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At least 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Lignin-First Biorefinery Development

Cost-effective biomass fractionation is an enabling, grand challenge for biorefining, especially when both carbohydrates and lignin are targeted for valorization. The advent of Reductive Catalytic Fractionation (RCF) - an active stabilization approach that solubilizes lignin from biomass and catalytically depolymerizes it into a narrow slate of monomers and oligomers - represents a potential step forward for this important goal. In the Lignin-First Biorefinery Development project, we are employing techno-economic analysis (TEA) and life cycle assessment (LCA) to guide bench-scale R&D efforts towards cost-effective RCF-based biorefining. This project is critical to lignin valorization efforts and could enable the use of woody feedstocks in a traditional biochemical conversion context. To date, we have conducted the first rigorous TEA and LCA study of the RCF process, developed a flow-through system to separate biomass and the chemical catalyst in RCF chemistry, developed models for solvolysis chemistry and transport phenomena for poplar, and co-led an international, authoritative perspective on guidelines for the research community on how to best practice lignin-first biorefining. The primary challenges for the lignin-first RCF process going forward are catalyst stability, the need to utilize, recover, and recycle high boiling point solvents to lower RCF reactor pressure, and the challenge of operating RCF continuously - all of which are being directly tackled by this project.

biomass↗
DOE OSTI2020

Lignin extraction and upgrading using deep eutectic solvents

Deep eutectic solvents (DESs) are a class of green solvents exhibiting low vapor pressure, high thermal stability,low toxicity, and biodegradability. These features make them attractive solvents for lignocellulosic biomassprocessing, especially for lignin valorization. DESs not only solubilize lignin from lignocellulose biomass, butalso confer extracted lignin with properties favorable to its further upgrading. This review summarizes recentadvances in biomass fractionation using DESs for lignin extraction. It also covers lignin upgrading in DESs interms of depolymerization and functionalization. The challenges of tailoring lignin properties by DESs for differentvalorization routes are also discussed.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

A new approach to zip–lignin: 3,4–dihydroxybenzoate is compatible with lignification

Renewed interests in the development of bioenergy, biochemicals, and biomaterials have elicited new strategies for engineering the lignin of biomass feedstock plants. Furthermore, this study shows, for the first time, that 3,4-dihydroxybenzoate (DHB) is compatible with the radical coupling reactions that assemble polymeric lignin in plants. We introduced a bacterial 3-dehydroshikimate dehydratase into hybrid poplar (Populus alba × grandidentata) to divert carbon flux away from the shikimate pathway, which lies upstream of lignin biosynthesis. Transgenic poplar wood had up to 33% less lignin with p-hydroxyphenyl units comprising as much as 10% of the lignin. Mild alkaline hydrolysis of transgenic wood released fewer ester-linked p-hydroxybenzoate groups than control trees, and revealed the novel incorporation of cell-wall-bound DHB, as well as glycosides of 3,4-dihydroxybenzoic acid (DHBA). Two-dimensional nuclear magnetic resonance (2D-NMR) analysis uncovered DHBA-derived benzodioxane structures suggesting that DHB moieties were integrated into the lignin polymer backbone. In addition, up to 40% more glucose was released from transgenic wood following ionic liquid pretreatment and enzymatic hydrolysis. This work highlights the potential of diverting carbon flux from the shikimate pathway for lignin engineering and describes a new type of ‘zip-lignin’ derived from the incorporation of DHB into poplar lignin.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2025

Integrated Biorefinery of Brewer’s Spent Grain for Second-Generation Ethanol, Mycoprotein, and Bioactive Vinasse Production

