METHOD FOR LOW WATER HYDROLYSIS OR PRETREATMENT OF POLYSACCHARIDES IN A LIGNOCELLULOSIC FEEDSTOCK

• US 20100056774A1
• Filed: 08/27/2009
• Published: 03/04/2010
• Est. Priority Date: 08/29/2008
• Status: Active Grant

• Current Assignee: Iogen Energy Corporation (Iogen Corporation)
• Original Assignee: Iogen Energy Corporation (Iogen Corporation)
• Inventors: Rowland, Stephen, Anand, Vijay Kumar, Foody, Patrick SR.
• Granted Patent: US 8,328,947 B2
• Time in Patent Office: Days
• US Class Current: 536/124
• CPC Class Codes: C08H 8/00 Macromolecular compounds derived from lignocellulosic materials pretreatment thereof B27N
• CPC Class Codes: C10G 2300/1014 of vegetal origin
• CPC Class Codes: C10G 2300/4012 Pressure
• CPC Class Codes: C10G 2300/807 Steam
• CPC Class Codes: C10L 1/02 essentially based on components consisting of carbon, hydrogen, and oxygen only
• CPC Class Codes: C12P 19/02 Monosaccharides 2-ketogulonic acid C12P7/60
• 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
• CPC Class Codes: Y02P 30/20 using bio-feedstock

Abstract

A method is provided for hydrolyzing polysaccharides in a lignocellulosic feedstock to produce monosaccharides or pretreating a lignocellulosic feedstock, in which an aqueous slurry of the lignocellulosic feedstock is fed into a pressurized dewatering zone wherein the feedstock is partially dewatered and then is compressed into a plug. The plug is introduced into a reaction zone that operates at a pressure (P_r) equal to greater than about 90 psia and under suitable temperature and pH conditions to hydrolyze the polysaccharides or pretreat the feedstock. The plug provides a pressure seal between the outlet of the dewatering zone and the reaction zone. The pressure (P_dwi) of the aqueous slurry of the lignocellulosic feedstock at the inlet of the dewatering device is related to P_r as follows:

• • 0≦ΔP<the lesser of [(P_r−20 psia) and 220 psia], and
  • where ΔP is the absolute difference in pressure between P_r and P_dwi in psia.

Claims

1. A method for hydrolyzing polysaccharides in a lignocellulosic feedstock to produce monosaccharides, comprising:

a) providing interconnected dewatering, plug formation and reaction zones, each of the dewatering, plug formation and reaction zones being provided with an inlet zone and an outlet zone, the outlet zone of the dewatering zone being operationally associated with the inlet zone of the plug formation zone and the outlet zone of the plug formation zone being operationally associated with the inlet zone to the reaction zone, wherein the pressure (P_r) in the reaction zone is from about 90 to about 680 psia;

b) feeding an aqueous slurry of the lignocellulosic feedstock to the dewatering zone to produce a partially dewatered lignocellulosic feedstock and an aqueous liquid, wherein the pressure (P_dwi) of the aqueous slurry of the lignocellulosic feedstock at the inlet zone of the dewatering zone is related to P_r as follows;

0≦

Δ

P<

the lesser of [(P_r−

20 psia) and 220 psia], and

where Δ

P is the absolute difference in pressure between P_r and P_dwi in psia

c) withdrawing, from the dewatering zone, a portion of the aqueous liquid to produce a withdrawn aqueous liquid, the withdrawn aqueous liquid being substantially free of solid lignocellulosic feedstock, and at a pressure which is lower than the pressure of the aqueous slurry of the lignocellulosic feedstock at the inlet zone of the dewatering zone;

d) moving the partially dewatered lignocellulosic feedstock from the outlet zone of the dewatering zone to the inlet zone of the plug formation zone;

e) forming a plug of lignocellulosic feedstock within the plug formation zone to provide a pressure seal between the outlet zone of the dewatering zone and the inlet zone of the reaction zone;

f) feeding the plug of lignocellulosic feedstock from the outlet zone of the plug formation zone to the inlet zone of the reaction zone, wherein the pressure at the outlet zone of the plug formation zone is substantially the same as the pressure at the inlet zone to the reaction zone;

g) maintaining suitable temperature and pH conditions in the reaction zone to hydrolyze polysaccharides in the lignocellulosic feedstock to produce the monosaccharides; and

h) recovering the monosaccharides produced in step g).

