Treatment method for fibrous lignocellulosic biomass using fixed stator device having nozzle tool with opposing coaxial toothed rings to make the biomass more susceptible to hydrolysis

• US 5,498,766 A
• Filed: 12/02/1994
• Issued: 03/12/1996
• Est. Priority Date: 12/17/1992
• Status: Expired due to Term

• Current Assignee: RA ENERGY, LTD., AFEX CORPORATION, EARNEST STUART, LINDA CLEBOSKI, TOM CAHALAN, BETTY ZOCH
• Original Assignee: Colorado State University Research Foundation
• Inventors: Stuart, Earnest D., Latimer, Vivian M.
• Primary Examiner(s): Naff, David M.
• Assistant Examiner(s): Meller, Michael V.
• Application Number:
  US08/348,453
• Time in Patent Office: 466 Days
• Field of Search: 435/99, 435/105, 435/277
• US Class Current: 435/99
• CPC Class Codes: C08H 8/00 Macromolecular compounds derived from lignocellulosic materials pretreatment thereof B27N
• CPC Class Codes: C13K 1/02 obtained by saccharification of cellulosic materials manufacture of fodder A23K10/32
• CPC Class Codes: Y02P 20/582 Recycling of unreacted starting or intermediate materials

Abstract

High-shear, microcavitation is used to shred and disintegrate fibrous lignocellulose-containing biomass to make the biomass more susceptible to hydrolysis. This process is preferably performed with the biomass particles dispersed in a slurry created using only water. The process can be performed on slurries created with other liquids such as liquid ammonia, aqueous solutions of acid or alkali reagents, or enzyme solutions containing cellulase, cellobiase or a combination thereof. High-shear microcavitation is carried out by subjecting the slurry to high-shear forces by injecting the slurry cross-currently into a turbulent Couette flow created in a high-frequency, rotor-stator device. This microcavitation shatters the fibrous structure of the biomass in the slurry thereby creating a sheared slurry. The device has a chamber containing a fixed stator equipped with a nozzle tool containing concentric rings having bore holes meshing with opposing coaxial tooth rings coupled to a rotor that is coupled to a rotatable shaft.

Claims

1. A method of treating a fibrous lignocellulosic biomass to make it more susceptible to hydrolysis, comprising the following steps:

a) providing a ground fibrous lignocellulosic biomass;

b) mixing said ground biomass with water to produce a slurry; and

c) subjecting said slurry to high-shear forces by injecting said slurry cross-currently into a turbulent Couette flow created in a high-frequency, rotor-stator device under conditions to microcavitate the slurry to shatter the fibrous structure of the biomass in the slurry creating a sheared slurry, said device comprising a chamber containing a fixed stator equipped with a nozzle tool containing concentric rings having bore holes meshing, with opposing coaxial toothed rings coupled to a rotor that is coupled to a rotatable shaft.

2. The method of claim 1, wherein the slurry of step (b) was formed in a medium-shear, mixer-grinder-pump then passed to step (c).

3. The method of claim 1, further comprising;

d) mixing the sheared slurry from step (c) with an enzyme to form a mixture; and

e) subjecting said mixture to said high-shear forces created by said device to form a sheared mixture.

4. The method of claim 3, wherein the enzyme comprises cellulase, cellobiase, or a combination of cellulase and cellobiase.

5. The method of claim 3, wherein said mixture further comprises a surfactant.

6. The method of claim 5, wherein the surfactant is an oleate ester of sorbitol.

7. The method of claim 3, further comprising the following steps:

f) separating said sheared mixture from step (e) to produce a filtrate and a retentate;

g) adding the retentate to a newly formed sheared slurry from step (c) forming a mixture; and

h) simultaneously adding an enzyme to said mixture and subjecting said mixture to said high-shear forces created by said device.

24. The method of claim 1, further comprising the following steps:

holding said slurry formed in step B in residence at a temperature of about 90°

C. for about 30 minutes;

titrating the pH of said slurry to a pH of about 5 and passing said slurry to said C.

