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US4248685A
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Method for making hydrophilic random interpolymer compositions
Assignee: Johnson and Johnson
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Filing: 1978-05-19
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Granted: 1981-02-03
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Expires: 1998-05-19
Abstract
Abstract Hydrocolloidal dispersions of random interpolymer compositions that have a capacity for absorbing water in amounts of from 10 to 125 times their own weight or greater and are also bacteriostatic are prepared by the polymerization in aqueous medium of a mixture of monomers comprising (1) up to about 90% by weight of an ester of an α,β-olefinically unsaturated carboxylic acid and a monohydric or polyhydric alcohol having a terminal quaternary ammonium group and (2) at least one α,β-olefinically unsaturated comonomer in the presence of a crosslinking agent comprising a difunctional monomer derived from an α,β-olefinically unsaturated carboxylic acid. The interpolymer compositions can be used for binding or coating nonwoven fabrics including paper to improve water absorbency, or cast into a structurally self-supporting film. A water dispersion of the interpolymer can also be formed into a gel, which can be shaped into useful articles or alternatively dried and pulverized into bacteriostatic hydrophilic particles.
Inventors
- 👤 Charles H. Beede
- 👤 Harold L. Waldman
- 👤 Theodore Blumig
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 06:55
CPC Classifications
C; C08; C08F; C08F220/00; C08F220/02; C08F220/08; A; A61; A61L; A61L15/00; A61L15/16; A61L15/22; A61L15/24; A61L15/42; A61L15/46; A61L2300/00; A61L2300/40; A61L2300/402
Claims Analysis
Total Claims: 14
Claim 1
Independent Claim
337 words
A process for preparing a random interpolymer derived from the polymerization of a mixture of monomers, said interpolymer having a water adsorbing capacity of at least about 10 times its own weight after having been dried at a temperature of about 100° C. for about 3 hours; this process comprising the steps of (1) selecting said mixture of monomers so that it comprises: (A) from about 10 to about 90% by weight of said mixture of a first monomer which is an ester of an α,β-olefinically unsaturated carboxylic acid and a monohydric or polyhydric alcohol having a terminal quaternary ammonium group and (B), correspondingly, from about 90 to about 10% by weight of said mixture of at least one α,β-olefinically unsaturated comonomer capable of being dispersed in aqueous media, said comonomer (B) comprising (1) at least 10% by weight of said mixture of monomers of an acid comonomer, or (2) at least 20% by weight of said mixture of monomers of an amide comonomer, or (3) at least 10% by weight of said mixture of monomers of a combination of acid and amide comonomers, said combination containing at least 5% by weight of said mixture of an acid monomer; (II) distributing said mixture of monomers in from about 9 to about 20 parts by weight of an aqueous medium per part of total monomers, said aqueous medium comprising at least 40% by weight of water and up to about 60% by weight of a water miscible organic solvent, and then (III) initiating said polymerization by means of a free radical initiator selected from the group consisting of high energy radiation, photochemical free radical initiators and chemical free radical initiators that are dispersible or soluble in said aqueous medium in the presence of (IV) at least 0.02% by weight, based on the weight of said mixture, of a cross-linking agent comprising a difunctional monomer which is capable of being dispersed or dissolved in said aqueous medium and is an ester or amide of an α,β-olefinically unsaturated carboxylic acid.
Claim 2
Dependent Claim
337 words
A process for preparing a random interpolymer derived from the polymerization of a mixture of monomers, said interpolymer having a water adsorbing capacity of at least about 10 times its own weight after having been dried at a temperature of about 100° C. for about 3 hours; this process comprising the steps of (1) selecting said mixture of monomers so that it comprises: (A) from about 10 to about 90% by weight of said mixture of a first monomer which is an ester of an α,β-olefinically unsaturated carboxylic acid and a monohydric or polyhydric alcohol having a terminal quaternary ammonium group and (B), correspondingly, from about 90 to about 10% by weight of said mixture of at least one α,β-olefinically unsaturated comonomer capable of being dispersed in aqueous media, said comonomer (B) comprising (1) at least 10% by weight of said mixture of monomers of an acid comonomer, or (2) at least 20% by weight of said mixture of monomers of an amide comonomer, or (3) at least 10% by weight of said mixture of monomers of a combination of acid and amide comonomers, said combination containing at least 5% by weight of said mixture of an acid monomer; (II) distributing said mixture of monomers in from about 9 to about 20 parts by weight of an aqueous medium per part of total monomers, said aqueous medium comprising at least 40% by weight of water and up to about 60% by weight of a water miscible organic solvent, and then (III) initiating said polymerization by means of a free radical initiator selected from the group consisting of high energy radiation, photochemical free radical initiators and chemical free radical initiators that are dispersible or soluble in said aqueous medium in the presence of (IV) at least 0.02% by weight, based on the weight of said mixture, of a cross-linking agent comprising a difunctional monomer which is capable of being dispersed or dissolved in said aqueous medium and is an ester or amide of an α,β-olefinically unsaturated carboxylic acid.