4. The method of claim 1, 2 or 3, wherein the aqueous slurry of the lignocellulosic feedstock has a weight ratio of water to dry lignocellulosic feedstock solids of about 5:

1 to about 33;

1 prior to entering the dewatering zone.

5. The method of claim 1, 2 or 3, wherein the aqueous slurry of the lignocellulosic feedstock has a weight ratio of water to dry lignocellulosic feedstock solids of about 7:

1 to about 24;

1 prior to entering the dewatering zone.

6. The method of any one of claims 1 to 5, wherein the partially dewatered lignocellulosic feedstock has a weight ratio of water to dry lignocellulosic feedstock solids of about 0.5:

1 to about 5;

1.

7. The method of any one of claims 1 to 5, wherein the partially dewatered lignocellulosic feedstock has a weight ratio of water to dry lignocellulosic feedstock solids of about 1.5:

1 to about 4;

1.

8. The method of any one of claims 1 to 7, wherein the plug of lignocellulosic feedstock at the outlet zone of the dewatering zone has a weight ratio of water to dry lignocellulosic feedstock solids of about 0.5:

1 to about 5;

1.

9. The method of any one of claims 1 to 7, wherein the plug of lignocellulosic feedstock at the outlet zone of the dewatering zone has a weight ratio of water to dry lignocellulosic feedstock solids of about 1.5:

1 to about 4;

1.

10. The method of any one of claims 1 to 9, wherein the pressure of the aqueous slurry of the lignocellulosic feedstock at the inlet of the dewatering zone is about 70 psia to about 900 psia.

11. The method of any one of claims 1 to 9, wherein the pressure of the aqueous slurry of the lignocellulosic feedstock at the inlet of the dewatering zone is about 70 psia to about 800 psia.

12. The method of any one of claims 1 to 9, wherein the pressure of the aqueous slurry of the lignocellulosic feedstock at the inlet zone of the dewatering zone is about 300 psia to about 800 psia.

13. The method of any one of claims 1 to 12, wherein the pressure of the aqueous liquid withdrawn from the dewatering zone is about 0.3 psia to about 50 psia lower than the pressure of the aqueous slurry of the lignocellulosic feedstock at the inlet zone of the dewatering zone.

14. The method of any one of claims 1 to 12, wherein the pressure of the aqueous liquid withdrawn from the dewatering zone is about 1 psia to about 50 psia lower than the pressure of the aqueous slurry of the lignocellulosic feedstock at the inlet zone of the dewatering zone.

15. The method of any one of claims 1 to 14, wherein the partially dewatered lignocellulosic feedstock is heated prior to its entry into the reaction zone, in the reaction zone or a combination thereof.

16. The method of any one of claims 1 to 14, wherein the partially dewatered lignocellulosic feedstock is at least partly heated by direct steam injection prior to its entry into the reaction zone, in the reaction zone or a combination thereof.

17. The method of any one of claims 1 to 16, wherein the lignocellulosic feedstock is reacted in the reaction zone under acidic conditions.

18. The method of claim 17, wherein the pH in the reaction zone is between 0 and about 3.0.

19. The method of claim 17, wherein the pH in the reaction zone is between about 0.2 and about 3.0.

20. The method of claim 17, wherein the pH in the reaction zone is between about 0.5 and about 3.0.

21. The method of any one of claims 17 to 20, wherein acid is added to the lignocellulosic feedstock prior to the entry of the plug of the lignocellulosic feedstock into the reaction zone.

