IP Library Granted Patent US 12,606,849
Granted Patent B2
US 12,606,849 · App. 17/998,759 · Granted Apr 21, 2026

Converting lignocellulosic feedstock to fuel

Inventors: Brian Foody (Ottawa, CA); Jeffrey S. Tolan (Ottawa, CA); Kristin Martens (Nepean, CA)
Assignee: Iogen Corporation
C12P7/06C08H8/00C10L1/02C12P5/026C12P19/02C12P19/14C10L2200/0469C10L2290/10C10L2290/12C10L2290/26C12P2201/00
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 12,606,849
App. No.
17/998,759
Granted
Apr 21, 2026
Kind
B2
Abstract

A process for converting lignocellulosic biomass to fuel, wherein lignocellulosic feedstock is soaked in a sulfuric acid solution to demineralize the feedstock, the demineralized feedstock is pretreated at a temperature between 150° C. and 230° C. and a pH between 1 and 2.5, at least part of the pretreated material is converted to a fermentation production such as ethanol, and at least a portion of a secondary stream, such as still bottoms from the distillation of ethanol, is converted to biogas by anaerobic digestion. Soaking the lignocellulosic feedstock in sulfuric acid solution reduces the amount of sulfuric acid required for the pretreatment, and thus the amount of sulfate carried downstream to the anaerobic digestion. This increases the biogas yield and/or xylose yield. A recycling process, wherein mineralized soaking liquid produced in the soaking process is fed to cation exchange to remove minerals, reduces excess waste of the sulfuric acid and water usage.

Claims (34)

1 . A process for converting lignocellulosic biomass to fuel, said process comprising:

(a) a demineralization, said demineralization comprising subjecting a feedstock to an acid soaking process, said feedstock comprising the lignocellulosic biomass, said acid soaking process comprising one or more acid soak stages, wherein each of the one or more acid soak stages comprises (i) contacting the feedstock with a soaking liquid to produce a soaked feedstock slurry, and (ii) subjecting the soaked feedstock slurry to a solids/liquid separation, wherein the soaking liquid in each of the one or more acid soak stages is an aqueous solution comprising sulfuric acid having a pH between 1 and 5;

(b) a pretreatment, said pretreatment comprising heating a slurry containing sulfuric acid and demineralized feedstock produced from the demineralization, said heating conducted at a temperature between 150° C. and 230° C. and at a pH between 1 and 2.5, said pretreatment producing a pretreated slurry;

(c) a first conversion, said first conversion comprising an enzymatic hydrolysis wherein cellulose in the pretreated slurry is converted to glucose, a fermentation wherein the glucose is converted to a fermentation product, and a fermentation product recovery, wherein the first conversion produces a secondary stream that contains one or more sulfur compounds derived from sulfuric acid used in the demineralization, the sulfuric acid used in pretreatment, or a combination thereof;

(d) a second conversion, said second conversion comprising feeding at least part of the secondary stream to an anaerobic digester and collecting biogas from the anaerobic digester, said biogas used as a fuel within the process, processed to provide a fuel, or a combination thereof, and

(e) a recycling process, said recycling process comprising feeding mineralized soaking liquid produced from step (a) to cation exchange wherein minerals are removed, and feeding clean sulfuric acid solution produced from the cation exchange to at least one acid soak stage in step (a).

2 . The process according to claim 1 , wherein the acid soaking process comprises a multi-stage countercurrent acid soak.

3 . The process according to claim 2 , wherein a pressate recycle fraction in at least one of the stages of the acid soaking process is greater than 10%.

4 . The process according to claim 1 , wherein the feedstock subjected to the acid soaking process has had at least 75% of the potassium originally present removed.

5 . The process according to claim 1 , wherein the conditions for the acid soaking process are selected to remove at least 70% of the calcium originally present in the lignocellulosic biomass.

6 . The process according to claim 1 , wherein the soaking liquid in each of the one or more acid soak stages has a pH between 1.2 and 4 and is at a temperature between 30° C. and 90° C.

7 . The process according to claim 1 , wherein step (i) of each acid soak stage is conducted at a consistency between 2% and 10% for at least 5 minutes.

8 . The process according to claim 1 , wherein step (ii) of each acid soak stage provides solids having a consistency of at least 15%.

9 . The process according to claim 1 , comprising a washing process upstream of the acid soaking process, said washing process comprising one or more washing stages, wherein each of the one or more washing stages comprises

(a) contacting the feedstock with a wash water, and

(b) a solids/liquid separation wherein the feedstock is separated from at least a portion of the wash water,

wherein the conditions for the washing process are selected to remove at least 70% of the potassium originally present in the feedstock.

