Recovery of inorganic salt during processing of lignocellulosic feedstocks

• US 8,247,203 B2
• Filed: 08/12/2009
• Issued: 08/21/2012
• Est. Priority Date: 04/13/2004
• Status: Active Grant

• Current Assignee: Iogen Energy Corporation (Iogen Corporation)
• Original Assignee: Iogen Energy Corporation (Iogen Corporation)
• Inventors: Foody, Brian, Tolan, Jeffrey S., Rahme, Ziyad, Anand, Vijay
• Primary Examiner(s): Weber, John P
• Assistant Examiner(s): UNDERDAHL, THANE E
• Application Number:
  US12/539,645
• Publication Number:
  US 20100003733A1
• Time in Patent Office: 1,105 Days
• Field of Search: 435/163, 435/164, 127/37, 127/39
• US Class Current: 435/163
• CPC Class Codes: B01B 1/005 Evaporation for physical or chemical purposes; Evaporation apparatus therefor, e.g. evaporation of liquids for gas phase reactions
• CPC Class Codes: B01D 15/1821 Simulated moving beds
• CPC Class Codes: B01D 15/365 Ion-exclusion
• CPC Class Codes: B01D 61/147 Microfiltration
• CPC Class Codes: B01D 61/44 Ion-selective electrodialysis
• CPC Class Codes: C01C 1/28 Methods of preparing ammonium salts in general
• CPC Class Codes: C01D 3/04 Chlorides
• CPC Class Codes: C01D 5/04 Preparation of sulfates with the aid of sulfurous acid or sulfites, e.g. Hargreaves process pyrosulfites or metabisulfites C01D5/145
• CPC Class Codes: C01D 5/16 Purification C01D5/145 takes precedence
• CPC Class Codes: C05B 7/00 Fertilisers based essentially on alkali or ammonium orthophosphates C05B11/00 takes precedence
• CPC Class Codes: C05C 3/00 Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
• CPC Class Codes: C05D 1/00 Fertilisers containing potassium C05D7/00 takes precedence
• CPC Class Codes: C05D 1/02 Manufacture from potassium chloride or sulfate or double or mixed salts thereof
• CPC Class Codes: C05D 5/00 Fertilisers containing magnesium C05D7/00 takes precedence
• CPC Class Codes: C05F 11/00 Other organic fertilisers
• CPC Class Codes: C12P 19/02 Monosaccharides 2-ketogulonic acid C12P7/60
• CPC Class Codes: C12P 2201/00 Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
• CPC Class Codes: C12P 3/00 Preparation of elements or inorganic compounds except carbon dioxide recovery of carbon dioxides as by-products C12F3/02
• CPC Class Codes: C12P 7/06 Ethanol, i.e. non-beverage
• CPC Class Codes: C12P 7/10 substrate containing cellulosic material
• CPC Class Codes: Y02E 50/10 : Biofuels, e.g. bio-diesel

Abstract

A method for recovering inorganic salt during processing of a lignocellulosic feedstock is provided. The method comprises pretreating the lignocellulosic feedstock by adding an acid to the feedstock to produce a pretreated lignocellulosic feedstock. A soluble base is then added to the pretreated lignocellulosic feedstock to adjust the pH and produce a neutralized feedstock. The neutralized feedstock is then enzymatically hydrolyzed to produce an enzyme hydrolyzed feedstock and a sugar stream. Inorganic salt is recovered from either a stream obtained from the lignocellulosic feedstock prior to the step of pretreating, a stream obtained from the pretreated lignocellulosic feedstock, a stream obtained from the neutralized feedstock, a stream obtained from the sugar stream, or a combination of these streams. The inorganic salt may be concentrated, clarified, recovered and purified by crystallization, electrodialysis drying, or agglomeration and granulation, and then used as desired, for example as a fertilizer.

Claims

1. A method for recovering inorganic salt during processing of a lignocellulosic feedstock comprising:

(a) pretreating the lignocellulosic feedstock by adding one or more than one acid to the lignocellulosic feedstock to produce a pretreated lignocellulosic feedstock, wherein at least a portion of hemicellulose in the feedstock is hydrolyzed to produce one or more than one sugar monomer selected from the group consisting of xylose, arabinose, mannose, galactose and a combination thereof;

(b) removing a sugar-acid mixture from the pretreated lignocellulosic feedstock;

(c) adding base to the removed sugar-acid mixture and then recovering inorganic salt therefrom;

(d) adding one or more than one soluble base to the pretreated lignocellulosic feedstock to adjust the pretreated lignocellulosic feedstock to a pH of about 4.0 to about 6.0 to produce a neutralized feedstock;

(e) enzymatically hydrolyzing the neutralized feedstock to produce a sugar stream and an enzyme hydrolyzed feedstock; and

(f) fermenting the sugar stream to produce a fermentation broth comprising alcohol.

