Methods of polymer impregnation

• US 5,340,614 A
• Filed: 02/11/1993
• Issued: 08/23/1994
• Est. Priority Date: 02/11/1993
• Status: Expired due to Term

• Current Assignee: 3M Company
• Original Assignee: 3M Company
• Inventors: Perman, Craig A., Riechert, Manfred E.
• Primary Examiner(s): Owens, Terry J.
• Assistant Examiner(s): CAMERON, ERMA C
• Application Number:
  US08/016,603
• Time in Patent Office: 558 Days
• Field of Search: 427/430.1, 427/2
• US Class Current: 427/2.24
• CPC Class Codes: A61K 9/1647 Polyesters, e.g. poly(lactide-co-glycolide)
• CPC Class Codes: A61K 9/1658 Proteins, e.g. albumin, gelatin
• CPC Class Codes: A61K 9/1694 resulting in granules or microspheres of the matrix type containing more than 5% of excipient
• CPC Class Codes: A61L 17/005 containing a biologically active substance, e.g. a medicament or a biocide
• CPC Class Codes: A61L 2300/252 Polypeptides, proteins, e.g. glycoproteins, lipoproteins, cytokines
• CPC Class Codes: A61L 2300/406 Antibiotics
• CPC Class Codes: A61L 2300/43 Hormones, e.g. dexamethasone
• CPC Class Codes: A61L 2300/442 Colorants, dyes
• CPC Class Codes: A61L 2300/622 Microcapsules
• CPC Class Codes: C08J 7/065 Low-molecular-weight organic substances, e.g. absorption of additives in the surface of the article
• CPC Class Codes: D06M 23/105 Processes in which the solvent is in a supercritical state
• CPC Class Codes: D06P 1/94 using dyes dissolved in solvents which are in the supercritical state
• CPC Class Codes: Y02P 20/54 using solvents, e.g. supercritical solvents or ionic liquids

Abstract

Methods of impregnating various polymer substrates with an impregnation additive, by simultaneously contacting the polymer substrate with an impregnation additive, carrier liquid, and supercritical fluid are provided. The impregnation additive is substantially insoluble in the supercritical fluid, and the carrier liquid is preferably substantially insoluble in the supercritical fluid.

Claims

1. A method of impregnating a polymeric substrate with an impregnation additive comprising:

(a) placing a polymeric substrate into a pressure vessel at atmospheric pressure;

(b) simultaneously contacting the polymeric substrate with a mixture of a carrier liquid and an impregnation additive, wherein the impregnation additive is substantially insoluble in a supercritical fluid;

(c) sealing the pressure vessel;

(d) exposing the polymeric substrate and the mixture of the carrier liquid and impregnation additive to the supercritical fluid in the pressure vessel for time sufficient to swell the polymeric substrate, such that the carrier liquid and impregnation additive at least partially penetrates the swollen polymeric substrate; and

(e) releasing the pressure in the pressure vessel so that the carrier liquid diffuses out of the swollen polymeric substrate, wherein an amount of the impregnation additive is entrapped within the polymeric substrate.

2. A method of impregnating a polymeric material according to claim 1, wherein the supercritical fluid comprises supercritical carbon dioxide.

3. A method of impregnating a polymeric material according to claim 1, wherein the polymeric material is selected from the group consisting of polyolefin polymers, polyamide polymers, polyurethane polymers, silicone polymers, protein derivative polymers, lactic acid polymers, glycolic acid polymers, and combinations thereof.

4. A method of impregnating a polymeric material according to claim 3, wherein the polyolefin polymer is selected from the group consisting of a low density polyethylene, linear low density polyethylene, polypropylene, and combinations thereof.

5. A method of impregnating a polymeric material according to claim 1, wherein the carrier liquid is selected from the group consisting of water, methanol, ethanol, isopropanol, hexane, and combinations thereof.