22. The method of any one of claims 17 to 20, wherein acid is added to the reaction zone.

23. The method of any one of claims 17 to 22, wherein the lignocellulosic feedstock is held in the reaction zone for a suitable time of about 10 seconds to about 20 minutes at a suitable temperature of about 180°

C. to about 260°

C. to hydrolyze the lignocellulosic feedstock.

24. The method of any one of claims 17 to 22, wherein the lignocellulosic feedstock is held in the reaction zone for suitable time of about 10 seconds to about 600 seconds at a suitable temperature of about 180°

C. to about 260°

C. to pretreat the lignocellulosic feedstock.

25. The method of any one of claims 17 to 22, wherein the lignocellulosic feedstock is held in the reaction zone for suitable time of about 10 seconds to about 180 seconds at a suitable temperature of about 180°

C. to about 260°

C. to pretreat the lignocellulosic feedstock.

26. The method of any one of claims 17 to 25, wherein acid that is added to the lignocellulosic feedstock is selected from the group consisting of sulfuric acid, sulfurous acid, hydrochloric acid, phosphoric acid or any combination thereof.

27. The method of any one of claims 17 to 25, wherein acid that is added to the lignocellulosic feedstock is sulfuric acid.

28. The method of any one of claims 1 to 16, wherein the lignocellulosic feedstock is reacted in the reaction zone under alkaline conditions.

29. The method of claim 28, wherein an alkali selected from the group consisting of ammonia, ammonium hydroxide, potassium hydroxide, sodium hydroxide or any combination thereof is added to the lignocellulosic feedstock prior to the entry of the plug of the lignocellulosic feedstock into the reaction zone, in the reaction zone or a combination thereof.

30. The method of claim 28 or claim 29, wherein the pH in the reaction zone is between about 9.5 and about 14.

31. The method of any one of claims 28 to 30, wherein the temperature in the reaction zone is between about 135°

C. and about 260°

C.

32. The method of any one of claims 28 to 30, wherein the temperature in the reaction zone is between about 120°

C. and about 220°

C. and the lignocellulosic feedstock is reacted for about 1 minute to about 120 minutes to pretreat the lignocellulosic feedstock.

33. The method of any one of claims 28 to 30, wherein the temperature in the reaction zone is between about 120°

C. and about 220°

C. and the lignocellulosic feedstock is reacted for about 2 minutes to about 60 minutes to pretreat the lignocellulosic feedstock.

34. The method of any one of claims 28 to 30, wherein the alkali is ammonia, ammonium hydroxide, or a combination thereof, the temperature in the reaction zone is between about 20°

C. and about 100°

C. and the lignocellulosic feedstock is reacted for about 1 minute to about 20 minutes to pretreat the lignocellulosic feedstock.

35. The method of any one of claims 28 to 30, wherein the alkali is ammonia, ammonium hydroxide, or a combination thereof, the temperature in the reaction zone is between about 20°

C. and about 150°

C. and the lignocellulosic feedstock is reacted for about 1 minute to about 20 minutes to pretreat the lignocellulosic feedstock.

36. The method of any one of claims 28 to 30, wherein the alkali is ammonia, ammonium hydroxide, or a combination thereof, the temperature in the reaction zone is between about 100°

C. and about 150°

C. and the lignocellulosic feedstock is reacted for about 1 minute to about 20 minutes to pretreat the lignocellulosic feedstock.

37. The method of any one of claims 28 to 30, wherein the alkali is potassium hydroxide, sodium hydroxide, or a combination thereof, the temperature in the reaction zone is between about 100°

C. and about 140°

C. and the lignocellulosic feedstock is reacted for about 15 minutes to about 120 minutes to pretreat the lignocellulosic feedstock.

38. The method of any one of claims 1 to 37, wherein the reacted lignocellulosic feedstock is cooled to a temperature equal to or less than 100°

C. after the reacted lignocellulosic feedstock is discharged from the reaction zone.

39. The method of claim 38, including the step of reducing the pressure of the reacted lignocellulosic feedstock to atmospheric pressure.

