# US 9,434,788 B2 · Bio-based fiber gums (BFGs) and processes for producing BFGs > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 9,434,788 B2 - Document ID: US9434788B2 - Status: Granted - Kind: B2 - Application number: 13/798,468 - Filed: 2013-03-13 - Published: 2014-01-16 - Granted: 2016-09-06 - Earliest claimed: 2012-07-11 - Assignees: The United States of America as represented by the Secretary of Agriculture - Applicants: The United States of America, as represented by the Secretary of Agriculture - Inventors: Madhav P. Yadav; Kevin B. Hicks; David Johnston; Kyle A. Hanah; Triveni P. Shukla - Web page: https://patentgrep.com/patent/US9434788B2 ## CPC - C08B 37/0003: {General processes for their isolation or fractionation, e.g. purification or extraction from biomass} - A23B 2/725: in the form of liquids or solids - A23D 7/005: characterised by ingredients other than fatty acid triglycerides - A23L 27/206: {Dairy flavours} - A23L 27/70: {Fixation, conservation, or encapsulation of flavouring agents} - A23L 29/206: of vegetable origin - C08B 37/00: Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof (cellulose D21; {microbiological processes C12P}) - C08B 37/0057: {beta-D-Xylans, i.e. xylosaccharide, e.g. arabinoxylan, arabinofuronan, pentosans; (beta-1,3)(beta-1,4)-D-Xylans, e.g. rhodymenans; Hemicellulose; Derivatives thereof} - C08B 37/006: {Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof} - C08L 3/02: Starch; Degradation products thereof, e.g. dextrin - C08B: POLYSACCHARIDES; DERIVATIVES THEREOF (polysaccharides containing less than six saccharide radicals attached to each other by glycosidic linkages C07H; fermentation or enzyme-using processes C12P19/00; sugar industry C13; production of cellulose D21) - A23B: PRESERVATION OF FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES; CHEMICAL RIPENING OF FRUIT OR VEGETABLES - A23D: EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS OR COOKING OILS (preservation thereof A23B20/00; production, refinement or preservation of animal or vegetable fats or oils C11B, C11C) - A23L: FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF (preservation thereof A23B) - C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06) ## Abstract Processes for the preparation of bio-based fiber gums and products produced by these processes and some of their uses. ## Claims ### Claim 1 A process for the preparation of bio-based fiber gums comprising: (a) mixing agricultural materials with a heated alkaline solution at temperatures in the range of about 75° to about 150° C. to form a slurry; (b) separating out the insoluble components from said slurry to yield a solution having a pH of about 9 to about 14 wherein said solution contains about 0.1 to about 10 wt % solids wherein said solids are alkaline soluble fractions; and one of the following: (c) evaporating said solution to about 16 to about 23 wt % solids and drying to a powder; (d) adjusting the pH of said solution to a pH of about 2 to about 12, evaporating said solution to about 16 to about 23 wt % solids and drying to a powder; (e) evaporating said solution to about 16 to about 23 wt % solids, adjusting the pH of said solution to a pH of about 2 to about 12 and drying to a powder; (f) evaporating said solution to about 16 to about 23 wt % solids and precipitating out said soluble components with about two to about five volumes of solvent to form a precipitate and a supernatant, and separately drying said precipitate and said supernatant; (g) evaporating said solution to about 16 to about 23 wt % solids, adjusting the pH of said solution to a pH of about 2 to about 12 and precipitating out said soluble components with one to five volumes of organic solvent to form a precipitate and a supernatant, and separately drying said precipitate and said supernatant; (h) adjusting the pH of said solution to a pH of about 2 to about 12, evaporating said solution to about 16 to about 23 wt % solids and precipitating out said soluble components with about one to five volumes of organic solvent to form a precipitate and a supernatant, and separately drying said precipitate and said supernatant; or (i) adjusting the pH of said solution to a pH of about 2 to about 5 to precipitate Hemicellulose A and the remaining solution is treated with about 2 volumes of solvent to form a precipitate and a supernatant, and separately drying said precipitate and said supernatant; and optionally the solution is pretreated with at least one of the following: (1) de-salting said solution and the de-salted solution becomes the solution; (2) processing said solution through at least one nano-filtration membrane or ultra-filtration membrane or diafiltration membrane and the permeate becomes the solution; or (3) processing said solution through at least one nano-filtration membrane or ultra-filtration membrane or diafiltration membrane and the retentate