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DOE OSTI2022

Opportunities for Utilization of Low-Cost Algae Resources: Techno-Economic Analysis Screening for Near-Term Deployment (Parts 1 and 2)

This report presents a comprehensive techno-economic analysis (TEA) for the production, collection, or procurement of several low-cost algae resources that may otherwise be considered "waste" biomass materials today, as well as the utilization of these materials through exemplary conversion processes to produce renewable fuels and chemicals. In contrast to conventional TEA models attributed to large-scale algae "farming" approaches, which may be able to produce substantially more biomass and thus fuels/products at a national scale in the future, this assessment focuses on understanding opportunities and costs for such "waste" algal biomass resources as may be available at considerably lower cost today. Economics for base case assumptions and a range of sensitivity scenarios are presented, employing conversion technologies that are simple and well understood, and thus may be deployed at smaller community scale in the near term, as a means to support and expand a nascent algae industry on the way to employing a larger commercial algae farm approach for commodity-scale production. Specifically, three algal biomass resources are considered in this assessment, as may be sourced from (1) municipal wastewater treatment (WWT) utilizing algae in place of more conventional technologies for nitrogen/phosphorus removal, (2) collection and removal of harmful algal bloom (HAB) biomass as proliferates in certain inland water bodies, and (3) procurement of residual biomass following commercial lipid extraction (EXT) operations performed at smaller scale by industry today focused on higher-value nutraceutical applications. These three resources are evaluated through two conversion pathways: (1) combined algal biomass processing (CAP) through a simple/low-complexity configuration, and (2) anaerobic digestion (AD). The CAP pathway produces liquid fuels and chemical coproducts (polymer for off-site upgrading to bioplastics), whereas the AD pathway produces biogas (specifically renewable natural gas [RNG]) and crop fertilizer coproducts. To streamline the discussion, this report is broken into two sections: Part 1 focuses on WWT-derived biomass, and Part 2 on HAB and EXT biomass.

09 BIOMASS FUELS↗

DOE OSTI2021

Microalgae Conversion to Biofuels and Biochemical via Sequential Hydrothermal Liquefaction (SEQHTL) and Bioprocessing: 2020 State of Technology

A preliminary techno-economic analysis (TEA) was developed for the fiscal year 2020 state of technology (SOT) assessment to evaluate the benefits and risks for a large-scale microalga hydrothermal liquefaction (HTL) system based on most recent testing results. The focus of the study is directed toward the conversion system, which consists of five processes: two-stage sequential HTL (SEQHTL), biocrude upgrading to final fuels, bioprocessing for co-product generation, hydrogen generation, and steam cycle. In this system, algae biomass with corn stover supplement during the lower algae productivity seasons (winter, fall, and spring) to match the maximum algae seasonal production rate in summer is employed to maintain a constant plant capacity in all the seasons. Algae only (summer season) or algae/corn stover blended feedstock (other seasons) are sent to a two-stage SEQHTL process. In stage I, the carbohydrates in the feedstock are extracted and separated from the residual solid. The residual solid from stage I is further converted to biocrude in the SEQHTL stage II step. The biocrude is upgraded to final fuel products in an upgrading process. The extract stream from HTL stage I is sent to the bioprocessing section for co-product generation via fermentation of carbohydrate. Lactic acid (LA) is assumed to be the co-product based on current bioprocessing testing results.

09 BIOMASS FUELS↗

DOE OSTI2024

Multi-stage pretreatment of hydrothermal liquefaction biocrude oil as a precursor for sustainable aviation fuel production

Not Available

09 BIOMASS FUELS↗

DOE OSTI2020

Influence of Ag metal dispersion on the thermal conversion of ethanol to butadiene over Ag-ZrO 2 /SiO 2 catalysts

