Method for production of cellulose nano crystals from cellulose-containing waste material
US-9464142-B2 · Oct 11, 2016 · US
US9434788B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9434788-B2 |
| Application number | US-201313798468-A |
| Country | US |
| Kind code | B2 |
| Filing date | Mar 13, 2013 |
| Priority date | Jul 11, 2012 |
| Publication date | Sep 6, 2016 |
| Grant date | Sep 6, 2016 |
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Processes for the preparation of bio-based fiber gums and products produced by these processes and some of their uses.
Opening claim text (preview).
We 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. 2. The process according to claim 1 , wherein said drying is by drum drying or spray drying. 3. The process according to claim 1 , wherein said process does not utilize oxidizing agents. 4. The process according to claim 3 , wherein said oxidizing agents are selected from the group consisting of hydrogen peroxide, sodium hypochlorite, and mixtures thereof. 5. 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. 6. 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
Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof (cellulose D21; {microbiological processes C12P}) · CPC title
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 · CPC title
General processes for their isolation or fractionation, e.g. purification or extraction from biomass · CPC title
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