Method of processing lignocellulosic feedstock for enhanced xylose and ethanol production

• US 7,901,511 B2
• Filed: 02/27/2002
• Issued: 03/08/2011
• Est. Priority Date: 02/28/2001
• Status: Active Grant

• Current Assignee: Iogen Energy Corporation (Iogen Corporation)
• Original Assignee: Iogen Energy Corporation (Iogen Corporation)
• Inventors: Anand, Vijay, Tolan, Jeffrey S., Griffin, Robert, Nicholson, Colin, Mott, Corinne
• Primary Examiner(s): Marx; Irene
• Assistant Examiner(s): UNDERDAHL, THANE E
• Application Number:
  US10/467,741
• Publication Number:
  US 20040231661A1
• Time in Patent Office: 3,296 Days
• Field of Search: None
• US Class Current: 127/37
• CPC Class Codes: A23L 33/21 Addition of substantially indigestible substances, e.g. dietary fibres
• CPC Class Codes: C12P 19/02 Monosaccharides 2-ketogulonic acid C12P7/60
• CPC Class Codes: C12P 19/14 produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase , e.g. by cellulase, hemicellulase
• CPC Class Codes: C12P 2201/00 Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
• CPC Class Codes: C12P 7/10 substrate containing cellulosic material
• CPC Class Codes: C13K 1/02 obtained by saccharification of cellulosic materials manufacture of fodder A23K10/32
• CPC Class Codes: Y02E 50/10 Biofuels, e.g. bio-diesel

Abstract

The present invention provides a method of producing xylose from lignocellulosic feedstock. The method comprises disrupting lignocellulosic feedstock; leaching the lignocellulosic feedstock by contacting the feedstock with at least one aqueous solution for a period greater than about 2 minutes to produce a leached feedstock and a leachate; removing the leachate from the leached feedstock; acidifying the leached feedstock to a pH between about 0.5 and about 3 to produce an acidified feedstock, and; reacting the acidified feedstock under conditions which disrupt fiber structure and hydrolyze a portion of hemicellulose and cellulose of the acidified feedstock, to produce a composition comprising xylose and a pretreated feedstock. The xylose may be purified from the pretreated feedstock or it may be converted to ethanol with the pretreated feedstock.

Claims

1. A method of producing xylose comprising, in this order:

a) leaching a lignocellulosic feedstock comprising greater than about 20% (w/w) cellulose, said leaching comprising contacting said feedstock with at least one aqueous solution of about pH 6 to about pH 9 for between about 2 minutes and about 5 hours, at a temperature of about 25°

C. to about 80°

C. to produce a leached feedstock and a leachate;

b) removing leachate from said leached feedstock; and

c) treating said leached feedstock with an aqueous solution at a temperature of at least about 100°

C. and at a pH of about 0.5 to about 2.5 to produce a composition comprising xylose and a treated feedstock.

2. The method of claim 1, wherein said lignocellulosic feedstock is selected from the group consisting of sugar beet bagasse, soybean stover, corn stover, rice straw, rice hulls, barley straw, corn cobs, wheat straw, wheat chaff, oat hulls, corn fiber, wood fiber, switch grass, cord grass, rye grass, miscanthus, and a combination thereof.

3. The method of claim 2, wherein said lignocellulosic feedstock comprises mechanically disrupted feedstock.

4. The method of claim 3, wherein said mechanically disrupted feedstock is capable of passing through about 20 mesh.

5. The method of claim 2, wherein said lignocellulosic feedstock has an AX/NSP ratio of about 0.35 to about 0.45.

6. The method of claim 5, wherein said feedstock comprises wheat straw, wheat chaff, switch grass, corn stover, corn cobs, oat hulls, or a combination thereof.

7. The method of claim 3, wherein said disrupted feedstock is produced by shredding, milling, chopping, chipping, grinding or a combination thereof.