Atomistic scale models were developed and coupled with experimental investigation to deliver a functional understanding of catalytic activity and selectivity in the conversion of ethanol to 1,3-butadiene over Ag/ZrO 2 /SiO 2 . A detailed evaluation of the structural and electronic properties of the resultant catalyst models led to the identification of critical active sites of the catalyst. More importantly, the extent of Ag dispersion on the SiO 2 support and relative proximity to ZrO 2 were found to vary with the oxidation state of Ag and local coordination environment (Ag-O SiO2 ) allowing for critical control of ethanol conversion towards butadiene or ethylene. Simulations revealed that less dispersed or clustered Ag contain predominantly Ag 0 charge state and promote conversion of ethanol to ethylene. The well-dispersed Ag/ZrO 2 /SiO 2 catalyst instead contain a larger fraction of cationic Ag δ+ , and predominantly promote ethanol dehydrogenation and subsequent production of butadiene. The theoretical insights drawn were validated and confirmed experimentally using TEM, XRD and reactivity measurements demonstrating the effect of Ag dispersion on the selectivity of ethanol conversion.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Tailored Bioblendstocks with Low Environmental Impact to Optimize MCCI Engines (Final Technical Report)

09 BIOMASS FUELS↗

DOE OSTI2020

Tailored Bioblendstocks with Low Environmental Impact to Optimize MCCI Engines

The overall objective of the project is to develop and demonstrate a microalgae bio-blendstock with greater than 60% greenhouse gas reduction potential relative to petroleum diesel, that can reduce sooting propensity, increase cetane number and improve engine thermal efficiency relative to a baseline diesel engine operating on conventional fuel. Specific objectives include: (1) development of a new framework for both LCA and TEA that explicitly considers temporal variation in productivity and the frequency of crop loss; (2) determination of how fuel compounds that can be produced from the algal biomass can be ‘bio-tailored’ based on the species composition and biological production process, and subsequent processing via HTL to biocrude, and upgrading of the biocrude; (3) execution of a feedback loop (algae production  biocrude refining  combustion optimization  feedback to refining stage), for optimization of fuels for MCCI combustion; (4) optimization of MCCI combustion and emissions performance, accounting first for the biological processes that dictate the chemical composition of biocrude oil, and second for the subsequent chemical processes that comprise mixing controlled compression ignition combustion; (6) simulation of MCCI engine combustion processes to demonstrate the incorporation of relevant fuel chemistry that captures the specific impacts of optimized algal fuels.

09 BIOMASS FUELS↗

DOE OSTI2026

Postanaerobic Digestion Manure Fibers as a Renewable Source of Lignin-Derived Aromatic Compounds for Microbial Upgrading

Abstract Postanaerobic digestion manure fibers are an abundant solid residue that remains underutilized. The substantial lignocellulosic content of digested manure opens the possibility of using it as a renewable resource for producing valuable products. In this study, we performed compositional and nuclear magnetic resonance analyses to determine lignin content and aromatic composition of these fibers. Additionally, alkaline-based treatment and reductive catalytic fractionation were evaluated as two different processes to produce aromatic-rich streams. The liquor from the alkaline treatment was subsequently utilized for microbial upgrading to produce 2-pyrone-4,6-dicarboxylic acid (PDC). The results showed that lignin in manure fibers represents 30% of the biomass (dry weight basis), with a ∼26% abundance of β-ether-linked aromatics and ∼13% p-coumarate moieties, indicating that the amount of lignin in the postanaerobic biomass is comparable to a moderately pretreated plant biomass. The alkaline treatment released 5.6 g aromatics/kg fibers, while reductive catalytic fractionation produced 14.0 g aromatics/kg fibers. A bioreactor operated in fed-batch mode produced a yield of ∼1 mol of PDC/mol measured aromatics at a rate of 0.2 g PDC/L·h and a titer of 2.6 g PDC/L. This study demonstrates how postanaerobic digestion manure fibers could be used in a circular bioeconomy by harnessing their lignocellulosic content to extract aromatic compounds and use them for obtaining valuable chemicals via microbial upgrading.