Claim 3
Dependent Claim
101 words
The process of claim 1 in which said first monomer is an ester selected from the group consisting of the compounds having the structural formula: ##STR6## wherein R is selected from the group consisting of hydrogen and C 1 to C 4 alkyl; R 1 is selected from the group consisting of C 1 to C 4 alkylene and hydroxy substituted C 1 to C 4 alkylene; each R 2 is selected from the group consisting of C 1 to C 4 alkyl; and X - represents an anion of an acid sufficiently acidic to form a salt with amino nitrogen.
Claim 4
Dependent Claim
16 words
The process of claim 2 in which the ester is 2-methylacryloyloxyethyltrimethylammonium methyl sulfate, or 2-hydroxy-3-methacryloyloxypropyltrimethylammonium chloride.
Claim 5
Dependent Claim
62 words
The process of claim 1 in which said comonomer is selected from the group consisting of the vinyl monomers, the α,β-olefinically unsaturated carboxylic acids of from 3 to 6 carbon atoms and the lower alkyl esters and amides thereof, 2-(C 1 -C 4 ) alkyl substituted acrylic and crotonic acids and esters and amides thereof, and N-substituted amides of the above acids.
Claim 6
Dependent Claim
23 words
The process of claim 4 in which said comonomer is selected from the group consisting of acrylic acid, methacrylic acid, acrylamide and methacrylamide.
Claim 7
Dependent Claim
68 words
The process of claim 4 in which said mixture of monomers comprises from about 10 to about 80% by weight of said first monomer, from about 5 to about 35% by weight of an acid comonomer selected from the group consisting of acrylic and methacrylic acids and from about 10 to about 85% by weight of an amide comonomer selected from the group consisting of acrylamide and methacrylamide.
Claim 8
Dependent Claim
149 words
The process of claim 1 in which said cross-linking agent is selected from the group consisting of the compounds defined by structural formulas I, II and III below: ##STR7## wherein R is hydrogen or C 1 to C 4 alkyl; R 3 is C 1 to C 6 alkylene; and n is an integer from 1 to 3; ##STR8## wherein R is hydrogen or C 1 to C 4 alkyl; and R 3 is C 1 to C 6 alkylene; and ##STR9## wherein R is hydrogen or C 1 to C 4 alkyl; and Y is selected from the group consisting of ##STR10## wherein R 4 is selected from the group consisting of hydrogen and C 1 to C 5 alkyl; and each R 5 is selected from the group consisting of hydrogen and --CH 2 OH, provided, however, that at least one R 5 is --CH 2 OH.
Claim 9
Dependent Claim
35 words
The process of claim 6 in which said crosslinking agent is N,N'-methylenebisacrylamide, and is present in an amount of from about 0.05 to about 1% by weight, based on the weight of the monomer mixture.
Claim 10
Dependent Claim
13 words
The process of claim 1 in which said water miscible solvent is methanol.
Claim 11
Dependent Claim
15 words
The process of claim 1 in which the free radical initiator is a chemical initiator.
Claim 12
Dependent Claim
13 words
The process of claim 10 in which said chemical initiator comprises ammonium persulfate.
Claim 13
Dependent Claim
28 words
The process of claim 11 in which the ammonium persulfate content is from about 0.5 to about 1% by weight based on the weight of the monomer mixture.
Claim 14
Dependent Claim
24 words
The process of claim 11 in which the polymerization is carried out at a temperature of from about 55° C. to about 75° C.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
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| 3.5 Years (Year 4) | 1984-02-03 | 1984-08-04 | 1985-02-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-02-03 | 1988-08-04 | 1989-02-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-02-03 | 1992-08-04 | 1993-02-03 | $7700.00 | Window Closed / Lapsed |