Hydrothermal conversion process with inertial cavitation

• US 9,968,904 B2
• Filed: 06/09/2016
• Issued: 05/15/2018
• Est. Priority Date: 06/10/2015
• Status: Active Grant

• Current Assignee: Alireza Shekarriz
• Original Assignee: Alireza Shekarriz
• Inventors: Shekarriz, Alireza
• Primary Examiner(s): Hendrickson, Stuart
• Application Number:
  US15/177,654
• Publication Number:
  US 20160361700A1
• Time in Patent Office: 705 Days
• CPC Class Codes: B01J 19/008 Processes for carrying out reactions under cavitation conditions
• CPC Class Codes: C01B 32/05 Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
• CPC Class Codes: C05F 11/00 Other organic fertilisers
• CPC Class Codes: C10L 2200/0469 Renewables or materials of biological origin
• CPC Class Codes: C10L 2250/06 Particle, bubble or droplet size
• CPC Class Codes: C10L 2290/06 Heat exchange, direct or indirect
• CPC Class Codes: C10L 2290/148 of steam
• CPC Class Codes: C10L 5/447 Carbonized vegetable substances, e.g. charcoal, or produced by hydrothermal carbonization of biomass
• CPC Class Codes: C10L 9/086 Hydrothermal carbonization
• CPC Class Codes: Y02E 50/10 Biofuels, e.g. bio-diesel
• CPC Class Codes: Y02E 50/30 Fuel from waste, e.g. synthetic alcohol or diesel

Abstract

Hydrothermal conversion is performed on organic feedstocks that include solids, by forming a slurry of the feedstock in water and subjecting the slurry to hydrothermal conversion conditions. The hydrothermal conversion conditions may be sufficient to product a carbonized solid and/or liquefaction products. The size of solids (either or both of feedstock or carbonized solids produced in the process) is reduced by conducting a series of bubble-forming and bubble-collapsing cycles on the slurry.

Claims

1. A hydrothermal conversion process comprising the steps of

a) combining a particulate solid organic feedstock with water to form a slurry of the organic feedstock particles in a liquid phase;

b) subjecting the slurry to hydrothermal conversion conditions including a temperature of at least 160°

C. and a superatmospheric pressure sufficient to maintain at least a portion of the water as a liquid, to convert at least a portion of the organic feedstock to one or more hydrothermal conversion products

wherein prior to, during and/or after step b), and at such a time as particles of the organic feedstock and/or a solid hydrothermal conversion product are dispersed in the liquid phase, the liquid phase with the dispersed particles is cycled through one or more bubble-forming and bubble-collapsing cycles while maintaining a liquid phase temperature of at least 100°

C., wherein each bubble-forming and bubble-collapsing cycle includes the steps of i) forming gas bubbles in the slurry and then ii) subjecting the gas bubbles to pressure and temperature conditions sufficient to condense gas in the gas bubbles and collapse the bubbles.

2. The process of claim 1, wherein each bubble-forming and bubble-collapsing cycle includes the steps of i) adjusting the pressure and/or temperature of the intermediate slurry such that a portion of the liquid phase volatilizes to form bubbles and then ii) re-adjusting the pressure and/or temperature to condense the volatilized liquid phase within the bubbles and collapse the bubbles.

3. The process of claim 1 wherein each bubble-forming and bubble-collapsing cycle includes the steps of establishing an operating temperature of at least 160°

C. and a pressure above the saturation pressure of at least one compound at the operating temperature, forming bubbles that include the at least one compound by reducing the pressure to below the saturation pressure of the at least one compound at the operating temperature such that a portion of the at least one compound volatilizes, and collapsing the bubbles by then increasing the pressure to above the saturation pressure of the at least one compound.

4. The process of claim 1 wherein each bubble-forming and bubble-collapsing cycle includes the steps of establishing an operating temperature of at least 160°

C. and a pressure above the saturation pressure of water at the operating temperature, forming bubbles that include water by reducing the pressure to below the saturation pressure of water at the operating temperature such that a portion of the water volatilizes, and collapsing the bubbles by then increasing the pressure to above the saturation pressure of water.

