OXYGEN ASSISTED ORGANOSOLV PROCESS, SYSTEM AND METHOD FOR DELIGNIFICATION OF LIGNOCELLULOSIC MATERIALS AND LIGNIN RECOVERY

• US 20160031921A1
• Filed: 08/01/2014
• Published: 02/04/2016
• Est. Priority Date: 08/01/2014
• Status: Active Grant

• Current Assignee: Agency For Science Technology and Research
• Original Assignee: Agency For Science Technology and Research
• Inventors: Manesh, Ali, Manesh, Mohammad Ali, Guenther, John H., Zoborowski, Edwin G., Braenner, Walter, Hawk, Lee J.
• Granted Patent: US 9,382,283 B2
• Time in Patent Office: Days
• US Class Current: 1/1
• CPC Class Codes: C07G 1/00 Lignin; Lignin derivatives
• CPC Class Codes: C08H 6/00 Macromolecular compounds derived from lignin, e.g. tannins, humic acids
• CPC Class Codes: C08H 8/00 Macromolecular compounds derived from lignocellulosic materials pretreatment thereof B27N
• CPC Class Codes: C08L 97/005 Lignin
• CPC Class Codes: D21C 1/00 Pretreatment of the finely-divided materials before digesting of waste paper D21C5/02
• CPC Class Codes: D21C 3/00 Pulping cellulose-containing materials digesters D21C7/00

Abstract

An oxygen assisted Organosolv process for a more efficient delignification and producing bio-products by decomposing lignocellulosic materials comprises providing a lignin solvent with water, an acid, an oxidant and one or more lignin dissolving chemicals. The process also includes placing biomass in contact with oxidant, acid, water, the lignin solvent in any order or combined to form a recyclable solvent, and recycling at least a portion of the recyclable solvent by circulating the recyclable solvent back into contact with the biomass. The circulating of the recyclable solvent occurs for a period of time, during which, acid and oxidant may be added if necessary as they may be consumed by the process, after which, the process then includes separating material such as chemicals and lignin from the recyclable solvent. The chemicals can be recycled as new lignin dissolving solvent or sold, while lignin can be used as natural and renewable colorant for polymers such as poly lactic acid, or mixed with other polymers as an additive and extruded or injected to consumable polymeric parts, or can be used and the natural source of renewable aromatics. Application of an oxidant will help the overall fractionation process by changing the chemical characteristics of the lignin and therefore allows more lignin to be removed from biomass. At the end, the lignin is separated from the lignin dissolving solvent by a separation process to also reclaim the lignin dissolving solvent for the next fractionation process.

Claims

1. An oxygen assisted organosolv process for delignification of lignocellulosic biomass materials comprising:

a) Placing a quantity of lignocellulosic biomass in contact with a quantity of oxidant such as hydrogen peroxide to partially or fully impregnate the biomass;

b) Placing a quantity of the partially or fully impregnated biomass in contact with a quantity of acid to acidify the impregnated biomass;

c) Adding a quantity of water to a quantity of the acidified impregnated biomass to make a mixture of biomass, water, acid, and oxidant,

d) Adding a quantity of lignin dissolving chemical or chemicals to a quantity of the mixture of biomass, water, acid, and oxidant to make a mixture of biomass and recyclable solvent that includes quantities of oxidant, acid, water, and lignin dissolving chemicals,

e) Effecting a separation of a quantity of the mixture of biomass and recyclable solvent into a recyclable solvent soluble phase and recyclable solvent insoluble phase; and

f) Effecting a separation of a quantity of the recyclable solvent soluble phase into aqueous and organic layers based on their specific densities differences; and

,

f) Effecting a removal of lignin from a quantity of the organic layer and use the remaining liquid as fresh lignin dissolving solvent for other applications or recycling it back into the fractionation process.

2. A process according to claim 1, wherein the impregnated and acidified biomass is mixed with lignin dissolving chemicals followed by adding water.

3. A process according to claim 1, wherein the impregnated biomass is mixed with water first followed by acidification and adding lignin dissolving chemicals.

4. A process according to claim 3, wherein the lignin dissolving chemicals is added prior to adding acid.

5. A process according to claim 1, wherein the impregnated biomass is mixed with lignin dissolving chemicals first followed by adding water and a quantity of acid to acidify the mixture.

6. A process according to claim 5, wherein the acid is added prior to adding water.

7. A process according to claim 1, wherein the biomass is acidified first followed by impregnation with oxidant, adding a quantity of water, and adding a quantity of lignin dissolving chemicals.

