IP Library Granted Patent US 12,644,055
Granted Patent B2
US 12,644,055 · App. 18/434,609 · Granted Jun 2, 2026

Carbon dioxide enhanced hydrothermal liquefaction

Inventors: Alan H. Zacher (Pasco, WA); Lisa A. Middleton-Smith (Pasco, WA); Todd R. Hart (Kennewick, WA); Andrew J. Schmidt (Richland, WA); Michael R. Thorson (Richland, WA); Samuel P. Fox (West Richland, WA); Dylan J. Cronin (Richland, WA)
Assignee: Battelle Memorial Institute
C10G3/40B01J4/007B01J8/085B01J8/087C02F11/18B01J2204/002B01J2208/00168B01J2208/00752C10G2300/1003C10G2300/1014
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Quick Facts
Patent No.
US 12,644,055
App. No.
18/434,609
Granted
Jun 2, 2026
Kind
B2
Abstract

A process where a liquid or supercritical CO2 co-solvent is used in a hydrothermal liquefaction (HTL) process. The process improves yield of the HTL process.

Claims (26)

1 . A method of producing liquid biocrude comprising:

providing an aqueous biomass slurry comprising biomass and water;

adding liquid CO 2 or supercritical CO 2 to the slurry to form a slurry with CO 2 cosolvent;

heating and pressurizing the slurry;

reacting the slurry in a HTL process in the presence of the CO 2 cosolvent under conditions where the CO 2 cosolvent is in the form of a liquid or is supercritical;

forming a product mixture from the step of reacting;

cooling the product mixture to form a cooled product mixture;

subjecting the cooled product mixture to a separation process; and

recovering a liquid product from the separation process.

2 . The method of claim 1 wherein the biomass comprises sewage sludge, food waste, algal biomass, wet agricultural residues, or a combination of these materials.

3 . The method of claim 1 wherein the method comprises a preheating step followed by a passing the preheated solution into a reactor where the step of reacting occurs.

4 . The method of claim 3 wherein the liquid or supercritical CO 2 is added to the slurry after the preheating step and before the reacting step.

5 . The method of claim 4 wherein the pressure in the reactor is in the range of 5 to 25 MPa.

6 . The method of claim 1 wherein separation process comprises a step of removing products in a stream of liquid CO 2 or supercritical CO 2 ; and wherein the stream of liquid CO 2 or supercritical CO 2 comes from the HTL process.

7 . The method of claim 1 wherein the pressure in the reactor is at least 10 MPa, or in the range of 10 to 100 MPa, or 10 to 50 MPa, or 12 to 30 MPa, or 13 to 20 MPa, or 10 to 15 MPa.

8 . The method of claim 1 where the step of reacting is conducted in the range of 300 to 370° C. or 350 to 370° C. or 300 to 330° C.

9 . The method of claim 1 wherein the aqueous biomass slurry comprises at least 5 wt % biomass, or in the range of 5 to 50 wt % biomass, or 10 to 30 wt % biomass, or 15 to 25 wt % biomass.

10 . The method of claim 1 wherein the mass of added liquid CO2 is at least 1.1 times to 4 times the mass of CO 2 that is generated in the method.

11 . The method of claim 1 wherein the separation process comprises a step of CO 2 gas removal wherein at least 1% (or at least 3%, or at least 5%) of carbon in the added CO 2 is present in the liquid product after the step of CO 2 gas removal.

12 . The method of claim 1 wherein the preheating is conducted in a vessel that is separate from a vessel where the slurry is reacted in the HTL process, and wherein the preheating is conducted to a temperature of at least 150° C. or at least 200° C.

13 . The method of claim 1 wherein liquid CO 2 is dispersed in the aqueous slurry.

14 . The method of claim 1 wherein the mass ratio of the added liquid CO 2 or supercritical CO 2 to the slurry is at least 0.01 or at least 0.03 or at least 0.05 and is 0.5 or less or 0.3 or less, or 0.1 or less.

15 . The method of claim 1 wherein the biocrude yield is at least 30%; or wherein the solids yield is 10% or less.

16 . The method of claim 1 wherein, as compared to a process that does not add CO 2 but is otherwise identical, the biocrude yield increases by at least 5% or at least 10% (for example, instead of 30 wt % yield, at least 33 wt % biocrude yield), or in the range of 5 to 20 to 5 to 15% increase, Likewise, the method can be characterized by any of these increases relative to an identical method conducted in the presence of an atmosphere of CO 2 but no liquid or supercritical CO 2 .

17 . The method of claim 1 wherein, as compared to a process that does not add CO 2 but is otherwise identical, the solids yield decreases by at least 5% or at least 10%, or in the range of 5 to 30 to 5 to 20% decrease, Likewise, the method can be characterized by any of these decreases relative to an identical method conducted in the presence of an atmosphere of CO 2 but no liquid or supercritical CO 2 .

