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Integrated Two-Stage Alkaline-Oxidative Pretreatment of Hybrid Poplar. Part 1: Impact of Alkaline Pre-Extraction Conditions on Process Performance and Lignin Properties

Journal Article · · Industrial and Engineering Chemistry Research
 [1];  [2];  [3];  [4];  [4];  [3];  [5]
  1. Montana State Univ., Bozeman, MT (United States); Michigan State University
  2. Montana State Univ., Bozeman, MT (United States)
  3. Michigan State Univ., East Lansing, MI (United States)
  4. Univ. of Wisconsin, Madison, WI (United States)
  5. Montana State Univ., Bozeman, MT (United States); Luleå Univ. (Sweden)

We previously demonstrated that a two-stage pretreatment comprising of an alkaline pre-extraction followed by a Cu-catalyzed alkaline–oxidative treatment is effective at pretreating hardwoods under relatively mild reaction conditions. In this work, we focus on characterizing how biomass source and reaction conditions used during the alkaline pre-extraction impact the subsequent processing stages as well as lignin yields and properties. Specifically, three hybrid poplars were subjected to the first stage alkaline pre-extraction under various conditions including differences in time (15–300 min), temperature (95–155 °C), and alkali loadings (50–200 mg NaOH/g biomass), and the impact on total mass solubilization, lignin recovery, and lignin purity was determined. Empirical correlations were developed between reaction conditions and mass solubilization and lignin recovery during the pre-extraction stage. For select conditions, lignin properties were assessed and include β-O-4 content determined by 13C NMR, molecular mass distributions as determined by gel permeation chromatography, and susceptibility to depolymerization to aromatic monomers using thioacidolysis and formic acid catalyzed depolymerization. We found alkaline pre-extraction performed at higher temperatures generated lignins exhibiting lower contamination by polysaccharides, lower aromatic monomer yields from depolymerization, lower molar masses, and lower β-O-4 contents relative to the lower temperature pre-extractions. Lastly, the pre-extracted biomass from select conditions was assessed for its response to the subsequent Cu-catalyzed alkaline–oxidative treatment and enzymatic hydrolysis. It was demonstrated that minor differences in delignification during pre-extraction have quantifiable impacts on the subsequent efficacy of the second stage of pretreatment and enzymatic hydrolysis with improved lignin removal during the first pre-extraction stage resulting in improved hydrolysis yields.

Research Organization:
Michigan State Univ., East Lansing, MI (United States)
Sponsoring Organization:
USDOE Office of Energy Efficiency and Renewable Energy (EERE)
Grant/Contract Number:
EE0008148; SC0018409
OSTI ID:
1877690
Alternate ID(s):
OSTI ID: 1612971
Journal Information:
Industrial and Engineering Chemistry Research, Journal Name: Industrial and Engineering Chemistry Research Journal Issue: 35 Vol. 58; ISSN 0888-5885
Publisher:
American Chemical Society (ACS)Copyright Statement
Country of Publication:
United States
Language:
English

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Figures / Tables (7)