US5470449A
Expired / Lapsed
US
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Microporous asbestos-free diaphragms/cathodes for electrolytic cells
Assignee: Chloralp SAS
•
Filing: 1994-07-14
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Granted: 1995-11-28
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Expires: 2014-07-14
Abstract
Abstract Microporous diaphragms adapted for wet-consolidation with composite cathodes for use in electrolytic cells, e.g., chlorine/soda electrolysis cells, comprise a sintered, fluoropolymer microconsolidated asbestos-free microporous fibrous sheet material, such sheet material including from 3% to 35% by weight of fluoropolymer binder, from 0% to 50% by weight of a uniformly distributed gel of an oxohydroxide of at least one metal of Groups IVA, IVB, VB and VIB of the Periodic Table or of the lanthanide or actinide series thereof, and from 20% to 95% by weight of a mixture of poly-tetrafluoroethylene (PTFE) fibers and inorganic fibers, such inorganic fibers constituting from 1% to 80% by weight of the mixture and such inorganic fibers including carbon, graphite or titanate fibers, or admixture thereof.
Inventors
- 👤 Jean Bachot
- 👤 Pascal Stutzmann
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 04:06
CPC Classifications
C; C25; C25B; C25B13/00; C25B13/04; C25B13/08; B; B01; B01D; B01D67/00; B01D67/0079; B01D71/00; B01D71/02; B01D71/06; C25B1/00; C25B1/01; C25B1/24; C25B1/26; Y; Y02; Y02E; Y02E60/00; Y02E60/10; Y02E60/30; Y02E60/50
Claims Analysis
Total Claims: 42
Claim 1
Independent Claim
156 words
A microporous diaphragm which comprises a sintered, fluoropolymer microconsolidated asbestos-free microporous fibrous sheet material, said sheet material comprising from 3% to 35% by weight of a fluoropolymer binder comprising a homopolymer or a copolymer derived at least partly from olefinic monomers completely substituted by fluorine atoms or completely substituted by a combination of fluorine atoms and of at least one of chlorine, bromine or iodine atoms per monomer, from 0% to 50% by weight of a gel of an oxohydroxide of at least one metal of Groups IVA, IVB, VB and VIB of the Periodic Table or of the lanthanide or actinide series thereof, and from 20% to 95% by weight of a mixture of polytetrafluoroethylene fibers and inorganic fibers, said inorganic fibers constituting from 1% to 80% by weight of such mixture and said inorganic fibers comprising titanate fibers, optionally in admixture with carbon or graphite fibers, or admixture thereof, wherein said diaphragm is non-conductive.
Claim 2
Dependent Claim
156 words
A microporous diaphragm which comprises a sintered, fluoropolymer microconsolidated asbestos-free microporous fibrous sheet material, said sheet material comprising from 3% to 35% by weight of a fluoropolymer binder comprising a homopolymer or a copolymer derived at least partly from olefinic monomers completely substituted by fluorine atoms or completely substituted by a combination of fluorine atoms and of at least one of chlorine, bromine or iodine atoms per monomer, from 0% to 50% by weight of a gel of an oxohydroxide of at least one metal of Groups IVA, IVB, VB and VIB of the Periodic Table or of the lanthanide or actinide series thereof, and from 20% to 95% by weight of a mixture of polytetrafluoroethylene fibers and inorganic fibers, said inorganic fibers constituting from 1% to 80% by weight of such mixture and said inorganic fibers comprising titanate fibers, optionally in admixture with carbon or graphite fibers, or admixture thereof, wherein said diaphragm is non-conductive.
Claim 3
Dependent Claim
26 words
The microporous diaphragm as defined by claim 1, said inorganic fibers comprising titanate fibers, in an amount of at least 5% by weight of such mixture.
Claim 4
Dependent Claim
19 words
The microporous diaphragm as defined by claim 2, comprising from 2% to 10% by weight of said oxohydroxide gel.
Claim 5
Dependent Claim
32 words
The microporous diaphragm as defined by claim 1, said inorganic fibers comprising carbon or graphite fibers monodisperse in length, in an amount ranging from 1% to 10% by weight of such mixture.
