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US5573994A Expired / Lapsed US ⏱️ 0.0 years remaining

Superabsorbent foams, and method for producing the same

Assignee: University of Cincinnati
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Filing: 1994-05-13
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Granted: 1996-11-12
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Expires: 2014-05-13
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Abstract

Abstract An absorbent, microporous foam comprising a crosslinked polymer having interconnected fluid cells distributed throughout its mass, wherein the fluid cells have a diameter of between about 0.1 and about 100 μm, and wherein the foam can rapidly absorb at least about twice its dry weight in fluid, is disclosed. A method for producing a microporous, absorbent foam is also disclosed. This method comprises the steps of: (a) mixing a cross-linkable polymer and a first solvent to form a stable solution, wherein the stable solution can be induced to phase separate; (b) inducing the stable solution to phase separate into a polymer-concentrated phase and a polymer-dilute phase after a predetermined period of time; (c) inducing crosslinking of said polymer, so that the polymer will crosslink in said concentrated phase for a predetermined period of time during phase separation to thereby form a microporous material; and (d) drying the microporous material to produce the absorbent foam.

Inventors

  • 👤 Bhagwati G. Kabra
  • 👤 Stevin H. Gehrke

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-31 22:17
CPC Classifications
A; A61; A61L; A61L15/00; A61L15/16; A61L15/22; A61L15/32; A61L15/26; A61L15/28; A61L15/42; A61L15/425; C; C08; C08J; C08J9/00; C08J9/28; Y; Y10; Y10S; Y10S264/00; Y10S264/16; Y10S264/18; Y10S502/00; Y10S502/514; Y10S521/00; Y10S521/905; Y10T; Y10T428/00; Y10T428/249921; Y10T428/249953; Y10T428/249954; Y10T428/249978; Y10T428/249979; Y10T428/249994; Y10T428/249995