Brewer’s spent grain (BSG), the main lignocellulosic by-product of the beer industry, represents an abundant yet underutilized resource with high potential for valorization. This study presents an integrated biorefinery approach to convert BSG into second-generation (2G) ethanol, bioactive vinasse for plant growth promotion, and fungal biomass as a potential mycoprotein source. The biomass was first subjected to biological delignification using the white-rot fungus Ganoderma lucidum, after which two valorization routes were explored: (i) evaluation of the fungal biomass as a mycoprotein candidate and (ii) alcoholic fermentation for ethanol production. For the latter, three pretreatment strategies were assessed (diluted sulfuric acid and two deep eutectic solvents (DESs) based on choline chloride combined with either glycerol or lactic acid) followed by a one-pot enzymatic saccharification and fermentation using Kluyveromyces marxianus SLP1. The highest ethanol yield on substrate (YP/S) was achieved with [Ch]Cl:lactic acid pretreatment (0.46 g/g, 89.32% of theoretical). Vinasse, recovered after distillation, was characterized for organic acid content and tested on Solanum lycopersicum seed germination, showing promising biostimulant activity. Overall, this work highlights the potential of BSG as a sustainable feedstock within circular economy models, enabling the production of multiple bio-based products from a single residue.

Ganoderma lucidum↗
DOE OSTI2023

Engineering Innovations, Challenges, and Opportunities for Lignocellulosic Biorefineries: Leveraging Biobased Polymer Production

Alternative polymer feedstocks are highly desirable to address environmental, social, and security concerns associated with petrochemical-based materials. Lignocellulosic biomass (LCB) has emerged as one critical feedstock in this regard because it is an abundant and ubiquitous renewable resource. LCB can be deconstructed to generate valuable fuels, chemicals, and small molecules/oligomers that are amenable to modification and polymerization. However, the diversity of LCB complicates the evaluation of biorefinery concepts in areas including process scale-up, production outputs, plant economics, and life-cycle management. We discuss aspects of current LCB biorefinery research with a focus on the major process stages, including feedstock selection, fractionation/deconstruction, and characterization, along with product purification, functionalization, and polymerization to manufacture valuable macromolecular materials. We highlight opportunities to valorize underutilized and complex feedstocks, leverage advanced characterization techniques to predict and manage biorefinery outputs, and increase the fraction of biomass converted into valuable products.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2020

Green chemistry design in polymers derived from lignin: review and perspective

The use of lignin for material and chemical applications has gained interest in recent times due to the environmental focus on using biomass for renewable materials as well as the motivation to valorize lignin as part of an integrated biorefinery. While a wealth of publications can be found for lignin-derived materials, and several reviews can be found on the topic, there are no reviews that outline and critically assess the sustainability of these protocols based on the criterion of the 12 Principles of Green Chemistry. This review assesses the literature for lignin- derived polymers over the past 20 years and highlights attempts to use biobased accompanying reagents, green solvents or solvent-less protocols, reports that replace traditionally toxic precursors (e.g. diisocyanates for polyurethanes), use mild conditions, valorize additional waste streams and prepare materials particularly biodegradable or recyclable. Here, the following work is a comprehensive and critical assessment of the green and sustainable nature of the state-of-the art of lignin-derived polymers (polyurethane, polyester, epoxy, phenolic resin, and others) utilizing actual biomass in the synthetic protocol. Each section of this review highlights and assesses published protocols that use a particularly green approach in one or more steps of the synthetic sequence. While many reports still contain traditional petroleum-derived and toxic methods along with more sustainable methods, the outline of all such green methods is able to create a landscape amidst lignin-derived polymer synthesis that points the way toward safer and more environmentally friendly materials.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Valorization of consolidated bioprocessing residues for bioplastics