Claim 6
Dependent Claim
23 words
The microporous diaphragm as defined by claim 1, comprising a gel of an oxohydroxide of at least one Group IVA and IVB metal.
Claim 7
Dependent Claim
16 words
The microporous diaphragm as defined by claim 1, comprising a gel of titanium or zirconium oxohydroxide.
Claim 8
Dependent Claim
13 words
The microporous diaphragm as defined by claim 1, said fluoropolymer binder comprising polytetrafluoroethylene.
Claim 9
Dependent Claim
26 words
The microporous diaphragm as defined by claim 1, comprising from 5% to 40% by weight of said fluoropolymer binder based on the total weight of fibers+binder.
Claim 10
Dependent Claim
24 words
An assembly adapted for incorporation in an electrolytic cell, comprising a composite cathode component consolidated with the microporous diaphragm as defined by claim 1.
Claim 11
Dependent Claim
43 words
The electrolytic assembly as defined by claim 9, said composite cathode component comprising an elementary cathode having a highly porous metal surface, said metal surface having deposited thereon a fluoropolymer microconsolidated microporous fibrous sheet material which comprises an amount of electrically conductive fibers.
Claim 12
Dependent Claim
20 words
The electrolytic assembly as defined by claim 10, said electrically conductive fibers comprising carbon or graphite fibers monodisperse in length.
Claim 13
Dependent Claim
14 words
The electrolytic assembly as defined by claim 10, the fluoropolymer binder material comprising polytetrafluoroethylene.
Claim 14
Dependent Claim
12 words
An electrolytic cell comprising the electrolytic assembly as defined by claim 9.
Claim 15
Dependent Claim
113 words
A process for the production of the micro-porous diaphragm as defined by claim 1, comprising (a) formulating an essentially aqueous dispersion of said fibers, particulates of said fluoropolymer binder and, optionally particulates of at least one precursor of an oxohydroxide of at least one metal of Groups IVA, IVB, VB and VIB of the Periodic Table or of the lanthanide or actinide series thereof, (b) depositing a sheet material by vacuum filtering said dispersion through a porous support substrate, (c) removing the liquid material therefrom and optionally drying the sheet material thus formed, (d) sintering said sheet material, and (e) treating said sintered sheet material with an aqueous solution of alkali metal hydroxide.
Claim 16
Dependent Claim
16 words
The process as defined by claim 14, said porous support substrate comprising a composite cathode component.
Claim 17
Dependent Claim
58 words
The process as defined by claim 14, said essentially aqueous dispersion comprising a poorly water-soluble salt of a metal of Groups IVA, IVB, VB and VIB of the Periodic Table or of the lanthanide or actinide series thereof, the anion of which comprising a phosphate, pyrophosphate, hydrogen phosphate or polyphosphate, optionally substituted by an alkali metal, and silicate.
Claim 18
Dependent Claim
14 words
The process as defined by claim 16, said oxohydroxide precursor comprising α-TiP or α-ZrP.
Claim 19
Dependent Claim
19 words
The process as defined by claim 14, said aqueous dispersion comprising from 5% to 40% by weight of silica.
Claim 20
Dependent Claim
110 words
A microporous diaphragm which comprises a sintered, fluoropolymer micro consolidated asbestos-free microporous fibrous sheet material, said sheet material comprising from 3% to 35% by weight of a fluoropolymer binder, an amount of from 5% to 25% by weight of a gel of an oxohydroxide of at least one metal of Groups IVA, IVB, VB and VIB of the Periodic Table or of the lanthanide or actinide series thereof, and from 20% to 95% by weight of a mixture of polytetrafluoroethylene fibers and inorganic fibers, said inorganic fibers constituting from 1% to 80% by weight of such mixture and said inorganic fibers comprising carbon, graphite or titanate fibers, or mixtures thereof.