8. The method of claim 7, wherein said milling comprises Szego milling, Hammer milling, Wiley milling, or a combination thereof.

9. The method of claim 1, wherein said leaching is performed for a period between about 2 minutes and about 2 hours.

10. The method of claim 1, wherein the amount of aqueous solution of step (a) added during said leaching is between about 0.25 to about 10 times the maximum water holding capacity of said lignocellulosic feedstock, wherein the maximum water holding capacity is measured by:

(i) mechanically disrupting a sample of the lignocellulosic feedstock;

(ii) adding water to a known dry mass of the mechanically disrupted feedstock until the point at which additional water added is free water;

(iii) determining the mass of water required to reach the point at which additional water added is free water; and

(iv) dividing the mass of water determined in step (iii) by the known dry mass of mechanically disrupted feedstock to obtain a value representing the maximum water holding capacity.

11. The method of claim 10, wherein the amount of aqueous solution added during said leaching is about 1.5 to 3 times the maximum water holding capacity of said lignocellulosic feedstock.

12. The method of claim 1, wherein said at least one aqueous solution of step (a) comprises water, mill water, process water, a leachate or a combination thereof.

13. The method of claim 1, wherein said pH of the at least one aqueous solution of step (a) is adjusted using NaOH, H₂SO₄, or a combination thereof.

14. The method of claim 1, wherein said leaching comprises a plurality of leaching stages.

15. The method of claim 14, wherein said leaching stages comprise 2 to 4 leaching stages.

16. The method of claim 14, wherein said plurality of leaching stages are performed such that leachate removed from a downstream leaching stage is added to an upstream leaching stage.

17. The method of claim 1, wherein said leaching removes between about 50% to about 100% of the total leachable buffering agents from the lignocellulosic feedstock.

18. The method of claim 1, wherein said leaching removes between about 70% to about 100% of the total leachable buffering agents from the lignocellulosic feedstock.

19. The method of claim 18, wherein said leaching removes between about 90% to about 100% of the total leachable buffering agents from the lignocellulosic feedstock.

20. The method of claim 1, wherein the treating of step (c) is performed using an acid selected from the group consisting of sulfuric acid, nitric acid and hydrochloric acid.

21. The method of claim 20, wherein said acid is sulfuric acid.

22. The method of claim 1, wherein said leachate is sampled during leaching, following leaching or both, and wherein conditions of the leaching are adjusted accordingly.

23. The method of claim 1, wherein the xylose is a xylose monomer.

24. The method of claim 1, wherein said composition produced from said method comprises a xylose concentration in the range of about 150 mg to about 260 mg of xylose per gram of feedstock.

25. The method of claim 1, wherein said treated feedstock has increased accessibility to being digested with cellulase enzymes.

26. The method of claim 1, wherein said method further comprises cellulase treatment of said treated feedstock.

27. The method of claim 10, wherein said method further comprises cellulase treatment of said treated feedstock.

28. The method of claim 1, wherein said at least one aqueous solution of step (a) comprises less than about 10 g/1 impurities.

29. The method of claim 1, wherein said lignocellulosic feedstock comprises cellulose in an amount greater than about 30% (w/w).

30. The method of claim 1, wherein said lignocellulosic feedstock comprises a lignin content in an amount greater than about 5% (w/w).

31. The method of claim 1, wherein said lignocellulosic feedstock comprises a combined sugar content of sucrose, fructose and starch of less than about 20% (w/w).

32. The method of claim 1, wherein said lignocellulosic feedstock comprises oat hulls, wheat straw, switch grass, or a combination thereof.

33. The method of producing xylose according to claim 3, wherein said contacting with said at least one aqueous solution is for a period of about 2 minutes to about 2 hours using a volume of the at least one aqueous solution which is between about 0.25 and about 10 times the maximum water holding capacity of said disrupted lignocellulosic feedstock per kilogram of dried feedstock.

