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US5067970A Expired / Lapsed US ⏱️ 0.0 years remaining

Asymmetric polyimide membranes

Assignee: WR Grace and Co Conn
•
Filing: 1990-05-11
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Granted: 1991-11-26
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Expires: 2010-05-11
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Abstract

Abstract An asymmetric membrane and a method for its preparation is disclosed. The membrane is suitable for gas separation, reverse osmosis and pervaporation applications and is characterized in that it is based on a fully imidized 5(6)-amino-1-(4'-aminophenyl)-1,3-trimethylindane polymer having pore diameters of less than 20 Å units, CO 2 /CH 4 selectivity of at least 20 and CO 2 permeability of at least 1.0 SCFH/ft 2 at 100 p.s.i.

Inventors

  • 👤 I-Fan Wang
  • 👤 Bhupender S. Minhas

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-10 01:18
CPC Classifications
C; C08; C08G; C08G73/00; C08G73/06; C08G73/10; C08G73/1075; C08G73/1082; B; B01; B01D; B01D67/00; B01D67/0002; B01D67/0009; B01D67/0011; B01D67/00111; B01D69/00; B01D69/02; B01D69/06; B01D69/08; B01D71/00; B01D71/06; B01D71/58; B01D71/62; B01D71/64; B01D2323/00; B01D2323/12; B01D2325/00; B01D2325/02; B01D2325/022; B01D2325/20