This study demonstrates an organic solvent-free processing strategy to valorize consolidated bioprocessing (CBP) residues, from switchgrass and poplar biomass, into functional poly(butylene succinate) (PBS)-based biocomposites using high-shear homogenization (HSH). HSH transformed the switchgrass and poplar CBP residues (CBP-R) into fine, uniformly distributed particles and microfibers. The composites of PBS with homogenized switchgrass residues (H-CBP-R-SG) or homogenized poplar residues (H-CBP-R-P) at a 70/30 weight ratio exhibited improved processability and mechanical integrity, with the Young's modulus for the PBS/H-CBP-R-SG and PBS/H-CBP-R-P nearly doubling to 0.66 ± 0.07 GPa and 0.65 ± 0.04 GPa, respectively, compared to neat PBS (0.36 ± 0.02 GPa). Dynamic Mechanical Analysis (DMA) reveals a significant suppression of the tan δ peak magnitude, indicating that HSH-mediated physical activation facilitates stress transfer in composites typical of covalent chemical grafting systems. While the transition to a stiffness-dominated profile reduces ductility, the resulting composites exhibit the dimensional stability and resistance to thermal warping required for high-fidelity FDM 3D printing and injection molding. Beyond material performance, comprehensive techno-economic analysis (TEA) and life cycle assessment (LCA) confirmed that diverting CBP residues into composite products can improve the economic viability of the biorefinery without substantially increasing biorefinery global warming potential (GWP). At a 30 wt% blend ratio, incorporating residuals into PBS yielded a minimum selling price for the composite of $\$4.07$ per kg compared to the conventional bioplastic price of $\$5.00$ per kg. This approach aligns with circular bioeconomy principles by converting waste streams into value-added products. Furthermore, this innovative strategy addresses key challenges in bioplastic development, including cost, compatibility, and performance, while simultaneously advancing waste minimization strategies for sustainable manufacturing systems.

09 BIOMASS FUELS↗
DOE OSTI2020

Bio-Restore Workshop Summary Report

This report summarizes the results of a Bioenergy Technologies Office-sponsored public workshop held at Argonne National Laboratory on September 25–26, 2019. The purpose of the Bio-Restore Workshop was to bring together experts to discuss the current state of the technology and to identify data and R&D relevant to the bio-restore concept. Specific topics included using dedicated energy crops and other biomass sources to provide environmental benefits, implementing algae technologies (e.g., wastewater treatment, direct bloom harvest, turf scrubbers, macroalgae), quantifying and valorizing ecosystem services, developing low-cost sensors and data management systems, and integrating “bio-restore biomass” with supply chain needs. For the purposes of the workshop, the term “bio-restore biomass” refers to terrestrial and algal biomass that provides environmental benefits when produced or harvested. For terrestrial biomass, this primarily includes energy crops (herbaceous and woody), other cellulosic biomass, and waste biomass. For algal biomass, this includes wastewater treatment algal biomass, algal blooms, algal turf scrubbers/attached growth systems, and macroalgae. Types of biomass not of interest to the workshop discussions include oilseed crops, crops generally grown for food or feed, and algae grown in artificial light conditions or other energy-intensive cultivation designs.

09 BIOMASS FUELS↗
DOE OSTI2022

Lignin Utilization

Valorization of lignin has massive potential economic and sustainability benefits for the lignocellulosic biorefinery. However, challenges remain to realize lignin conversion to coproducts, especially related to selective, high yield depolymerization to monomers and quantitative analytics on lignin, the latter of which is critical for accurate process modeling. Towards these goals, the Lignin Utilization project focuses on catalytic lignin deconstruction chemistries for C-O and C-C bond cleavage, development of analytical chemistry techniques to quantitatively characterize lignin, and syntheses of requisite model compounds for understanding lignin transformations. This work is done with and supports multiple BETO projects, including the Biological Lignin Valorization (BLV) project, the Separations Consortium, and others. Outcomes of Lignin Utilization for analytics and synthesis include 1) development of new mass spectrometry (MS) methods to characterize lignin dimers/oligomers in process streams, 2) deployment of a computational-experimental tool (with Biochemical Process Modeling and Simulation) to identify lignin-derived compounds with high fidelity from MS, and 3) delivery of >40 unique compounds. From a catalysis perspective, we have developed new oxidative approaches to cleave C-O and C-C bonds and produce >50% bio-available aromatic monomers for biological funneling for the BLV project and have developed recoverable bases for base-catalyzed deconstruction of lignin.