34. The method of claim 1, further comprising, prior to said leaching step (a), heating said lignocellulosic feedstock to about 80°

C.

35. The method of claim 1, wherein in said leaching step (a), the lignocellulosic feedstock is incubated within a leaching bath and debris is removed.

36. The method of claim 35, wherein in said leaching step (a), said lignocellulosic feedstock is incubated from about 5 to about 30 minutes.

37. The method of claim 1, wherein said step (b) of removing said leachate from said leached feedstock comprises crushing said leached feedstock to produce a pressate and a solid feedstock, said pressate comprising soluble protein which is further processed for animal feed.

38. A method of producing ethanol comprising, in this order:

a) preparing said composition comprising xylose and treated feedstock according to claim 1;

b) treating said composition comprising xylose and treated feedstock with cellulase under conditions which hydrolyse cellulose in said treated feedstock to glucose, producing a sugar solution comprising xylose and glucose; and

c) fermenting said sugar solution to ethanol.

39. A method of producing ethanol, comprising:

a) preparing said composition comprising xylose and treated feedstock according to claim 1; and

b) treating said composition with a microorganism under conditions which permit fermentation of said xylose in said composition to ethanol.

40. A method of producing ethanol comprising, in this order:

a) preparing said composition comprising xylose and treated feedstock according to claim 1;

b) separating said treated feedstock from said composition;

c) treating said treated feedstock with cellulase under conditions that hydrolyze cellulose in said treated feedstock to glucose, producing a sugar solution comprising glucose; and

d) fermenting said sugar solution to ethanol.

41. The method of claim 1, wherein leaching is performed at a temperature of about 60°

C. to about 80°

C.

42. The method of claim 41, wherein said at least one aqueous solution of step (a) comprises about 0.25 to about 10 times the maximum water holding capacity per kilogram of dry lingocellulosic feedstock.

43. The method of claim 1, wherein leaching is performed for a period between about 10 minutes and about 30 minutes.

44. The method of claim 42, wherein leaching is performed at a temperature of about 70°

C.

45. The method of claim 42, wherein the aqueous solution has a pH of about 6 to about 7.

46. The method of claim 42, wherein said leached feedstock is treated in step (c) at a temperature of about 100°

C. to about 220°

C.

47. The method of claim 46, wherein said leached feedstock is treated for about 5 seconds to about 60 minutes.

48. The method of claim 1, wherein said treatment of step (c) comprises a first stage at a temperature between about 100°

C. to about 180°

C. followed by a second stage at a temperature between about 180°

C. to about 270°

C.

49. The method of claim 48, wherein said first stage is performed between about 0.25 to about 24 hours.

50. The method of claim 49, wherein said second stage is performed between about 5 to about 120 seconds.

52. The method of claim 1, wherein during step (b), between about 20 % and about 100% of the leachate is removed from the leached feedstock.

51. A method of producing xylose and glucose comprising, in this order:

a) leaching a mechanically-disrupted or preconditioned lignocellulosic feedstock comprising greater than about 20% (w/w) cellulose, said leaching being conducted prior to any chemical treatment of said lignocellulosic feedstock, comprising contacting said feedstock with at least one aqueous solution of pH 6 to 9 for a period greater than 2 minutes at a temperature of 25°

C. to about 80°

C. to produce a leached feedstock and a leachate;

b) removing the leachate from said leached feedstock; and

c) treating said leached feedstock with an aqueous solution at a temperature of at least about 100°

C. with ammonia under conditions which disrupt fiber structure of the leached feedstock and hydrolyze a portion of hemicellulose in said leached feedstock to produce a composition comprising a treated feedstock; and

d) treating said composition with an enzyme comprising cellulase under conditions which hydrolyze cellulose in said leached feedstock to glucose, thereby producing a sugar solution comprising xylose and glucose.

53. The method of claim 51, wherein said leaching is conducted for a period of between about 10 minutes and about 5 hours.