Dilute acid/metal salt hydrolysis of lignocellulosics

• US 6,423,145 B1
• Filed: 08/09/2000
• Issued: 07/23/2002
• Est. Priority Date: 08/09/2000
• Status: Expired due to Term

• Current Assignee: Alliance For Sustainable Energy LLC
• Original Assignee: Midwest Research Institute
• Inventors: Nguyen, Quang A., Tucker, Melvin P.
• Primary Examiner(s): BRUNSMAN, DAVID M
• Application Number:
  US09/634,978
• Time in Patent Office: 713 Days
• Field of Search: 127/37, 106/164.5, 106/164.53
• US Class Current: 127/37
• CPC Class Codes: C12P 2201/00 Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
• CPC Class Codes: C12P 7/08 produced as by-product or from waste or cellulosic material substrate
• 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: Y02E 50/30 Fuel from waste, e.g. synthetic alcohol or diesel

Abstract

A modified dilute acid method of hydrolyzing the cellulose and hemicellulose in lignocellulosic material under conditions to obtain higher overall fermentable sugar yields than is obtainable using dilute acid alone, comprising:

impregnating a lignocellulosic feedstock with a mixture of an amount of aqueous solution of a dilute acid catalyst and a metal salt catalyst sufficient to provide higher overall fermentable sugar yields than is obtainable when hydrolyzing with dilute acid alone;

loading the impregnated lignocellulosic feedstock into a reactor and heating for a sufficient period of time to hydrolyze substantially all of the hemicellulose and greater than 45% of the cellulose to water soluble sugars; and recovering the water soluble sugars.

Claims

1. A modified dilute acid method of hydrolyzing the cellulose and hemicellulose in lignocellulosic material under conditions to obtain higher overall fermentable sugar yields than is obtainable using dilute acid alone, comprising:

impregnating a lignocellulosic feedstock with a mixture of an amount of aqueous solution of a dilute acid catalyst and a metallic salt catalyst sufficient to hydrolyze the hemicellulose and cellulose fractions to provide higher overall fermentable sugar yields than is obtainable when hydrolyzing with dilute acid alone;

loading said impregnated lignocellulosic feedstock into a reactor and heating for a sufficient period of time to hydrolyze substantially all of the hemicellulose and greater than 45% of the cellulose to water soluble sugars; and

recovering said water soluble sugars.

2. The process of claim 1 wherein said reactor is a batch steam explosion reactor.

3. The process of claim 1 wherein said reactor is a continuous reactor.

4. The process of claim 1 wherein said lignocellulosic feedstock is selected from the group consisting of softwood, hardwood, agricultural residues, corn refining residues and grasses.

5. The process of claim 4 wherein said softwood is Douglas Fir, White fir and Ponderosa pine.

6. The process of claim 1 wherein said dilute acid catalyst is selected from the group consisting of H₂SO₄, HCl, HNO₃, SO₂ or any strong acid which effect pH values below about 3, and said metal salt catalyst is selected from the group consisting of ferrous sulfate, ferric sulfate, ferric chloride, aluminum sulfate, aluminum chloride, and magnesium sulfate.

7. The process of claim 6 wherein said amount of aqueous mixture of catalysts sufficient to provide higher overall fermentable sugar yields than is obtainable when hydrolyzing with dilute acid alone is between about 0.2-4.0 weight percent range and between about 0.2 to about 25.0 mmole/L for said metal salt catalyst.

8. The process of claim 7 wherein said dilute acid catalyst is H₂SO₄ and said metal salt is ferrous sulfate.

9. The process of claim 8 wherein said heating of the lignocellulosic material for a sufficient period of time is at a temperature of between about 120°

C. to about 240°

C. for about 1 to about 30 minutes.

10. The process of claim 9 wherein, subsequent to said heating step and prior to recovering water soluble sugars, the mixture is cooled to less than about 105°

C. to minimize degradation of sugars.

11. The process of claim 1 wherein said lignocellulosic feedstock is milled prior to impregnation.

12. The process of claim 11 wherein said hydrolysis is conducted in a single stage.

13. The process of claim 11 wherein the hydrolysis is conducted in two stages with an inter-stage washing step to recover soluble sugars from first-stage hydrolysate.

14. A combination of a dilute acid catalyst and a metal salt catalyst at a sufficient temperature to hydrolyze greater than 45% cellulose and substantially all of the hemicellulose in a lignocellulosic material in a single stage to obtain higher overall fermentable sugar yields than is obtainable using dilute acid alone.

15. The combination of claim 14 wherein said dilute acid catalyst is present in a concentration range of from about 0.2 to about 4% by weight and said metal salt catalyst is present in a concentration range of from about 0.2 to about 25 mmole/L.