8. A method for treating lignocellulosic biomass to make it more susceptible to hydrolysis, comprising the steps of:

a) mixing a ground lignocellulosic biomass with water to produce a slurry; and

b) subjecting said slurry to high-shear forces by injecting said slurry cross-currently into a turbulent Couette flow created in a high-frequency, rotor-stator device under conditions to microcavitate said slurry to shatter the fibrous structure of the biomass in the slurry creating a sheared slurry, said device comprising a chamber containing a fixed stator equipped with a nozzle tool containing concentric rings having bore holes meshing with opposing coaxial toothed rings coupled to a rotor that is coupled to a rotatable shaft.

9. The method of claim 8, further comprising:

c) mixing the sheared slurry from step (b) with an enzyme to form a mixture; and

d) subjecting said mixture to said high-shear forces created by said device to form a sheared mixture.

10. The method of claim 9, wherein the enzyme comprises cellulase, cellobiase, or a combination of cellulase and cellobiase.

11. The method of claim 9, wherein said mixture further comprises a surfactant.

12. The method of claim 11, wherein said surfactant is an oleate ester of sorbitol.

13. The method of claim 9, further comprising the following steps:

f) separating said sheared mixture from step (d) to produce a filtrate and a retentate;

g) adding the retentate to a newly formed sheared slurry from step (b) forming a mixture; and

h) simultaneously adding an enzyme to said mixture and subjecting said mixture to said high-shear forces created by said device.

14. A method of treating lignocellulosic biomass to make it more susceptible to hydrolysis, comprising the following steps:

a) providing a ground fibrous lignocellulosic biomass;

b) mixing said ground biomass with water in a medium-shear, mixer-grinder-pump to produce a slurry;

c) holding said slurry in residence at a temperature of about 90°

C. for about 30 minutes;

d) titrating the pH of said slurry to pH of about 5;

e) subjecting said slurry to high-shear forces by injecting said slurry cross-currently into a turbulent Couette flow created in a high-frequency, rotor-stator device under conditions to microcavitate the slurry to shatter the fibrous structure of the biomass in the slurry creating a sheared slurry, said device comprising a chamber containing a fixed stator equipped with a nozzle tool containing concentric rings having bore holes meshing with opposing coaxial toothed rings coupled to a rotor that is coupled to a rotatable shaft;

cooling said sheared slurry to a temperature of about 50°

C.;

g) mixing said sheared slurry with an enzyme, selected from the group cellulase, cellobiase, and a combination of cellulase and cellobiase, and a surfactant to form a first mixture;

h) subjecting said first mixture to said high-shear forces created by said device;

i) separating said first mixture producing a filtrate and a retentate;

j) adding the retentate to a newly formed sheared slurry from step (c) forming a second mixture; and

k) simultaneously adding an enzyme, selected from the group cellulase, cellobiase, and a combination of cellulase and cellobiase, and a surfactant to said second mixture and subjecting said second mixture to said high-shear forces created by said device.

15. The method of claim 14, wherein the surfactant is an oleate ester of sorbitol.

16. A method of hydrolyzing lignocellulosic biomass, comprising the following steps:

a) mixing a ground lignocellulosic biomass, water, an enzyme capable of converting cellulose and hemicellulose to sugars, and a surfactant to form a slurry;

b) subjecting said slurry to high-shear forces by injecting said slurry cross-currently into a turbulent Couette flow created in a high-frequency, rotor-stator device under conditions to microcavitate said slurry to shatter the fibrous structure of the biomass in the slurry creating a sheared slurry, said device comprising a chamber containing a fixed stator equipped with a nozzle tool containing concentric rings having bore holes meshing with opposing coaxial toothed rings coupled to a rotor coupled to a rotatable shaft.

17. The method of claim 16, further comprising the following steps:

c) separating said sheared slurry from step (b) to produce a filtrate and a retentate;

d) adding the retentate to a newly formed sheared slurry from step (b) forming a mixture; and

e) simultaneously adding an enzyme selected from the group cellulase, cellobiase and a combination of cellulase and cellobiase and a surfactant to said mixture and subjecting said mixture to said high-shear forces created by said device.