10 . The process according to claim 1 , wherein the secondary stream comprises at least part of still bottoms from the fermentation product recovery.

11 . The process according to claim 10 , wherein the still bottoms are subjected to a solids/liquid separation that provides solids and liquids, where the secondary stream comprises liquid produced from the solids/liquid separation of the still bottoms.

12 . The process according to claim 1 , wherein the first conversion comprises subjecting the pretreated slurry to a solids/liquid separation, and wherein the secondary stream comprises liquid from the solids/liquid separation of the pretreated slurry.

13 . The process according to claim 1 , wherein the enzymatic hydrolysis in the first conversion is conducted on unwashed demineralized feedstock.

14 . The process according to claim 1 , wherein the fermentation product is ethanol.

15 . The process according to claim 1 , wherein the second conversion comprises producing renewable natural gas from the biogas.

16 . The process according to claim 1 , wherein the amount of sulfuric acid provided in pretreatment is not more than 12 kg H 2 SO 4 /ton of dry lignocellulosic biomass.

17 . The process according to claim 1 , wherein the secondary stream has a sulfate concentration that is not more than 5 g/L.

18 . The process according to claim 1 , wherein the secondary stream has a biologically degraded chemical oxygen demand to sulfate ratio of at least 7 to 1.

19 . A process for converting lignocellulosic biomass to fuel, said process comprising:

subjecting a feedstock comprising lignocellulosic biomass to a washing process to provide a washed feedstock,

subjecting the washed feedstock to an acid soaking process to produce a demineralized feedstock, said acid soaking process comprising a multi-stage countercurrent acid soak, each stage of the multi-stage acid soak comprising (a) contacting the feedstock with an aqueous sulfuric acid solution having a pH not more than 3, and (ii) a solids/liquid separation that provides a pressate and solids, said solids having a consistency of at least 20%, wherein a pressate recycle fraction in at least one stage of the multi-stage countercurrent acid soak is greater than 10% by weight;

pretreating the demineralized feedstock to produce a pretreated slurry comprising cellulose, said pretreating comprising heating a slurry containing sulfuric acid and the demineralized feedstock at a temperature between 150° C. and 230° C. and at a pH between 1 and 2.5;

converting at least part of the pretreated slurry to ethanol, said converting comprising hydrolyzing the cellulose to glucose in an enzymatic hydrolysis, fermenting the glucose to ethanol, and recovering the ethanol in a distillation that produces concentrated ethanol and still bottoms;

feeding a stream comprising at least part of the still bottoms to an anaerobic digestion, said stream comprising sulfate derived from sulfuric acid used in the acid soaking process, sulfate derived from sulfuric acid used in pretreatment, or a combination thereof;

collecting biogas from the anaerobic digester, said collected biogas used as a fuel within the process, processed to provide a transportation fuel, or a combination thereof; and

