US20070128425A1 - Reinforced ion-conductive membranes - Google Patents

Reinforced ion-conductive membranes Download PDF

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Publication number
US20070128425A1
US20070128425A1 US11/295,764 US29576405A US2007128425A1 US 20070128425 A1 US20070128425 A1 US 20070128425A1 US 29576405 A US29576405 A US 29576405A US 2007128425 A1 US2007128425 A1 US 2007128425A1
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Prior art keywords
ionomer
layer
substrate
ion
conductive membrane
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Abandoned
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US11/295,764
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English (en)
Inventor
Ilyess Hadj Romdhane
Scott Ciliske
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3M Innovative Properties Co
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3M Innovative Properties Co
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Application filed by 3M Innovative Properties Co filed Critical 3M Innovative Properties Co
Priority to US11/295,764 priority Critical patent/US20070128425A1/en
Assigned to 3M INNOVATIVE PROPERTIES COMPANY reassignment 3M INNOVATIVE PROPERTIES COMPANY ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CILISKE, SCOTT L., RADJ ROMDHANE, IIYESS
Assigned to 3M INNOVATIVE PROPERTIES COMPANY reassignment 3M INNOVATIVE PROPERTIES COMPANY RE-RECORD TO CORRECT THE NAME OF THE FIRST ASSIGNOR, PREVIOUSLY RECORDED ON REEL 017333 FRAME 0928. Assignors: CILISKE, SCOTT L., HADJ ROMDHANE, ILYESS
Priority to EP06838446.0A priority patent/EP1957567B1/en
Priority to JP2008544368A priority patent/JP5129152B2/ja
Priority to CN2006800464419A priority patent/CN101326220B/zh
Priority to PCT/US2006/045481 priority patent/WO2007067385A1/en
Publication of US20070128425A1 publication Critical patent/US20070128425A1/en
Priority to US12/340,899 priority patent/US7906052B2/en
Abandoned legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12—Composite membranes; Ultra-thin membranes
    • B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12—Composite membranes; Ultra-thin membranes
    • B01D69/1216—Three or more layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
    • B01D67/00091—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching by evaporation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
    • B01D67/0013—Casting processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
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    • B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
    • B01D67/0016—Coagulation
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D69/14—Dynamic membranes
    • B01D69/141—Heterogeneous membranes, e.g. containing dispersed material; Mixed matrix membranes
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    • B01D69/1411—Heterogeneous membranes, e.g. containing dispersed material; Mixed matrix membranes containing dispersed material in a continuous matrix
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    • B01D71/06—Organic material
    • B01D71/30—Polyalkenyl halides
    • B01D71/32—Polyalkenyl halides containing fluorine atoms
    • C—CHEMISTRY; METALLURGY
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    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/20—Manufacture of shaped structures of ion-exchange resins
    • C08J5/22—Films, membranes or diaphragms
    • C08J5/2206—Films, membranes or diaphragms based on organic and/or inorganic macromolecular compounds
    • C08J5/2275—Heterogeneous membranes
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    • H01M8/103—Polymeric electrolyte materials characterised by the chemical structure of the main chain of the ion-conducting polymer having nitrogen, e.g. sulfonated polybenzimidazoles [S-PBI], polybenzimidazoles with phosphoric acid, sulfonated polyamides [S-PA] or sulfonated polyphosphazenes [S-PPh]
    • H—ELECTRICITY
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    • H01M8/1032—Polymeric electrolyte materials characterised by the chemical structure of the main chain of the ion-conducting polymer having sulfur, e.g. sulfonated-polyethersulfones [S-PES]
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M8/1041—Polymer electrolyte composites, mixtures or blends
    • H01M8/1046—Mixtures of at least one polymer and at least one additive
    • H01M8/1048—Ion-conducting additives, e.g. ion-conducting particles, heteropolyacids, metal phosphate or polybenzimidazole with phosphoric acid
    • H—ELECTRICITY
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    • H01M8/1041—Polymer electrolyte composites, mixtures or blends
    • H01M8/1053—Polymer electrolyte composites, mixtures or blends consisting of layers of polymers with at least one layer being ionically conductive
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
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    • H01M8/1058—Polymeric electrolyte materials characterised by a porous support having no ion-conducting properties
    • H01M8/106—Polymeric electrolyte materials characterised by a porous support having no ion-conducting properties characterised by the chemical composition of the porous support
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M8/1062—Polymeric electrolyte materials characterised by a porous support having no ion-conducting properties characterised by the physical properties of the porous support, e.g. its porosity or thickness
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M8/1067—Polymeric electrolyte materials characterised by their physical properties, e.g. porosity, ionic conductivity or thickness
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
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    • H01M8/1069—Polymeric electrolyte materials characterised by the manufacturing processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/60—Co-casting; Co-extrusion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/14—Membrane materials having negatively charged functional groups
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D2325/00—Details relating to properties of membranes
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    • B01D2325/42—Ion-exchange membranes
    • C—CHEMISTRY; METALLURGY
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
    • C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • H01M2300/0094—Composites in the form of layered products, e.g. coatings
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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    • Y10T428/00—Stock material or miscellaneous articles
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    • Y10T428/249955—Void-containing component partially impregnated with adjacent component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T428/24996—With internal element bridging layers, nonplanar interface between layers, or intermediate layer of commingled adjacent foam layers