Riascos, Brayan D. [University of Wisconsin-Madiso↗

DOE OSTI2022

Standard Analytical Methods for Pyrolysis Bio-Oils

There has been significant recent interest in the production of renewable fuels and chemicals from biomass and waste feedstocks. Pyrolysis pathways produce a liquid bio-oil product, which must be processed further, or upgraded, to yield fuel or chemical products. Bio-oils are very complex and often unstable samples, and research and development on upgrading processes needs reliable analytical information. In particular, chemical characterization techniques are needed to quantify both functional groups and individual compounds present in bio-oils. Reliable analytics are also needed to enable the bioenergy industry, as industrial facilities often have different analytical needs and capabilities than research facilities. In this presentation, we will discuss the development of a suite of standard analytical methods for pyrolysis bio-oils. Analytical methods to be discussed include: Determination of Carbon, Hydrogen, Nitrogen, and Oxygen in bio-oils; Accelerated Aging of Fast Pyrolysis Bio-oil using Carbonyl Titration; Determination of Water Content in Bio-oils by Volumetric Karl Fischer Titration; Determination of Carbon Functional Groups; Elemental Analysis of Bio-oils by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) - Na, K, Mg, Ca, S, P, and Fe; Determination of Phenolic Groups in Bio-oils using Revised Folin-Ciocalteu Methods: Single Cuvette and Plate Reader; Corrosivity of Bio-oils: Screening Test using Metal Leaching; Determination of Biogenic Content by 14C Measurement using Liquid Scintillation Counter. These new analytical methods are publicly available as Laboratory Analytical Procedures (https://www.nrel.gov/bioenergy/bio-oil-analysis.html), along with previously developed standard methods: GC-MS, Acid Titration, Carbonyl Titration, and 31P NMR. Additionally, the development of diffusion ordered NMR for characterization of bio-oil molecular weight will be discussed. Collectively, this suite of analytical methods represents the most comprehensive set of standard methods available for pyrolysis bio-oils. These standard methods are commonly used by the bioenergy community, and provide reliable information that enables research, scaleup, and industrial processing of biomass to produce renewable fuels and chemicals.

analytical↗

DOE OSTI2023

DOE Bioenergy Technologies Office (BETO) 2023 Project Peer Review: WBS 2.4.1.100 Bench Scale Research & Development

Bench Scale Integration develops and optimizes fermentation processes to produce bio-based fuels and chemicals for commercial scale-up. The project uses fermentation science to achieve high titers and production rates by, for example, manipulating how the microorganisms are fed biomass sugars and nutrients, modifying fermentation conditions (pH, temperature, aeration) or developing online control strategies for better fermentation operations and high titer, rates, and yield (TRY). For this period of performance, we continued our development of a commercial-ready 2,3-butanediol (BDO) fermentation from biomass sugars utilizing NREL's proprietary Zymomonas mobilis microorganism. The engineered Z. mobilis can use all the main sugars in corn stover biomass, which are glucose, xylose, and arabinose. BDO is a versatile, low-carbon chemical which can be catalytically upgraded to a variety of hydrocarbon fuels and chemicals. The project had three goals during this review period; evaluate the technical feasibility of using whole slurry pretreated corn stover to achieve the techno-economic analysis (TEA) performance goals, continue optimizing a liquor-based fed-batch fermentation process for high titer, and develop strategies to enable scale-up. After evaluating different iterations of a whole slurry fermentation that did not meet the TEA goals, a Go/No-Go decision was made to pivot to liquor-only with new TEA performance targets, the main one being 140 g/L titer. We successfully met this goal, producing 141 g/L BDO at 1 g/L-hr productivity and 84% process yield. This titer and productivity attracted industrial interest to scale the fermentation resulting in a Technology Commercialization Fund project award in 2022. We used an NREL developed near-infra red (NIR) spectroscopy method for rapid analysis which allowed for changes to aeration levels and sugar feeding during the fermentation to maximize BDO production. The NIR analysis can be done using a hand-held spectrometer, essentially taking the analysis on to the plant floor during scale-up and preliminary work shows the feasibility of using an online probe for continuous monitoring and control. The other scale-up tool is mapping oxygen transfer coefficient (kLa) and oxygen transfer rate (OTR) in various vessels to find conditions that match the optimized 500 mL vessels. Showing a correlation to the mapping work, which is done with water and a dissolved oxygen probe, can reduce the risk of failed fermentations during scale-up. Our end-of-project goal is to meet the design target BDO titer (140-150 g/L) from DMR corn stover liquor at 1000L or larger scale to demonstrate BDO process design case and transfer the technology to industrial fermentation stakeholders for commercialization.