5. The process of claim 1 wherein the bubble-forming and bubble-collapsing cycle includes a step of injecting steam into the liquid phase above the saturation pressure of water at the temperature of the liquid phase, such that the steam forms bubbles in the liquid phase and the steam bubbles collapse.

6. The process of claim 1, wherein the one or more bubble-forming and bubble-collapsing cycles are performed under hydrothermal conversion conditions.

7. The process of claim 1, wherein 10 to 10,000,00 bubble-forming and bubble-collapsing cycles are performed.

8. The process of claim 1 wherein the hydrothermal conversion step includes a hydrothermal carbonization step that produces an at least partially carbonized solid, and at least one of the one or more of the bubble-forming and bubble-collapsing cycles is performed before carbonized solids are formed to reduce the size of at least some of the feedstock solids.

9. The process of claim 1 wherein the hydrothermal conversion step includes a hydrothermal carbonization step that produces an at least partially carbonized solid, and at least one of the one or more bubble-forming and bubble-collapsing cycles is performed simultaneously with the hydrothermal carbonization step to reduce the size of at least some of the organic feedstock particles and/or of at least some of the at least partially carbonized solid.

10. The process of claim 1 wherein the hydrothermal conversion step includes a hydrothermal carbonization step that produces an at least partially carbonized solid, and at least one of the one or more bubble-forming and bubble-collapsing cycles is performed after the hydrothermal conversion step to reduce the size of the at least partially carbonized solid.

11. The process of claim 1 wherein the hydrothermal conversion step includes a hydrothermal liquefaction step, a wet-air oxidation step, or both a hydrothermal liquefaction step and a wet-air oxidation step, and the at least one bubble-forming and bubble-collapsing cycle is performed before and/or during the hydrothermal liquefaction step, wet-air oxidation step or the hydrothermal liquefaction and wet-air oxidation steps, while solid organic feedstock particles are present.

12. The process of claim 1, wherein the hydrothermal conversion step includes a first hydrothermal carbonization step and at least one subsequent hydrothermal liquefaction step and/or wet-air oxidation step.

13. The process of claim 12, wherein hydrothermal conditions are maintained from the start of the first hydrothermal carbonization step to the end of the last hydrothermal liquefaction and/or wet-air oxidation step, including any intermediate bubble-forming and bubble-collapsing steps.

14. The process of claim 12, wherein at least one of the one or more bubble-forming and bubble-collapsing cycles is performed during the first hydrothermal carbonization step.

15. The process of claim 12, wherein at least one of the one or more bubble-forming and bubble-collapsing cycles is performed during the at least one subsequent hydrothermal liquefaction step and/or wet-air oxidation step.

16. The process of claim 12, wherein at least one of the one or more bubble-forming and bubble-collapsing cycles is performed as an intermediate step after the first hydrothermal carbonization step and before at least one subsequent hydrothermal liquefaction step and/or wet-air oxidation step.

17. The process of claim 1, wherein the at least one bubble-forming and bubble-collapsing cycle produces particles having surface areas of 0.03 cm² or less.

18. The process of claim 1, wherein the hydrothermal conversion conditions include a temperature of 160 to 400°

C. and a pressure above the saturation temperature of water at the temperature.

19. The process of claim 1, wherein the bubble-forming and bubble-collapsing cycles increase the rate of reaction by reducing the particle size and de-agglomerating the feedstock and/or carbonized solids, by improving bulk mixing and/or by providing localized heating due to the heat released when the bubbles collapse.

20. The process of claim 1, wherein each bubble-forming and bubble-collapsing cycle is performed under conditions sufficient to maintain at least a portion of the water in the liquid phase as a liquid.

21. The process of claim 1 which includes multiple steps of subjecting the slurry to hydrothermal conversion conditions, and wherein hydrothermal conditions are maintained continuously from the start of the first step of subjecting the slurry to hydrothermal conversion conditions to the end of the last step of subjecting the slurry to hydrothermal conversion conditions, including any intermediate bubble-forming and bubble-collapsing steps.