2. A method for hydrolyzing polysaccharides in a lignocellulosic feedstock to produce monosaccharides, comprising:

a) providing interconnected dewatering, plug formation and reaction zones, each of the dewatering, plug formation and reaction zones being provided with an inlet zone and an outlet zone, the outlet zone of the dewatering zone being operationally associated with the inlet zone of the plug formation zone and the outlet zone of the plug formation zone being operationally associated with the inlet zone to the reaction zone, wherein the pressure (P_r) in the reaction zone is from about 300 to about 680 psia;

b) feeding an aqueous slurry of the lignocellulosic feedstock to the dewatering zone to produce a partially dewatered lignocellulosic feedstock and an aqueous liquid, wherein the pressure (P_dwi) of the aqueous slurry of the lignocellulosic feedstock at the inlet zone of the dewatering zone is related to P_r as follows;

0≦

Δ

P<

220 psia, and

where Δ

P is the absolute difference in pressure between P_r and P_dwi in psia

c) withdrawing, from the dewatering zone, a portion of the aqueous liquid to produce a withdrawn aqueous liquid, the withdrawn aqueous liquid being substantially free of solid lignocellulosic feedstock, and at a pressure which is lower than the pressure of the aqueous slurry of the lignocellulosic feedstock at the inlet zone of the dewatering zone;

d) moving the partially dewatered lignocellulosic feedstock from the outlet zone of the dewatering zone to the inlet zone of the plug formation zone;

e) forming a plug of lignocellulosic feedstock within the plug formation zone to provide a pressure seal between the outlet zone of the dewatering zone and the inlet zone of the reaction zone;

f) feeding the plug of lignocellulosic feedstock from the outlet zone of the plug formation zone to the inlet zone of the reaction zone, wherein the pressure at the outlet zone of the plug formation zone is substantially the same as the pressure at the inlet zone to the reaction zone;

g) maintaining suitable temperature and pH conditions in the reaction zone to hydrolyze polysaccharides in the lignocellulosic feedstock to produce the monosaccharides; and

h) recovering the monosaccharides produced in step g).

3. A method for producing a pretreated lignocellulosic feedstock comprising:

a) providing interconnected dewatering, plug formation and reaction zones, each of the dewatering, plug formation and reaction zones being provided with an inlet zone and an outlet zone, the outlet zone of the dewatering zone being operationally associated with the inlet zone of the plug formation zone and the outlet zone of the plug formation zone being operationally associated with the inlet zone to the reaction zone, wherein the pressure (P_r) in the reaction zone is from about 90 to about 680 psia;

b) feeding an aqueous slurry of the lignocellulosic feedstock to the dewatering zone to produce a partially dewatered lignocellulosic feedstock and an aqueous liquid, wherein the pressure (P_dwi) of the aqueous slurry of the lignocellulosic feedstock at the inlet zone of the dewatering zone is related to P_r as follows;

0≦

Δ

P<

the lesser of [(P_r−

20 psia) and 220 psia], and

where Δ

P is the absolute difference in pressure between P_r and P_dwi in psia

c) withdrawing, from the dewatering zone, a portion of the aqueous liquid to produce a withdrawn aqueous liquid, the withdrawn aqueous liquid being substantially free of solid lignocellulosic feedstock, and at a pressure that is lower than the pressure of the aqueous slurry of the lignocellulosic feedstock at the inlet zone of the dewatering zone;

d) moving the partially dewatered lignocellulosic feedstock from the outlet zone of the dewatering zone to the inlet zone of the plug formation zone;

e) forming a plug of lignocellulosic feedstock within the plug formation zone to provide a pressure seal between the outlet zone of the dewatering zone and the inlet zone of the reaction zone;

f) feeding the plug of lignocellulosic feedstock from the outlet zone of the plug formation zone to the inlet zone of the reaction zone, wherein the pressure at the outlet zone of the plug formation zone is substantially the same as the pressure at the inlet zone to the reaction zone; and

g) pretreating the lignocellulosic feedstock in the reaction zone to produce the pretreated feedstock.