becomes the solution wherein said process does not utilize oxidizing agents and wherein said product contains feruloyl-arabinoxylans. ### Claim 2 (depends on 1) The process according to claim 1, wherein said drying is by drum drying or spray drying. ### Claim 3 (depends on 1) The process according to claim 1, wherein said process does not utilize oxidizing agents. ### Claim 4 (depends on 3) The process according to claim 3, wherein said oxidizing agents are selected from the group consisting of hydrogen peroxide, sodium hypochlorite, and mixtures thereof. ### Claim 5 (depends on 1) The process according to claim 1, wherein said agricultural materials is selected from the group consisting of corn bran, corn fiber, oat bran, oat fiber, wheat bran, wheat fiber, barley straw, barley hull, switchgrass, sugar cane bagasse, miscanthus, corn stover, wheat straw, sorghum bran, and mixtures thereof. ### Claim 6 (depends on 1) The process according to claim 1, said process comprising: (a) mixing agricultural materials with a heated alkaline solution at temperatures in the range of about 75° C. to about 150° C. to form a slurry; (b) separating out the insoluble components from said slurry to yield a solution having a pH of about 9 to about 14 wherein said solution contains about 0.1 to about 10 wt % solids wherein said solids are alkaline soluble fractions; and at least one of the following: (c) evaporating said solution to about 16 to about 23 wt % solids and drying to a powder; (d) adjusting the pH of said solution to a pH of about 2 to about 12, evaporating said solution to about 16 to about 23 wt % solids and drying to a powder, (e) evaporating said solution to about 16 to about 23 wt % solids, adjusting the pH of said solution to a pH of about 2 to about 12 and drying to a powder; (f) evaporating said solution to about 16 to about 23 wt % solids and precipitating out said soluble components with about two to about five volumes of organic solvent to form a precipitate and a supernatant, and separately drying said precipitate and said supernatant; (g) adjusting the pH of said solution to a pH of about 2 to about 12, evaporating said solution to about 16 to about 23 wt % solids and precipitating out said soluble components with two to about five volumes of organic solvent to form a precipitate and a supernatant, and separately drying said precipitate and said supernatant; (h) evaporating said solution to about 16 to about 23 wt % solids, adjusting the pH of said solution to a pH of about 2 to about 12, precipitating out said soluble components with organic solvent to form a precipitate and a supernatant, and separately drying said precipitate and said supernatant; (i) adjusting the pH of said solution to a pH of about 2 to about 5 to precipitate Hemicellulose A and treating the remaining solution with 2 volumes of organic solvent to form a precipitate and a supernatant, and separately drying said precipitate and said supernatant; and optionally the solution is pretreated with at least one of the following: (1) processing said solution through a 10,000 Dalton MWCO ultrafiltration membrane to form a permeate which becomes a solution containing alkaline soluble fractions with molecular weight<10,000 Daltons; (2) processing said solution through a 10,000 Dalton MWCO ultrafiltration membrane to form a retentate and a permeate, and processing said retentate through a 50,000 Dalton membrane to form a permeate which becomes a solution containing alkaline soluble fractions with molecular weights between 10,000 and 50,000 Daltons; (3) processing said solution through a 10,000 Dalton MWCO ultrafiltration membrane to form a first retentate, and processing said first retentate through a 50,000 Dalton MWCO membrane to form a second retentate, and processing said second retentate through a 100,000 Dalton MWCO membrane and the permeate becomes a solution containing alkaline soluble fractions with molecular weights between 50,000 and 100,000 Daltons; (4) processing said solution through a 10,000 Dalton MWCO ultrafiltration membrane to form a first retentate, and processing said first retentate through a 50,000 Dalton MWCO membrane to form a second retentate, and processing said second retentate through a 100,000 Dalton MWCO membrane to form a third retentate which becomes a solution containing alkaline soluble fractions with molecular weight greater than 100,000 Daltons; (5) processing said solution through a 10,000 Dalton MWCO ultrafiltration membrane to from a first retentate, and processing said first retentate through a 50,000 Dalton MWCO membrane to form a second retentate, and processing said second retentate through a 100,000 Dalton MWCO membrane to form a third retentate and adjusting the pH of said third retentate to a pH of about 2 to about 5 to precipitate out a precipitant which is then dried to yield hemicellulose-A and the remaining solution contains