Porous polymer structures

• US 8,222,308 B2
• Filed: 04/05/2007
• Issued: 07/17/2012
• Est. Priority Date: 04/07/2006
• Status: Expired due to Fees

• Current Assignee: The University of Queensland
• Original Assignee: The University of Queensland
• Inventors: Cooper-White, Justin John, Cao, Yang
• Primary Examiner(s): Kugel, Timothy J.
• Application Number:
  US12/296,178
• Publication Number:
  US 20090270519A1
• Time in Patent Office: 1,930 Days
• Field of Search: 521/63, 521/61, 521/64, 516/98, 516/99
• US Class Current: 521/63
• CPC Class Codes: C08J 2201/052 Inducing phase separation by thermal treatment, e.g. cooling a solution
• CPC Class Codes: C08J 9/28 by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum

Abstract

A method of preparing a porous polymer structure comprising the steps of: forming a liquid composition comprising at least one polymer dissolved in at least one solvent; subjecting the liquid composition to stress, and if necessary also to a reduction in temperature, to cause the liquid composition to form a bi-continuous phase separated composition, the bi-continuous phase separated composition comprising a polymer rich phase and a polymer poor phase; solidifying the at least one polymer in the polymer rich phase; and removing the polymer poor phase from the polymer rich phase to provide the porous polymer structure having a bi-continuous morphology from the polymer rich phase.

Claims

1. A method of preparing a porous polymer structure comprising the steps of:

forming a liquid composition comprising at least one polymer dissolved in at least one solvent;

subjecting the liquid composition to stress, to cause the liquid composition to form a bi-continuous phase separated composition, the bi-continuous phase separated composition comprising a polymer rich phase and a polymer poor phase;

solidifying the at least one polymer in the polymer rich phase; and

removing the polymer poor phase from the polymer rich phase to provide the porous polymer structure having a bi-continuous morphology from the polymer rich phase.

2. The method of claim 1 wherein the liquid composition is prepared by heating the at least one polymer and at least one solvent to a temperature required to dissolve an amount of at least one polymer in the solvent.

3. The method of claim 2 wherein all of the at least one polymer is dissolved in the at least one solvent to form a homogeneous solution.

4. The method of claim 2 wherein the amount of polymer dissolved in the liquid composition is about 0.5 to about 50 wt % based on the total weight of the liquid composition.

5. The method of claim 1 wherein the liquid composition further comprises additives selected from the list of dyes, pigments, stabilizers and bioactive substances.

6. The method of claim 5 further comprising the step of adding the additives to the liquid composition prior to forming the bi-continuous phase separated composition.

7. The method of claim 1, further include a step of subjecting the liquid composition to a reduction in temperature;

wherein the temperature is reduced during the step of subjecting the liquid composition to stress.

8. The method of claim 1 wherein the stress is at least one form selected from the group of shear stress, compressive stress and extensional stress.

9. The method of claim 1 wherein the bi-continuous morphology of the porous polymer structure is a plurality of interconnected pores having a cellular structure.

10. The method of claim 1 wherein the bi-continuous phase separated composition comprises greater than 50% of the polymer rich phase.

11. The method of claim 1 wherein the bi-continuous phase separated composition comprises greater than 60% of the polymer rich phase.

12. The method of claim 1 wherein the bi-continuous phase separated composition comprises greater than 80% of the polymer rich phase.

13. The method of claim 1 wherein the liquid composition further comprises a non-solvent, the non-solvent being miscible with the at least one solvent.

38. A porous polymer structure produced by the method of any one of claim 1, 14 or 26, wherein at least a portion of the polymer has a bi-continuous morphology comprising a plurality of interconnected pores having a cellular structure.

14. A method of preparing a porous polymer structure comprising the steps of:

forming a liquid composition comprising at least one polymer dissolved in at least one solvent;

subjecting the liquid composition to stress to decrease the Gibbs free energy of mixing of the composition and form a homogeneous solution;

simultaneously or consecutively decreasing the temperature of the liquid composition to form a bi-continuous phase separated composition, the bi-continuous phase separated composition comprising a polymer rich phase and a polymer poor phase;

solidifying the at least one polymer in the polymer rich phase; and

removing the polymer poor phase from the polymer rich phase to provide the porous polymer structure having a bi-continuous morphology from the polymer rich phase.

