Process for producing microporous powders and membranes

• US 4,968,733 A
• Filed: 09/01/1989
• Issued: 11/06/1990
• Est. Priority Date: 09/01/1988
• Status: Expired due to Term

• Current Assignee: Membrana GmbH (Asahi Kasei Corporation)
• Original Assignee: Akzo Nobel N.V. (Nouryon BV)
• Inventors: Muller, Heinz-Joachim, Wechs, Friedbert
• Primary Examiner(s): NOT, DEFINED
• Assistant Examiner(s): Sridharan, Anang
• Application Number:
  US07/401,854
• Time in Patent Office: 431 Days
• Field of Search: 521/50, 521/64, 521/90, 521/61, 524/98
• US Class Current: 521/64
• CPC Class Codes: B01D 2323/12 Specific ratios of components used
• CPC Class Codes: B01D 2325/022 Asymmetric membranes
• CPC Class Codes: B01D 67/0018 Thermally induced processes [TIPS]
• CPC Class Codes: B01D 67/003 by selective elimination of components, e.g. by leaching
• CPC Class Codes: B01D 71/68 Polysulfones; Polyethersulfones
• CPC Class Codes: C08J 2201/052 Inducing phase separation by thermal treatment, e.g. cooling a solution
• CPC Class Codes: C08J 2201/0544 the non-solvent being aqueous
• CPC Class Codes: C08J 3/14 by precipitation from solutions C08J3/122 takes precedence
• 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: Y10S 424/07 Microporous membranes

Abstract

A process produces microporous powders or shaped articles, in particular membranes in the form of flat films, tubular films or hollow fibers, which may be used for controlled release of an active compound, for dialysis, gas separation, ultrafiltration or microfiltration, from polyvinylidene fluoride and/or polyphenylene sulfide and/or polysulfone and/or polyacrylonitrile and/or ethylene/vinyl alcohol copolymer and/or ethylene/chlorotrifluoroethylene copolymer and/or polyethersulfone and/or polyether-imide and/or polymethyl methacrylate and/or polycarbonate and/or cellulose triacetate. The process utilizes phase separation by means of thermally induced triggering or triggering induced by a non-solvent of a solution of the polymer in a mixture containing ε-caprolactam as the essential dissolving constituent. The solution may be formed before the phase separation is triggered.

Claims

1. A process for producing microporous powders or shaped articles, comprising preparing a solution of at least one polymer selected from the group consisting of polyvinylidene fluoride, polyphenylene sulfide, polysulfone, polyacrylonitrile, ethylene/vinyl alcohol copolymer, ethylene/chlorotrifluoroethylene copolymer, polyether-sulfone, polyether-imide, polymethyl methacrylate, polycarbonate, cellulose triacetate and copolymers thereof in a solvent mixture containing e-caprolactam as the essential dissolving constituent, forming said solution, and triggering phase separation thermally or by a non-solvent.

2. The process as claimed in claim 1, wherein the solvent mixture contains at least 10% by weight of e-caprolactam.

3. The process as claimed in claim 2, wherein the solvent mixture contains 20-65% by weight of e-caprolactam.

4. The process as claimed in claim 1, wherein the polymer is dissolved at temperatures of 60°

to 240°

C.

5. The process as claimed in claim 1, wherein the phase separation is effected by spontaneous crystallization of the solvent mixture after supercooling.

6. The process as claimed in claim 1, wherein the phase separation is triggered by coagulation in a non-solvent bath.

7. The process as claimed in claim 1, wherein the solvent mixture is comprised of ε

-caprolactam, a latent solvent and a non-solvent, and forms a homogeneous phase with the polymer at elevated temperatures, this homogeneous phase forming two separate liquid phases after cooling to a lower temperature, and wherein the homogeneous phase of polymer and solvent mixture is cooled in such a way that initially a segregation into two liquid phases takes place before solidification of the polymer occurs.

8. The process as claimed in claim 7, wherein said shaped article is a membrane.

9. The process as claimed in claim 7, wherein said solvent mixture is further comprised of a thickener and auxiliaries.

10. The process as claimed in claim 1, wherein said shaped article is a membrane.

11. The process as claimed in claim 10, wherein said membrane is in the form of a flat film, tubular film or hollow fiber.