a BFG product with a molecular weight greater than 100,000 Dalton and is soluble at all pH values; (6) processing said solution through a 10,000 Dalton MWCO ultrafiltration membrane to form (a) a permeate that is evaporated and dried to yield a product with molecular weight<10,000 Daltons and (b) a retentate which is evaporated and dried to yield a product with molecular weight>10,000 Daltons; (7) processing the solution through a 50,000 Dalton MWCO ultrafiltration membrane to form (a) a permeate that is evaporated and dried to yield a product with molecular weight<50,000 Daltons and (b) a retentate which is evaporated and dried to yield a product with molecular weight>50,000 Daltons; (8) processing the solution through a 100,000 Dalton MWCO ultrafiltration membrane to form (a) a permeate that is evaporated and dried to yield a product with molecular weight<100,000 Daltons and (b) a retentate which is evaporated and dried to yield a product with molecular weight>100,000 Daltons; (9) processing the solution through a 100,000 Dalton MWCO ultrafiltration membrane to form a retentate containing a product with molecular weight>100,000 Daltons and adjusting the pH of said retentate to a pH of about 2 to about 5 to form (a) a precipitate which is then dried to form hemicellulose-A and (b) a solution containing a product with a molecular weight greater than 100,000 Daltons that is soluble at all pH values; (10) removing salts and ash from said solution; (11) removing salts and ash from said solution and evaporating said solution to about 16 to about 23 wt % solids and then drying; (12) removing salts and ash from said solution and adjusting the pH of the solution to a pH of about 2 to about 5 to form (a) a precipitant which is then dried to form hemicellulose-A and (b) a solution containing hemicellulose B; or (13) pretreating said solution by ultrafiltration or diafiltration or nanofiltration with or without pH adjustment before or after said ultrafiltration or said diafiltration or said nanofiltration to form (a) a retentate or retentates which becomes the solution and (b) the resulting permeate or permeates becomes the solution. ### Claim 7 A product produced by a process of comprising (a) mixing agricultural materials with a heated alkaline solution at temperatures in the range of about 75° to about 150° C. to form a slurry; (b) separating out the insoluble components from said slurry to yield a solution having a pH of about 9 to about 14 wherein said solution contains about 0.1 to about 10 wt % solids wherein said solids are alkaline soluble fractions; and one of the following: (c) evaporating said solution to abort 16 to about 23 wt % solids and drying to a powder; (d.) adjusting the pH of said solution to a pH of about 2 to about 12, evaporating said solution to about 16 to about 23 wt % solids and drying to a powder; (c) evaporating said solution to about 16 to about 23 wt % solids, adjusting of said solution to a pH of about 2 to about 12 and drying to a powder; (f) evaporating said solution to about 16 to about 23 wt % solids and precipitating out said soluble components with about two to about five volumes of organic solvent to form a precipitate and a supernatant, and separately drying said precipitate and said supernatant; (g) evaporating said solution to about 16 to about 23 wt % solids, adjusting the pH of said solution to a pH of about 2 to about 12 and precipitating out said soluble components with one to five volumes of organic solvent to form a precipitate and a supernatant, and separately drying said precipitate and said supernatant; (h) adjusting the pH of said solution to a pH of about 2 to about 12, evaporating said solution to about 16 to about 23 wt % solids and precipitating out said soluble components with about one to five volumes of organic solvent to form a precipitate and a supernatant, and separately drying said precipitate and said supernatant; or (i) adjusting the pH of said solution to a pH of about 2 to about 5 to precipitate Hemicellulose A and the remaining solution is treated with about 2 volumes of organic solvent to form a precipitate and a. supernatant, and separately drying said precipitate and said supernatant; and optionally the solution is pretreated with at least one of the following: (1) de-salting said solution and the de-salted solution becomes the solution; (2) processing said solution through at least one nano-filtration membrane or ultra-filtration membrane or diafiltration membrane and the permeate becomes the solution; or (3) processing said solution through at least one nano-filtration membrane or ultra-filtration membrane or diafiltration membrane and the retentate becomes the solution; wherein said process does not utilize oxidizing agents and wherein said product contains feruloyl-arabinoxylans. ### Claim 8 (depends on 7) The product according to claim 7, wherein said. product contains