Process for the production of alcohols

• US 9,217,184 B2
• Filed: 04/20/2010
• Issued: 12/22/2015
• Est. Priority Date: 05/07/2009
• Status: Active Grant

• Current Assignee: Silvanova LLC
• Original Assignee: Weyland AS
• Inventors: Weydahl, Karl Ragnar
• Primary Examiner(s): DRODGE, JOSEPH W
• Application Number:
  US13/318,302
• Publication Number:
  US 20120190840A1
• Time in Patent Office: 2,072 Days
• Field of Search: 443/07, 443/13, 445/89, 446/05, 210/202, 210/209, 210/259, 210/511, 210/634, 210/639, 210/749, 210/773, 210/806, 422/187, 422/256, 536/127, 536/128, 568/902, 530/422, 530/427
• US Class Current: 1/1
• CPC Class Codes: B01D 11/0426 Counter-current multistage extraction towers in a vertical or sloping position
• CPC Class Codes: B01D 11/0488 Flow sheets
• CPC Class Codes: B01D 11/0492 Applications, solvents used
• CPC Class Codes: B01D 2011/002 Counter-current extraction
• CPC Class Codes: C07C 29/09 by hydrolysis
• CPC Class Codes: C07H 1/06 Separation; Purification
• 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

Abstract

The invention provides a process for alcohol production from a cellulosic material wherein a said cellulosic material is subjected to acid hydrolysis to yield an aqueous hydrolysate, said hydrolysate is introduced into a separator at a hydrolysate inlet, an extraction solvent is introduced into said separator at at least two extraction solvent inlets, a residue containing oligosaccharides is removed from said separator at a residue discharge outlet, and acid-containing extraction solvent is removed from said separator at an extraction solvent discharge outlet, wherein removal of said extraction solvent from said separator through said discharge outlet occurs downstream of at least one said extraction solvent inlet and upstream of at least one other said extraction solvent inlet.

Claims

1. A process for alcohol production from a cellulosic material or for the production of an oligosaccharide-containing residue from a cellulosic material comprising the steps of subjecting a said cellulosic material to acid hydrolysis to yield an aqueous hydrolysate, introducing said hydrolysate into a separator at a hydrolysate inlet, said separator having at least two sections;

introducing an extraction solvent into at least two separator sections at at least two extraction solvent inlets, removing a residue containing oligosaccharides from said separator at a residue discharge outlet, and removing acid-containing extraction solvent from said separator at an extraction solvent discharge outlet, wherein removal of said extraction solvent from said separator through said discharge outlet occurs downstream of at least one said extraction solvent inlet and upstream of at least one other said extraction solvent inlet.

2. The process of claim 1, wherein when said extraction solvent is removed at at least 2 outlets located between the extraction solvent inlets, extraction solvent removed at one such outlet is returned to the separator through one of the inlets.

3. The process of claim 2, wherein in oligosaccharide flow direction the solvent inlet and outlet order is second inlet, second outlet, first outlet, first inlet;

and wherein the second outlet is the outlet from which the acid-containing extraction solvent is discharged from the separator.

4. The process of claim 1, further comprising a time delay of at least 10 seconds between the earliest point of contact between the hydrolysate and the extraction solvent and said acid containing extraction solvent reaching the extraction solvent discharge outlet.

5. The process of claim 4, wherein said time delay is at least 60 seconds.

6. The process of claim 1, wherein said extraction solvent comprises a ketone having up to eight carbons per molecule.

7. The process of claim 6, wherein said extraction solvent comprises methyl ethyl ketone.

8. The process of claim 1, wherein said acid hydrolysis is with an inorganic acid, and wherein said extraction solvent comprises an ether and/or a ketone having up to 8 carbons per molecule.

9. A process for alcohol production from a cellulosic material or for the production of an oligosaccharide-containing residue from a cellulosic material, comprising the steps of subjecting a said cellulosic material to acid hydrolysis to yield an aqueous hydrolysate, introducing said hydrolysate into a separator at a hydrolysate inlet, said separator having at least two sections;

introducing an extraction solvent into at least two separator sections at an extraction solvent inlet, removing a residue containing oligosaccharides from said separator at a residue discharge outlet, and removing acid-containing extraction solvent from said separator at an extraction solvent discharge outlet, wherein;

(a) said hydrolysate inlet and said extraction solvent discharge outlet are so positioned that the time of flow from said hydrolysate inlet to said extraction solvent discharge outlet is at least 10 seconds;

or

(b) said hydrolysate inlet and said extraction solvent discharge outlet are positioned above said extraction solvent inlet, said hydrolysate inlet is positioned at or below said extraction solvent discharge outlet, and said separator has an internal cross-sectional area that is higher at said hydrolysate inlet or between said hydrolysate inlet and said extraction solvent discharge outlet than the average between said extraction solvent inlet and said extraction solvent discharge outlet;

or

(c) said hydrolysate inlet is positioned in said separator below at least 10% of the flow path of extraction solvent from said extraction solvent inlet to said extraction solvent discharge outlet.

