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Method of preparing acrylic ion-transfer membranes

Assignee: Electrochemical Technology Corp
•
Filing: 1982-06-28
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Granted: 1984-02-28
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Expires: 2002-06-28
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Abstract

Abstract Ion exchange resins can be prepared by co-polymerizing a major amount (>88 mol %) of non-ionic acrylic monomer, such as methyl methacrylate, with a minor amount (3 to 12 mol %) of an ionogenous monomer such as methacrylamidopropyltrimethylammonium chloride or 2-acrylamido-2-methyl propane sulfonic acid. The resultant anion-conductive or cation conductive membranes exhibit low swelling in water and high ion-transference numbers. The membranes may be applied as coatings on neural prosthesis electrodes.

Inventors

  • 👤 Cindy L. Ballestrasse
  • 👤 Robert T. Ruggeri

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-03 12:43
CPC Classifications
C; C08; C08J; C08J5/00; C08J5/20; C08J5/22; C08J5/2206; C08J5/2218; C08J5/2231; B; B01; B01J; B01J47/00; B01J47/12; G; G01; G01N; G01N27/00; G01N27/26; G01N27/28; G01N27/30; G01N27/333; G01N27/3335; C08J2333/00; C08J2333/04; C08J2333/06; C08J2333/10; C08J2333/12; H; H01; H01M; H01M50/00; H01M50/40; H01M50/46; Y; Y02; Y02E; Y02E60/00; Y02E60/10