BIOMASS FUELS↗
DOE OSTI2024

Sustainable aviation fuels from biomass and biowaste via bio- and chemo-catalytic conversion: Catalysis, process challenges, and opportunities

Sustainable aviation fuel (SAF) production from biomass and biowaste streams is an attractive option for decarbonizing the aviation sector, one of the most-difficult-to-electrify transportation sectors. Despite ongoing commercialization efforts using ASTM-certified pathways (e.g., lipid conversion, Fischer-Tropsch synthesis), production capacities are still inadequate due to limited feedstock supply and high production costs. New conversion technologies that utilize lignocellulosic feedstocks are needed to meet these challenges and satisfy the rapidly growing market. Combining bio- and chemo-catalytic approaches can leverage advantages from both methods, i.e., high product selectivity via biological conversion, and the capability to build C-C chains more efficiently via chemical catalysis. Herein, conversion routes, catalysis, and processes for such pathways are discussed, while key challenges and meaningful R&D opportunities are identified to guide future research activities in the space. Bio and chemo-catalytic conversion primarily utilize the carbohydrate fraction of lignocellulose, leaving lignin as a waste product. This makes lignin conversion to SAF critical in order to utilize whole biomass, thereby lowering overall production costs while maximizing carbon efficiencies. Thus, lignin valorization strategies are also reviewed herein with vital research areas identified, such as facile lignin depolymerization approaches, highly integrated conversion systems, novel process configurations, and catalysts for the selective cleavage of aryl C–O bonds. The potential efficiency improvements available via integrated conversion steps, such as combined biological and chemo-catalytic routes, along with the use of different parallel pathways, are identified as key to producing all components of a cost-effective, 100% SAF.

09 BIOMASS FUELS↗
DOE OSTI2021

Degradation of aromatic compounds and lignin by marine protist Thraustochytrium striatum

This paper aimed at studying a novel high biomass strain (HBS) of marine protist, Thraustochytrium striatum, for lignin valorization to lipids and carotenoids. In the screening of 15 aromatic compounds, T. striatum HBS can utilize most compounds while achieving the best growth on 3,4-dihydroxybenzoic acid (3,4-DHBA) and 4-hydroxybenzoic acid (4-HBA). The maximum cell mass concentration reached 2-3 g/L under 5 g/L of 3,4-DHBA or 2 g/L of 4-HBA, which was comparable to that under equivalent concentration of glucose. The long-chain fatty acids content was 13 % and 7 % with 3,4-DHBA and 4-HBA, respectively. The adoption of fed-batch fermentation mode improved the degradation of carbon source and prevented the inhibitory effect caused by overloading of aromatic compounds. Further, both final cellular fatty acids and carotenoids contents were doubled in the fermentation of 3,4-DHBA. T. striatum HBS exhibited limited lignin depolymerization (~24 %) ability on technical lignins.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2025

Lignin-Derived Phenolic Compounds and Water Are Effective Cosolvents for Reductive Catalytic Fractionation

Reductive catalytic fractionation (RCF) is an effective lignin-first biorefining method to extract lignin as a stabilized oil from lignocellulosic biomass. To realize RCF at scale, process modeling has shown that minimizing the use of exogenous organic solvents is critical. To this end, here we investigate the ability of lignin-derived monomers to act as either solvents or cosolvents for RCF. We begin by examining the influence of lignin-derived aromatic compounds (4-propylguaiacol, 4-propylphenol, and propylbenzene) on RCF monomer yields and subsequently extend our analysis to mixtures of 4-propylguaiacol and either methanol or water. Here, we demonstrate that 4-propylguaiacol is an effective solvent for lignin extraction and depolymerization during RCF, especially when used in combination with water as a cosolvent. Cosolvent mixtures of 4-propylguaiacol and water enable up to 81% lignin extraction, monomer yields up to 25 wt %, and postreaction phase separation. However, unlike methanol, water as a cosolvent fails to inhibit aromatic ring hydrogenation when conducted over Ru/C as a catalyst, potentially leading to excess hydrogen consumption in a process utilizing this approach. Nonetheless, these results suggest a promising strategy for eliminating external organic solvents from RCF by utilizing mixtures of lignin-derived compounds and water as alternative extraction solvents.

