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Title: Pilot-Scale Batch Alkaline Pretreatment of Corn Stover

Abstract

The goal of biomass pretreatment is to increase the enzymatic digestibility of the plant cell wall polysaccharides to produce sugars for upgrading to biofuels. Alkaline pretreatment has the ability to solubilize much of the lignin in biomass while the carbohydrates remain insoluble. With an increased research focus to produce high-value products from lignin, a low molecular weight, lignin-rich stream in a biorefinery is desirable. Here, this work reports on batch alkaline pretreatment of corn stover conducted using a three-factor, two-level central composite experimental design in a pilot-scale reactor to determine the relationship between sodium hydroxide (NaOH) loading, temperature, and anthraquinone (AQ) charge on solids solubilization, component yields, and enzymatic digestibility of the residual solids. Operating conditions were 100 to 140 °C, 40 to 70 mg NaOH/g dry corn stover, and 0.05% to 0.2% (w/w) AQ loading. An enzymatic hydrolysis screening study was performed at 2% cellulose loading. Empirical modeling results showed that NaOH loading and temperature are both significant factors, solubilizing 15% to 35% of the solids and up to 54% of the lignin. Enzymatic hydrolysis of the residual solids produced good monomeric glucose (>90%) and xylose (>70%) yields at the more severe pretreatment conditions. We also found that themore » AQ charge was not a significant factor at the conditions studied, so efforts to reduce xylan and increase lignin solubilization using this compound were not successful. Lastly, while good lignin solubilization was achieved, effectively recovering this stream remains a challenge, and demonstrating performance in continuous reactors is still needed.« less

Authors:
 [1];  [1];  [1];  [1]
  1. National Renewable Energy Lab. (NREL), Golden, CO (United States). National Bioenergy Center
Publication Date:
Research Org.:
National Renewable Energy Lab. (NREL), Golden, CO (United States)
Sponsoring Org.:
USDOE Office of Energy Efficiency and Renewable Energy (EERE), Transportation Office. Bioenergy Technologies Office
OSTI Identifier:
1241508
Report Number(s):
NREL/JA-5100-65012
Journal ID: ISSN 2168-0485
Grant/Contract Number:  
AC36-08GO28308
Resource Type:
Accepted Manuscript
Journal Name:
ACS Sustainable Chemistry & Engineering
Additional Journal Information:
Journal Volume: 4; Journal Issue: 3; Journal ID: ISSN 2168-0485
Publisher:
American Chemical Society (ACS)
Country of Publication:
United States
Language:
English
Subject:
09 BIOMASS FUELS; lignocellulose; pretreatment; alkaline; aodium hydroxide; lignin; scale-up; enzymatic hydrolysis

Citation Formats

Kuhn, Erik M., O’Brien, Marykate H., Ciesielski, Peter N., and Schell, Daniel J.. Pilot-Scale Batch Alkaline Pretreatment of Corn Stover. United States: N. p., 2015. Web. https://doi.org/10.1021/acssuschemeng.5b01041.
Kuhn, Erik M., O’Brien, Marykate H., Ciesielski, Peter N., & Schell, Daniel J.. Pilot-Scale Batch Alkaline Pretreatment of Corn Stover. United States. https://doi.org/10.1021/acssuschemeng.5b01041
Kuhn, Erik M., O’Brien, Marykate H., Ciesielski, Peter N., and Schell, Daniel J.. Fri . "Pilot-Scale Batch Alkaline Pretreatment of Corn Stover". United States. https://doi.org/10.1021/acssuschemeng.5b01041. https://www.osti.gov/servlets/purl/1241508.
@article{osti_1241508,
title = {Pilot-Scale Batch Alkaline Pretreatment of Corn Stover},
author = {Kuhn, Erik M. and O’Brien, Marykate H. and Ciesielski, Peter N. and Schell, Daniel J.},
abstractNote = {The goal of biomass pretreatment is to increase the enzymatic digestibility of the plant cell wall polysaccharides to produce sugars for upgrading to biofuels. Alkaline pretreatment has the ability to solubilize much of the lignin in biomass while the carbohydrates remain insoluble. With an increased research focus to produce high-value products from lignin, a low molecular weight, lignin-rich stream in a biorefinery is desirable. Here, this work reports on batch alkaline pretreatment of corn stover conducted using a three-factor, two-level central composite experimental design in a pilot-scale reactor to determine the relationship between sodium hydroxide (NaOH) loading, temperature, and anthraquinone (AQ) charge on solids solubilization, component yields, and enzymatic digestibility of the residual solids. Operating conditions were 100 to 140 °C, 40 to 70 mg NaOH/g dry corn stover, and 0.05% to 0.2% (w/w) AQ loading. An enzymatic hydrolysis screening study was performed at 2% cellulose loading. Empirical modeling results showed that NaOH loading and temperature are both significant factors, solubilizing 15% to 35% of the solids and up to 54% of the lignin. Enzymatic hydrolysis of the residual solids produced good monomeric glucose (>90%) and xylose (>70%) yields at the more severe pretreatment conditions. We also found that the AQ charge was not a significant factor at the conditions studied, so efforts to reduce xylan and increase lignin solubilization using this compound were not successful. Lastly, while good lignin solubilization was achieved, effectively recovering this stream remains a challenge, and demonstrating performance in continuous reactors is still needed.},
doi = {10.1021/acssuschemeng.5b01041},
journal = {ACS Sustainable Chemistry & Engineering},
number = 3,
volume = 4,
place = {United States},
year = {2015},
month = {12}
}

