Porous polymer beads and process

• US 5,314,923 A
• Filed: 08/29/1991
• Issued: 05/24/1994
• Est. Priority Date: 11/23/1988
• Status: Expired due to Fees

• Current Assignee: Cytec Technology Corp.
• Original Assignee: Cytec Technology Corp.
• Inventors: Hiscock, Laura J., Cooke, Michael T.
• Primary Examiner(s): Kight, III, John
• Assistant Examiner(s): COONEY, JOHN M
• Application Number:
  US07/752,915
• Time in Patent Office: 999 Days
• Field of Search: 521/56, 521/60, 521/64, 521/84.1, 521/89, 521/142, 521/143, 521/144, 521/147, 521/149, 428/402, 428/409, 528/491
• US Class Current: 521/64
• CPC Class Codes: B01J 20/26 Synthetic macromolecular compounds
• CPC Class Codes: C08J 2201/052 Inducing phase separation by thermal treatment, e.g. cooling a solution
• CPC Class Codes: C08J 3/12 Powdering or granulating
• CPC Class Codes: C08J 9/28 by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
• CPC Class Codes: Y10T 428/2982 Particulate matter [e.g., sphere, flake, etc.]
• CPC Class Codes: Y10T 428/31 Surface property or characteristic of web, sheet or block

Abstract

Isotropic porous polymer beads having a high surface porosity and large pore diameters from about 0.002 to about 5 microns are produced from solutions of a polymer or a copolymer by a thermally-induced phase separation process. The use of mixed solvent-non-solvent combinations as solvents for the polymers, produces high pore content, substantially spherical beads having a morphology ideally suited to the chromatography of large molecules, such as proteins, and for enzyme-binding.

Claims

1. A process for the preparation of isotropic polymer beads, said process comprising:

(i) heating and mixing a polymer or copolymer selected from the group consisting of vinyl addition polymers, condensation polymers and oxidation polymers which are soluble in a liquid medium and form rigid structures at the temperatures at which said beads will be used with a mixture comprising an organic or inorganic liquid solvent capable of dissolving said polymer or copolymer without permanent chemical transformation and a liquid non-solvent which is immiscible with said polymer or copolymer to form a homogeneous solution;

(ii) breaking said homogenous solution into droplets;

(iii) cooling said droplets, optionally in the presence of an inert liquid, to bring about phase separation and solidification of the polyerm or copolymer in the droplets; and

(iv) separating the droplets from any inert liquid and the solvent-non-solvent mixture to produce isotropic porous beads.

2. A process as defined in claim 1 wherein said solvent is dimethyl sulfone, the non-solvent is urea, water, propylene glycol, ethylene glycol or a mixture thereof and step (i) is carried out at a temperature of at least about 130°

C.

3. A process as defined in claim 1 wherein the inert liquid is mineral oil, heptane or a mixture thereof.

4. A process as defined in claim 2 wherein the beads are extracted with acetone, methanol, water or a mixture of any of the foregoing.

5. A process as defined in claim 1 wherein said polymer is polymerized methyl methacrylate or polysulfone.

6. A process as defined in claim 1 wherein said homogeneous solution contains less then about 10 weight percent of polymer or copolymer.

7. A process as defined in claim 1 or 6 wherein the polymer is polyacrylonitrile.

8. A process as defined in claim 1 wherein said isotropic porous polymer beads are skinless.

9. A process as defined in claim 1 wherein the homogeneous solution of step (i) contains less than about 10 weight percent total polymer or copolymer solids and the isotropic porous polymer beads are skinless.

10. The product of the process of claim 1.

11. The product of the process of claim 6.

12. The product of the process of claim 7.

13. The product of the process of claim 8.

14. The product of the process of claim 9.