2 3-butanediol↗

DOE OSTI2021

Upgrading of C1 Building Blocks

This project is developing the centerpiece technology for a market-responsive, integrated biorefinery concept based on the conversion of renewable C1 intermediates (e.g., syngas, CO2, methanol) to a suite of fuels and co-products with improved carbon efficiency, reduced capital expense, and control of the product distribution to meet market demand. Advanced upgrading technologies of syngas are critically needed for the successful commercialization of fuel production at a scale relevant for biomass gasification. Research tasks within this project leverage complementary catalyst and process design for the conversion of CO2-rich syngas (15-20% CO2 in syngas) to achieve high carbon yields of gasoline and jet fuels as the major products. The conversion pathways generate high quality fuels (e.g., high octane gasoline with low aromatics, desirable jet-range hydrocarbons), and potential to achieve favorable cost targets by 2022. Research progress is compared against the Mobil Olefin to Gasoline and Distillate (MOGD) process, which also offers control over the gasoline and distillate products, as an industrial benchmark. The pathway for direct conversion of CO2-rich syngas to hydrocarbon fuels seeks to exceed the carbon efficiency of biomass-sourced MOGD (31.8%). Recent catalyst and process development achievements are highlighted by improvements in carbon-selectivity to fuels and carbon yields, along with evidence of incorporation of carbon from CO2 into the hydrocarbon products.

bioenergy↗

DOE OSTI2023

A Machine Learning Model for Predicting Composition of Catalytic Coprocessing Products from Molecular Beam Mass Spectra

Demand for the development of an automated and integrated refining process for biofuels has increased in recent years due to the lack of generalized process inspection tools. In bio-oil upgrading processes, all process variables are maintained based on the offline specification of intermediates and products. A lack of real-time product specifications in batch-wise monitoring can cause process failure and wasted resources. Therefore, there is a need for a fast and accurate intermediates/product specification tool that can be used for real-time specification to reduce waste and mitigate the risk of process failure. Here, to address this gap, we developed a machine learning (ML) model for predicting speciated bio-oil composition, including paraffin, iso-paraffins, olefins, naphthene, and aromatics. The model is trained using the mass spectra from upgraded products collected in the vapor phase before condensation and predicts the composition of the condensed product. Training ML models using raw mass spectra is challenging due to numerous overlapped peaks originating from different parent compounds. With this in mind, we propose a protocol that (i) transforms raw mass spectra to chemistry-inspired predefined features and (ii) trains decision tree-based models using these features. Our results show that the random forest model was robust against overfitting and had the highest accuracy compared to other models. Moreover, a stochastic ablation method determined the eight most significant features while maximizing the accuracy. Our protocol facilitates real-time compositional analysis of upgraded bio-oils and thus real-time process monitoring. Additionally, this protocol enables the rational design of efficient catalysts and the determination of optimal process conditions.

09 BIOMASS FUELS↗

DOE OSTI2024

Phenotypic and genomic characterization of Methanothermobacter wolfeii strain BSEL, a CO 2 -capturing archaeon with minimal nutrient requirements