8. A process according to claim 7, wherein the lignin dissolving chemicals is added prior to adding water.

9. A process according to claim 1, wherein the biomass is acidified first followed by adding water, oxidant, and lignin dissolving chemicals.

10. A process according to claim 9, wherein the lignin dissolving chemicals is added prior to adding water.

11. A process according to claim 1, wherein the biomass is acidified first followed by adding lignin dissolving chemicals, water, and oxidant.

12. A process according to claim 11, wherein the oxidant is added prior to adding water.

13. A process according to claim 1, wherein biomass is first soaked in water followed by impregnation with oxidant, acidification, and adding lignin dissolving chemicals.

14. A process according to claim 13, wherein the lignin dissolving chemicals is added prior to acidification.

15. A process according to claim 1, wherein biomass is first soaked in water followed by acidification, impregnation and adding lignin dissolving chemicals.

16. A process according to claim 15, wherein the lignin dissolving chemicals is added prior to impregnation with oxidant.

17. A process according to claim 1, wherein biomass is first soaked in water followed by adding the lignin dissolving chemicals, acidification, and impregnation.

18. A process according to claim 17, wherein the impregnation with oxidant is done prior to acidification.

19. A process according to claim 1, wherein the biomass is first soaked in lignin dissolving chemicals, followed by adding water, impregnation with oxidant, and acidification.

20. A process according to claim 19, wherein the acidification is done prior to impregnation with oxidant.

21. A process according to claim 1, wherein biomass is first soaked in lignin dissolving chemicals followed by acidification, impregnation and adding water.

22. A process according to claim 21, wherein the water is added prior to impregnation with oxidant.

23. A process according to claim 1, wherein biomass is first soaked in lignin dissolving chemicals followed by adding oxidant, water, and acidification.

24. A process according to claim 23, wherein the acidification is done prior to adding water.

27. A process according to claim 1, wherein a quantity of the recyclable solvent can be circulated without any separation of lignin or other chemicals.

25. An oxygen assisted organosolv process for delignification of lignocellulosic biomass materials comprising:

a) placing a quantity of lignocellulosic biomass in contact with a quantity of acid to acidify the biomass;

b) Placing a quantity of the acidified biomass in contact with a quantity of water to make a mixture of biomass, acid, and water;

c) Adding a quantity of lignin dissolving chemical or chemicals to a quantity of the mixture of biomass, water, and acid to make a mixture of biomass and recyclable solvent that includes quantities of acid, water, and lignin dissolving chemicals,

d) Keep the recyclable solvent in contact with biomass under an atmosphere that includes a quantity of oxygen O2, for a period of time at a temperature above boiling point of water.

e) effecting a separation of a quantity of the mixture of biomass and recyclable solvent into a recyclable solvent soluble phase and recyclable solvent insoluble phase; and

f) effecting a separation of a quantity of the recyclable solvent soluble phase into aqueous and organic layers based on their specific density differences; and

,

f) effecting a removal of lignin from a quantity of the organic layer and use the remaining liquid as fresh lignin dissolving solvent for other applications or recycling it back into the fractionation process.

26. A process according to claim 25, where in the biomass can be soaked in water, lignin dissolving chemicals, hydrogen peroxide, or a combination of them prior to acidification.

28. A process according to claim 25, wherein a quantity of the recyclable solvent can be circulated without any separation of lignin or other chemicals.

29. A process for isolating lignin from lignin dissolving solvent, wherein the process comprising:

(a) Mixing lignin dissolving solvent with a quantity of water to helps some of the lignin dissolving solvents float on top.

(b) Evaporate the mixture by applying heat

(c) collect and condense the vapor, with or without vacuum, to reclaim lignin dissolving solvent and water; and

,

(d) effecting a removal of lignin from a quantity of the lignin dissolving solvent.

30. A process according to claim 29, wherein the additional water is added at the beginning of evaporation process

31. A process according to claim 29, wherein the additional water is added at any point after the beginning of evaporation process

32. A process for isolating lignin from lignin dissolving solvent, wherein the separation process comprises;

solvent extraction, chromatography, distillation, filtration, pressing, recrystallization, and/or solvent-solvent partitioning.

33. A plastic consisting essentially a quantity of an isolated lignin as an additive, filler, or colorant, mixed with and a quantity of one or several different polymers.

34. A product according to claim 33, wherein the product comprises a plastic, and wherein the plastic comprises a quantity of the isolated lignin.