Claim 21
Dependent Claim
110 words
A microporous diaphragm which comprises a sintered, fluoropolymer micro consolidated asbestos-free microporous fibrous sheet material, said sheet material comprising from 3% to 35% by weight of a fluoropolymer binder, an amount of from 5% to 25% by weight of a gel of an oxohydroxide of at least one metal of Groups IVA, IVB, VB and VIB of the Periodic Table or of the lanthanide or actinide series thereof, and from 20% to 95% by weight of a mixture of polytetrafluoroethylene fibers and inorganic fibers, said inorganic fibers constituting from 1% to 80% by weight of such mixture and said inorganic fibers comprising carbon, graphite or titanate fibers, or mixtures thereof.
Claim 22
Dependent Claim
158 words
A microporous diaphragm which comprises a sintered, fluoropolymer microconsolidated asbestos-free microporous fibrous sheet material, said sheet material comprising from 30 to 35% by weight of a fluoropolymer binder comprising a homopolymer or a copolymer derived at least partly from olefinic monomers completely substituted by fluorine atoms or completely substituted by a combination of fluorine atoms and of at least one of chlorine, bromine or iodine atoms per monomer, from 0 to 50% by weight of a gel of an oxohydroxide of at least one metal of Groups IVA, IVB, VB and VIB of the Periodic Table or of the lanthanide or actinide series thereof, and from 20 to 95% by weight of a mixture of polytetrafluoroethylene fibers and inorganic fibers, said inorganic fibers constituting from 1% to 80% by weight of such mixture and said inorganic fibers comprising at least 5% by weight of titanate fibers or from 1 to 10% by weight of carbon or graphite fibers.
Claim 23
Dependent Claim
158 words
A microporous diaphragm which comprises a sintered, fluoropolymer microconsolidated asbestos-free microporous fibrous sheet material, said sheet material comprising from 30 to 35% by weight of a fluoropolymer binder comprising a homopolymer or a copolymer derived at least partly from olefinic monomers completely substituted by fluorine atoms or completely substituted by a combination of fluorine atoms and of at least one of chlorine, bromine or iodine atoms per monomer, from 0 to 50% by weight of a gel of an oxohydroxide of at least one metal of Groups IVA, IVB, VB and VIB of the Periodic Table or of the lanthanide or actinide series thereof, and from 20 to 95% by weight of a mixture of polytetrafluoroethylene fibers and inorganic fibers, said inorganic fibers constituting from 1% to 80% by weight of such mixture and said inorganic fibers comprising at least 5% by weight of titanate fibers or from 1 to 10% by weight of carbon or graphite fibers.
Claim 24
Dependent Claim
108 words
A microporous diaphragm which comprises a sintered, fluoropolymer microconsolidated asbestos-free microporous fibrous sheet material, said sheet material comprising from 3% to 35% by weight of a fluoropolymer binder, from 2% to 50% by weight of a gel of an oxohydroxide of at least one metal of Groups IVA, IVB, VB and VIB of the Periodic Table or of the lanthanide or actinide series thereof, and from 20% to 95% by weight of a mixture of polytetrafluoroethylene fibers and inorganic fibers, said inorganic fibers constituting from 1% to 80% by weight of such mixture and said inorganic fibers comprising carbon, graphite or admixture thereof, wherein said diaphragm is non-conductive.
Claim 25
Dependent Claim
108 words
A microporous diaphragm which comprises a sintered, fluoropolymer microconsolidated asbestos-free microporous fibrous sheet material, said sheet material comprising from 3% to 35% by weight of a fluoropolymer binder, from 2% to 50% by weight of a gel of an oxohydroxide of at least one metal of Groups IVA, IVB, VB and VIB of the Periodic Table or of the lanthanide or actinide series thereof, and from 20% to 95% by weight of a mixture of polytetrafluoroethylene fibers and inorganic fibers, said inorganic fibers constituting from 1% to 80% by weight of such mixture and said inorganic fibers comprising carbon, graphite or admixture thereof, wherein said diaphragm is non-conductive.
Claim 26
Dependent Claim
19 words
The microporous diaphragm as defined by claim 21 comprising from 2% to 10% by weight of said oxohydroxide gel.
