Catalytic fast pyrolysis process with impurity removal

• US 10,703,649 B2
• Filed: 06/26/2019
• Issued: 07/07/2020
• Est. Priority Date: 06/30/2015
• Status: Active Grant

• Current Assignee: Anellotech, Inc.
• Original Assignee: Anellotech, Inc.
• Inventors: Shi, Jian, Sorensen, Charles, Mazanec, Terry, Song, Ruozhi, Goud, Sandeep, Han, Scott, Cheng, Yu-Ting, Frank, Victoria L., Igoe, Jr., William F., Schneidkraut, Marc
• Primary Examiner(s): McCaig, Brian A
• Application Number:
  US16/453,371
• Publication Number:
  US 20190315636A1
• Time in Patent Office: 377 Days
• CPC Class Codes: C02F 1/04 by distillation or evaporation
• CPC Class Codes: C02F 1/42 by ion-exchange ion-exchange in general B01J
• CPC Class Codes: C02F 1/441 by reverse osmosis
• CPC Class Codes: C02F 11/10 by pyrolysis
• CPC Class Codes: C02F 2101/10 Inorganic compounds
• CPC Class Codes: C02F 2101/101 Sulfur compounds
• CPC Class Codes: C02F 2101/12 Halogens or halogen-containing compounds
• CPC Class Codes: C02F 2101/16 Nitrogen compounds, e.g. ammonia
• CPC Class Codes: C02F 2303/10 Energy recovery
• CPC Class Codes: C02F 2303/18 Removal of treatment agents after treatment
• CPC Class Codes: C02F 2303/26 Reducing the size of particles, liquid droplets or bubbles, e.g. by crushing, grinding, spraying, creation of microbubbles or nanobubbles
• CPC Class Codes: C02F 9/00 Multistage treatment of water, waste water or sewage
• CPC Class Codes: C10B 49/22 according to the "fluidised bed" technique
• CPC Class Codes: C10B 53/02 of cellulose-containing material production of pyroligneous acid C10C5/00
• CPC Class Codes: C10B 57/06 containing additives
• CPC Class Codes: C10B 57/08 Non-mechanical pretreatment of the charge C10L9/00 takes precedence, e.g. desulfurization
• CPC Class Codes: C10G 1/002 in combination with oil conversion- or refining processes
• CPC Class Codes: C10G 1/02 by distillation
• CPC Class Codes: C10G 2300/1014 of vegetal origin
• CPC Class Codes: D21C 3/22 Other features of pulping processes
• CPC Class Codes: Y02E 50/10 : Biofuels, e.g. bio-diesel
• CPC Class Codes: Y02P 20/145 : the feedstock being materials of biological origin
• CPC Class Codes: Y02P 30/20 : using bio-feedstock
• CPC Class Codes: Y02W 10/30 : Wastewater or sewage treatment systems using renewable energies

Abstract

The present invention provides an improved catalytic fast pyrolysis process for increased yield of useful and desirable products. In particular, the process comprises an improved catalytic fast pyrolysis process for producing aromatic compounds, such as, for example, benzene, toluene and xylenes, from biomass feedstock containing impurities, such as, for example alkali and alkaline earth metal, sulfur and nitrogen components.

Claims

1. A process for treating biomass containing at least 500 ppm alkali and alkaline earth metal components to reduce alkali and alkaline earth metal content to result in treated biomass comprising steps 1) sizing the biomass to ≤

20 cm size particles,

     2) washing the sized biomass of step

     1) in at least one washing cycle with a washing fluid comprising acidified water having a pH from 2 to 5 sufficiently to reduce the content of alkali and alkaline earth metals by at least 90%, including a mass ratio of washing fluid to biomass of at least 3,

     3) rinsing the washed biomass of step

     2) with rinsing fluid comprising water which comprises ≤

5 ppm K or ≤

20 ppm Ca, or both,

     4) drying the rinsed biomass of step

     3) to reduce water content, wherein the temperature of step

     2) is maintained at a temperature of no more than 90°

C.

2. The process of claim 1 wherein the washing fluid is recirculated through the biomass in step 2) in a continuous manner.

3. The process of claim 1 wherein a BET surface area measured by gas adsorption of the dried biomass from step 4) is from 10 to 200 m²/g, or has increased by at least 1.5 times compared to the untreated biomass.

4. The process of claim 1 wherein a pore volume measured by gas adsorption of the dried biomass from step 4) is from 0.01 to 0.5 cc/g, or has increased by at least 1.5 times compared to the untreated biomass.

5. The process of claim 1 wherein a contacting time of an individual washing cycle of step 2) is ≤

60 minutes.

6. The process of claim 1 wherein a sum of all contacting times of all washing cycles, or a contacting time of a continuous washing cycle, is ≤

120 minutes.

7. The process of claim 1 wherein a contacting time of rinsing step 3) is ≤

30 minutes.

8. The process of claim 1 wherein a total elapsed time of washing step 2) and rinsing step 3) is ≤

10 hours.

9. The process of claim 1 wherein a particle size distribution of at least 50% of the sized biomass of step 1) is from 1 to 1400 microns as measured by laser diffraction.

10. The process of claim 1 wherein an average aspect ratio of the particles of the sized biomass of step 1) is from 1.1 to at least 40.

11. The process of claim 1 wherein a cellulose/hemicellulose ratio in the washed biomass of step 2) is changed from the cellulose/hemicellulose ratio in the sized biomass of step 1) by no more than 10%.

12. The process of claim 1 wherein the washing in step 2) is conducted as a counter-current washing process, wherein the flows of biomass to be washed and the washing fluid are flowing in opposite directions as they encounter each other.

13. A process for treating biomass containing at least 500 ppm alkali and alkaline earth metal components to reduce alkali and alkaline earth metal content to result in a treated biomass comprising steps:

1) sizing the biomass to less than or equal to 20 cm size particles,

     2) extracting and washing the sized biomass of step

     1) in at least one extraction and washing cycle with an extracting and washing fluid comprising acidified water having a pH less than or equal to 2 sufficiently to reduce the content of the alkali and alkaline earth metals by at least 90%, including a mass ratio of extraction and washing fluid to biomass of at least 3, wherein the mass ratio of cellulose to hemicellulose in the washed biomass compared to that found in the untreated biomass has changed by no more than 10%;

     3) rinsing the washed biomass of step

     2) with rinsing fluid comprising water which comprises less than or equal to 5 ppm K or less than or equal to 20 ppm Ca, or both,

     4) drying the biomass of step

     3) to reduce the water content to less than or equal to 10%, wherein the temperature of step

     2) is maintained at a temperature of no more than 90°

C. and wherein the washing fluid is an aqueous solution.

14. The process of claim 13 wherein the washing step is conducted in a countercurrent configuration wherein a flow of biomass to be washed and the washing fluid are flowing in opposite directions as they encounter each other.