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Works referenced in this record:

Comparative sugar recovery and fermentation data following pretreatment of poplar wood by leading technologies
journal, March 2009

  • Wyman, Charles E.; Dale, Bruce E.; Elander, Richard T.
  • Biotechnology Progress, Vol. 25, Issue 2
  • DOI: 10.1002/btpr.142

Energy, wealth, and human development: Why and how biomass pretreatment research must improve
journal, July 2012

  • Dale, Bruce E.; Ong, Rebecca G.
  • Biotechnology Progress, Vol. 28, Issue 4
  • DOI: 10.1002/btpr.1575

Coordinated development of leading biomass pretreatment technologies
journal, December 2005


Summary of findings from the Biomass Refining Consortium for Applied Fundamentals and Innovation (CAFI): corn stover pretreatment
journal, June 2009


Comparative sugar recovery data from laboratory scale application of leading pretreatment technologies to corn stover
journal, December 2005


A bioethanol process development unit: initial operating experiences and results with a corn fiber feedstock
journal, January 2004


Lignin Valorization: Improving Lignin Processing in the Biorefinery
journal, May 2014

  • Ragauskas, A. J.; Beckham, G. T.; Biddy, M. J.
  • Science, Vol. 344, Issue 6185, p. 1246843-1246843
  • DOI: 10.1126/science.1246843

Lignin as a base material for materials applications: Chemistry, application and economics
journal, March 2008


Life cycle assessment of corn grain and corn stover in the United States
journal, January 2009

  • Kim, Seungdo; Dale, Bruce E.; Jenkins, Robin
  • The International Journal of Life Cycle Assessment, Vol. 14, Issue 2
  • DOI: 10.1007/s11367-008-0054-4

Monitoring switchgrass composition to optimize harvesting periods for bioenergy and value-added products
journal, September 2013


A new method for stabilizing softwood kraft lignin fibers for carbon fiber production
journal, October 2012

  • Norberg, Ida; Nordström, Ylva; Drougge, Rickard
  • Journal of Applied Polymer Science, Vol. 128, Issue 6
  • DOI: 10.1002/app.38588

Oxidative stabilisation of kraft lignin for carbon fibre production
journal, February 2012

  • Brodin, Ida; Ernstsson, Marie; Gellerstedt, Göran
  • Holzforschung, Vol. 66, Issue 2
  • DOI: 10.1515/HF.2011.133

Kraft Lignin-Based Rigid Polyurethane Foam
journal, July 2012


Improved Lignin Polyurethane Properties with Lewis Acid Treatment
journal, May 2012

  • Chung, Hoyong; Washburn, Newell R.
  • ACS Applied Materials & Interfaces, Vol. 4, Issue 6
  • DOI: 10.1021/am300425x