Claim 27
Dependent Claim
33 words
The microporous diaphragm as defined by claim 21 wherein said inorganic fibers comprise carbon or graphite fibers monodisperse in length, in an amount ranging from 1% to 10% by weight of such mixture.
Claim 28
Dependent Claim
19 words
The microporous diaphragm as defined by claim 23, comprising from 5% to 25% by weight of said oxohydroxide gel.
Claim 29
Dependent Claim
23 words
The microporous diaphragm as defined by claim 21, comprising a gel of an oxohydroxide of at least one Group IVA and IVB metal.
Claim 30
Dependent Claim
16 words
The microporous diaphragm as defined by claim 21, comprising a gel of titanium or zirconium oxohydroxide.
Claim 31
Dependent Claim
14 words
The microporous diaphragm as defined by claim 21 wherein said fluoropolymer binder comprises polytetrafluorethylene.
Claim 32
Dependent Claim
26 words
The microporous diaphragm as defined by claim 21, comprising from 5% to 40% by weight of said fluoropolymer binder based on the total weight of fibers+binder.
Claim 33
Dependent Claim
23 words
An assembly for incorporation in an electrolytic cell, comprising a composite cathode component consolidated with the microporous diaphragm as defined by claim 21.
Claim 34
Dependent Claim
44 words
The electrolytic assembly as defined by claim 29, wherein said composite cathode component comprises an elementary cathode having a highly porous metal surface, said metal surface having deposited thereon a fluoropolymer microconsolidated microporous fibrous sheet material which comprises an amount of electrically conductive fibers.
Claim 35
Dependent Claim
21 words
The electrolytic assembly as defined by claim 30, wherein said electrically conductive fibers comprise carbon or graphite fibers monodisperse in length.
Claim 36
Dependent Claim
15 words
The electrolytic assembly as defined by claim 30, wherein the fluoropolymer binder material comprises polytetrafluoroethylene.
Claim 37
Dependent Claim
12 words
An electrolytic cell comprising the electrolytic assembly as defined by claim 29.
Claim 38
Dependent Claim
112 words
A process for the production of the micro-porous diaphragm as defined by claim 21, comprising (a) formulating an essentially aqueous dispersion of said fibers, particulates of said fluoropolymer binder and, particulates of at least one precursor of an oxohydroxide of at least one metal of Groups IVA, IVB, VB and VIB of the Periodic Table or of the lanthanide or actinide series thereof, (b) depositing a sheet material by vacuum filtering said dispersion through a porous support substrate, (c) removing the liquid material therefrom and optionally drying the sheet material thus formed, (d) sintering said sheet material, and (e) treating said sintered sheet material with an aqueous solution of alkali metal hydroxide.
Claim 39
Dependent Claim
16 words
The process as defined by claim 34, said porous support substrate comprising a composite cathode component.
Claim 40
Dependent Claim
58 words
The process as defined by claim 34, said essentially aqueous dispersion comprising a poorly water-soluble salt of a metal of Groups IVA, IVB, VB and VIB of the Periodic Table or of the lanthanide or actinide series thereof, the anion of which comprising a phosphate, pyro-phosphate, hydrogen phosphate or polyphosphate, optionally substituted by an alkali metal, and silicate.
Claim 41
Dependent Claim
14 words
The process as defined by claim 36, said oxohydroxide precursor comprising α-TiP or α-ZrP.
Claim 42
Dependent Claim
19 words
The process as defined by claim 34, said aqueous dispersion comprising from 5% to 40% by weight of silica.
References Cited (Backward Citations)
FR2213850A1
Cited
FR2229739A1
Cited
FR2280609A1
Cited
FR2280435A1
Cited
US4105516A
Cited
US4243504A
Cited
EP0132425A1
Cited
EP0214066A1
Cited
US4775551A
Cited
US4720334A
Cited
US4810345A
Cited
EP0296076A1
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1998-11-27 | 1999-05-29 | 1999-11-28 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2002-11-27 | 2003-05-29 | 2003-11-28 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2006-11-27 | 2007-05-29 | 2007-11-28 | $7700.00 | Window Closed / Lapsed |