A new variant of Methanothermobacter wolfeii was isolated from an anaerobic digester using enrichment cultivation in anaerobic conditions. Here, the new isolate was taxonomically identified via 16S rRNA gene sequencing and tagged as M. wolfeii BSEL. The whole genome of the new variant was sequenced and de novo assembled. Genomic variations between the BSEL strain and the type strain were discovered, suggesting evolutionary adaptations of the BSEL strain that conferred advantages while growing under a low concentration of nutrients. M. wolfeii BSEL displayed the highest specific growth rate ever reported for the wolfeii species (0.27 ± 0.03 h –1 ) using carbon dioxide (CO 2 ) as unique carbon source and hydrogen (H 2 ) as electron donor. M. wolfeii BSEL grew at this rate in an environment with ammonium (NH 4 + ) as sole nitrogen source. The minerals content required to cultivate the BSEL strain was relatively low and resembled the ionic background of tap water without mineral supplements. Optimum growth rate for the new isolate was observed at 64°C and pH 8.3. In this work, it was shown that wastewater from a wastewater treatment facility can be used as a low-cost alternative medium to cultivate M. wolfeii BSEL. Continuous gas fermentation fed with a synthetic biogas mimic along with H 2 in a bubble column bioreactor using M. wolfeii BSEL as biocatalyst resulted in a CO 2 conversion efficiency of 97% and a final methane (CH 4 ) titer of 98.5%v, demonstrating the ability of the new strain for upgrading biogas to renewable natural gas.

09 BIOMASS FUELS↗

DOE OSTI2022

Developing a High Value Chemical Coproduct: Bio-Base Insecticides from Catalytic Fast Pyrolysis

Coproduction of biochemicals from the thermochemical conversion of biomass is a strategy to reduce biofuel costs and improve bio-oil quality in an integrated biorefinery. (Challenge) Cost effective separations of coproducts from thermochemical conversion streams remains a challenge largely due to the heterogenous nature and stability of thermochemical conversion streams. (Solution) Bio-based insecticides isolated from catalytic fast pyrolysis (CFP) oils are a viable coproduct that can overcome the oil is more stable, they are a high value product, and they can remain a mixture of components. (Approach) This work focuses on the development of a bio-based insecticide coproduct that is distilled from a catalytic fast pyrolysis bio-oil produced using a platinum on titanium dioxide (Pt/TiO2) catalyst to upgrade pyrolysis vapors.

BIOMASS FUELS↗

DOE OSTI2020

TAILORED BIOBLENDSTOCKS WITH LOW ENVIRONMENTAL IMPACT TO OPTIMIZE MCCI ENGINES

09 BIOMASS FUELS↗

DOE OSTI2021

Process Intensification and Scale-Up of a Continuous Enzymatic Hydrolysis and Separation Process

Combining separate unit operations into one where the best of each part can be maximized is one of the benefits of process intensification. An example is the combination of lignocellulosic biomass enzymatic hydrolysis with the downstream solid-liquid separation step to produce clarified sugars ready for fermentation or catalytic upgrading. The productivity and endpoint yield of enzymatic hydrolysis both enjoy the benefits of reduced feedback inhibition through the continuous removal of sugars by incorporating separations into the reactor. Likewise, the efficiency of recovering clarified sugars from the enzymatic hydrolysis slurry can be enhanced by operating separations equipment at steady-state conditions simultaneously with the continuously fed hydrolysis process. A key parameter that enables greater processing capacity while also raising the risks of failure is the solids loading or concentration. Higher solids loading allows for smaller reactor vessels and results in clarified sugars of higher concentration; however, required pumping power increases, reactor agitation may become ineffective, and membrane flux suffers. Feedstock material attributes influenced by upstream pretreatment must also be scrutinized more carefully: dilute-acid pretreated and deacetylated-and-disc-refined feedstocks exhibit different characteristics that affect agitation and pumping. The authors invite you to further explore the process science enabling the scale-up of this technology from conceptual work at the bench to pilot-scale industrially-relevant equipment where the challenges and solutions of integration and process optimization are expounded upon.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

DOE OSTI2021

Computational Fluid Dynamics Modeling to Simulate a Combined Reforming Process for Syngas and Hydrogen Production

