Extraction and fractionation of biopolymers and resins from plant materials

• US 7,259,231 B2
• Filed: 10/12/2005
• Issued: 08/21/2007
• Est. Priority Date: 10/12/2004
• Status: Active Grant

• Current Assignee: Yulex Corporation
• Original Assignee: Yulex Corporation
• Inventors: Marentis, Rodger T., Martin, Jeffrey A., Cornish, Katrina, Plamthottam, Sebastian
• Primary Examiner(s): WOODWARD, ANA LUCRECIA
• Application Number:
  US11/249,884
• Publication Number:
  US 20060106183A1
• Time in Patent Office: 678 Days
• Field of Search: 528/1, 528930-931, 528/937, 528/483, 528/489, 528/499, 528/500, 528/502.A, 528/502.C, 528/490, 528/493, 528/494, 528/495, 528/496, 209/19, 209/21, 209/133
• US Class Current: 528/483
• CPC Class Codes: B01D 11/0203 with a supercritical fluid
• CPC Class Codes: B01D 11/0219 Fixed bed of solid material
• CPC Class Codes: B01D 11/0288 Applications, solvents
• CPC Class Codes: B01D 11/0292 Treatment of the solvent
• CPC Class Codes: C08C 2/02 Purification
• CPC Class Codes: C09F 1/00 Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
• CPC Class Codes: Y02P 20/54 using solvents, e.g. supercritical solvents or ionic liquids
• CPC Class Codes: Y10S 528/93 Guayule rubber

Abstract

A method for the extraction, separation, fractionation and purification of biopolymers from plant materials using supercritical and/or subcritical solvent extractions is disclosed. Specifically, the process can be used for the separation of resins and rubber from guayule shrub (Parthenium argentatum), and other rubber and/or resin containing plant materials, using supercritical solvent extraction, for example supercritical carbon dioxide extraction. Additionally, polar and/or non-polar co-solvents can be used with supercritical carbon dioxide to enhance the selective extraction of resins and rubbers from the shrub.

Claims

1. A method for removing a non-resin biopolymer from plant material, comprising:

contacting plant material with a compressed gas solvent compressed from about 1,500 psi to about 10,000 psi, wherein the temperature and pressure of the solvent are at supercritical conditions;

maintaining the supercritical conditions for a sufficient time, wherein the biopolymer solubilizes with the solvent forming a supercritical solution; and

extracting the biopolymer by percolation of the supercritical solution through a bed of the plant material and wherein the plant material is guayule.

2. The method of claim 1, wherein the solvent is carbon dioxide.

3. The method of claim 2, further including contacting the plant material with a co-solvent.

4. The method of claim 3, wherein the co-solvent is a polar co-solvent.

5. The method of claim 3, wherein the co-solvent is a non-polar co-solvent.

6. The method of claim 3, wherein the step of contacting with the solvent and the step of contacting with the co-solvent are performed either sequentially or in reverse order.

7. The method of claim 3, wherein the step of contacting with the solvent and the step of contacting with the co-solvent are performed at approximately the same time.

8. The method of claim 1, wherein the pressure is between about 5,000 and 10,000 psi.

9. The method of claim 1, wherein the temperature is between 60 and 100 degrees centigrade.

10. The method of claim 1, further comprising contacting the plant material with a co-solvent.

11. The method of claim 10, wherein the co-solvent is a polar co-solvent.

12. The method of claim 10, wherein the co-solvent is a non-polar co-solvent.

13. The method of claim 10, wherein the step of contacting with the compressed gas solvent and the step of contacting with the co-solvent are performed either sequentially or in reverse order.

14. The method of claim 10, wherein the step of contacting with the compressed gas solvent and the step of contacting with the co-solvent are performed at approximately the same time.

15. The method of claim 1, further comprising extracting a resin from the plant material to form a non-resin biopolymer and resin extraction.

16. The method of claim 15, further comprising fractionating the nonresin biopolymer and resin extraction into a non-resin biopolymer fraction and a resin fraction.

17. A method for removing a non-resin biopolymer from plant material, comprising:

contacting plant material with a compressed gas solvent compressed from about 1,500 psi to about 10,000 psi, wherein the temperature and pressure of the solvent are at supercritical conditions;

maintaining the supercritical conditions for a sufficient time, wherein the biopolymer solubilizes with the solvent forming a supercritical solution; and

extracting the biopolymer by percolation of the supercritical solution through a bed of the plant material and wherein the biopolymer is rubber.

18. The method of claim 17, wherein the solvent is carbon dioxide.

19. The method of claim 17, wherein the pressure is between about 5,000 and 10,000 psi.

20. The method of claim 17, wherein the temperature is between 60 and 100 degrees centigrade.

21. The method of claim 17, further including extracting a resin from the plant material to form a non-resin biopolymer and resin extraction.

22. The method of claim 21, further comprising fractionating the non-resin biopolymer and resin extraction into a biopolymer fraction and a resin fraction.

23. A method for removing a biopolymer from plant material, comprising:

contacting plant material with a compressed gas solvent compressed from about 1,500 psi to about 10,000 psi, wherein the temperature and pressure of the solvent are at subcritical liquid conditions;

maintaining the subcritical liquid conditions for a sufficient time, wherein the biopolymer and the solvent form a subcritical liquid solvent solution; and

extracting the biopolymer by percolation of the subcritical liquid solvent solution through a bed of the plant material and wherein the plant material is guayule.

24. The method of claim 23, further comprising using an inert percolation aid.

25. The method of claim 24, wherein the percolation aid is diatomaceous earth.

26. The method of claim 23, wherein the solvent is carbon dioxide.

27. The method of claim 23, wherein the solvent is water.

28. A method for removing a biopolymer from plant material, comprising:

contacting plant material with a compressed gas solvent compressed from about 1,500 psi to about 10,000 psi, wherein the temperature and pressure of the solvent are at subcritical liquid conditions;

maintaining the subcritical liquid conditions for a sufficient time, wherein the biopolymer and the solvent form a subcritical liquid solvent solution; and

extracting the biopolymer by percolation of the subcritical liquid solvent solution through a bed of the plant material and wherein the biopolymer is rubber.

29. The method of claim 28, further comprising using an inert percolation aid.

30. The method of claim 29, wherein the percolation aid is diatomaceous earth.

31. The method of claim 28, wherein the solvent is carbon dioxide.

32. The method of claim 28, wherein the solvent is water.

33. A method for removing a non-polar rubber and a polar resin from guayule, comprising:

contacting guayule with carbon dioxide in an extraction vessel, wherein the temperature in the extraction vessel is between 60 and 100 degrees centigrade and the pressure in the extraction vessel is between 5,000 and 10,000 psi;

further contacting the guayule with a co-solvent in the extraction vessel, wherein the contact with the co-solvent occurs at approximately the same time as the contact with the carbon dioxide; and

extracting the rubber and resin by percolation of a formed supercritical solution through a bed of guayule, to form a rubber-resin extraction.

34. The method of claim 33, wherein the co-solvent is a non-polar solvent.

35. The method of claim 34, further comprising a third solvent, wherein the third solvent is a polar solvent.

36. The method of claim 33, wherein the co-solvent is a polar solvent.

37. The method of claim 33, further comprising fractionating the rubber-resin extraction into a rubber fraction and a resin fraction.

38. The method of claim 33, wherein the co-solvent ratio is between 3 to 10 times a pre-determined feedstock weight.