Process for making low density hydrogel materials having high surface areas

• US 5,541,234 A
• Filed: 06/05/1995
• Issued: 07/30/1996
• Est. Priority Date: 12/20/1991
• Status: Expired due to Fees

• Current Assignee: Alliedsignal Inc. (Honeywell International Inc.)
• Original Assignee: Alliedsignal Inc. (Honeywell International Inc.)
• Inventors: Unger, Peter D., Rohrbach, Ronald P.
• Primary Examiner(s): Raimund, Christopher W.
• Application Number:
  US08/461,087
• Time in Patent Office: 421 Days
• Field of Search: 521/66, 521/65, 521/141, 521/155, 521/170, 521/186, 521/187
• US Class Current: 521/66
• CPC Class Codes: B01J 20/24 Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
• CPC Class Codes: B01J 20/26 Synthetic macromolecular compounds
• CPC Class Codes: C08J 2300/14 Water soluble or water swellable polymers, e.g. aqueous gels
• CPC Class Codes: C08J 3/12 Powdering or granulating
• CPC Class Codes: C08J 9/28 by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum

Abstract

A process for making a crosslinked, highly porous body derived from a water-soluble, hydrogel polymer, wherein the porous body is characterized in that it has an open-celled 3-dimensional lattice structure, a density of less than about 1.0 g/cm³, a surface area of equal to or greater than about 30 m² /g, and a compression strength of equal to or less than about 75% yield at 300 psi.

Claims

1. A process for making a crosslinked, highly porous body comprising the steps of:

a) dissolving a hydrogel polymer in a gelling solvent, said hydrogel polymer selected from the group consisting of alginates, gums, starch, dextrins, agar, gelatins, casein, collagen, polyvinyl alcohol, polyethylenimine, acrylate polymers, starch/acrylate copolymers, and mixtures and copolymers thereof,

b) forming a gel from the dissolved polymer solution into a desired configuration,

c) gradually replacing said gelling solvent with a crosslinking solvent by employing a concentration gradient solvent exchange process,

d) adding a crosslinking agent to crosslink said gel, and

e) isolating the crosslinked gel from said crosslinking solvent,

wherein said porous body is characterized in that it has an open-celled 3-dimensional lattice structure, a density of less than about 1.0 g/cm³, a surface area of equal to or greater than about 30 m² /g, and a compression strength of equal to or less than about 75% yield at 300 psi.

2. The process of claim 1, wherein said hydrogel polymer is selected from the group consisting of alginates, gums, dextrins, agar, gelatins, casein, collagen, polyvinyl alcohol, starch/acrylate copolymers, and mixtures thereof.

3. The process of claim 1, wherein said crosslinking solvent is selected from the group consisting of acetone, chloroform, dimethyl sulfoxide, toluene, pyridine, and xylene.

4. The process of claim 1, wherein said concentration gradient solvent exchange process utilizes an intermediate solvent that is miscible to both said gelling solvent and said crosslinking solvent.

5. The process of claim 1, wherein said intermediate solvent is selected from the group consisting of alcohols, acetates, ketones, DMSO, DMF, methylene chloride, ethylene chloride, tetrahydrofuran, and dioxane.

6. The porous body of claim 1, wherein said crosslinking agent selected from the group consisting of diisocyanates, diacid halides, diepoxides, epichlorohydrin, aldehydes, dialdehydes, trimetaphosphates, vinyl sulfones, urea-formaldehydes and di-halogenated aliphatics.

7. A process for making a crosslinked, highly porous body comprising the steps of:

a) dissolving a hydrogel polymer in a gelling solvent that contains an additive selected from the group consisting of surfactants, elastomeric additives, and polyols, said hydrogel polymer selected from the group consisting of alginates, gums, starch, dextrins, agar, gelatins, casein, collagen, polyvinyl alcohol, polyethylenimine, acrylate polymers, starch/acrylate copolymers, and mixtures and copolymers thereof,

b) forming a gel from the dissolved polymer solution into a desired configuration,

c) freeze-drying said gel,

d) adding a crosslinking solvent to the freeze-dried gel,

e) adding a crosslinking agent to said crosslinking solvent, and

e) isolating the crosslinked gel from said crosslinking solvent,

wherein said porous body is characterized in that it has an open-celled 3-dimensional lattice structure, a density of less than about 1.0 g/cm³, a surface area of equal to or greater than about 30 m² /g, and a compression strength of equal to or less than about 75% yield at 300 psi.

8. The process of claim 7, wherein said hydrogel polymer is selected from the group consisting of alginates, gums, dextrins, agar, gelatins, casein, collagen, polyvinyl alcohol, starch/acrylate copolymers, and mixtures thereof.

9. The process of claim 7, wherein said crosslinking solvent is selected from the group consisting of acetone, chloroform, dimethyl sulfoxide, toluene, pyridine, and xylene.

10. The process of claim 7, wherein said crosslinking agent is selected from the group consisting of diisocyanates, diacid halides, diepoxides, epichlorohydrin, aldehydes, dialdehydes, trimetaphosphates, vinyl sulfones, urea-formaldehydes and di-halogenated aliphatics.