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US4131576A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for the preparation of graft copolymers of a water soluble monomer and polysaccharide employing a two-phase reaction system

Assignee: Ingredion Inc
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Filing: 1977-12-15
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Granted: 1978-12-26
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Expires: 1997-12-15
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Abstract

Abstract Graft copolymers of a water soluble monomer and polysaccharide are prepared employing a two-phase reaction system under controlled conditions. The resultant graft copolymers are formed at high grafting efficiency and high conversion and obtained as precipitated solid beads.

Inventors

  • 👤 Carmine P. Iovine
  • 👤 Dilip K. Ray-Chaudhuri

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-28 20:01
CPC Classifications
C; C08; C08F; C08F251/00

Claims Analysis

Total Claims: 12
Claim 1
Independent Claim 190 words
A process for the production of a graft copolymer of a polysaccharide and water-soluble monomer comprising the steps of: (a) suspending the polysaccharide in an organic solvent, which solvent has a boiling point at or above the temperature of the polymerization reaction, is immiscible with water and does not dissolve the polysaccharide, monomer or graft copolymer; (b) adding thereto an aqueous solution of the monomer thereby forming a suspension of discrete aqueous spheres in the organic solvent phase; (c) deoxygenating and heating the reaction mixture in the presence of a free radical polymerization catalyst to a temperature of 40 to 100° C. to initiate polymerization; (d) continuing the polymerization for from 0.5 to 6 hours; and (e) isolating the resultant graft copolymer from the reaction mixture in the form of solid beads; wherein it is required that either the aqueous solution or the polysaccharide suspension or both contain a cationic, anionic or nonionic surfactant, that the solids content of the aqueous polymerization mixture is greater than 50% by weight, and that the polysaccharide be present in the final graft copolymer in an amount of from 10 to 90% by weight.
Claim 2
Dependent Claim 190 words
A process for the production of a graft copolymer of a polysaccharide and water-soluble monomer comprising the steps of: (a) suspending the polysaccharide in an organic solvent, which solvent has a boiling point at or above the temperature of the polymerization reaction, is immiscible with water and does not dissolve the polysaccharide, monomer or graft copolymer; (b) adding thereto an aqueous solution of the monomer thereby forming a suspension of discrete aqueous spheres in the organic solvent phase; (c) deoxygenating and heating the reaction mixture in the presence of a free radical polymerization catalyst to a temperature of 40 to 100° C. to initiate polymerization; (d) continuing the polymerization for from 0.5 to 6 hours; and (e) isolating the resultant graft copolymer from the reaction mixture in the form of solid beads; wherein it is required that either the aqueous solution or the polysaccharide suspension or both contain a cationic, anionic or nonionic surfactant, that the solids content of the aqueous polymerization mixture is greater than 50% by weight, and that the polysaccharide be present in the final graft copolymer in an amount of from 10 to 90% by weight.
Claim 3
Dependent Claim 26 words
The process of claim 1 wherein the monomer solution contains a water-soluble surfactant in an amount of 0.5 to 12% by weight of the polysaccharide substrate.
Claim 4
Dependent Claim 26 words
The process of claim 1 wherein the polysaccharide suspension contains a solvent-soluble surfactant in an amount of 1 to 12% by weight of the organic solvent.
Claim 5
Dependent Claim 47 words
The process of claim 1 wherein the surfactant is selected from the group consisting of hydroxyethylated nonyl phenols, hydroxyethylated long-chain monocarboxylic acids, hydroxyethylated long-chain fatty acids, fatty acid esters of sorbitol, hydroxyethylated fatty acid esters of sorbitol, alkyl aryl sulfonates, linear alkyl sulfonates and linear alkyl sulfates.
Claim 6
Dependent Claim 56 words
The process of claim 1 wherein the water-soluble monomer is selected from the group consisting of acrylic acid, methacrylic acid, acrylamide, methacryloxyethyl trimethyl ammonium methosulfate, methacrylamidopropyl trimethyl ammonium chloride, ammonium styrene sulfonate, sodium styrene sulfonate, sulfonatoethyl methacrylate, dimethyldiallyl ammonium chloride, dipotassium methacryloxyethyl phosphate, vinyl pyrrolidone, hydroxymethyl acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate and sodium 2-acrylamide-2-methyl propane sulfonate.
Claim 7
Dependent Claim 15 words
The process of claim 1 wherein the polysaccharide is a starch or starch conversion product.
Claim 8
Dependent Claim 18 words
The process of claim 1 wherein the polysaccharide is cellulose or a cellulose derivative or a plant gum.
Claim 9
Dependent Claim 22 words
The process of claim 1 wherein the polysaccharide is present in the final graft copolymer in an amount of 40-70% by weight.
Claim 10
Dependent Claim 24 words
The process of claim 1 wherein the solids content is within the range of 60 to 80% by weight of the aqueous polymerization system.
Claim 11
Dependent Claim 26 words
The process of claim 1 wherein the organic solvent is selected from the group consisting of benzene, dichlorobenzene, toluene, xylene, 1,2-dichloroethane, heptane, octane, isooctane and nonane.
Claim 12
Dependent Claim 10 words
The graft copolymer produced by the process of claim 1.

References Cited (Backward Citations)

US3211708A Cited
US3656884A Cited
US3809664A Cited
US3957739A Cited
US3976552A Cited
US4028290A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1981-12-25 1982-06-26 1982-12-26 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1985-12-25 1986-06-26 1986-12-26 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1989-12-25 1990-06-26 1990-12-26 $7700.00 Window Closed / Lapsed

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