subjecting mineralized soaking liquid produced from the acid soaking process to cation exchange to remove one or more minerals therefrom and recycling clean sulfuric acid solution produced by cation exchange within the acid soaking process.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 17, 2022
From: FOODY, BRIAN; TOLAN, JEFFREY S.; MARTENS, KRISTIN
To: IOGEN CORPORATION
Reel/Frame 061809/0517 →
Continuity (2)
Provisional Application 63028888 · May 22, 2020
Related Publication 20230340543A1 · Oct 26, 2023
References Cited (95)
US 4168988A · Riehm et al. · 1979 [cited by applicant]
US 4461648A · Foody · 1984 [cited by applicant]
US 4908067A · Just · 1990 [cited by applicant]
US 7198925B2 · Foody · 2007 [cited by applicant]
US 7503981B2 · Wyman et al. · 2009 [cited by applicant]
US 7585652B2 · Foody et al. · 2009 [cited by applicant]
US 7670813B2 · Foody et al. · 2010 [cited by applicant]
US 7709042B2 · Foody et al. · 2010 [cited by applicant]
US 7754457B2 · Foody et al. · 2010 [cited by applicant]
US 7901511B2 · Griffin et al. · 2011 [cited by applicant]
US 7993463B2 · Griffin et al. · 2011 [cited by applicant]
US 8101024B2 · Wyman et al. · 2012 [cited by applicant]
US 8123864B2 · Christensen et al. · 2012 [cited by applicant]
US 8273181B2 · Foody et al. · 2012 [cited by applicant]
US 8298796B2 · Tolan et al. · 2012 [cited by applicant]
US 8328947B2 · Anand et al. · 2012 [cited by applicant]
US 8404355B2 · Jansen et al. · 2013 [cited by applicant]
US 8500910B2 · Brady et al. · 2013 [cited by applicant]
US 8603789B2 · Harlick · 2013 [cited by applicant]
US 8652261B2 · O'Connor · 2014 [cited by applicant]
US 8709770B2 · Harlick et al. · 2014 [cited by applicant]
US 8785155B2 · Retsina et al. · 2014 [cited by applicant]
US 8980599B2 · Tolan et al. · 2015 [cited by applicant]
US 9315427B2 · Foody et al. · 2016 [cited by applicant]
US 9335043B2 · Nguyen · 2016 [cited by applicant]
US 9476066B2 · Foody · 2016 [cited by applicant]
US 9493851B2 · Jansen et al. · 2016 [cited by applicant]
US 9574212B2 · Foody et al. · 2017 [cited by applicant]
US 9783861B2 · Jansen et al. · 2017 [cited by applicant]
US 9809866B2 · Ottonello et al. · 2017 [cited by applicant]
US 9862893B2 · Gray et al. · 2018 [cited by applicant]
US 10179971B2 · Griffin et al. · 2019 [cited by applicant]
US 10202622B2 · Foody et al. · 2019 [cited by applicant]
US 10336628B2 · Shi et al. · 2019 [cited by applicant]
US 10421667B2 · Foody et al. · 2019 [cited by applicant]
US 10513714B2 · Foody et al. · 2019 [cited by applicant]
US 10612048B2 · Foody et al. · 2020 [cited by applicant]
US 10654235B2 · Miller et al. · 2020 [cited by applicant]
US 10889795B2 · Rowland et al. · 2021 [cited by applicant]
US 11008598B2 · Foody · 2021 [cited by examiner]
US 20130071900A1 · Mackay et al. · 2013 [cited by applicant]
US 20130071903A1 · Rowland et al. · 2013 [cited by applicant]
US 20130143278A1 · Tolan et al. · 2013 [cited by applicant]
US 20130143285A1 · Tolan et al. · 2013 [cited by applicant]
US 20130157334A1 · Van Der Heide et al. · 2013 [cited by applicant]
US 20140315258A1 · Nguyen · 2014 [cited by applicant]
US 20150191758A1 · Larsen et al. · 2015 [cited by applicant]
US 20170362618A1 · Nguyen · 2017 [cited by applicant]
US 20180355387A1 · Javers et al. · 2018 [cited by applicant]
US 20190032094A1 · Yu et al. · 2019 [cited by applicant]
US 20190144773A1 · Ribeiro de Lima et al. · 2019 [cited by applicant]
US 20190248962A1 · Satlewal et al. · 2019 [cited by applicant]
US 20190315636A1 · Shi et al. · 2019 [cited by applicant]
US 20190323096A1 · Jansen et al. · 2019 [cited by applicant]
WO WO2006026863 · 2006 [cited by applicant]
WO WO2012019306 · 2012 [cited by applicant]
WO WO2015142399A1 · 2015 [cited by applicant]
WO WO2016113221A1 · 2016 [cited by applicant]
WO WO2016145529 · 2016 [cited by applicant]
WO WO2017100907 · 2017 [cited by applicant]
WO WO2017174093A9 · 2017 [cited by applicant]
WO WO2019090413A1 · 2019 [cited by applicant]
WO WO2019090414A1 · 2019 [cited by applicant]
WO WO2019191828A1 · 2019 [cited by applicant]
WO WO2021232143 · 2021 [cited by applicant]
Heinone et al, Performance evaluation of a recycle-integrated process for the production and purification of monosaccharides from lignocellulosic mass. Separation and Purification Technol., 2015, vol. 156: 561-571. (Yea… [cited by examiner]
Oriez et al., Lignocellulosic Biomass fractionation by mineral acids and resulting extract purification processes: conditions, yields, and purities. Molecules, 2019, vol. 24, 4273, pp. 1-21. (Year: 2019). [cited by examiner]
