Process for controlled liquefaction of a biomass feedstock by treatment in hot compressed water

• US 9,738,943 B2
• Filed: 10/28/2011
• Issued: 08/22/2017
• Est. Priority Date: 11/01/2010
• Status: Active Grant

• Current Assignee: Renmatix, Inc.
• Original Assignee: Renmatix, Inc.
• Inventors: Ekman, Rune, Gram, Andreas, Johannesson, Haukur
• Primary Examiner(s): Mayes, Melvin C
• Assistant Examiner(s): COHEN, STEFANIE J
• Application Number:
  US13/882,868
• Publication Number:
  US 20160053337A1
• Time in Patent Office: 2,125 Days
• CPC Class Codes: B01J 2219/00029 Batch processes
• CPC Class Codes: B01J 2219/00036 Intermittent processes
• CPC Class Codes: B01J 2219/00177 controlling the pH
• CPC Class Codes: B01J 3/008 Processes carried out under supercritical conditions
• CPC Class Codes: C08B 1/003 Preparation of cellulose solutions, i.e. dopes, with different possible solvents, e.g. ionic liquids solutions used in the manufacture of monocomponent artificial filaments or cellulose or derivatives thereof D01F2/02
• 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: 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: C13K 11/00 Fructose separation from invert sugar C13K3/00
• CPC Class Codes: C13K 13/00 Sugars not otherwise provided for in this class
• CPC Class Codes: C13K 13/007 Separation of sugars provided for in subclass C13K C13K3/00 takes precedence
• CPC Class Codes: D21B 1/021 by chemical means
• CPC Class Codes: Y02E 50/10 Biofuels, e.g. bio-diesel
• CPC Class Codes: Y02P 20/54 using solvents, e.g. supercritical solvents or ionic liquids

Abstract

The present invention describes a process for a controlled conversion of a biomass feedstock, wherein the process comprises the steps of:

• • loading the biomass feedstock to at least one reactor;
  • liquefaction of the biomass feedstock into a monomer and/or oligomer sugar mixture in said reactor by treatment in hot compressed liquid water (HCW) at sub- and/or super-critical condition; and
  • removal of the monomer and/or oligomer sugar mixture, being the product molecules, to avoid continued detrimental decomposition.

Claims

1. Process for a controlled conversion of a biomass feedstock, wherein the process comprises:

loading the biomass feedstock to at least one reactor;

liquefaction of the biomass feedstock into a monomer and/or oligomer sugar mixture in said reactor by treatment in hot compressed liquid water at sub- and/or super-critical condition; and

removal of the monomer and/or oligomer sugar mixture to avoid continued detrimental decomposition;

wherein the liquefaction is performed at a temperature of at least 280°

C. during a reaction time t of from 1.5 to 30 s; and

wherein the liquefaction is performed in one cycle or by repeated cycles by injection of hot compressed water; and

further

wherein each injection of hot compressed water applies a temperature pulse at a sub- or super-critical condition in the reactor to allow for liquefaction of the biomass feedstock, said pulse involving applying a pulse start temperature during a temperature increase time and allowing for liquefaction reaction to occur during the reaction time t.

2. Process according to claim 1, wherein the liquefaction is performed at a temperature of below 374°

C.

3. Process according to claim 1, wherein the liquefaction is performed at a temperature in the range of 280-350°

C.

4. Process according to claim 1, wherein the liquefaction is performed at a temperature in the range of 300-350°

C.

5. Process according to claim 1, wherein

loading of the biomass feedstock is performed by preloading biomass into a batch reactor;

liquefaction is performed in one cycle or repeated cycles by injection of hot compressed water to the batch reactor; and

solubilized material is discharged from the batch reactor after the reaction time t for each cycle.

6. Process according to claim 1, wherein

loading of the biomass feedstock is performed by cyclic loading of biomass into a single batch reactor or into a series of batch reactors so that said reactor(s) is refilled after complete biomass liquefaction;

liquefaction is performed in one cycle or by repeated cycles by injection of hot compressed water to the batch reactor or series of batch reactors; and

solubilized material is discharged from the batch reactor after the reaction time t for each cycle.

7. Process according to claim 1, wherein

loading of the biomass feedstock is performed by cyclic loading of biomass into at least one flow reactor;

liquefaction is performed by injection of hot compressed water to said flow reactor by one cycle; and

solubilized material is flowed downstreams from the flow reactor to a non-reactive zone.

8. Process according to claim 1, wherein separation of a lignin component is performed by removal of non-solubilized material from at least one reactor.

9. Process according to claim 1, wherein

loading of the biomass feedstock is performed by continuous loading of biomass into at least one flow reactor;

liquefaction is performed by continuously injecting hot compressed water to said flow reactor; and

solubilized material is flowed downstreams from the flow reactor to a non-reactive zone.

10. Process according to claim 7, wherein several flow reactors are used and wherein at least one flow reactor is a loading reactor and at least one flow reactor is a reaction reactor.

11. Process according to claim 1, wherein

the biomass feedstock is a slurry which is continuously loaded to a flow reactor;

said slurry is rapidly warmed to sub- or super-critical condition; and

solubilized material is flowed downstreams from the flow reactor to a non-reactive zone.

12. Process according to claim 1, wherein the process further comprises

removal of non-solubilized material;

wherein lignin is separated at the step of removal of non-solubilized material, and

wherein the removed non-solubilized material is reprocessed.

13. Process according to claim 1, wherein the process is performed free from any chemicals besides hot compressed water and the biomass feedstock.

14. Process according to claim 1, wherein at least one pH lowering additive is added to the process.

15. Process according to claim 1, wherein the pulse start temperature is at least 280°

C.

16. Process according to claim 1, wherein the pulse start temperature is in the range of 300°

C.-350°

C. and the reaction time t is 1.5 to 15 s.

17. Process according to claim 1, wherein the process further comprises a subsequent step of hydrolysis, fermentation, or a combination thereof.

18. Process according to claim 1, wherein the biomass feedstock is a lignocellulosic biomass feedstock.

19. Process according to claim 9, wherein several flow reactors are used and wherein at least one flow reactor is a loading reactor and at least one flow reactor is a reaction reactor.

20. Process according to claim 1, wherein the liquefaction is performed at a pressure held at a level high enough so that the hot compressed water is in liquid form.