10. The process of claim 9, wherein said extraction solvent comprises a ketone having up to eight carbons per molecule.

11. The process of claim 10, wherein said extraction solvent comprises methyl ethyl ketone.

12. The process of claim 9, further comprising a time delay of at least 60 seconds between the earliest point of contact between the hydrolysate and the extraction solvent and said acid containing extraction solvent reaching the extraction solvent discharge outlet.

13. Apparatus for oligosaccharide production from a cellulosic material, said apparatus comprising an acid hydrolysis reactor and a separator having an oligosaccharide flow path therethrough, said separator having:

a hydrolysate inlet arranged to receive hydrolysate from said reactor;

at least two sections with at least two of the sections having an extraction solvent inlet for introduction of an extraction solvent;

a residue discharge outlet for removal of a residue containing oligosaccharides; and

an extraction solvent discharge outlet for removal of acid-containing extraction solvent, wherein said extraction solvent discharge outlet is downstream on said flow path of at least one said extraction solvent inlet and upstream on said flow path of at least one other said extraction solvent inlet; and

wherein said hydrolysate inlet and said extraction solvent discharge outlet are positioned above said extraction solvent inlets, said hydrolysate inlet is positioned at or below said extraction solvent discharge outlet, and said separator has an internal cross-sectional area that is higher at said hydrolysate inlet or between said hydrolysate inlet and said extraction solvent discharge outlet than the average between said extraction solvent inlets and said extraction solvent discharge outlet.

14. The apparatus according to claim 13 for alcohol production from a cellulosic material.

15. The apparatus of claim 13, said apparatus comprising at least two outlets located between the extraction solvent inlets, with the solvent removal at one such outlet being returned to the separator through one of the inlets.

16. The apparatus of claim 15, wherein in the oligosaccharide flow direction the solvent inlet and outlet order is second inlet, second outlet, first outlet, first inlet;

and wherein the second outlet is the outlet from which the acid-containing extraction solvent is discharged from the separator.

17. The apparatus of claim 13, wherein said apparatus involves a time delay of at least 10 seconds between the earliest point of contact between the hydrolysate and the extraction solvent and said acid containing extraction solvent reaching the extraction solvent discharge outlet.

18. The apparatus of claim 17, wherein said time delay is at least 60 seconds.

19. The apparatus of claim 13, wherein said extraction solvent comprises a ketone having up to eight carbons per molecule.

20. The apparatus of claim 19, wherein said extraction solvent comprises methyl ethyl ketone.

21. The apparatus of claim 13, wherein said acid hydrolysis reactor is for use with inorganic acid, and said extraction solvent comprises an ether and/or ketone having up to 8 carbons per molecule.

22. Apparatus for oligosaccharide production from a cellulosic material, said apparatus comprising an acid hydrolysis reactor and a separator having an oligosaccharide flow path therethrough, said separator having:

a hydrolysate inlet arranged to receive hydrolysate from said reactor;

at least two sections, with an extraction solvent inlet for introduction of an extraction solvent;

a residue discharge outlet for removal of a residue containing oligosaccharides; and

an extraction solvent discharge outlet for removal of acid-containing extraction solvent, wherein

said hydrolysate inlet and said extraction solvent discharge outlet are positioned above said extraction solvent inlet, said hydrolysate inlet is positioned at or below said extraction solvent discharge outlet, and said separator has an internal cross-sectional area that is higher at said hydrolysate inlet or between said hydrolysate inlet and said extraction solvent discharge outlet than the average between said extraction solvent inlet and said extraction solvent discharge outlet.

23. The apparatus according to claim 22 for alcohol production from a cellulosic material.

24. The apparatus of claim 22, wherein said extraction solvent comprises a ketone having up to eight carbons per molecule.

25. The apparatus of claim 24, wherein said extraction solvent comprises methyl ethyl ketone.

26. The apparatus of claim 22, wherein said apparatus involves a time delay of at least 60 seconds between the earliest point of contact between the hydrolysate and the extraction solvent and said acid containing extraction solvent reaching the extraction solvent discharge outlet.

27. The apparatus of claim 22, wherein said hydrolysate inlet is positioned in said separator below at least 10% of the flow path of extraction solvent from said extraction solvent inlet to said extraction solvent outlet.