol, glycerol and any mixture thereof.

14. The method according to claim 1 , wherein said plant fibers are cotton fibers.

15. The method according to claim 1 , wherein said polymer matrix is depolymerized.

16. The method according to claim 6 , wherein said mixture of water and alcohol has a water/alcohol volume ratio of between 50:50 and 60:40.

17. The method according to claim 1 , wherein said mixture and said composite material are placed in contact for 45 to 75 minutes.

18. The method according to claim 1 , further comprising the recovery of effluent produced by the solvolysis and discharged outside said reactor; and the burning of the effluent to heat said reactor.

19. A method for recovering organic fibers from a composite material consisting of a polymer matrix and organic fibers, the method comprising the following steps:
providing a solution comprising a mixture of water and alcohol;
disposing said composite material inside a reactor;
placing said mixture in contact with said composite material in order to carry out a solvolysis reaction of said polymer matrix of said composite material;
recovering said organic fibers;
wherein the organic fibers are selected from aramid fibers or plant fibers;
wherein the pressure and temperature in said reactor are adjusted so as to fall within the homogeneous subcritical region of the phase diagram, within the supercritical region, or within 50° C. of the critical temperature and within 50 bar of the critical pressure;
wherein the temperature is below the degradation temperature of the organic fibers and is set to at most 300° C.; and
wherein said mixture of water and alcohol has a water/alcohol volume ratio of between 50:50 and 75:25.

20. A method for recovering organic fibers from a composite material consisting of a polymer matrix, organic fibers and filler, the method comprising the following steps:
providing a solution comprising a mixture of water and alcohol;
disposing said composite material inside a reactor;
placing said mixture in contact with said composite material in order to carry out a solvolysis reaction of said polymer matrix of said composite material;
recovering said organic fibers;
wherein the organic fibers are selected from aramid fibers or plant fibers;
wherein the pressure and temperature in the reactor are adjusted so as to fall within the homogeneous subcritical region of the phase diagram, within the supercritical region, or within 50° C. of the critical temperature and within 50 bar of the critical pressure;
wherein the temperature is below the degradation temperature of the organic fibers and is set to at most 300° C.; and
wherein said mixture of water and alcohol has a water/alcohol volume ratio of between 50:50 and 75:25.

21. A method for recovering organic fibers from a composite material comprising a polymer matrix and organic fibers, the method comprising the following steps:
providing a solution comprising a mixture of water and alcohol;
disposing the composite material inside a reactor;
placing the mixture in contact with said composite material in order to carry out a solvolysis reaction of said polymer matrix of said composite material;
recovering said organic fibers;
wherein said organic fibers are selected from aramid fibers, plant fibers and any mixture thereof;
wherein the pressure and temperature in said reactor are adjusted so as to fall within the homogeneous subcritical region of the phase diagram, within the supercritical region, or within 50° C. of the critical temperature and within 50 bar of the critical pressure;
wherein said temperature is below the degradation temperature of the organic fibers and is set to at most 300° C.;

wherein said alcohol is selected from the group consisting of methanol, ethanol, n-propanol, isopropanol, glycerol or a mixture thereof; and
wherein said mixture of water and alcohol has a water/alcohol volume ratio of between 50:50 and 75:25.

Assignees

• Centre Nat Rech Scient
• Univ Bordeaux
• Airbus Operations Sas
• Univ Bordeaux
• Airbus Operations Sas

Inventors

• Aymonier Cyril
• Loppinet Serani Anne
• Debeauvais Antoine

Classifications

• C08J2300/22

  Thermoplastic resins · CPC title

• C08J2377/00

  Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers · CPC title

• B29B2017/0293

  Dissolving the materials in gases or liquids · CPC title

• Y02W30/704

  Cross-Sectional Technologies · mapped topic

• B29B17/02

  Separating plastics from other materials · CPC title