Claims Analysis

Total Claims: 27
Claim 1
Independent Claim 242 words
A process for forming ion-transfer membranes which comprises the following steps in sequence: preparing a reaction mixture consisting essentially of: (A) a major, non-ionic component selected from the group consisting of a hydrophobic acrylic monomer having the formula: ##STR4## where R is H or CH 3 and R 1 is methyl, ethyl or butyl, and mixtures of two or more of said hydrophobic monomers; (B) a minor, ionogenous acrylic monomer component selected from the group consisting of: (i) acrylic acid; (ii) methacrylic acid; (iii) monomers represented by the formula: ##STR5## wherein: R is H or CH 3 , and X is ##STR6## R 1 is alkylene or hydroxyalkylene R 2 , R 3 and R 4 are hydrogen, alkyl, or hydroxyalkyl, and Z - is a halide, acetate, or methyl sulfate ion; and, (iv) mixtures of two or more of said ionogenous acrylic monomers; and (C) an organic solvent, wherein the concentration of said major, non-ionic component in said solvent is in the range 2.5 to 7.5 molar, and the concentration of said minor, ionogenous component in said solvent is in the range 0.10 to 0.75 molar, and wherein the molar concentration of said ionogenous component is between 3 and 12% of the total monomer content in said reaction mixture; depositing a thin film of said reaction mixture on a substrate; and heating said deposited film in a substantially oxygen-free environment at a temperature between 55 degrees C. and 80 degrees C.
Claim 2
Dependent Claim 242 words
A process for forming ion-transfer membranes which comprises the following steps in sequence: preparing a reaction mixture consisting essentially of: (A) a major, non-ionic component selected from the group consisting of a hydrophobic acrylic monomer having the formula: ##STR4## where R is H or CH 3 and R 1 is methyl, ethyl or butyl, and mixtures of two or more of said hydrophobic monomers; (B) a minor, ionogenous acrylic monomer component selected from the group consisting of: (i) acrylic acid; (ii) methacrylic acid; (iii) monomers represented by the formula: ##STR5## wherein: R is H or CH 3 , and X is ##STR6## R 1 is alkylene or hydroxyalkylene R 2 , R 3 and R 4 are hydrogen, alkyl, or hydroxyalkyl, and Z - is a halide, acetate, or methyl sulfate ion; and, (iv) mixtures of two or more of said ionogenous acrylic monomers; and (C) an organic solvent, wherein the concentration of said major, non-ionic component in said solvent is in the range 2.5 to 7.5 molar, and the concentration of said minor, ionogenous component in said solvent is in the range 0.10 to 0.75 molar, and wherein the molar concentration of said ionogenous component is between 3 and 12% of the total monomer content in said reaction mixture; depositing a thin film of said reaction mixture on a substrate; and heating said deposited film in a substantially oxygen-free environment at a temperature between 55 degrees C. and 80 degrees C.
Claim 3
Dependent Claim 14 words
The process of claim 1 wherein said organic solvent is a water soluble alcohol.
Claim 4
Dependent Claim 14 words
The process of claim 1 wherein said organic solvent is a water soluble acid.
Claim 5
Dependent Claim 20 words
The process of claim 1 wherein said organic solvent is selected from the group consisting of ethanol and acetic acid.
Claim 6
Dependent Claim 14 words
The process of claim 1 wherein said reaction mixture further includes a polymerization initiator.
Claim 7
Dependent Claim 13 words
The process of claim 1 wherein said reaction mixture further includes a cross-linker.
Claim 8
Dependent Claim 11 words
The process of claim 5 wherein said polymerization initiator is azobisisobutyronitrile.
Claim 9
Dependent Claim 98 words
A process for forming ion-transfer membranes which comprises the following steps in sequence: preparing a reaction mixture consisting essentially of: (A) a major, non-ionic component selected from the group consisting of a hydrophobic acrylic monomer having the formula: ##STR7## where R is H or CH 3 and R 1 is methyl, ethyl or butyl, and mixtures of two or more of said hydrophobic monomers; (B) a minor, ionogenous acrylic monomer component selected from the group consisting of: (i) acrylic acid; (ii) methacrylic acid; (iii) monomers represented by the formula: ##STR8## wherein: R is H or CH 3 ,
Claim 10
Dependent Claim 98 words
A process for forming ion-transfer membranes which comprises the following steps in sequence: preparing a reaction mixture consisting essentially of: (A) a major, non-ionic component selected from the group consisting of a hydrophobic acrylic monomer having the formula: ##STR7## where R is H or CH 3 and R 1 is methyl, ethyl or butyl, and mixtures of two or more of said hydrophobic monomers; (B) a minor, ionogenous acrylic monomer component selected from the group consisting of: (i) acrylic acid; (ii) methacrylic acid; (iii) monomers represented by the formula: ##STR8## wherein: R is H or CH 3 ,
Claim 11
Dependent Claim 168 words
and X is ##STR9## R 1 is alkylene or hydroxyalkylene R 2 , R 3 and R 4 are hydrogen, alkyl, or hydroxyalkyl, and Z - is a halide, acetate, or methyl sulfate ion; and, (iv) mixtures of two or more of said ionogenous monomers; and (C) an organic solvent, wherein the concentration of said major, non-ionic component in said solvent is in the range 2.5 to 7.5 molar, and the concentration of said minor, ionogenous component in said solvent is in the range 0.10 to 0.75 molar, and wherein the molar concentration of said ionogenous component is between 2 and 12% of the total monomer content in said reaction mixture; heating said reaction mixture to a viscous consistency at a temperature between 55 and 80 degrees C. in a substantially oxygen-free environment; coating a substrate with a film of said viscous reaction mixture; and heating said deposited film to a temperature between 55 and 80 degrees C. in a substantially oxygen-free environment until said film becomes rubbery.
Claim 12
Dependent Claim 168 words