6. A method of impregnating a polymeric material according to claim 1, wherein the carrier liquid is substantially insoluble in the supercritical fluid.

7. A method of impregnating a polymeric material according to claim 1, wherein the carrier liquid is substantially insoluble in the polymeric material.

8. A method of impregnating a polymeric material according to claim 1, wherein the impregnation additive is substantially insoluble in the polymeric material.

9. A method of impregnating a polymeric material according to claim 1, wherein the impregnation additive is selected from the group consisting of a dye, a protein, a polypeptide, a nucleotide, a drug, a monomer, and combinations thereof.

11. A method of impregnating a polymeric material according to claim 9, wherein the impregnation additive comprises a drug selected from the group consisting of antibiotics, antiinflanunatory agents, cardiovascular agents, analgesics, calcium channel blockers, beta-blockers, antidepressants, antacids, antidiabetics, cerebral stimulants, sedatives, anti-parasitics, decongestants, muscle relaxants, anti-Parkinsonism agents, antiviral agents, bronchodialators, vitamins, dietary supplements, and combinations thereof.

10. A method of impregnating a polymeric substrate with an impregnation additive comprising;

(a) placing a polymeric substrate into a pressure vessel at atmospheric pressure;

(b) simultaneously contacting the polymeric substrate with a mixture of a carrier liquid and an impregnation additive, wherein the impregnation additive is substantially insoluble in a supercritical fluid and comprises a dye selected from the group consisting of fluorescein dyes, indigo dyes, and combinations thereof;

(c) sealing the pressure vessel;

(d) exposing the polymeric substrate and the mixture of the carrier liquid and impregnation additive to the supercritical fluid in the pressure vessel for time sufficient to swell the polymeric substrate, such that the carrier liquid and impregnation additive at least partially penetrates the swollen polymeric substrate; and

(e) releasing the pressure in the pressure vessel so that the carrier liquid diffuses out of the swollen polymeric substrate, wherein an amount of the impregnation additive is entrapped within the polymeric substrate.

12. A method of impregnating a polymeric substrate with a hydrophilic impregnation additive comprising:

(a) placing a polymeric substrate into a pressure vessel at atmospheric pressure;

(b) simultaneously contacting the polymeric substrate with a mixture of a carrier liquid and a hydrophilic impregnation additive;

(c) sealing the pressure vessel;

(d) exposing the polymeric substrate and the mixture of the carrier liquid and hydrophilic impregnation additive to a lipophilic supercritical fluid in the pressure vessel for time sufficient to swell the polymeric substrate, such that the carrier liquid and hydrophilic impregnation additive at least partially penetrates the swollen polymeric substrate; and

(e) releasing the pressure in the pressure vessel so that the carrier liquid diffuses out of the swollen polymeric substrate, wherein an amount of the hydrophilic impregnation additive is entrapped within the polymeric substrate.

13. A method of impregnating a polymeric material according to claim 12, wherein the carrier liquid comprises water.

14. A method of impregnating a polymeric material according to claim 12, wherein the lipophilic supercritical fluid comprises supercritical carbon dioxide.

15. A method of impregnating a polymeric material according to claim 12, wherein the polymeric material is selected from the group consisting of polyolefin polymers, polyamide polymers, polyurethane polymers, silicone polymers, protein derivative polymers, lactic acid polymers, glycolic acid polymers, and combinations thereof.

16. A method of impregnating a polymeric material according to claim 12, wherein the carrier liquid is substantially insoluble in the lipophilic supercritical fluid.

17. A method of impregnating a polymeric material according to claim 12, wherein the carrier liquid is substantially insoluble in the polymeric material.

18. A method of impregnating a polymeric material according to claim 12, wherein the impregnation additive is substantially insoluble in the polymeric material.

19. A method of impregnating a polymeric material according to claim 12, wherein the impregnation additive is selected from the group consisting of a dye, a protein, a polypeptide, a nucleotide, a drug, a monomer, and combinations thereof.