about 24 to about 27% arabinose. ### Claim 9 (depends on 7) The product according to claim 7, wherein said product contains about 6 to about 14% glucose. ### Claim 10 (depends on 7) The product according to claim 7, wherein said product has a ratio of arabinose/xylose of about 0.5. ### Claim 11 (depends on 1) A composition comprising (a) a product produced by the process of claim 1 as a binder and (b) carbonaceous materials. ### Claim 12 An oil-in-water or water-in-oil composition comprising (a) a product as an emulsifier, (b) oil and (c) water; wherein said product is prepared by a process comprising (a) mixing agricultural materials with a heated alkaline solution at temperatures in the range of about 75° to about 150°C to form a slurry; (b) separating out the insoluble components from said slurry to yield a solution having a pH of about 9 to about 14 wherein said solution contains about 0.1 to about 10 wt % solids wherein said solids are alkaline soluble fractions; and one of the following: (c) evaporating said solution to about 16 to about 23 wt % solids and drying to a powder; (d) adjusting the pH of said solution to a pH of about 2 to about 12, evaporating said solution to about 16 to about 23 wt % solids and drying to a powder; (e) evaporating said solution to about 16 to about 23 wt % solids, adjusting the pH of said so ion to a pH of about 2 to about 12 and drying to a powder; (f) evaporating said solution to about 16 to about 23 wt % solids and precipitating out said soluble components with about two to about five volumes of organic solvent to fonn a precipitate and a supernatant, and separately drying said precipitate and said supernatant; (g) evaporating said solution to about 16 to about 23 wt h% solids, adjusting the pH of said solution to a pH of about 2 to about 12 and precipitating out said soluble components with one to five volumes of organic solvent to form a precipitate and a supernatant, and separately drying said precipitate and said supernatant; (h) adjusting the pH of said solution to a pH of about 2 to about 12, evaporating said solution to about 16 to about 23 wt % solids and precipitating out said soluble components with about one to five volumes of organic solvent to form a precipitate and a supernatant, and separately drying said precipitate and said supernatant; or (i) adjusting the pH of said solution to a pH of about 2 to about 5 to precipitate Hemicellulose A and the remaining solution is treated with about 2 volumes of organic solvent to form a precipitate and a supernatant, and separately drying said precipitate and said supernatant; and optionally the solution is pretreated with at least one of the following: (1) de-salting said solution and the de-salted solution becomes the solution; (2) processing said solution through at least one nano-filtration membrane or ultra-filtration membrane or diafiltration membrane and the permeate becomes the solution; or (3) processing said solution through at least one nano-filtration membrane or ultra-filtration membrane or diafiltration membrane and the retentate becomes the solution; wherein said process does not utilize oxidizing agents and wherein said product contains feruloyl-arabinoxylans. ### Claim 13 (depends on 12) The oil-in-water or water-in-oil composition according to claim 12, wherein said product contains about 24 to about 27% arabinose. ### Claim 14 (depends on 12) The oil-in-water or water-in-oil composition according to claim 12, wherein said product contains about 6 to about 14% glucose. ### Claim 15 (depends on 12) The oil-in-water or water-in-oil composition according to claim 12, wherein said product has a. ratio of arabinose/xylose of about 0.5. ### Claim 16 (depends on 1) A composition comprising (a) a product produced by the process of claim 1 as an antioxidant and (b) a material that is oxidizable. ### Claim 17 (depends on 1) A method of reducing oxidation of a composition that is oxidizable, said method comprising adding the product produced by the process of claim 1 to a composition that is oxidizable. ### Claim 18 (depends on 1) A method of binding carbonaceous materials, said method comprising adding the product produced by the process of claim 1 to carbonaceous materials, and pelletizing. ### Claim 19 (depends on 1) A method for stabilizing an oil-in-water or water-in-oil emulsion, said method comprising adding the product produced by the process of claim 1 to oil and water. ### Claim 20 (depends on 1) A method for producing plywood with less phenol-formaldehyde resin, said method comprising adding the product produced by the process of claim 1 to plywood formulations, pressing and heating. ### Claim 21 (depends on 1) A method of stabilizing oxidizable material, said method comprising adding the product produced by the process of claim 1 to the oxidizable material to form an emulsion and spray drying to form an encapsulated product.