Targeted down-regulation of cytochrome P450 enzymes for forage quality improvement in alfalfa (Medicago sativa L.)
journal, November 2005

  • Reddy, M. S. S.; Chen, F.; Shadle, G.
  • Proceedings of the National Academy of Sciences, Vol. 102, Issue 46
  • DOI: 10.1073/pnas.0505749102

Improved Sugar Conversion and Ethanol Yield for Forage Sorghum (Sorghum bicolor L. Moench) Lines with Reduced Lignin Contents
journal, August 2009


Loosening lignin's grip on biofuel production
journal, July 2007

  • Chapple, Clint; Ladisch, Michael; Meilan, Rick
  • Nature Biotechnology, Vol. 25, Issue 7, p. 746-748
  • DOI: 10.1038/nbt0707-746

Solvent fractionation of renewable woody feedstocks: Organosolv generation of biorefinery process streams for the production of biobased chemicals
journal, October 2011


Biomass Fractionation for the Biorefinery: Heteronuclear Multiple Quantum Coherence–Nuclear Magnetic Resonance Investigation of Lignin Isolated from Solvent Fractionation of Switchgrass
journal, September 2011

  • Bozell, Joseph J.; O'Lenick, C. J.; Warwick, Stacy
  • Journal of Agricultural and Food Chemistry, Vol. 59, Issue 17
  • DOI: 10.1021/jf201850b

Impact of high biomass loading on ionic liquid pretreatment
journal, January 2013

  • Cruz, Alejandro G.; Scullin, Chessa; Mu, Chen
  • Biotechnology for Biofuels, Vol. 6, Issue 1
  • DOI: 10.1186/1754-6834-6-52

Comparison of dilute acid and ionic liquid pretreatment of switchgrass: Biomass recalcitrance, delignification and enzymatic saccharification
journal, July 2010


Dissolution of Cellose with Ionic Liquids
journal, May 2002

  • Swatloski, Richard P.; Spear, Scott K.; Holbrey, John D.
  • Journal of the American Chemical Society, Vol. 124, Issue 18, p. 4974-4975
  • DOI: 10.1021/ja025790m

Distillable Acid-Base Conjugate Ionic Liquids for Cellulose Dissolution and Processing
journal, May 2011

  • King, Alistair W. T.; Asikkala, Janne; Mutikainen, Ilpo
  • Angewandte Chemie International Edition, Vol. 50, Issue 28
  • DOI: 10.1002/anie.201100274

Networks with large solvent recycle: Dynamics, hierarchical control, and a biorefinery application
journal, July 2011

  • Jogwar, Sujit S.; Torres, Ana I.; Daoutidis, Prodromos
  • AIChE Journal, Vol. 58, Issue 6
  • DOI: 10.1002/aic.12708

Biomass pretreatment: Fundamentals toward application
journal, November 2011


The impacts of deacetylation prior to dilute acid pretreatment on the bioethanol process
journal, January 2012

  • Chen, Xiaowen; Shekiro, Joseph; Franden, Mary Ann
  • Biotechnology for Biofuels, Vol. 5, Issue 1
  • DOI: 10.1186/1754-6834-5-8

Improved Xylan Hydrolysis of Corn Stover by Deacetylation with High Solids Dilute Acid Pretreatment
journal, December 2011

  • Chen, Xiaowen; Shekiro, Joseph; Elander, Rick
  • Industrial & Engineering Chemistry Research, Vol. 51, Issue 1
  • DOI: 10.1021/ie201493g

Development of a high-throughput method to evaluate the impact of inhibitory compounds from lignocellulosic hydrolysates on the growth of Zymomonas mobilis
journal, December 2009


Inhibition of growth of Zymomonas mobilis by model compounds found in lignocellulosic hydrolysates
journal, January 2013

  • Franden, Mary Ann; Pilath, Heidi M.; Mohagheghi, Ali
  • Biotechnology for Biofuels, Vol. 6, Issue 1
  • DOI: 10.1186/1754-6834-6-99

Electron Transfer Reactions in Pulping Systems (I): Theory and Applicability to Anthraquinone Pulping
journal, January 1985