40. A system for the pretreatment or hydrolysis of a lignocellulosic feedstock including interconnected dewatering, plug formation and reactor devices wherein the pressure (P_r) in the reaction device is from about 90 to about 680 psia, comprising:

a pump or pumps for pumping an aqueous slurry of the lignocellulosic feedstock into the dewatering device at a pressure between about 70 psia and about 900 psia and wherein the pressure (P_dwi) of the aqueous slurry of the lignocellulosic feedstock at the inlet of the dewatering device is related to P_r as follows;

0≦

Δ

P<

the lesser of [(P_r−

20 psia) and 220 psia], and

where Δ

P is the absolute difference in pressure between P_r and P_dwi in psia;

means within the dewatering device for removing aqueous liquid from the aqueous slurry of the lignocellulosic feedstock to form a partially dewatered lignocellulosic feedstock;

means for withdrawing aqueous liquid from within the dewatering device;

means for urging the partially dewatered lignocellulosic feedstock from the dewatering device into the plug formation device to form a plug of the lignocellulosic feedstock; and

means for discharging the plug of lignocellulosic feedstock from the plug formation device and feeding the lignocellulosic feedstock into the reaction device which is at a pressure that is substantially the same as the pressure of the plug of lignocellulosic feedstock that is discharged from the plug formation device.

41. The system of claim 40, wherein, when the system is in operation, the aqueous slurry of the lignocellulosic feedstock is pumped into the dewatering device at a pressure between about 70 psia and about 800 psia.

42. The system of claim 40 or 41, including means to break up the plug of lignocellulosic material prior to feeding the lignocellulosic feedstock into the reaction device.

43. The system of any one of claims 40 to 42, wherein the dewatering device and the plug formation device are integrated into a combined dewatering and plug formation device.

44. A method for producing a pretreated lignocellulosic feedstock comprising:

a) providing interconnected dewatering, plug formation and reaction zones, each of the dewatering, plug formation and reaction zones being provided with an inlet zone and an outlet zone, the outlet zone of the dewatering zone being operationally associated with the inlet zone of the plug formation zone and the outlet zone of the plug formation zone being operationally associated with the inlet zone to the reaction zone, wherein the pressure (P_r) in the reaction zone is from about 90 to about 680 psia;

b) feeding an aqueous slurry of the lignocellulosic feedstock to the dewatering zone to produce a partially dewatered lignocellulosic feedstock and an aqueous liquid, wherein the pressure (P_dwi) of the aqueous slurry of the lignocellulosic feedstock at the inlet zone of the dewatering zone is related to P_r as follows;

0≦

Δ

P<

the lesser of [(P_r−

20 psia) and 220 psia], and

where Δ

P is the absolute difference in pressure between P_r and P_dwi in psia

c) withdrawing, from the dewatering zone, a portion of the aqueous liquid to produce a withdrawn aqueous liquid, the withdrawn aqueous liquid being substantially free of solid lignocellulosic feedstock, and at a pressure which is lower than the pressure of the aqueous slurry of the lignocellulosic feedstock at the inlet zone of the dewatering zone;

d) moving the partially dewatered lignocellulosic feedstock from the outlet zone of the dewatering zone to the inlet zone of the plug formation zone;

e) forming a plug of lignocellulosic feedstock within the plug formation zone to provide a pressure seal between the outlet zone of the dewatering zone and the inlet zone of the reaction zone;

f) feeding the plug of lignocellulosic feedstock from the outlet zone of the plug formation zone to the inlet zone of the reaction zone, wherein the pressure at the outlet zone of the plug formation zone is substantially the same as the pressure at the inlet zone to the reaction zone;

g) adding acid to the partially dewatered lignocellulosic feedstock prior to the entry of the plug of the lignocellulosic feedstock into the reaction zone or to the reaction zone; and

h) maintaining a temperature of between about 180°

C. and about 260°

C., a pH of between about 0.5 and about 3 for between about 10 seconds and about 600 seconds to pretreat the lignocellulosic feedstock thereby hydrolyzing hemicellulose contained in the feedstock to xylose.