KRZYWANSKI ROMUALD S (US)
30 AMENDED CLAIMS received by the International Bureau on 22 November 2016 (22.11.2016) What is claimed is: 1. A process for making a hydrogel forming material from an unbleached cellulose pulp byproduct of the pulp and paper industry comprised of pulp fines, hemicellulose compounds and lignin comprising: isolating pulp fines from the cellulose pulp by screening and/or dissolved air filtration, wherein said isolated pulp fines comprise hemicellulose compounds, lignin, flocculant, and cellulose fibers having fiber length in the range of 0.005 mm to 0.2 mm, a Kappa number in the range of 2.0 to 20.0, and said hemicellulose compounds have a concentration between 2.0% and 10% on a dry weight basis; reacting the isolated pulp fines with alkaline hydroxide to form an alkali cellulose composition; preparing a heterogeneous mixture comprising the alkali cellulose composition and at least one etherifying agent; and reacting the etherifying agent and the alkali cellulose composition at a temperature in the range of 30°C to 100°C for about 0.5 hours to about 12 hours to produce a hydrogel forming material. 2. The process of Claim 1, wherein on a dry basis the pulp fines comprise 50 to 90% by weight cellulose polymer and 2 to 8% by weight hemicellulose polymers. 3. The process of Claim 2, wherein the hemicellulose polymers in the pulp fines comprise monomers of glucose, xylose, mannose, arabinose, and fucose. 4. The process of Claim 3, wherein the glucose monomer comprises 50% to 90% by weight of the hemicellulose polymers in the pulp fines. 5. The process of Claim 2, wherein the pulp fines comprise cellulose fibers having a length in the range of 0.02 mm to 0.2 mm. 6. The process of Claim 2, wherein the cellulose fiber component of the pulp fines has a weight average molecular (Mw) weight from 500 kDa to 900 kDa and the hemicellulose polymers have a weight average molecular weight (Mw) from 2.0 kDa to 15 kDa . 7. The process of Claim 2, wherein the pulp fines comprise not more than 1% by weight polyacrylamide and not more than 1% by weight of each starch and alum. 8. The process of Claim 1, wherein the isolated pulp fines have a Kappa number not exceeding 18. 9. The process of Claim 1, further comprising the step of washing the hydrogel forming material and neutralizing it to a pH from 3 to 12. 10. The process of Claim 9, further comprising the step of drying the washed and neutralized hydrogel forming material to a water concentration of not more than 20% by weight. 11. The process of Claim 1, wherein an organic cross-linking agent is added to the heterogeneous mixture of the alkali cellulose composition and etherifying agent, and is reacted with the alkali cellulose. 12. The process of Claim 1, further comprising the step of cross-linking the hydrogel forming material with a polyvalent metal cross-linking agent. 13. The process of Claim 1 , wherein the etherifying agent comprises an alkyl halide, halocarboxylic acid, halofatty acid, haloalkylsulphonic acid, haloalkylammonium compound, halohydin, chloroacetic acid, epoxychlorohdrin, epoxy carboxylic acid, a salt of one of the foregoing, chloromethane or alkylene oxide. 14. The process of Claim 11, wherein the organic cross-linking agent comprises ethylene glycol diglycidyl ether, glycerol triglycidyl ether, glycerol diglycidyl ether, glycerol propoxylate triglycidyl ether, polyethylen glycol diglycidyl ether, propylene glycol glycidyl ether or 1,4-cyclohexanoldimethanol diglycidyl ether. 33 15. The process of Claim 11 , wherein the organic cross-linking agent comprises ethylene glycol diglycidyl ether, glycerol triglycidyl ether, or glycerol diglycidyl ether. 16. The process of Claim 15, wherein the weight ratio of organic cross-linking agent to etherifying agent is from 0.1:10 to 1:10. 17. The process of Claim 12, wherein the polyvalent metal cross-linking agent comprises titanium(IV) oxysulfate, titanium (IV) tetrachloride, titanium sulfate, tetrakis(isopropoxy)-titanium, aluminum sulfate, zirconium oxychloride, zirconium orthosulfate, zirconium acetate, zirconium tetrachloride, zirconium ortho-sulfate, zirconium carbonate, zirconium ammonium carbonate, titanium dioxide, zirconium acetylacetonate, titanium citrate, titanium malate, titanium tartrate, zirconium lactate, aluminum acetate, sodium borate, sodium tetraborate, disodium tetraborate, potassium borate or potassium tetraborate. 18. The process of Claim 17, wherein the polyvalent metal cross-linking agent comprises less than 10% by weight of the hydrogel forming material on a dry basis. 19. The process of Claim 1 , wherein the pulp fines have cellulosic chains containing anhydroglucose repeat units and the alkaline hydroxide is present in the reaction 34 in an amount that affords from 1.5 to 6.0 moles of hydroxide anion per mole of anhydroglucose repeat unit of cellulosic chains of the pulp fines. 20. The process of Claim 13, wherein the alkaline hydroxide comprises sodium hydroxide (NaOH), lithium hydroxide (LiOH), potassium hydroxide (KOH), and rubidium hydroxide (RbOH), or benzyltrimethylammonium hydroxide (BTMOH). 21. The process of Claim 1 , wherein the hydrogel forming material produced has a viscosity of at least 1000 cp, at 20°C, 20 rpm when in an aqueous solution at a concentration of 2.5% by weight. 22. The process of Claim 21, wherein the hydrogel forming material has Derivatizing Density of not less than 20% by weight. |
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