Liquefaction of biomass at low pH

• US 9,783,565 B2
• Filed: 11/08/2012
• Issued: 10/10/2017
• Est. Priority Date: 11/08/2011
• Status: Active Grant

• Current Assignee: Renmatix, Inc.
• Original Assignee: Renmatix, Inc.
• Inventors: Carlius, Anders, Gram, Andreas, Granath, Corinne, Jhannesson, Haukur, Karlsson, Gran
• Primary Examiner(s): Call, Douglas B
• Assistant Examiner(s): CALL, DOUGLAS BRYANT
• Application Number:
  US14/356,388
• Publication Number:
  US 20140323716A1
• Time in Patent Office: 1,797 Days
• CPC Class Codes: B01D 11/0203 with a supercritical fluid
• CPC Class Codes: C07H 1/00 Processes for the preparation of sugar derivatives
• CPC Class Codes: C07H 3/02 Monosaccharides
• CPC Class Codes: C07H 3/10 Anhydrosugars, e.g. epoxides
• CPC Class Codes: C08H 6/00 Macromolecular compounds derived from lignin, e.g. tannins, humic acids
• 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 3/003 with organic compounds D21C3/20 and D21C3/222 take precedence
• CPC Class Codes: D21C 3/04 with acids, acid salts or acid anhydrides D21C3/003 and D21C3/222 take precedence
• CPC Class Codes: D21C 5/02 Working-up waste paper mechanical part D21B1/08, D21B1/32
• CPC Class Codes: D21C 9/007 by mechanical or physical means
• CPC Class Codes: Y02P 20/54 using solvents, e.g. supercritical solvents or ionic liquids
• CPC Class Codes: Y02W 30/64 Paper recycling

Abstract

The present invention relates to regulation of the p H of a liquefaction process. Presented is a method for treatment of a biomass feedstock wherein the biomass feedstock is subjected to liquefaction, at a p H of at most 4, by treatment with hot compressed liquid water (HCW) at subcritical and/or supercritical conditions to improve the conversion efficiency. The present invention is also directed to quenching of a liquefaction process according to above, preventing, minimizing or eliminating clogging and/or fouling of sticky biomass components in process equipment during processing as according to above, and to the use of additives in a biomass liquefaction process.

Claims

1. A method for treatment of a biomass feedstock comprising

subjecting the biomass feedstock to liquefaction, by treatment with hot compressed liquid water (HCW) at a subcritical condition;

wherein the liquefaction is carried out

at a temperature of from 330°

C. to below 374°

C.,

at a pH below 3.0, and

for a reaction time below 1 minute.

2. A method according to claim 1, also comprising subjecting the biomass feedstock to a subsequent quenching step.

3. A method according to claim 2, wherein the quenching step is made to avoid continued detrimental decomposition, and wherein the quenching is performed by injection of water into a monomer and/or oligomer sugar mixture solution produced after the treatment with hot compressed liquid water (HCW) at subcritical conditions, for a rapid cooling of the solution so that liquid lignin components or liquid lignin derivative components are solidified.

4. A method according to claim 3, wherein the liquid lignin components or liquid lignin derivative components are solidified into particles.

5. A method according to claim 3, wherein the produced solid lignin components or lignin derivative components are separated.

6. A method according to claim 2, wherein the quenching is performed by injection of water into the monomer and/or oligomer sugar mixture solution to a post-quenching temperature below 165°

C.

7. A method according to claim 6, wherein the quenching is performed so that the post-quenching temperature is reached within a time of maximum 10 seconds.

8. A method according to claim 7, wherein the post-quenching temperature is reached within a time of maximum 2 seconds.

9. A method according to claim 2, wherein the quenching is performed by injection of water into the monomer and/or oligomer sugar mixture solution to a post-quenching temperature below 150°

C.

10. The method according to claim 1, wherein inorganic and/or organic acids are added to the biomass feedstock before and/or during the liquefaction.

11. The method according to claim 10, wherein the inorganic acids are chosen from sulfuric acid, sulfonic acid, phosphoric acid, phosphonic acid, nitric acid, nitrous acid, hydrochloric acid, hydrofluoric acid, hydrobromic acid, and hydroiodic acid, or any combination.

12. The method according to claim 10, wherein the organic acids are chosen from aliphatic carboxylic acids, aromatic carboxylic acids, dicarboxylic acids, aliphatic fatty acids, aromatic fatty acids, and amino acids, or any combination.

13. The method according to claim 1, wherein the liquefaction is performed sequentially in at least two separate reactors, and wherein separation of a liquid phase is performed after each reactor.

14. A method according to claim 13, also comprising a step wherein an additive selected from a dispersing agent and/or a caustic solution is added to the treated biomass feedstock before a separation of a liquid phase from a solid phase is performed.

15. The method according to claim 14, wherein the caustic solution is chosen from sodium hydroxide or potassium hydroxide, or a combination.

16. The method according to claim 14, wherein the dispersing agent is chosen from lignosulphonates, polyacrylates, sulphonates, carboxylates, salts of lecithin, and sodium allyl sulphonate/maleic acid copolymer (SASMAC).

17. The method according to claim 16, wherein the lignosulphonates are chosen from ammonium lignosulphonate, sodium lignosulphonate, calcium lignosulphonate, magnesium lignosulphonate, and ferrochrome lignosulphonate, or any combination thereof.

18. The method according to claim 16, wherein the polyacrylates are chosen from sodium, potassium, lithium and ammonium polyacrylates, or any combination thereof.

19. The method according to claim 16, wherein the polyacrylates are chosen from polymers formed from the monomers acrylic acid, methacrylate, acrylonitrile, methyl acrylate, ethyl acrylate, 2-chloroethyl vinyl ether, 2-ethylhexyl acrylate, hydroxyethyl methacrylate, butyl acrylate, butyl methacrylate, or trimethylolpropane triacrylate (TMPTA), or any combination thereof.

20. The method according to claim 1, wherein the liquefaction is performed in a continuous flow system.

21. The method according to claim 1, wherein the method is performed free from any other added solvents besides HCW.

22. The method according to claim 1, wherein the pH value is increased during and/or after the liquefaction to slow down or quench the liquefaction reaction by the use of a base.

23. The method according to claim 1, wherein the reaction time of the liquefaction is set to between 1 and 45 seconds.

24. A method according to claim 1, wherein the method also comprises removal of any material not solubilized.

25. A method according to claim 1, also comprising a step for preventing, minimizing or eliminating clogging and/or fouling of sticky biomass components in process equipment, wherein an alkaline liquid is washed through the process equipment, either as a sole solution between regular process operations of a biomass process flow in a liquid solution, or as added directly into the liquid solution for dissolving biomass components which are or otherwise may become sticky.

26. A method according to claim 25, wherein the alkaline liquid is processed separately from the biomass process flow solution after the washing or the addition thereof.

27. A method according to claims 25, wherein the alkaline liquid is recovered after the washing or addition thereof, for further washing or addition.

28. A method according to claim 25, wherein the alkaline liquid is a liquid based on caustic liquor or ammonia.

29. A method according to claim 25, wherein an oxidizing agent also is added in the alkaline liquid.