An Oxygen Transport Membrane (OTM) combined reforming technology for producing syngas and hydrogen integrates the advantages of multiple processes—steam methane reforming (SMR), autothermal reforming (ATR), an air separation unit (ASU)—into a single integrated technology. The OTM consists of a primary reforming tube, in which desulfurized natural gas is partially reformed by steam at high pressure in the presence of a metal catalyst. This process is followed in series by a ceramic OTM with a secondary reformer, in which residual methane reforms and O 2 - ions react with a portion of the CO and H 2 fuel to provide the heat to support both primary and secondary reforming. Although the OTM combined reformer technology for syngas and H 2 production has been substantially developed in the last decade, several challenges that affect the overall production efficiency and reliability are yet to be fully understood, addressed, and resolved. Therefore, developing Computational Fluid Dynamics (CFD) models that incorporate fluid dynamics, mass transport, kinetics, heat transport, and structural mechanics is critical to understanding and minimizing the probability of tube failures during the startup and operation. In this report, an exhaustive literature review was performed to survey the current state of technology for producing syngas and H 2 using either conventional or renewable energy sources. The feedstocks reviewed include natural gas and coal for the conventional technologies, whereas biomass, solar, wind, and nuclear energy for the renewable technologies. The existing industry-grade COMSOL multiphysics models of OTM were upgraded for the latest software release. In addition, they were improved to help achieve grid and solver independence and were successfully ported on the ORNL high-performance computing clusters to speed up their run times. A 42% reduction in the simulation run time was achieved. A new higher-fidelity CFD model of an OTM tube was developed in the StarCCM+ simulation platform. This new model was designed to simulate various physics using first principles, e.g., turbulent flow, heat transfer, and chemical reactions while avoiding unnecessary simplifications. The resulting predictions were qualitatively assessed and provided useful insights into the multiphysics complexity of an OTM tube.

08 HYDROGEN↗

DOE OSTI2020

Response of Pseudomonas putida to Complex, Aromatic-Rich Fractions from Biomass

There is strong interest in the valorization of lignin to produce valuable products; however, its structural complexity has been a conversion bottleneck. Chemical pretreatment liberates lignin-derived soluble fractions that may be upgraded by bioconversion. Here, cholinium ionic liquid pretreatment of sorghum produced soluble, aromatic-rich fractions that were converted by Pseudomonas putida (P. putida), a promising host for aromatic bioconversion. Growth studies and mutational analysis demonstrated that P. putida growth on these fractions was dependent on aromatic monomers but unknown factors also contributed. Proteomic and metabolomic analyses indicated that these unknown factors were amino acids and residual ionic liquid; the oligomeric aromatic fraction derived from lignin was not converted. A cholinium catabolic pathway was identified, and the deletion of the pathway stopped the ability of P. putida to grow on cholinium ionic liquid. This work demonstrates that aromatic-rich fractions obtained through pretreatment contain multiple substrates; conversion strategies should account for this complexity.

09 BIOMASS FUELS↗

DOE OSTI2021

Pilot-scale hydrotreating of catalytic fast pyrolysis biocrudes: process performance and product analysis

Catalytic fast pyrolysis (CFP) is a technology option for producing advanced biofuels from hydrocarbon-rich biocrude intermediates. The relatively high oxygen content of biocrudes compared to petroleum intermediates increases hydrogen consumption and the lower thermal stability accelerates catalyst deactivation and reactor fouling hindering the adaptation of hydrotreating technology for biocrude upgrading into biofuels. In this study, four chemically different biocrude feeds were upgraded in a pilot scale hydroprocessing unit at similar process conditions using a commercial hydrodeoxygenation (HDO) catalyst. The biocrude feeds and hydrotreated products were characterized using standard ASTM procedures and advanced analytical techniques (GCxGC-FID and GCxGC-MS). HDO catalyst activity was monitored by changes in physical properties and chemical composition of the upgraded products as a function of time on stream. Aliphatic acids, ketones, aldehydes, and furan derivatives were completely converted during the hydrotreating tests while the concentration of aromatics, aliphatic hydrocarbons and phenolics increased during the hydrotreating tests. The oxygen content, nitrogen content, specific gravity, viscosity and the heavy end of the boiling point range (determined by simulated distillation) of the upgraded products increased with increasing time on stream during hydrotreating. The deactivation rate was the lowest for the biocrude feed that contained the most aliphatic and aromatic hydrocarbons and was the highest for the biocrude feed that had the most anhydrosugars. Overall, the HDO deactivation rate correlates with the total amount of oxygen in the feed (17 wt% to 29 wt%, on a wet basis).

09 BIOMASS FUELS↗