15. The method of claim 14 wherein different levels of stress are applied to different regions of the liquid composition to cause differing morphologies to form in the bi-continuous phase separated composition.

16. The method of claim 15 wherein a continuous level of stress variation is applied across the liquid composition.

17. The method of claim 15 wherein a discreet level of stress variation is applied across the liquid composition.

18. The method of claim 15 wherein a temperature gradient is applied across the liquid composition while the liquid composition is subjected to stress.

19. The method of claim 14 wherein the bi-continuous phase separated composition is formed at a temperature above the glass transition temperature of at least one polymer and the freezing temperature of the solvent.

20. The method of claim 19 wherein the liquid composition is held at said temperature for a pre-determined time.

21. The method of claim 14 wherein a stress gradient is established in the liquid composition to cause different morphologies to form across the stress gradient.

22. The method of claim 14 wherein the bi-continuous phase separated composition is held at a temperature below either the glass transition temperature of the at least one polymer or the freezing temperature of the at least one solvent.

23. The method of claim 14 wherein the solidification of the bi-continuous phase separated composition includes the step of reducing the temperature of the liquid composition to a temperature below the glass transition temperature of the at least one polymer and/or below the freezing temperature of the at least one solvent.

24. The method of claim 14 wherein the solidification of the bi-continuous phase separated composition includes the step of subjecting the liquid composition to sufficient pressure to induce solvent crystallisation and/or causing the at least one polymer to solidify.

25. The method of claim 14 wherein the step of removing the polymer poor phase includes the steps of:

adding a further solvent, the further solvent being miscible or soluble with the at least one solvent and a non-solvent of the polymer structure; and

extracting or leaching the further solvent from the polymer rich phase.

26. A method of preparing a porous polymer structure comprising the steps of:

forming a liquid composition comprising at least one polymer dissolved in at least one solvent, the liquid composition being a homogeneous solution at a predetermined temperature;

subjecting the liquid composition to stress at the predetermined temperature to increase the Gibbs-free energy of mixing of the composition causing the liquid composition to form a bi-continuous phase separated composition at the predetermined temperature, the bi-continuous phase separated composition comprising a polymer rich phase and a polymer poor phase;

solidifying the at least one polymer in the polymer rich phase; and

removing the polymer poor phase from the polymer rich phase to provide the porous polymer structure having a bi-continuous morphology from the polymer rich phase.

27. A porous polymer structure produced by the method of claim 26, wherein at least a portion of the polymer has a bi-continuous morphology comprising a plurality of interconnected pores having a cellular structure.

28. The method of claim 26 wherein the bi-continuous phase separated composition is held at a temperature below either the glass transition temperature of the at least one polymer or the freezing temperature of the at least one solvent.

29. The method of claim 26 wherein the solidification of the bi-continuous phase separated composition includes the step of reducing the temperature of the liquid composition to a temperature below the glass transition temperature of the at least one polymer and/or below the freezing temperature of the at least one solvent.

30. The method of claim 26, wherein the solidification of the bi-continuous phase separated composition includes the step of subjecting the liquid composition to a pressure to induce solvent crystallisation and/or causing the at least one polymer to solidify.

31. A porous polymer structure wherein at least a portion of the polymer has a bi-continuous morphology comprising a plurality of interconnected pores having a cellular structures;

wherein the polymer has regions of different morphology.

32. The porous polymer structure of claim 31 wherein the plurality of interconnected pores forms an interconnected pore network.

33. The porous polymer structure of claim 32 wherein the structure forms at least part of a tissue scaffold in tissue engineering or tissue guided regeneration applications.

34. The porous polymer structure of claim 31 wherein the polymer incorporates an additive into the walls of the cellular structure.

35. The porous polymer structure of claim 34 wherein the additive is selected from the group consisting of dyes, pigments, stabilizers and bioactive substances.

36. The porous polymer structure of claim 34 wherein the structure forms at least part of a tissue scaffold in tissue engineering or tissue guided regeneration applications.

37. The porous polymer structure of claim 31 wherein the polymer has a uniform cellular structure.