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

(g) distilling the fermentation broth to produce concentrated alcohol and still bottoms.

3. The method of claim 2, further comprising a step of recovering the inorganic salt from the still bottoms followed by purifying the inorganic salt.

4. The method of claim 3, wherein, prior to the step of recovering the inorganic salt from the still bottoms, the concentration of the still bottoms is increased by evaporation, membrane filtration, or a combination thereof, to produce concentrated still bottoms, followed by a step of ion exclusion chromatography using a simulated moving bed process.

5. The method of claim 4, wherein the concentrated still bottoms are clarified by microfiltration, plate and frame filtration or centrifugation, prior to the step of ion exclusion chromatography.

6. The method of claim 5, wherein the step of purifying the inorganic salt comprises crystallization of the inorganic salt, electrodialysis, drying, or agglomeration and granulation.

7. The method of claim 1, wherein the lignocellulosic feedstock is selected from the group consisting of corn stover, wheat straw, barley straw, canola straw, rice straw, oat straw, soybean stover, grass, switch grass, miscanthus, cord grass, reed canary grass, aspen wood, sawdust, bagasse and beet pulp.

8. The method of claim 1, wherein the lignocellulosic feedstock contains from about 0.2% to about 4% (w/w) potassium.

9. The method of claim 1, wherein said inorganic salt is recovered by ion exclusion.

10. The method of claim 9, wherein the recovered inorganic salt is electrodialyzed, dried or agglomerated and granulated.

11. The method of claim 1, wherein the recovered inorganic salt comprises ammonium sulfate salts, ammonium phosphate salts, potassium sulfate salts, ammonium sulfite salts, potassium sulfite salts, sodium sulfate salts, sodium sulfite salts, magnesium sulfate, ammonium chloride, potassium chloride, magnesium chloride or a mixture thereof.

12. The method of claim 11, wherein the salt comprises said ammonium sulfate salts, potassium sulfate salts, or said mixture thereof.

13. The method of claim 11, wherein the ammonium sulfite salts, sodium sulfite salts, potassium sulfite salts, or said mixture thereof are converted to sulfate salts by oxidation before or after the step of recovering.

14. The method of claim 9, wherein the inorganic salt is concentrated by evaporation, membrane filtration, or a combination thereof prior to recovery to produce a concentrated solution comprising the inorganic salt.

15. The method of claim 14, wherein the concentrated solution is clarified by microfiltration, plate and frame filtration, or centrifugation prior to recovery.

16. The method of claim 1, wherein the step of pretreatment comprises a method selected from the group consisting of batch dilute acid hydrolysis, continuous dilute acid hydrolysis, steam explosion and extrusion.

17. The method of claim 1, wherein, in the step of pretreatment, the acid is selected from the group consisting of sulfuric acid, sulfurous acid, sulfur dioxide, phosphoric acid, and a combination thereof.

18. The method of claim 17, wherein the acid is sulfuric acid.

19. The method of claim 1, wherein, in step d., the soluble base is selected from the group consisting of ammonia, ammonium hydroxide, potassium hydroxide, and sodium hydroxide.

20. The method of claim 1, wherein the step of pretreating is performed at a temperature from about 160°

C. to about 280°

C., at a pH from about pH 0.4 to about 2.0 and/or for a time period of from about 0.1 to about 30 minutes.

21. The method of claim 1, wherein, prior to the step of pretreatment, the lignocellulosic feedstock is pressed, leached, or a combination thereof to produce a leachate and wherein the leachate is combined with the sugar-acid mixture to produce a combined salt stream.

22. The method of claim 21, wherein the salt present in the combined salt stream is concentrated by evaporation, membrane filtration, or a combination thereof, to produce a concentrated salt solution.

23. The method of claim 22, wherein the concentrated salt solution is clarified to produce a clarified salt solution.

24. The method of claim 23, wherein the inorganic salt is recovered from the clarified salt solution by ion exclusion chromatography.

25. The method of claim 1, wherein, after the step of enzymatically hydrolyzing, the sugar stream is separated from the enzyme hydrolyzed feedstock to form a solid residue and a sugar hydrolyzate stream.

26. The method of claim 24, wherein the inorganic salt is concentrated by evaporation, membrane filtration, or a combination thereof.

27. The method of claim 1, wherein, in the step of enzymatically hydrolyzing, one or more than one cellulase enzyme is added to the neutralized feedstock so that at least a portion of cellulose in the neutralized feedstock is hydrolyzed to produce glucose.

28. The method of claim 1, wherein the inorganic salt is soluble.

29. The method of claim 1, further comprising fermenting sugar originating from said sugar-acid mixture, said fermenting being conducted after the steps of adding base to the sugar-acid mixture and recovering inorganic salt therefrom.