Process Operations for Biomass Fractionation

• US 20160002851A1
• Filed: 02/26/2014
• Published: 01/07/2016
• Est. Priority Date: 02/27/2013
• Status: Active Grant

• Current Assignee: Bio-Sep Limited
• Original Assignee: Bio-Sep Limited
• Inventors: Gates, Malcolm Gilbert, McGarel-Groves, Anthony Robin, Anderson, Nigel Donald, Day, Kenneth John Coryton, Leahy, Patrick, Drage, Geoffrey Nicholas
• Granted Patent: US 9,863,090 B2
• Time in Patent Office: Days
• US Class Current: 1/1
• CPC Class Codes: C07G 1/00 Lignin; Lignin derivatives
• CPC Class Codes: 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
• 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: D21C 1/00 Pretreatment of the finely-divided materials before digesting of waste paper D21C5/02
• CPC Class Codes: D21C 1/04 with acid reacting compounds
• CPC Class Codes: D21C 1/10 Physical methods for facilitating impregnation
• CPC Class Codes: D21C 11/0007 Recovery of by-products, i.e. compounds other than those necessary for pulping, for multiple uses or not otherwise provided for volatile compounds obtained by decomposition of spent liquors in order to regenerate them D21C11/125; compounds obtained by fractionating the liquors in order to regenerate them D21C11/0042
• CPC Class Codes: D21C 3/00 Pulping cellulose-containing materials digesters D21C7/00
• CPC Class Codes: D21C 5/00 Other processes for obtaining cellulose, e.g. cooking cotton linters obtaining fibres for spinning D01C; Processes characterised by the choice of cellulose-containing starting materials
• CPC Class Codes: Y02P 30/20 using bio-feedstock
• CPC Class Codes: Y02P 70/10 Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working

Abstract

There is described a method of fractionating a biomass material comprising: (i) blending the biomass material with an acid catalyst to form a slurry; (ii) mixing the slurry with an organosolv reagent optionally under an inert atmosphere to form a pre-treatment mix; (iii) subjecting the pre-treatment mix to sonication; (iv) optionally heating the product of step (iii) in an autoclave under pressure; (v) separating the solid and liquid components of the fractionation mix; (vi) optionally washing the solid; (vii) optionally drying the solid component; (viii) separating the liquid component into organic and aqueous components; and (ix) isolating lignin from the organic component and/or isolating hemi-cellulose from the aqueous component.

Claims

1. A method of fractionating a biomass material comprising the steps of:

(i) blending the biomass material with an acid catalyst to form a slurry (stage

     1);

(ii) mixing the slurry (stage

     1) with an organosolv reagent optionally under an inert atmosphere to form a pre-treatment mix (stage

     2);

(iii) subjecting the pre-treatment mix (stage

     2) to sonication and, optionally, heat (stage

     3);

(iv) optionally heating stage 3 in an autoclave under pressure;

(stage 3a)

(v) separating the solid (stage 4a) and liquid (stage 4b) components of the fractionation mix of stage 3 or stage 3a;

(vi) optionally washing the solid (stage 4a);

(vii) optionally drying the solid component (stage 4a and stage 7a) (to retrieve cellulosic materials);

(viii) separating the liquid component (stage 4b) into organic (stage 5a) and aqueous (stage 5b) components; and

(ix) isolating lignin from the organic component (stage 5a) and/or isolating hemi-cellulose from the aqueous component (stage 5b).

3. A method according to claim 1 which comprises the steps of:

(i) blending the biomass material with an acid catalyst to form a slurry (stage

     1);

(ii) mixing the slurry (stage

     1) with a de-aerated organosolv reagent, optionally under an inert atmosphere, to form a pre-treatment mix (stage

     2);

(iii) subjecting the de-aerated pre-treatment mix (stage

     2) to sonication and, optionally, heat (stage

     3);

(iv) subjecting the sonicated mixture to thermal or ultrasonic digestion and separating the solid (stage 4a) and liquid (stage 4b) components of the digestion mix by fractionation of stage 3 or stage 3a;

(v) optionally washing the solid (stage 4a);

(vi) optionally drying the solid component (stage 4a) (to retrieve cellulosic materials);

(vii) fractionating the liquid component (stage 4b) into organic (stage 5a) and aqueous (stage 5b) components; and

(viii) isolating lignin from the organic component (stage 5a) and/or isolating hemi-cellulose from the aqueous component (stage 5b).

5. A method according to claim 1 which comprises the steps of:

(i) blending the biomass material with an acid catalyst to form a slurry (stage

     1);

(ii) mixing the slurry (stage

     1) with an organosolv reagent to form a pre-treatment mix (stage

     2);

(iii) subjecting the pre-treatment mix (stage

     2) to sonication and, optionally, heat (stage

     3);

(iv) digesting stage 3 in an autoclave under pressure;

(stage 3a)

(v) separating the solid (stage 4a) and liquid (stage 4b) components of the fractionation mix of stage 3 or stage 3a;

(vi) optionally drying the solid component (stage 4a) (to retrieve cellulosic materials);

(vii) separating the liquid component (stage 4b) into organic (stage 5a) and aqueous (stage 5b) components; and

(viii) isolating lignin from the organic component (stage 5a) and/or isolating hemi-cellulose from the aqueous component (stage 5b).

7. A method according to claim 1 wherein a wash stage solid (stage 4a) is included.

8. A method according to claim 1 wherein the blending (stage 1) comprises mixing the biomass material with an aqueous organic acid.

9. A method according to claim 1 wherein the blending (stage 1) comprises mixing the biomass material with aqueous oxalic acid.

10. A method according to claim 1 wherein the biomass material is comminuted to a mean particle size of from about 0.5 to about 10 mm prior to blending.

13. A method according to claim 1 wherein the biomass material is dried prior to blending.

14. A method according to claim 1 wherein the water content in the slurry (stage 1) is from about 30 to about 60 wt. %.

15. A method according to claim 1 wherein the fractionation mix is de-aerated with an inert gas and is subjected to a first sonication step and a second sonication step.

17. A method according to claim 15 wherein the first sonication step is carried out at an elevated pressure of from about >

1 bar to about 10 bar.

20. A method according to claim 1 wherein the sonicator operates at a frequency in the range of from about 10 to about 250 kHz.

22. A method according to claim 1 wherein the sonicator operates at an energy output of from about 50 to about 400 W.

24. A method according to claim 1 wherein the sonicator comprises a three-dimensional arrangement of a plurality of transducers.

25. A method according to claim 1 wherein the fractionation mix is subjected to a first sonication step.

26. A method according to claim 1 wherein the fractionation mix is subjected to a first and a second sonication step.

30. A method according to claim 1 wherein the volume to mass ratio of organosolv reagent to separated solid (pulp) is about 10:

1 v/w.

32. A method according to claim 15 wherein the autoclave step is carried out at a pressure of from about >

5 bar to about 20 bar.

33. A method according to claim 1 wherein the organosolv reagent comprises a ketone, such as, methylisobutylketone (MIBK);

an alcohol, such as ethanol; and

aqueous oxalic acid.

34. A method according to claim 1 wherein the lignin component is recovered by isolating and evaporating the ketone component of the organosolv reagent after fractionation.

35. A method according to claim 1 wherein the hemi-cellulose component is recovered by isolating the aqueous/alcohol component of the organosolv reagent after fractionation and subjecting it to chromatographic separation.

36. A method according to claim 1 wherein the acid catalyst is recovered by crystallisation from the aqueous/alcohol component of the organosolv reagent.

2. (canceled)

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37-45. -45. (canceled)