Hydrolysis and fractionation of lignocellulosic biomass

• US 6,022,419 A
• Filed: 09/30/1996
• Issued: 02/08/2000
• Est. Priority Date: 09/30/1996
• Status: Expired due to Term

• Current Assignee: Alliance For Sustainable Energy LLC
• Original Assignee: Midwest Research Institute
• Inventors: Wyman, Charles E., Hatzis, Christos, Padukone, Nandan, Torget, Robert W.
• Primary Examiner(s): Bell, Mark L.
• Assistant Examiner(s): Hailey, Patricia L.
• Application Number:
  US08/723,399
• Time in Patent Office: 1,226 Days
• Field of Search: 127/1, 127/37, 435/105, 536/56, 536/124, 536/127
• US Class Current: 127/37
• CPC Class Codes: C07G 99/00 Subject matter not provided for in other groups of this subclass
• 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: D21C 3/04 with acids, acid salts or acid anhydrides D21C3/003 and D21C3/222 take precedence

Abstract

A multi-function process is described for the hydrolysis and fractionation of lignocellulosic biomass to separate hemicellulosic sugars from other biomass components such as extractives and proteins; a portion of the solubilized lignin; cellulose; glucose derived from cellulose; and insoluble lignin from said biomass comprising one or more of the following: optionally, as function 1, introducing a dilute acid of pH 1.0-5.0 into a continual shrinking bed reactor containing a lignocellulosic biomass material at a temperature of about 94 to about 160° C. for a period of about 10 to about 120 minutes at a volumetric flow rate of about 1 to about 5 reactor volumes to effect solubilization of extractives, lignin, and protein by keeping the solid to liquid ratio constant throughout the solubilization process; as function 2, introducing a dilute acid of pH 1.0-5.0, either as virgin acid or an acidic stream from another function, into a continual shrinking bed reactor containing either fresh biomass or the partially fractionated lignocellulosic biomass material from function 1 at a temperature of about 94-220° C. for a period of about 10 to about 60 minutes at a volumetric flow rate of about 1 to about 5 reactor volumes to effect solubilization of hemicellulosic sugars, semisoluble sugars and other compounds, and amorphous glucans by keeping the solid to liquid ratio constant throughout the solubilization process; as function 3, optionally, introducing a dilute acid of pH 1.0-5.0 either as virgin acid or an acidic stream from another function, into a continual shrinking bed reactor containing the partially fractionated lignocellulosic biomass material from function 2 at a temperature of about 180-280° C. for a period of about 10 to about 60 minutes at a volumetric flow rate of 1 to about 5 reactor volumes to effect solubilization of cellulosic sugars by keeping the solid to liquid ratio constant throughout the solubilization process; and as function 4, optionally, introducing a dilute acid of pH 1.0-5.0 either as virgin acid or an acidic stream from another function, into a continual shrinking bed reactor containing the partially fractionated lignocellulosic biomass material from function 3 at a temperature of about 180-280° C. for a period of about 10 to about 60 minutes at a volumetric flow rate of about 1 to about 5 reactor volumes to effect solubilization of cellulosic sugars by keeping the solid to liquid ratio constant throughout the solubilization process.

Claims

1. A multi-function process for hydrolysis and fractionation of lignocellulosic biomass to separate hemicellulosic sugars from other biomass components comprising extractives and proteins;

a portion of a solubilized lignin;

cellulose;

glucose derived from cellulose; and

insoluble lignin from said biomass comprising;

A) introducing a dilute acid liquid of pH 1.0-5.0 into a continual shrinking bed reactor containing either solid fresh biomass or solid partially fractionated lignocellulosic biomass material at a temperature of from about 140 to about 220°

C. for a period of about 10 to about 60 minutes at a volumetric flow rate sufficient to keep the solid and liquid at a constant ratio throughout said process so as to increase the linear velocity, keep a constant volumetric flow rate to effect solubilization of hemicellulosic sugars and amorphous glucans, to improve hemicellulosic sugar yields.

2. The process of claim 1 wherein said flow rate is from about 1 to about 5 reactor volumes.

3. The process of claim 2 wherein said dilute acid is a mineral acid.

4. The process of claim 3, wherein said mineral acid is selected from the group consisting of sulfuric acid, phosphoric acid or nitric acid.

5. The process of claim 4 wherein said dilute acid is carbonic acid.

6. The process of claim 3 wherein said mineral acid is introduced in stages.

7. The process of claim 2 wherein the continual shrinking bed reactor is a conical shaped flow-thru reactor in which the lignocellulosic biomass is conveyed as a solid toward a narrower end of the conical shaped flow-thru reactor.

8. The process of claim 2 wherein the continual shrinking bed reactor is a series of flow-thru reactors of decreasing volumetric capacity in which the solids are moved from a larger capacity reactor to a smaller capacity reactor as a function of the hydrolysis and/or fractionation of the biomass.

9. The process of claim 2 wherein the continual shrinking bed reactor is a cylindrical flow-thru reactor comprising an activated piston or weighted internal movable top to decrease reactor volume as hydrolysis progresses.

10. The process of claim 2 wherein the continual shrinking bed reactor is a screw reactor that conveys lignocellulosic solids co-current to the acid hydrolysis liquor feed.

11. The process of claim 10, wherein said screw reactor conveys lignocellulosic solids counter-current to the acid hydrolysis liquor feed.

12. The process of claim 2 wherein prior to step A), a dilute acid liquid of about pH 1.0-5.0 is introduced into a continual shrinking bed reactor containing a solid lignocellulosic biomass material at a temperature of from about 94 to about 160°

C. for a period of about 10 to about 120 minutes at a volumetric flow rate of from about 1 to about 5 reactor volumes to effect solubilization of extractives, lignin, and protein while keeping the solid to liquid ratio constant throughout the solubilization process.

13. The process of claim 12, subsequent to step A), a liquid dilute acid pH 1.0-5.0 is introduced into a continual shrinking bed reactor containing a solid partially fractionated lignocellulosic biomass material from step A) at a temperature of from about 180-280°

C. for a period of about 10 to about 60 minutes and at a volumetric flow rate of 1 to about 5 reactor volumes to effect solubilization of cellulosic sugars while keeping the solid to liquid ratio constant throughout the solubilization process.

14. The process of claim 13 wherein, as a last step, a liquid dilute acid of pH 1.0-5.0 is introduced into a continual shrinking bed reactor containing a solid partially fractionated lignocellulosic biomass material at a temperature of from about 180-280°

C. for a period of about 10 to about 60 minutes at a volumetric flow rate of about 1 to about 5 reactor volumes to effect solubilization of cellulosic sugars while keeping the solid to liquid ratio constant throughout the solubilization process.