09 BIOMASS FUELS↗
DOE OSTI2020

Reductive catalytic fractionation of agricultural residue and energy crop lignin and application of lignin oil as antimicrobials

Cheap and abundant waste from bioethanol and agricultural processing industries are an alluring alternative feedstock for biorefineries. In this work, we employ reductive catalytic fractionation (RCF) to depolymerize, over Ru/C powder and Ru/Al 2 O 3 pellets, five herbaceous biomass feedstocks, namely corn stover, miscanthus, switchgrass, sugarcane bagasse, and wheat straw into phenolic monomers with high yields (~40 wt.% based on total (Klason + acid soluble) lignin and > 50 wt.% when stabilized using aldehydes), leaving behind a carbohydrate pulp residue. Interestingly, a polar solvent is sufficient to solubilize and fragment the lignin polymer into monomers without any catalyst. Here, contrary to woody biomass, where the monomer yields are positively correlated with the S-content of lignin, principal component analysis indicates that the monomer yields from herbaceous biomass depend on the content of lignin crosslinker – ferulate. Using NMR, we further identify α – 6 C-C linked oligomers formed from condensation reactions, explaining the unexpected low monomer yields of high β-O-4 herbaceous biomass. Recyclability experiments indicate that catalyst deactivation occurs through sintering, leaching, and fouling. Lignin oil from herbaceous biomass exhibits bacteriostatic effects against Staphylococcus aureus, highlighting a potential application in functional food development and as food or feed preservative.

09 BIOMASS FUELS↗
DOE OSTI2021

Protocols for isolating and characterizing polysaccharides from plant cell walls: a case study using rhamnogalacturonan-II

Abstract Background In plants, a large diversity of polysaccharides comprise the cell wall. Each major type of plant cell wall polysaccharide, including cellulose, hemicellulose, and pectin, has distinct structures and functions that contribute to wall mechanics and influence plant morphogenesis. In recent years, pectin valorization has attracted much attention due to its expanding roles in biomass deconstruction, food and material science, and environmental remediation. However, pectin utilization has been limited by our incomplete knowledge of its structure. Herein, we present a workflow of principles relevant for the characterization of polysaccharide primary structure using nature’s most complex polysaccharide, rhamnogalacturonan-II (RG-II), as a model. Results We outline how to isolate RG-II from celery and duckweed cell walls and from red wine using chemical or enzymatic treatments coupled with size-exclusion chromatography. From there, we applied mass spectrometry (MS)-based techniques to determine the glycosyl residue and linkage compositions of the intact RG-II and derived oligosaccharides including special considerations for labile monosaccharides. In doing so, we demonstrated that in the duckweed Wolffiella repanda the arabinopyranosyl (Ara p ) residue of side chain B is substituted at O- 2 with rhamnose. We used electrospray-MS techniques to identify non-glycosyl modifications including methyl-ethers, methyl-esters, and acetyl-esters on RG-II-derived oligosaccharides. We then showed the utility of proton nuclear magnetic resonance spectroscopy ( 1 H-NMR) to investigate the structure of intact RG-II and to complement the RG-II dimerization studies performed using size-exclusion chromatography. Conclusions The complexity of pectic polysaccharide structures has hampered efforts aimed at their valorization. In this work, we used RG-II as a model to demonstrate the steps necessary to isolate and characterize polysaccharides using chromatographic, MS, and NMR techniques. The principles can be applied to the characterization of other saccharide structures and will help inform researchers on how saccharide structure relates to functional properties in the future.