Claims Analysis

Total Claims: 12
Claim 1
Independent Claim 76 words
An asymmetric polyimide membrane comprising a unitary membrane having a thin dense skin supported on a porous substructure, characterized in that (a) said skin and substructure are composed of a fully imidized polymer based on 5(6)-amino-1-(4'-aminophenyl)-1,3-trimethylindane; (b) it has a pre diameter of less than 20 Å; (c) it has a CO 2 /CH 4 selectivity of at least 20; and (d) it has CO 2 permeability of at least 1 SCFH/ft 2 at 100 psi.
Claim 2
Dependent Claim 76 words
An asymmetric polyimide membrane comprising a unitary membrane having a thin dense skin supported on a porous substructure, characterized in that (a) said skin and substructure are composed of a fully imidized polymer based on 5(6)-amino-1-(4'-aminophenyl)-1,3-trimethylindane; (b) it has a pre diameter of less than 20 Å; (c) it has a CO 2 /CH 4 selectivity of at least 20; and (d) it has CO 2 permeability of at least 1 SCFH/ft 2 at 100 psi.
Claim 3
Dependent Claim 34 words
The asymmetric polyimide polymer membrane according to claim 1 wherein said CO 2 /CH 4 selectivity is at least 30 and said CO 2 permeability is at least 2.0 SCFH/ft 2 at 100 p.s.i..
Claim 4
Dependent Claim 21 words
The asymmetrical polyimide polymer membrane according to claims 1 or 2 characterized in that it is formed into a flat sheet.
Claim 5
Dependent Claim 22 words
The as polyimide polymer membrane according to claims 1 or 2 characterized in that it is formed into a hollow fiber configuration.
Claim 6
Dependent Claim 18 words
The membrane of claim 1 having mechanical strength sufficient to withstand a pressure of at least 500 psi.
Claim 7
Dependent Claim 279 words
The process of preparing a polyimide polymer membrane having a pore diameter of less than 20 Å units, a CO 2 /CH 4 selectivity of at least about 20, and a CO 2 permeability of at least 1.0 SCFH/ft 2 at 100 p.s.i., said process comprising the steps of: (a) preparing a polyimide dope solution consisting essentially of: (1) a fully imidized polyimide polymer based on 5(6)-amino-1-(4'-aminophenyl)-1,3-trimethylindane present in amounts of 20 to 28% by weight of said dope solution; (2) a solvent system for said polyimide which is water miscible and is selected from the group consisting essentially of N-methyl-2-pyrrolidone, tetrahydrofuran, N,N-dimethylformamide, dioxane, γ-butyrolactone or a mixture thereof; (3) a low molecular weight non-solvent system present in amounts of less than 10% by weight of said dope solution consisting essentially of water, ketones, alcohols, or formamide; (4) a viscosity enhancer present in amounts of less than 3% by weight of said dope solution consisting essentially of polyvinyl pyrrolidones, polyethylene glycols or urethanes; (5) a void supressor present in amounts of less than 5% by weight of said dope solution consisting essentially of maleic acid; casting a film of said polyimide dope solution onto a supporting substrate; (c) evaporating said solvent system under conditions of time, temperature and air flow rate sufficient to produce a polyimide membrane final product characterized by a CO 2 /CH 4 selectivity of at least about 20 and a CO 2 permeability of at least about 1.0 SCFH/ft 2 at 100 p.s.i.; (d) immersing said film cast on said substrate into a coagulating medium consisting essentially of water, alcohol, ketones or mixtures thereof; and (e) washing and drying the thusly prepared asymmetric polyimide membrane.
Claim 8
Dependent Claim 279 words
The process of preparing a polyimide polymer membrane having a pore diameter of less than 20 Å units, a CO 2 /CH 4 selectivity of at least about 20, and a CO 2 permeability of at least 1.0 SCFH/ft 2 at 100 p.s.i., said process comprising the steps of: (a) preparing a polyimide dope solution consisting essentially of: (1) a fully imidized polyimide polymer based on 5(6)-amino-1-(4'-aminophenyl)-1,3-trimethylindane present in amounts of 20 to 28% by weight of said dope solution; (2) a solvent system for said polyimide which is water miscible and is selected from the group consisting essentially of N-methyl-2-pyrrolidone, tetrahydrofuran, N,N-dimethylformamide, dioxane, γ-butyrolactone or a mixture thereof; (3) a low molecular weight non-solvent system present in amounts of less than 10% by weight of said dope solution consisting essentially of water, ketones, alcohols, or formamide; (4) a viscosity enhancer present in amounts of less than 3% by weight of said dope solution consisting essentially of polyvinyl pyrrolidones, polyethylene glycols or urethanes; (5) a void supressor present in amounts of less than 5% by weight of said dope solution consisting essentially of maleic acid; casting a film of said polyimide dope solution onto a supporting substrate; (c) evaporating said solvent system under conditions of time, temperature and air flow rate sufficient to produce a polyimide membrane final product characterized by a CO 2 /CH 4 selectivity of at least about 20 and a CO 2 permeability of at least about 1.0 SCFH/ft 2 at 100 p.s.i.; (d) immersing said film cast on said substrate into a coagulating medium consisting essentially of water, alcohol, ketones or mixtures thereof; and (e) washing and drying the thusly prepared asymmetric polyimide membrane.
Claim 9
Dependent Claim 55 words
The process of preparing a polyimide polymer membrane according to claim 6 under conditions of time, temperature, and air flow rate sufficient to produce a polyimide membrane final product characterized by a CO 2 /CH 4 selectivity of at least 30 and a CO 2 permeability of at least 2.0 SCFH/ft 2 at 100 p.s.i.
Claim 10
Dependent Claim 82 words
The process of claim 6 characterized in that said solvent system consists of a mixture of two solvents, one solvent having a boiling point of less than 102° C. selected from the group consisting essentially of tetrahydrofuran and dioxane and the other solvent having a boiling point of greater than 150° C. selected from the group of N-methyl-2-pyrrolidone, N,N-dimethylformamide and γ-butyrolactone wherein the proportions of said high boiling point solvent to said low boiling point solvent present are from 25:75 to 75:25.
Claim 11
Dependent Claim 26 words
The asymmetric polyimide polymer membrane prepared according to the process of claim 6 or 7 characterized in that it is formed into a flat sheet configuration.
Claim 12
Dependent Claim 26 words
The asymmetric polyimide polymer membrane prepared according to the process of claim 6 or 7 characterized in that it is formed into a hollow fiber configuration.

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1994-11-25 1995-05-27 1995-11-26 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1998-11-25 1999-05-27 1999-11-26 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2002-11-25 2003-05-27 2003-11-26 $7700.00 Window Closed / Lapsed

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