Claims Analysis

Total Claims: 40
Claim 1
Independent Claim 90 words
A method for producing a microporous, absorbent foam, comprising the steps of: (a) mixing a cross-linkable polymer and a first solvent to form a stable solution, wherein said stable solution can be induced to phase separate; (b) inducing said stable solution to phase separate into a polymer-concentrated phase and a polymer-dilute phase; (c) inducing chemical crosslinking of said polymer, so that said polymer will crosslink in said concentrated phase during said phase separation to thereby form a microporous material; and (d) drying said microporous material to produce said absorbent foam.
Claim 2
Independent Claim 90 words
A method for producing a microporous, absorbent foam, comprising the steps of: (a) mixing a cross-linkable polymer and a first solvent to form a stable solution, wherein said stable solution can be induced to phase separate; (b) inducing said stable solution to phase separate into a polymer-concentrated phase and a polymer-dilute phase; (c) inducing chemical crosslinking of said polymer, so that said polymer will crosslink in said concentrated phase during said phase separation to thereby form a microporous material; and (d) drying said microporous material to produce said absorbent foam.
Claim 3
Dependent Claim 15 words
The method of claim 1, wherein said stable solution is a substantially homogeneous, single-phase solution.
Claim 4
Dependent Claim 19 words
The method of claim 2, wherein said phase separation is induced by changing the temperature of said stable solution.
Claim 5
Dependent Claim 21 words
The method of claim 2, wherein said phase separation is induced by adding a phase separation enhancer to said stable solution.
Claim 6
Dependent Claim 36 words
The method of claim 4, wherein said phase separation enhancer is either another solute or an additional solvent, and wherein said additional solvent is a non-solvent for said polymer and is miscible with said first solvent.
Claim 7
Dependent Claim 25 words
The method of claim 3, wherein said crosslinking is induced prior to said phase separtion, such that crosslinking will occur prior to said phase separation.
Claim 8
Dependent Claim 39 words
The method of claim 3, wherein said single-phase solution exhibits a lower consolute solution temperature, and wherein said phase separation is induced by increasing the temperature of said single-phase solution to a point above said lower consolute solution temperature.
Claim 9
Dependent Claim 39 words
The method of claim 3, wherein said single-phase solution exhibits an upper consolute solution temperature, and wherein said phase separation is induced by decreasing the temperature of said single-phase solution to a point below said upper consolute solution temperature.
Claim 10
Dependent Claim 24 words
The method of claim 3 further comprising the step of adding a phase-separation enhancer to said single-phase solution prior to inducing said phase separation.
Claim 11
Dependent Claim 25 words
The method of claim 3, further comprising the step of removing the uncrosslinked sol fraction present in said microporous material prior to said drying step.
Claim 12
Dependent Claim 13 words
The method of claim 3, wherein said drying step is accomplished by air-drying.
Claim 13
Dependent Claim 13 words
The method of claim 3, wherein said drying step is accomplished by freeze-drying.
Claim 14
Dependent Claim 53 words
The method of claim 3, wherein said drying step is accomplished by placing said microporous material in a second solvent, thereby swelling said material with said second solvent and replacing any of said first solvent which is present in said material, followed by air-drying said material so that said second solvent will evaporate.
Claim 15
Dependent Claim 48 words
The method of claim 13, wherein said drying step further comprises the step of placing said microporous material swollen with said second solvent in a third solvent, thereby replacing said second solvent with said third solvent, and thereafter air-drying said material so that said third solvent will evaporate.
Claim 16
Dependent Claim 43 words
The method of claim 3, wherein said polymer is chosen from the group consisting of: hydrophobically modified carbohydrate polymers, poly(vinyl alcohol-co-vinyl acetate), poly(methacrylic acid), cyanoethylated or partially formalized poly(vinyl alcohol), poly-N-vinyl-2-oxazolidone, polypeptides, acrylate (or analogous methacrylate) copolymers, and N-alkylacrylamide (or analogous N-alkylmethacrylamide) derivatives.
Claim 17
Dependent Claim 73 words
The method of claim 15, wherein said hydrophobically modified carbohydrate polymers include: hydroxypropyl dextran, hydroxypropyl guar, hydroxypropyl starch, hydroxypropyl cellulose (HPC), hydroxyethyl cellulose (HEC), methyl cellulose, hydroxypropylmethyl cellulose, and ethylhydroxyethyl cellulose; wherein said polypeptides include: poly(L-proline), and poly(valine-proline-glycine-X-glycine), wherein X=any amino acid; wherein said acrylate (or analogous methacrylate) copolymers include: hydroxypropyl acrylate-co-acrylamide, diacetone acrylamide-co-hydroxyethyl acrylate, and hydroxypropyl acrylate-co-hydroxyethyl acrylate; and wherein said N-alkylacrylamide (or analogous N-alkylmethacrylamide) derivatives include: ethylacrylamide, cyclopropylacrylamide, n-propylacrylamide, and isopropylacrylamide.
Claim 18
Dependent Claim 13 words
The method of claim 16, wherein said polymer is either HPC or HEC.
Claim 19
Dependent Claim 14 words
The method of claim 3, wherein said crosslinking is further accomplished by physical means.
Claim 20
Dependent Claim 18 words
The method of claim 2, wherein crosslinking is induced by adding a suitable crosslinking agent to said solution.
Claim 21
Dependent Claim 10 words
The method of claim 2, wherein said solution is photo-crosslinked.
Claim 22
Dependent Claim 26 words
The method of claim 19, wherein said physical crosslinking is accomplished by employing a polymer having hydrophobic polymer side chains capable of interacting with one another.
Claim 23
Dependent Claim 26 words
The method of claim 19, wherein said physical crosslinking is accomplished through hydrogen-bonding, van der Waals interactions, ionic bonding, hydrogen bonding, coordination interactions, or salt bridges.
Claim 24
Dependent Claim 39 words
