High purity lignin, lignin compositions, and higher structured lignin
US-10059730-B2 · Aug 28, 2018 · US
US10858712B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10858712-B2 |
| Application number | US-201816104513-A |
| Country | US |
| Kind code | B2 |
| Filing date | Aug 17, 2018 |
| Priority date | Jan 19, 2010 |
| Publication date | Dec 8, 2020 |
| Grant date | Dec 8, 2020 |
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Methods are disclosed for the continuous treatment of biomass comprising a pretreatment step, wherein said biomass is contacted with a first supercritical, near-critical, or sub-critical fluid to form a solid matrix and a first liquid fraction; and a hydrolysis step, wherein said solid matrix formed in said pretreatment step is contacted with a second supercritical or near-supercritical fluid to produce a second liquid fraction and an insoluble lignin-containing fraction. Also disclosed are apparatuses for the continuous conversion of biomass comprising a pretreatment reactor and a hydrolysis reactor associated with said pretreatment reactor.
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What is claimed is: 1. A method of treating a fractionated biomass, comprising: providing a slurry comprising the fractionated biomass; water; cellulose; and insoluble lignin; contacting the slurry with a second reaction fluid to form a reaction mixture comprising a second solid fraction comprising insoluble lignin; and a second liquid fraction comprising a saccharide selected from the group consisting of cello-oligosaccharides, glucose, and mixtures thereof; wherein the second reaction fluid comprises water and the second reaction fluid having a temperature and a pressure at near the critical point of water, the subcritical point of water, the critical point of water, or above the critical point of water; and reducing the temperature of the reaction mixture to a temperature below near the critical point of water or below the subcritical point of water. 2. The method of claim 1 , wherein the slurry is pre-heated to a temperature less than near the critical point of water, less than the subcritical point of water, or less than the critical point of water prior to the contacting step. 3. The method of claim 2 , wherein the pre-heating is carried out at a temperature of about 180° C. to about 260° C. and a pressure of about 200 bar to about 260 bar. 4. The method of claim 1 , wherein the contacting the slurry with the second reaction fluid is carried out in a hydrolysis step, and the hydrolysis step occurs at a temperature of about 275° C. to about 450° C. 5. The method of claim 1 , further comprising separation of the second solid fraction from the second liquid fraction, and wherein the separation comprises extrusion. 6. The method of claim 1 , wherein the second liquid fraction comprises cello-oligosaccharides and the method comprises hydrolyzing cello-oligosaccharides to form glucose. 7. The method of claim 6 , wherein the hydrolyzing comprises contacting the second liquid fraction with hot compressed water, or a third near-critical or sub-critical fluid, to produce a third liquid fraction comprising glucose monomers; wherein the third near-critical or sub-critical fluid comprises water; and optionally, wherein the hot compressed water or the third near-critical or sub-critical fluid comprises acid. 8. The method of claim 7 , wherein the acid is present in an amount of about 0.1% to about 1.5% by weight, based on the weight of the hot compressed water, or the third near-critical or sub-critical fluid, whichever is employed in the hydrolyzing the second liquid fraction. 9. The method of claim 7 , wherein the hydrolyzing employs the hot compressed water; and the hot compressed water has a temperature of about 50° C. to about 250° C. and a pressure sufficient to maintain the hot compressed water in a liquid state; and wherein the hot compressed water comprises acid. 10. The method of claim 7 , wherein the third near-critical or sub-critical fluid comprises carbon dioxide. 11. The method of claim 6 , wherein the hydrolyzing comprises addition of acid. 12. The method of claim 1 , wherein prior to providing the slurry, the biomass comprises a first liquid fraction and a first solid fraction. 13. The method of claim 12 , wherein the first solid fraction comprises cellulose and insoluble lignin and is used to provide the slurry. 14. The method of claim 12 , wherein the first liquid fraction comprises xylo-oligosaccharides, wherein the first liquid fraction is contacted with a second hot compressed water, or a fourth near-critical or sub-critical fluid, to produce a fourth liquid fraction comprising xylose monomers; wherein the fourth near-critical or sub-critical fluid comprises water; and optionally, wherein the second hot compressed water or the fourth near-critical or sub-critical fluid comprises acid. 15. The method of claim 14 , wherein the acid is present in an amount of about 0.1% to about 1.5% by weight, based on the weight of the second hot compressed water, or the fourth near-critical or sub-critical fluid, whichever is employed. 16. The method of claim 14 , wherein the first liquid fraction is contacted with the second hot compressed water; and the second hot compressed water has a temperature of about 50° C. to about 250° C. and a pressure sufficient to maintain the second hot compressed water in a liquid state; and wherein the second hot compressed water comprises acid. 17. The method of claim 12 , wherein the first liquid fraction comprises xylo-oligosaccharide and the method further comprises addition of acid to the first liquid fraction. 18. The method of claim 1 , wherein the method is continuous. 19. The method of claim 1 , wherein the biomass is produced by subjecting lignocellulosic biomass to a supercritical, near-critical, or sub-critical fluid, and wherein the supercritical, near-critical, or sub-critical fluid comprises water. 20. The method of claim 1 , wherein the second reaction fluid further comprises carbon dioxide.
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