18 . The method of claim 3 wherein the aqueous slurry is mechanically stirred in a preheater section prior to passage into a HTL reactor.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 15, 2025
From: ZACHER, ALAN H.; MIDDLETON-SMITH, LISA A.; HART, TODD R.; SCHMIDT, ANDREW J.; THORSON, MICHAEL R.; FOX, SAMUEL P.; CRONIN, DYLAN J.
To: BATTELLE MEMORIAL INSTITUTE
Reel/Frame 072587/0627 →
CONFIRMATORY LICENSE Recorded Jun 12, 2024
From: BATTELLE MEMORIAL INSTITUTE
To: U. S. DEPARTMENT OF ENERGY
Reel/Frame 067702/0356 →
Continuity (2)
Provisional Application 63443512 · Feb 6, 2023
Related Publication 20240287390A1 · Aug 29, 2024
References Cited (18)
US 11505772B1 · Perry · 2022 [cited by examiner]
US 20170166819A1 · Choi · 2017 [cited by examiner]
US 20210284916A1 · Iversen · 2021 [cited by examiner]
US 20240191143A1 · Bobbili · 2024 [cited by examiner]
US 20240400910A1 · Engelthon · 2024 [cited by examiner]
US 20250320428A1 · Floan · 2025 [cited by examiner]
WO WO2016036948A1 · 2016 [cited by examiner]
Elliott, D.C., P. Biller, A.B. Ross, A.J. Schmidt, S.B. Jones, “Hydrothermal liquefaction of biomass: Developments from batch to continuous process”, Bioresource Technol, 178 (2015) 147-156. [cited by applicant]
Snowden-Swan, L.J., J.M. Billing, M.R. Thorson, A.J. Schmidt, Y. Jiang, D.M. Santosa, T.E. Seiple, R.C. Daniel, C. A. Burns, S. Li, “Wet Waste Hydrothermal Liquefaction and Biocrude Upgrading to Hydrocarbon Fuels: 2020 … [cited by applicant]
Yuan, X.Z., J.Y. Wang, G.M. Zeng, H.J. Huang, X.K. Pei, Z.F. Liu, M.H. Cong, “Comparative studies of thermochemical liquefaction characteristics of microalgae using different organic solvents”, Energy, 36 (2011) 6406-64… [cited by applicant]
Zhang, J.X., W.T. Chen, P. Zhang, Z.Y. Luo, Y.H. Zhang, “Hydrothermal liquefaction of Chlorella pyrenoidosa in sub-and supercritical ethanol with heterogeneous catalysts”, Bioresource Technol, 133 (2013) 389-397. [cited by applicant]
Huang, H.J., X.Z. Yuan, G.M. Zeng, J.Y. Wang, H. Li, C.F. Zhou, X.K. Pei, Q.A. You, L.A. Chen, “Thermochemical liquefaction characteristics of microalgae in sub- and supercritical ethanol”, Fuel Process Technol, 92 (201… [cited by applicant]
Jin, B.B., P.G. Duan, C.C. Zhang, Y.P. Xu, L. Zhang, F. Wang, “Non-catalytic liquefaction of microalgae in sub-and supercritical acetone”, Chem Eng J, 254 (2014) 384-392. [cited by applicant]
Reddy, H.K., T. Muppaneni, P.D. Patil, S. Ponnusamy, P. Cooke, T. Schaub, S.G. Deng, “Direct conversion of wet algae to crude biodiesel under supercritical ethanol conditions”, Fuel, 115 (2014) 720-726. [cited by applicant]
Singh, R., T. Bhaskar, B. Balagurumurthy, “Effect of solvent on the hydrothermal liquefaction of macro algae Ulva fasciata”, Process Saf Environ, 93 (2015) 154-160. [cited by applicant]
Montesantos, N., T.H. Pedersen, R.P. Nielsen, L. Rosendahl, M. Maschietti, “Supercritical carbon dioxide fractionation of bio-crude produced by hydrothermal liquefaction of pinewood”, J Supercrit Fluid, 149 (2019) 97-10… [cited by applicant]
Yi, W., D Zheng, X. Wang, Y. Chen, J. Hu, H. Yang, J. Shao, S. Zhang, H. Chen, Biomass Hydrothermal conversion under CO2 atmosphere: A way to improve the regulation of hydrothermal products, Science of the Total Environ… [cited by applicant]
Montesantos, N et al. “Supercritical Carbon Dioxide Extraction of Lignocellulosic Bio-Oils: The Potential of Fuel Upgrading and Chemical Recovery”, Energies 2020, 13, 1600. [cited by applicant]