Silva et a., Influence of COD/SO42-ratio on vinasse treatment performance by two-stage anaerobic membrane bioreactor. J. Environ. Management., 2020, vol. 259, 110034, pp. 1-11. (Year: 2020). [cited by examiner]
Aslam, Umair et al., “Effect of demineralization on the physiochemical structure and thermal degradation of acid treated indigenous rice husk”, Pol. J. of Chem. Tech., vol. 80 (2016), pp. 117-121. [cited by applicant]
Aston, John E et al., “Performance Assessment of Dilute-Acid Leaching to Improve Corn Stover Quality for Thermochemical Conversion”, (2016). [cited by applicant]
Bondesson, Pia-Maria et al., “Ethanol and biogas production after steam pretreatment of corn stover with or without the addition of sulphuric acid”, Biotechnol Biofuels, vol. 6 (2013), pp. 1-11. [cited by applicant]
Cesaro, Alessandra et al., “Combined biogas and bioethanol production: Opportunities and challenges for industrial application,” Energies, V 8 (2015), pp. 8121-8144. [cited by applicant]
Horhammer, Hanna et al., “Removal of non-structural components from poplar whole-tree chips to enhance hydrolysis and fermentation performance,” Biotechnol Biofuels, V 11 (2018), pp. 1-22. [cited by applicant]
Humbird, D., “Process design and economics for biochemical conversion of lignocellulosic biomass to ethanol—Dilute-acid pretreatment and enzymatic hydrolysis of corn stover,” Technical Report NREL/TP-5100-47764, (2011). [cited by applicant]
Joelsson, Elisabeth et al., “Combined production of biogas and ethanol at high solids loading from wheat straw impregnated with acetic acid: experimental study and techno-economic evaluation,” Sustain Chem Process, vol.… [cited by applicant]
Kang, Qian et al., “Bioethanol from lignocellulosic biomass: current findings determine research priorities,” Scientific World Journal, (2014). [cited by applicant]
Le, Duy Michael, “Biorefining of wheat straw: accounting for the distribution of mineral elements in pretreated biomass by an extended pretreatment-severity equation,” Biotechnol Biofuels, V 7 (2014), 1-13. [cited by applicant]
Luque, Luis, et al., “Comparison of ethanol production from corn cobs and switchgrass following a pyrolysis-based biorefinery approach,” Biotechnol Biofuels, V 9 (2016), pp. 1-14. [cited by applicant]
Mahmood, Hamayoun et al., “Recent advances in the pretreatment of lignocellulosic biomass for biofuels and value-added products,” Green and Sustainable Chemistry V 20 (2019) pp. 18-24. [cited by applicant]
Moraes, Bruna S. et al., “Anaerobic digestion of vinasse from sugarcane ethanol production in Brazil: challenges and perspectives,” Renewable and Sustainable Energy Reviews, vol. 44 (2015), pp. 888-903. [cited by applicant]
Persson, H. et al., “Catalytic pyrolysis of demineralized lignocellulosic biomass,” Fuel, V252 (2019) pp. 200-209. [cited by applicant]
Reza, M. Toufiq, et al., “Ash reduction of corn stover by mild hydrothermal preprocessing,” Biomass Conv. Bioref, V 5 (2015), pp. 21-31. [cited by applicant]
Roeleveld, P.J. et al., “Experience with guidelines for wastewater characterisation in the Netherlands,” Water Science and Technology, V 45 (2002) pp. 77-87. [cited by applicant]
Shan, Lili et al., “Performance of SCTR-EGSB-SBR system for treating sulfate-rich cellulosic ethanol wastewater and microbial community analysis,” Environ Sci Pollut Res (2017). [cited by applicant]
Sluiter, A. et al., “Determination of Ash in Biomass,” Technical Report NREL/TP-510-42622 (2008). [cited by applicant]
Tian, Zhuoli et al., “Anaerobic digestion for treatment of stillage from cellulosic bioethanol production,” Bioresource Technology V 144 (2013) pp. 387-395. [cited by applicant]
Visser, Andre, “The anaerobic treatment of sulfate containing wastewater,” Thesis. [cited by applicant]
Wilkie, Ann C., “Stillage characterization and anaerobic treatment of ethanol stillage from conventional and cellulosic feedstocks,” Biomass and Bioenergy V 19 (2000) pp. 63-102. [cited by applicant]
Written Opinion for PCT/CA2021/050555 dated Jun. 23, 2021. [cited by applicant]
International Search Report for PCT/CA2021/050555 dated Jun. 23, 2021. [cited by applicant]
IPRP for PCT/CA2021/050555 dated Nov. 17, 2022. [cited by applicant]
Sluiter et al., “Determination of Structural Carbohydrates and Lignin in Biomass,” NREL Technical Report NREL/TP-510-42618, Aug. 2012, in 18 pages. [cited by applicant]
European Office Action in EP Application No. 21807899.6 dated Nov. 14, 2023. [cited by applicant]
Yoon, S.-Y. et al., “The effect of hemicelluloses and lignin on acid hydrolysis of cellulose”, Energy, Feb. 2014, vol. 77, pp. 19-24. [cited by applicant]
European Office Action in EP Application No. 21807899.6 dated Jul. 18, 2025. [cited by applicant]