09 BIOMASS FUELS↗
DOE OSTI2022

Enabling Production of Algal Biofuels by Techno-Economic Optimization of Co-Product Suites

Recent techno-economic analysis (TEA) has underscored that for algal biofuels to be cost competitive with petroleum fuels, co-products are necessary to offset the cost of fuel production. The co-product suite must scale with fuel production while also maximizing value from the non-fuel precursor components. The co-product suite also depends on algal biomass composition, which is highly dynamic and depends on environmental conditions during cultivation. Intentional shifts in composition during cultivation are often associated with reduced biomass productivity, which can increase feedstock production costs for the algae-based biorefinery. The optimal algae-based biorefinery configuration is thus a function of many factors. We have found that comprehensive TEA, which requires the construction of process models with detailed mass and energy balances, along with a complete accounting of capital and operating expenditures for a commercial-scale production facility, provides invaluable insight into the viability of a proposed biorefinery configuration. This insight is reflected in improved viability for one biorefining approach that we have developed over the last 10 years, namely, the Combined Algal Processing (CAP) approach. This approach fractionates algal biomass into carbohydrate-, lipid-, and protein-rich fractions, and tailors upgrading chemistry to the composition of each fraction. In particular, transitioning from valorization of only the lipids to a co-product suite from multiple components of high-carbohydrate algal biomass can reduce the minimum fuel selling price (MFSP) from more than $8/gallon of gasoline equivalent (GGE) to $2.50/GGE. This paper summarizes that progress and discusses several surprising implications in this optimization approach.

09 BIOMASS FUELS↗
DOE OSTI2020

Synthesis and Characterization of Lignin-grafted-poly(ε-caprolactone) from Different Biomass Sources

Modification of lignin with poly(ε-caprolactone) is a promising approach to valorize industrial low-value lignins and to advance the bioeconomy. We have synthesized lignin grafted poly(ε-caprolactone) (lignin-g-PCL) copolymers via ring-opening polymerization of ε-caprolactone with different types of lignins of varying botanical sources (G-type pine lignin, S/G-type poplar lignin, and C-type Vanilla seeds lignin) and lignin extraction methods (Kraft and ethanol organosolv pulping). The lignin-g-PCL copolymer showed remarkably improved compatibility and dispersion in acetone, chloroform, and toluene in comparison to non-modified lignins. The structure and thermal properties of the lignin-g-PCL were investigated using Fourier-transform infrared spectroscopy (FTIR), 31 P nuclear magnetic resonance (NMR), 2D heteronuclear single quantum correlation (HSQC) NMR, gel permeation chromatography (GPC), and differential scanning calorimetry (DSC). Furthermore, we have found that all the technical lignins were reactive to the copolymerization reaction regardless of their plant source and isolation methods. The molecular weights of the synthesized lignin-g-PCL copolymers were positively correlated with the content of aliphatic lignin hydroxyls, suggesting that the copolymerization reaction tends to occur preferentially at the aliphatic hydroxyls rather than the phenolic hydroxyls of lignin. Thermal analyses of the lignin-g-PCL copolymers were studied, and in general, a reduction of melting temperature and crystallinity percentage in comparison to the neat PCL was observed. However, the thermal behavior of lignin-g-PCL copolymers varied depending on the lignin feedstocks employed in the copolymerization reaction.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2021

Integrated Biorefinery for Valorization of Engineered Bioenergy Crops—A Review

Biorefinery allows production of multiple bioproducts from various biomass and streams using suitable unit operations to improve the economics of process while minimizing waste generation. Biorefinery holds importance in the biofuel industry because multiple coproducts can allow to produce biofuels at a price which is competitive of fossil fuels. Newer generations of cellulosic biomasses are being developed to accumulate lipids and pigments. Such crops, which can be cultivated on land unsuitable for row crops, are aimed to provide drop-in fuels to reduce dependency on fossil fuels and food crops. This review describes the potential of recovery and value addition to different constituents of engineered crops besides producing drop-in fuels. As a result, the work also provides the market value of different products which can be obtained from engineered crops to make an informed decision.

09 BIOMASS FUELS↗