Definitions

  • FIG. 4 is an expanded view of section 4 taken in FIG. 3 .
  • ICM 14 may be formed by initially dissolving or dispersing the reinforcement polymer and the ionomers in solvents to form solutions.
  • the solutions used to form anode layer 28 , substrate 30 , and cathode layer 32 are respectively referred to herein as ionomer solution 28 s , reinforcement polymer solution 30 s , and ionomer solution 32 s .
  • the term “solution” is herein defined to include full dissolutions, partial dissolutions, and dispersions.
  • the reinforcement polymer used to provide reinforcement polymer solution 30 s is substantially dissolved in the corresponding solvent to further promote the ionomer-induced phase separation.
  • the resulting ICM 14 is mechanically reinforced by the reinforcement polymer of substrate 30 , and exhibits good proton conductivity from the ionomers of anode layer 28 , cathode layer 32 , and the ionomers interpenetrated within substrate 30 .
  • the ionomer-induced phase separation allows substrate 30 to be filled with ionomer materials in a single-step process, and provides for a more uniform filling of the micropores compared to standard techniques of impregnating ionomers within pre-formed porous polymers.
  • Core layer 150 compositionally also includes one or more ionomers, and functions as a proton-transport core region of ICM 114 . This allows ICM 114 to achieve greater membrane thicknesses without sacrificing proton conductivity. Examples of suitable ionomers for core layer 150 are also the same as those discussed above for anode layer 28 and cathode layer 32 .
  • a particularly suitable arrangement for ICM 114 includes using high equivalent weight ionomers for anode layer 146 and cathode layer 154 , and a low equivalent weight ionomer for core layer 150 . This arrangement provides a combination of high mechanical strengths and good proton conductivity.
  • TABLE 1 provides the volumetric flow rates of the upper, middle, and lower slots of the tri-die system, and the resulting coating speeds of the wet cast multilayer film for ICMs of Examples 1A-14.
  • TABLE 1 Middle Coating Upper slot flow slot flow Lower slot flow speed Example rate (ml/min) rate (ml/min) rate (ml/min) (fpm)
  • Example 1A 23.4 4.1 23.4 10
  • Example 1B 23.4 4.1 23.4 10
  • Example 2 23.4 8.0 23.4 5
  • Example 3 24.0 8.0 24.0 5
  • Example 4 24.0 5.0 24.0 5
  • Example 5 24.0 5.0 24.0 10
  • Example 6 40.0 5.0 40.0 5
  • Example 7 23.4 8.1 23.4 10
  • Example 8 24.0 5.0 24.0 10
  • Example 9 24.0 5.0 24.0 10
  • Example 10 23.4 8.0 23.4 5
  • Example 11 23.4 6.0 23.4 5
  • Example 12 24.0 10.0 24.0 10
  • Example 13 24.0 10.0 24.0 5
  • Example 14 40.0
  • the ICM of Example 16 was prepared by laminating two pre-formed ICMs of Example 9 with a fuel cell lamination technique. This involved releasing each of the ICM's of Example 9 from the respective polyimide liners by immersion in ambient water. The ICM's of Example 9 were then placed between a pair of 50-micrometer silicone liner sheets. The resulting assembly was then introduced between two rolls in a hot roll laminator where the top roll is preheated at 140° C., the bottom roll at 132° C., and the pressure is set at 3.4 MegaPascals (about 500 pounds/inch 2 ), thereby forming the ICM of Example 16 disposed between the silicone liner sheets.

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  • Life Sciences & Earth Sciences (AREA)
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US11/295,764 2005-12-07 2005-12-07 Reinforced ion-conductive membranes Abandoned US20070128425A1 (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
US11/295,764 US20070128425A1 (en) 2005-12-07 2005-12-07 Reinforced ion-conductive membranes
EP06838446.0A EP1957567B1 (en) 2005-12-07 2006-11-27 Method of forming ion-conductive membranes
JP2008544368A JP5129152B2 (ja) 2005-12-07 2006-11-27 強化されたイオン導電性膜
CN2006800464419A CN101326220B (zh) 2005-12-07 2006-11-27 增强的离子传导膜
PCT/US2006/045481 WO2007067385A1 (en) 2005-12-07 2006-11-27 Reinforced ion-conductive membranes
US12/340,899 US7906052B2 (en) 2005-12-07 2008-12-22 Reinforced ion-conductive membranes

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US11/295,764 US20070128425A1 (en) 2005-12-07 2005-12-07 Reinforced ion-conductive membranes

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US12/340,899 Expired - Fee Related US7906052B2 (en) 2005-12-07 2008-12-22 Reinforced ion-conductive membranes

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EP (1) EP1957567B1 (ja)
JP (1) JP5129152B2 (ja)
CN (1) CN101326220B (ja)
WO (1) WO2007067385A1 (ja)

Cited By (16)

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