The method of claim 2, wherein said crosslinking agent is chosen from the group consisting of: acetaldehyde, formaldehyde, glutaraldehyde, diglycidyl ether, divinyl sulfone, diisocyanates, dimethyl urea, epichlorohydrin, oxalic acid, phosphoryl chloride, trimetaphosphate, trimethylomelamine, polyacrolein, and ceric ion redox systems.
Claim 25
Dependent Claim 12 words
The method of claim 23, wherein said crosslinking agent is divinyl sulfone.
Claim 26
Independent Claim 119 words
A method for producing a microporous, open-celled foam, comprising the steps of: (a) mixing hydroxypropyl cellulose (HPC) and water to form a substantially homogeneous, single-phase solution: (b) inducing crosslinking of said HPC by adding a suitable crosslinking agent to said single-phase solution; (c) inducing phase separation of said single-phase solution into a polymer-concentrated phase and a polymer-dilute phase, wherein said phase separation is induced by increasing the temperature of said single-phase solution to above the lower consolute solution temperature of said single-phase solution; (d) permitting said crosslinking to continue, so that said HPC will crosslink in said concentrated phase during said phase separation to thereby form a microporous material; and (e) drying said microporous material to produce said foam.
Claim 27
Independent Claim 119 words
A method for producing a microporous, open-celled foam, comprising the steps of: (a) mixing hydroxypropyl cellulose (HPC) and water to form a substantially homogeneous, single-phase solution: (b) inducing crosslinking of said HPC by adding a suitable crosslinking agent to said single-phase solution; (c) inducing phase separation of said single-phase solution into a polymer-concentrated phase and a polymer-dilute phase, wherein said phase separation is induced by increasing the temperature of said single-phase solution to above the lower consolute solution temperature of said single-phase solution; (d) permitting said crosslinking to continue, so that said HPC will crosslink in said concentrated phase during said phase separation to thereby form a microporous material; and (e) drying said microporous material to produce said foam.
Claim 28
Dependent Claim 13 words
The method of claim 25, wherein said crosslinking agent is divinyl sulfone (DVS).
Claim 29
Dependent Claim 35 words
The method of claim 26, wherein the concentration of HPC is between about 1.9 and about 25 weight percent of said single-phase solution, and wherein the pH of said single-phase solution is above about 11.
Claim 30
Dependent Claim 23 words
The method of claim 27, wherein the concentration of DVS is between about 0.2 and about 5.5 weight percent of said single-phase solution.
Claim 31
Dependent Claim 23 words
The method of claim 28, wherein said phase separation is induced by increasing the temperature of said solution to above about 40° C.
Claim 32
Dependent Claim 44 words
The method of claim 29, wherein said phase separation is induced after said crosslinking has proceeded for between about 1 and about 45 minutes, and said crosslinking is permitted to continue after inducing said phase separation for between about 0.3 and about 100 hours.
Claim 33
Independent Claim 151 words
A method for producing a microporous, open-celled foam, comprising the steps of: (a) mixing hydroxyethyl cellulose (HEC), water and a phase-separation enhancer to form a substantially homogeneous, single-phase solution, wherein said phase-separation enhancer is chosen from the group consisting of: a salt, a water-soluble organic solvent, and a combination of a salt and a water-soluble organic solvent; (b) inducing crosslinking of said HEC by adding a suitable crosslinking agent to said single-phase solution; (c) inducing phase separation of said single-phase solution into a polymer-concentrated phase and a polymer-dilute phase, wherein said phase separation is induced by increasing the temperature of said single-phase solution to above the lower consolute solution temperature of said single-phase solution; and (d) permitting said crosslinking to continue, so that said HEC will crosslink in said concentrated phase during said phase separation to thereby form a microporous material; and (e) drying said microporous material to produce said foam.
Claim 34
Independent Claim 151 words
A method for producing a microporous, open-celled foam, comprising the steps of: (a) mixing hydroxyethyl cellulose (HEC), water and a phase-separation enhancer to form a substantially homogeneous, single-phase solution, wherein said phase-separation enhancer is chosen from the group consisting of: a salt, a water-soluble organic solvent, and a combination of a salt and a water-soluble organic solvent; (b) inducing crosslinking of said HEC by adding a suitable crosslinking agent to said single-phase solution; (c) inducing phase separation of said single-phase solution into a polymer-concentrated phase and a polymer-dilute phase, wherein said phase separation is induced by increasing the temperature of said single-phase solution to above the lower consolute solution temperature of said single-phase solution; and (d) permitting said crosslinking to continue, so that said HEC will crosslink in said concentrated phase during said phase separation to thereby form a microporous material; and (e) drying said microporous material to produce said foam.
Claim 35
Dependent Claim 13 words
The method of claim 31, wherein said crosslinking agent is divinyl sulfone (DVS).
Claim 36
Dependent Claim 13 words
The method of claim 32, wherein said phase separation enhancer is sodium chloride.
Claim 37
Dependent Claim 23 words
The method of claim 32, wherein said phase separation is induced by increasing the temperature of said solution to above about 94° C.
Claim 38
Dependent Claim 35 words
The method of claim 34, wherein the pH of said single-phase solution is above about 11, and wherein the concentration of HEC is between about 1.3 and about 18 weight percent of said single-phase solution.
Claim 39
Dependent Claim 19 words
The method of claim 35, wherein the concentration of DVS is between about 0.4 and about 2 weight percent.
Claim 40
Dependent Claim 42 words
The method of claim 36, wherein said phase separation is induced after said crosslinking has proceeded for between about 1 and about 3 minutes, and said crosslinking is permitted to continue after said inducing for between about 20 and about 60 minutes.

References Cited (Backward Citations)

US4089800A Cited
EP0060138A1 Cited
US4444922A Cited
US4782097A Cited
US4917845A Cited
US5126382A Cited
US5328935A Cited

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