and X is ##STR9## R 1 is alkylene or hydroxyalkylene R 2 , R 3 and R 4 are hydrogen, alkyl, or hydroxyalkyl, and Z - is a halide, acetate, or methyl sulfate ion; and, (iv) mixtures of two or more of said ionogenous monomers; and (C) an organic solvent, wherein the concentration of said major, non-ionic component in said solvent is in the range 2.5 to 7.5 molar, and the concentration of said minor, ionogenous component in said solvent is in the range 0.10 to 0.75 molar, and wherein the molar concentration of said ionogenous component is between 2 and 12% of the total monomer content in said reaction mixture; heating said reaction mixture to a viscous consistency at a temperature between 55 and 80 degrees C. in a substantially oxygen-free environment; coating a substrate with a film of said viscous reaction mixture; and heating said deposited film to a temperature between 55 and 80 degrees C. in a substantially oxygen-free environment until said film becomes rubbery.
Claim 13
Dependent Claim 264 words
A process for forming ion-transfer membranes which comprises the following steps in sequence preparing a reaction mixture consisting essentially of: (A) a major, non-ionic component selected from the group consisting of a hydrophobic acrylic monomer having the formula: ##STR10## where R is H or CH 3 and R 1 is methyl, ethyl or butyl and mixtures of two or more of said hydrophobic monomers; (B) a minor, ionogenous acrylic monomer component selected from the group consisting of: (i) acrylic acid; (ii) methacrylic acid; (iii) monomers represented by the formula: ##STR11## wherein: R is H or CH 3 , and X is ##STR12## R 1 is alkylene or hydroxyalkylene R 2 , R 3 and R 4 are hydrogen, alkyl, or hydroxyalkyl, and Z - is a halide, acetate, or methyl sulfate ion; and, (iv) mixtures of two or more of said ionogenous monomers; and (C) an organic solvent, wherein the concentration of said major, non-ionic component in said solvent is in the range 2.5 to 7.5 molar, and the concentration of said minor, ionogenous component in said solvent is in the range 0.10 to 0.75 molar, and wherein the molar concentration of said ionogenous component is between 3 and 12% of the total monomer content in said reaction mixture; introducing a quantity of said reaction mixture into a mold cavity and thereafter maintaining said mold cavity in a substantially oxygen-free condition; heating said mold cavity to a temperature between 55 and 80 degrees C. and maintaining said temperature until the mold cavity contents becomes rubbery; and removing said rubbery contents from said mold cavity.
Claim 14
Dependent Claim 264 words
A process for forming ion-transfer membranes which comprises the following steps in sequence preparing a reaction mixture consisting essentially of: (A) a major, non-ionic component selected from the group consisting of a hydrophobic acrylic monomer having the formula: ##STR10## where R is H or CH 3 and R 1 is methyl, ethyl or butyl and mixtures of two or more of said hydrophobic monomers; (B) a minor, ionogenous acrylic monomer component selected from the group consisting of: (i) acrylic acid; (ii) methacrylic acid; (iii) monomers represented by the formula: ##STR11## wherein: R is H or CH 3 , and X is ##STR12## R 1 is alkylene or hydroxyalkylene R 2 , R 3 and R 4 are hydrogen, alkyl, or hydroxyalkyl, and Z - is a halide, acetate, or methyl sulfate ion; and, (iv) mixtures of two or more of said ionogenous monomers; and (C) an organic solvent, wherein the concentration of said major, non-ionic component in said solvent is in the range 2.5 to 7.5 molar, and the concentration of said minor, ionogenous component in said solvent is in the range 0.10 to 0.75 molar, and wherein the molar concentration of said ionogenous component is between 3 and 12% of the total monomer content in said reaction mixture; introducing a quantity of said reaction mixture into a mold cavity and thereafter maintaining said mold cavity in a substantially oxygen-free condition; heating said mold cavity to a temperature between 55 and 80 degrees C. and maintaining said temperature until the mold cavity contents becomes rubbery; and removing said rubbery contents from said mold cavity.
Claim 15
Dependent Claim 15 words
The process of claim 1, 8, or 9, wherein said ionogenous monomer is methacrylamidopropyltrimethylammonium chloride.
Claim 16
Dependent Claim 14 words
The process of claim 8 wherein said organic solvent is a water soluble alcohol.
Claim 17
Dependent Claim 14 words
The process of claim 8 wherein said organic solvent is a water soluble acid.
Claim 18
Dependent Claim 20 words
The process of claim 8 wherein said organic solvent is selected from the group consisting of ethanol and acetic acid.
Claim 19
Dependent Claim 14 words
The process of claim 8 wherein said reaction mixture further includes a polymerization initiator.
Claim 20
Dependent Claim 13 words
The process of claim 8 wherein said reaction mixture further includes a cross-linker.
Claim 21
Dependent Claim 11 words
The process of claim 8 wherein said polymerization initiator is azobisisobutyronitrile.
Claim 22
Dependent Claim 14 words
The process of claim 9 wherein said organic solvent is a water soluble alcohol.
Claim 23
Dependent Claim 14 words
The process of claim 9 wherein said organic solvent is a water soluble acid.
Claim 24
Dependent Claim 20 words
The process of claim 9 wherein said organic solvent is selected from the group consisting of ethanol and acetic acid.
Claim 25
Dependent Claim 14 words
The process of claim 9 wherein said reaction mixture further includes a polymerization initiator.
Claim 26
Dependent Claim 13 words
The process of claim 9 wherein said reaction mixture further includes a cross-linker.
Claim 27
Dependent Claim 11 words
The process of claim 9 wherein said polymerization initiator is azobisisobutyronitrile.

References Cited (Backward Citations)

US2567836A Cited
US2980657A Cited
US3718500A Cited
US3725291A Cited
US4139684A Cited
US4009201A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1987-02-27 1987-08-29 1988-02-28 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1991-02-27 1991-08-29 1992-02-28 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1995-02-27 1995-08-29 1996-02-28 $7700.00 Window Closed / Lapsed

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