System and process for efficient separation of biocrudes and water in a hydrothermal liquefaction system

Patent metadata

Field	Value
Publication number	US-9404063-B2
Application number	US-201414534010-A
Country	US
Kind code	B2
Filing date	Nov 5, 2014
Priority date	Nov 6, 2013
Publication date	Aug 2, 2016
Grant date	Aug 2, 2016

Abstract

A system and process are described for clean separation of biocrudes and water by-products from hydrothermal liquefaction (HTL) product mixtures of organic and biomass-containing feedstocks at elevated temperatures and pressures. Inorganic compound solids are removed prior to separation of biocrude and water by-product fractions to minimize formation of emulsions that impede separation. Separation may be performed at higher temperatures that reduce heat loss and need to cool product mixtures to ambient. The present invention thus achieves separation efficiencies not achieved in conventional HTL processing.

First claim

What is claimed is:

1. A method for processing a hydrothermal liquefaction (HTL) product mixture derived from an HTL feedstock, the method separating a biocrude from a water by-product present in a hydrothermal liquefaction (HTL) product mixture and including:
removing precipitated inorganic compounds and/or mineral solids present in the HTL product mixture at a first temperature and a first pressure;
after removing the precipitated inorganic compounds and/or mineral solids, cooling the HTL product mixture to a second temperature selected below the first temperature to phase separate the biocrude from the water by-product in the HTL product mixture; and
separating the biocrude and the water by-product phases in the absence of an extraction solvent into separate biocrude and water by-product fractions without a further change in temperature and pressure.

2. The method of claim 1 , wherein the first temperature is between about 300° C. and 370° C. and the first pressure is between about 100 bar (1.00×10 4 kPa) and 210 bar (2.10×10 4 kPa).

3. The method of claim 1 , wherein the first temperature is about 350° C. and the first pressure is about 207 bar (2.07×10 4 kPa).

4. The method of claim 1 , wherein the second temperature is between about 175° C. and about 275° C. and the second pressure is above about 20 bar (2.0×10 3 kPa) up to about 100 bar (1.00×10 4 kPa).

5. The method of claim 1 , wherein the second temperature is up to about 250° C. and the second pressure is up to about 60 bar (6.0×10 3 kPa).

6. The method of claim 1 , wherein the second temperature is selected between about 40° C. to about 90° C.

7. The method of claim 1 , wherein removal of the precipitated inorganic compounds and/or mineral solids from the HTL product mixture includes settling and accumulating the precipitated solids.

8. The method of claim 1 , wherein removal of the precipitated inorganic compounds and/or mineral solids is performed in a separation vessel or settling vessel.

9. The method of claim 1 , wherein removal of the precipitated inorganic compounds and/or mineral solids is performed after heat-up to the first temperature and first pressure and after liquefaction of the HTL feedstock.

10. The method of claim 1 , wherein removal of the precipitated inorganic compounds and/or mineral solids is performed after liquefaction of the HTL feedstock prior to separation of the biocrude and water by-product from the HTL product mixture into separate fractions.

11. The method of claim 1 , wherein removal of the precipitated inorganic compounds and/or mineral solids includes holding the HTL product mixture at a non-turbulent (quiescent) condition for a time sufficient to settle and accumulate the precipitated solids.

12. The method of claim 1 , wherein removal of the precipitated inorganic compounds and/or mineral solids includes growing particles of the solids in a quiescent condition to a size sufficient to settle and accumulate the particles prior to removal thereof.

13. The method of claim 12 , wherein growth of the solid particles includes a dwell time in the quiescent condition of at least about 10 minutes or greater.

14. The method of claim 1 , wherein removal of the precipitated inorganic compounds and/or mineral solids includes settling and accumulating the solids in a settling vessel or a separation vessel.

15. The method of claim 14 , wherein removal of the precipitated inorganic compounds and/or mineral solids includes separation of the precipitated inorganic compounds and/or mineral solids from the bottom of the settling vessel or the separation vessel.

16. The method of claim 1 , wherein the precipitated inorganic compounds and/or mineral solids include a divalent cation and an anion selected from the group consisting of: sulfate, phosphate, carbonate, and combinations thereof.

17. The method of claim 1 , further including delivering one or both of the separated biocrude and water by-product fractions to a subsequent processing stage or process for further processing at a temperature at or above the second temperature.

Assignees

• Battelle Memorial Institute
• Genifuel Corp

Inventors

• Elliott Douglas C
• Hart Todd R
• Neuenschwander Gary G
• Oyler James R
• Rotness Jr Leslie J
• Schmidt Andrew J
• Zacher Alan H

Classifications

• B01J19/24

  Stationary reactors without moving elements inside (B01J19/08, B01J19/26 take precedence; with stationary particles B01J8/02) · CPC title

• C10G33/06

  with mechanical means, e.g. by filtration · CPC title

• C10G3/40

  Thermal non-catalytic treatment · CPC title

• B01J2219/24

  Stationary reactors without moving elements inside · CPC title

• B01J19/18

  Stationary reactors having moving elements inside (B01J19/08, B01J19/26 take precedence) · CPC title