Methods and apparatus for hydrolyzing cellulosic material

• US 8,496,754 B2
• Filed: 10/21/2008
• Issued: 07/30/2013
• Est. Priority Date: 11/01/2007
• Status: Active Grant

• Current Assignee: Eau-Viron Incorporated
• Original Assignee: Eau-Viron Incorporated
• Inventors: Titmas, James
• Primary Examiner(s): Brunsman, David M
• Application Number:
  US12/452,605
• Publication Number:
  US 20100121047A1
• Time in Patent Office: 1,743 Days
• Field of Search: 127/1, 127/37
• US Class Current: 127/37
• CPC Class Codes: C08H 8/00 Macromolecular compounds derived from lignocellulosic materials pretreatment thereof B27N
• CPC Class Codes: C12P 2201/00 Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
• CPC Class Codes: C13K 1/02 obtained by saccharification of cellulosic materials manufacture of fodder A23K10/32
• CPC Class Codes: D21C 1/06 with alkaline reacting compounds
• CPC Class Codes: D21C 11/0007 Recovery of by-products, i.e. compounds other than those necessary for pulping, for multiple uses or not otherwise provided for volatile compounds obtained by decomposition of spent liquors in order to regenerate them D21C11/125; compounds obtained by fractionating the liquors in order to regenerate them D21C11/0042
• CPC Class Codes: D21C 3/04 with acids, acid salts or acid anhydrides D21C3/003 and D21C3/222 take precedence
• CPC Class Codes: Y02E 50/10 Biofuels, e.g. bio-diesel
• CPC Class Codes: Y02P 20/582 Recycling of unreacted starting or intermediate materials

Abstract

A method of hydrolyzing woody cellulosic material containing lignin and air pockets involves impregnating the woody cellulosic material a first alkali having a pH of from 10 to 14 such that the first alkali is in contact with the lignin within the woody cellulosic material. Thereafter, the woody cellulosic material is advanced through a gravity pressure vessel for the acid hydrolysis conversion of cellulosic material to sugars. In accordance with other methods, ultrasound may be introduced during impregnation or at the gravity pressure vessel or both.

Claims

1. A method of hydrolyzing woody cellulosic material containing lignin and air pockets, the method comprising the steps of:

impregnating the woody cellulosic material with a first alkali having a pH of from 10 to 14 such that the first alkali is in contact with the lignin within the lignin-containing woody cellulosic material and, thereafter, advancing the woody cellulosic material through a gravity pressure vessel whereby the woody cellulosic material is acid hydrolyzed to sugars.

2. The method of claim 1, wherein said step of impregnating includes:

creating a process stream of the woody cellulosic material and the first alkali as carrier fluid;

applying a vacuum to the process stream thereby removing air from the air pockets of the woody cellulosic material, and thereafter

increasing the pressure to which the process stream is subjected such that a portion of the first alkali of the process stream enters air pockets within the woody cellulosic material while the remainder of the first alkali remains as first alkali carrier fluid.

3. The method of claim 2, wherein, after said step of impregnating the woody cellulosic material with a first alkali, the method further comprises the step of substantially removing the first alkali carrier fluid and replacing it with a secondary alkali carrier fluid having a pH of from 7 to 8.5.

4. The method of claim 2, wherein said step of impregnating further comprises:

subjecting the process stream of the woody cellulosic material and the first alkali to ultrasound.

5. The method of claim 3, wherein said gravity pressure vessel includes:

a tubular casing having a lower closed end, and

a counterflow tubular casing positioned within the tubular casing and having an lower open end whereby an outer reaction annulus is formed between the tubular casing and the counterflow tubular casing and a starved oxidation reaction zone is formed proximate the lower closed end of the tubular casing; and

the method further comprises introducing ultrasound at the starved oxidation reaction zone.

6. The method of claim 5, further comprising adding oxygen proximate the starved oxidation reaction zone.

7. A method of hydrolyzing woody cellulosic material containing lignin and air pockets, the method comprising the steps of:

introducing woody cellulosic material into a gravity pressure vessel and impregnating the woody cellulosic material with a first alkali having a pH of from 10 to 14, such that the first alkali is in contact with the lignin within the lignin-containing woody cellulosic material, wherein the gravity pressure vessel includes;

a tubular casing having a lower closed end,

a counterflow tubular casing positioned within the tubular casing and having an lower open end whereby an outer reaction annulus is formed between the tubular casing and the counterflow tubular casing, and

a starved oxidation reaction zone proximate the lower closed end of the tubular casing; and

introducing ultrasound at the starved oxidation reaction zone, whereby the woody cellulosic material is acid hydrolyzed to sugars.

8. The method of claim 7, further comprising adding oxygen proximate the starved oxidation reaction zone.

9. The method of claim 7, wherein said step of impregnating the woody cellulosic material comprises:

creating a process stream of the woody cellulosic material and the first alkali as carrier fluid;

applying a vacuum to the process stream thereby removing air from the air pockets of the woody cellulosic material, and thereafter

increasing the pressure to which the process stream is subjected such that a portion of the first alkali of the process stream enters air pockets within the woody cellulosic material while the remainder of the first alkali remains as first alkali carrier fluid.

10. The method of claim 9, wherein, after said step of impregnating the woody cellulosic material with a first alkali, the step of introducing the cellulosic material further comprises the step of substantially removing the first alkali carrier fluid and replacing it with a secondary alkali carrier fluid having a pH of from 7 to 8.5.

11. The method of claim 9, wherein said step of impregnating further comprises:

subjecting the process stream of the woody cellulosic material and the first alkali to ultrasound.

12. A method of hydrolyzing woody cellulosic material containing lignin and air pockets, the method comprising the steps of:

impregnating the woody cellulosic material with a first alkali having a pH of from 10 to 14 such that the first alkali is in contact with the lignin within the woody cellulosic material, and thereafter

introducing the woody cellulosic material into a gravity pressure vessel, wherein the gravity pressure vessel includes;

a tubular casing having a lower closed end,

a counterflow tubular casing positioned within the tubular casing and having an lower open end whereby an outer reaction annulus is formed between the tubular casing and the counterflow tubular casing, and

a starved oxidation reaction zone proximate the lower closed end of the tubular casing; and

introducing ultrasound at the starved oxidation reaction zone, whereby, upon advancing the cellulosic material through the gravity pressure vessel, the cellulosic material is acid hydrolyzed to sugars.