Dissolving Reactions of Anthraquinone at High Temperatures
journal, January 1986

  • Storgard-envall, Carola; Dimmed, Donald R.
  • Journal of Wood Chemistry and Technology, Vol. 6, Issue 3
  • DOI: 10.1080/02773818608085233

Electron Transfer Reactions in Pulping Systems (II): Electrochemistry of Anthraquinone/Lignin Model Quinonemethides
journal, January 1985

  • Dinmel, Donald R.; Perry, Lois F.; Palasz, Peter D.
  • Journal of Wood Chemistry and Technology, Vol. 5, Issue 1
  • DOI: 10.1080/02773818508085179

Lignin and Lignans
book, August 2010


Alkaline Pretreatment of Corn Stover: Bench-Scale Fractionation and Stream Characterization
journal, May 2014

  • Karp, Eric M.; Donohoe, Bryon S.; O’Brien, Marykate H.
  • ACS Sustainable Chemistry & Engineering, Vol. 2, Issue 6, p. 1481-1491
  • DOI: 10.1021/sc500126u

Enzymatic Conversion of Xylan Residues from Dilute Acid-Pretreated Corn Stover
journal, July 2012

  • Shekiro, Joseph; Kuhn, Erik M.; Selig, Michael J.
  • Applied Biochemistry and Biotechnology, Vol. 168, Issue 2
  • DOI: 10.1007/s12010-012-9786-5

Two-Stage Dilute-Acid Pretreatment of Softwoods
journal, January 2000

  • Nguyen, Quang A.; Tucker, Melvin P.; Keller, Fred A.
  • Applied Biochemistry and Biotechnology, Vol. 84-86, Issue 1-9
  • DOI: 10.1385/ABAB:84-86:1-9:561

Characterization of Lignins Isolated from Alkali Treated Prehydrolysate of Corn Stover
journal, April 2013


Cellulose solvent-based biomass pretreatment breaks highly ordered hydrogen bonds in cellulose fibers of switchgrass
journal, November 2010

  • Sathitsuksanoh, Noppadon; Zhu, Zhiguang; Wi, Sungsool
  • Biotechnology and Bioengineering, Vol. 108, Issue 3
  • DOI: 10.1002/bit.22964

Dilute-Sulfuric Acid Pretreatment of Corn Stover in Pilot-Scale Reactor: Investigation of Yields, Kinetics, and Enzymatic Digestibilities of Solids
journal, January 2003

  • Schell, Daniel J.; Farmer, Jody; Newman, Millie
  • Applied Biochemistry and Biotechnology, Vol. 105, Issue 1-3, p. 69-86
  • DOI: 10.1385/ABAB:105:1-3:69

The effects of lignin removal and drying on the porosity and enzymatic hydrolysis of sugarcane bagasse
journal, August 2013

  • Junior, Celso Santi; Milagres, Adriane Maria Ferreira; Ferraz, André
  • Cellulose, Vol. 20, Issue 6
  • DOI: 10.1007/s10570-013-0032-2

    Works referencing / citing this record:

    Effects of Corn Stover Pretreated with NaOH and CaO on Anaerobic Co-Digestion of Swine Manure and Corn Stover
    journal, December 2018

    • You, Zhaoyang; Zhang, Shujuan; Kim, Hyunook
    • Applied Sciences, Vol. 9, Issue 1
    • DOI: 10.3390/app9010123

    A review of the potential of pretreated solids to improve gas biofuels production in the context of an OFMSW biorefinery: A review of the potential of pretreated solids
    journal, October 2016

    • Romero-Cedillo, Leticia; Poggi-Varaldo, Hector M.; Ponce-Noyola, Teresa
    • Journal of Chemical Technology & Biotechnology, Vol. 92, Issue 5
    • DOI: 10.1002/jctb.5116

    Comparative analysis of key technologies for cellulosic ethanol production from Brazilian sugarcane bagasse at a commercial scale
    journal, March 2019

    • Chandel, Anuj K.; Albarelli, Juliana Q.; Santos, Diego T.
    • Biofuels, Bioproducts and Biorefining, Vol. 13, Issue 4
    • DOI: 10.1002/bbb.1990