18. The method of claim 17, wherein the surfactant is an oleate ester of sorbitol.

19. A method of treating lignocellulosic biomass to make it more susceptible to hydrolysis, comprising the following steps:

a) providing a ground lignocellulosic biomass;

b) mixing said ground biomass with liquid ammonia to produce a slurry;

c) subjecting said slurry to high-shear forces by injecting said slurry cross-currently into a turbulent Couette flow created in a high-frequency, rotor-stator device under conditions to microcavitate said slurry to shatter the fibrous structure of the biomass in the slurry creating a sheared slurry, said device comprising a chamber containing a fixed stator equipped with a nozzle tool containing concentric rings having bore holes meshing with opposing coaxial toothed rings coupled to a rotor coupled to a rotatable shaft; and

d) removing said liquid ammonia from said slurry to form a particulate substrate.

20. The method of claim 19, wherein the removal of liquid ammonia is accomplished by filter pressing, gasification, water absorption, heat drying, pressure reduction, or any combination thereof.

21. The method of claim 19, further comprising the following steps:

e) mixing said particulate substrate from step (d) with water and an enzyme and a surfactant to form a mixture;

f) subjecting said mixture to said high-shear forces created by said device to form a sheared mixture;

g) separating said sheared mixture to produce a filtrate and a retentate;

h) adding the retentate to a newly formed slurry from step (e); and

i) simultaneously adding an enzyme and a surfactant to said slurry and subjecting said slurry to said high-shear forces created by said device.

22. The method of claim 21, wherein the enzyme comprises cellulase, cellobiase, or a combination of cellulase and cellobiase.

23. The method of claim 21, wherein the surfactant is an oleate ester of sorbitol.

25. A method of treating a fibrous lignocellulosic biomass to make it more susceptible to hydrolysis, comprising the following steps.

a) providing a ground fibrous lignocellulosic biomass;

b) mixing said ground biomass with an alkali solution containing from 1% to 10% alkali by weight to produce a slurry;

c) holding said slurry in residence for a period of time sufficient to swell said biomass; and

d) subjecting said slurry to high-shear forces by injecting said slurry cross-currently into a turbulent Couette flow created in a high-frequency, rotor-stator device under conditions to microcavitate the slurry to shatter the fibrous structure of the biomass in the slurry creating a sheared slurry, said device comprising a chamber containing a fixed stator equipped with a nozzle tool containing concentric rings having bore holes meshing with opposing coaxial toothed rings coupled to a rotor that is coupled to a rotatable shaft.

26. The method of claim 25, wherein the alkali comprises calcium hydroxide or sodium hydroxide.

27. The method of claim 25, wherein said slurry is held in residence for a period of time from 30 minutes to 3 hours at a temperature ranging from about 75°

C. to about 90°

C.

28. A method of treating a fibrous lignocellulosic biomass to make it more susceptible to hydrolysis, comprising the following steps:

a) providing a ground fibrous lignocellulosic biomass;

b) mixing said ground biomass with from about 1% to 4% concentrated acid by weight to form a slurry;

c) maintaining the pH of said slurry in a range from a pH of about 1.8 to a pH of about 5.2;

d) holding said slurry in residence for a period of time sufficient to swell said biomass;

e) subjecting said slurry to high-shear forces by injecting said slurry cross-currently into a turbulent Couette flow created in a high-frequency, rotor-stator device under conditions to microcavitate the slurry to shatter the fibrous structure of the biomass in the slurry creating a sheared slurry, said device comprising a chamber containing a fixed stator equipped with a nozzle tool containing concentric rings having bore holes meshing with opposing coaxial toothed rings coupled to a rotor that is coupled to a rotatable shaft; and

f) centrifuging said sheared slurry to separate said acid from said biomass.

29. The method of claim 28, wherein said fibrous lignocellulosic biomass contains 18% or more lignin, said concentrated acid is about 4% by weight, said slurry is maintained at a pH ranging from about 1.8 to about 4.2, and said slurry is held in residence for a period of time ranging from about 30 minutes to about 3 hours at a temperature ranging from about 75°

C. to about 120°

C.

30. The method of claim 28, wherein said fibrous lignocellulosic biomass is a hay, said concentrated acid is about 2% by weight, said slurry is maintained at a pH ranging from about 2.8 to about 5.2, and said slurry is held in residence for a period of time ranging from about 30 minutes to about 3 hours at a temperature ranging from about 75°

C. to about 90°

C.