Multilayer interfacial composite membrane

• US 5,049,167 A
• Filed: 12/13/1989
• Issued: 09/17/1991
• Est. Priority Date: 12/13/1989
• Status: Expired due to Term

• Current Assignee: Membrane Technology and Research, Inc.
• Original Assignee: Membrane Technology and Research, Inc.
• Inventors: Castro, Robert P., Wijmans, Johannes G., Baker, Richard W.
• Primary Examiner(s): SPITZER, ROBERT H
• Application Number:
  US07/450,278
• Time in Patent Office: 643 Days
• Field of Search: 55/16, 55/68, 55/158
• US Class Current: 95/55
• CPC Class Codes: B01D 69/125 In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
• CPC Class Codes: B01D 69/1251 by interfacial polymerisation

Abstract

A composite membrane particularly useful for gas separation or pervaporation. The membrane has three layers: a microporous substrate, an intermediate sealing layer, and a top permselective layer. The permselective layer is made by interfacial polymerization directly on the sealing layer. The sealing layer prevents penetration of the interfacial polymerization reagents into the substrate pores during membrane preparation and provides a gutter layer in the finished membrane.

Claims

1. A separation process, comprising the steps of:

(a) providing a separation membrane having a feed side and a permeate side, said membrane comprising;

a microporous substrate layer;

a sealing layer coating said microporous substrate layer;

an interfacially polymerized permselective layer formed on said sealing layer;

(b) contacting said feed side with a feed fluid mixture comprising component A and component B;

(c) withdrawing from said permeate side a gas mixture enriched in component A compared with said feed fluid mixture.

2. The process of claim 1, wherein said component A is hydrogen.

3. The process of claim 1, wherein said component A is hydrogen and said component B is carbon dioxide.

4. The process of claim 1, wherein said membrane has a selectivity for component A over component B of at least 10.

5. The process of claim 1, wherein said sealing layer comprises a polymer that takes no part in a reaction used to form said permselective layer.

6. The process of claim 1, wherein said permselective layer is selectively permeable to hydrogen over carbon dioxide.

7. A membrane suitable for use in gas separation or pervaporation, comprising:

a microporous substrate layer;

a sealing layer coating said microporous substrate layer;

an interfacially polymerized permselective layer formed on said sealing layer.

8. The membrane of claim 7, wherein said permselective layer is produced by reacting a first reagent and a second reagent, both reagents having two or more functional groups.

9. The membrane of claim 8, wherein said first reagent has two functional groups and said second reagent has three functional groups.

10. The membrane of claim 8, wherein said first reagent is a diamine.

11. The membrane of claim 10, wherein said diamine is 1,6-hexane diamine.

12. The membrane of claim 8, wherein said second reagent is a trifunctional acyl halide.

13. The membrane of claim 12, wherein said trifunctional acyl halide is 1,3,5-benzene tricarbonyl trichloride.

14. The membrane of claim 7, having a sealing layer comprising a rubbery polymer.

15. The membrane of claim 7, having a sealing layer comprising silicone rubber.

16. The membrane of claim 7, characterized in that the membrane exhibits a selectivity for a more permeable gas over a less permeable gas of at least 10.

17. The membrane of claim 16, wherein said more permeable gas is hydrogen.

18. The membrane of claim 17, wherein said less permeable gas is carbon dioxide.

19. The membrane of claim 7, wherein said sealing layer comprises a polymer that takes no part in a reaction used to form said permselective layer.

20. The membrane of claim 7, wherein said permselective layer is selectively permeable to hydrogen over carbon dioxide.

21. A process for preparing a separation membrane, comprising:

providing a microporous substrate;

coating said substrate with a sealing layer, to form a composite support membrane;

contacting said composite support membrane with a first solution containing a first reagent for a first contact period; and

contacting said composite support membrane with a second solution containing a second reagent for a second contact period.

22. The process of claim 21, wherein said first solution comprises an organic solvent.

23. The process of claim 22, wherein said organic solvent comprises hexane.

24. The process of claim 21, wherein said first solution comprises water.

25. The process of claim 21, wherein said first reagent has at least two functional groups.

26. The process of claim 21, wherein said first reagent is a diamine.

27. The process of claim 21, wherein said first reagent is 1,6-hexane diamine.

28. The process of claim 21, wherein said first reagent is trifunctional acyl halide.

29. The process of claim 21, wherein said trifunctional acyl halide is 1,3,5-benzene tricarbonyl trichloride.

30. The process of claim 21, wherein said first contact time is up to 30 minutes.

31. The process of claim 21, wherein said second contact time is up to 10 minutes.