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At least 433 records · Page 24

Titania Deposition on PMR-15

The formation, degree of crystallinity and adherence of dense titania (TiO2) thin film coatings on a high-temperature polyimide resin (PMR-15) can be influenced by the chemical composition of the polymer surface. Furthermore, solution deposition conditions can be adjusted to provide additional control over the morphology and crystallinity of the titania films. Recipes for solution-based titania deposition that used a slowly-hydrolyzing titanium fluoride salt in the presence of boric acid as a fluoride scavenger allowed growth of films up to 750 nm thick in 22 h. By adjusting solution pH and temperature, either amorphous titania or oriented crystalline anatase films could be formed. Surface sulfonate groups enhance the adhesion of solution-deposited oxide thin film coatings. While most sulfonation procedures severely damaged the PMR-15 surface, the use of chlorosulfonic acid followed by hydrolysis of the installed chlorosulfonyl groups provided effective surface sulfonation without significant surface damage. In some cases, the oxide deposition solution caused partial hydrolysis of the polymer surface, which itself was sufficient to allow adhesion of the titania film through chelation of titanium ions by exposed benzoic acid groups on the polymer surface.

Meador, Mary B.↗

Hematite Spherules in Basaltic Tephra Altered Under Aqueous, Acid-Sulfate Conditions on Mauna Kea Volcano, Hawaii: Possible Clues for the Occurrence of Hematite-Rich Spherules in the Burns Formation at Meridiani Planum, Mars

Iron-rich spherules (>90% Fe2O3 from electron microprobe analyses) approx.10-100 microns in diameter are found within sulfate-rich rocks formed by aqueous, acid-sulfate alteration of basaltic tephra on Mauna Kea volcano, Hawaii. Although some spherules are nearly pure Fe, most have two concentric compositional zones, with the core having a higher Fe/Al ratio than the rim. Oxide totals less than 100% (93-99%) suggest structural H2O and/or /OH. The transmission Moessbauer spectrum of a spherule-rich separate is dominated by a hematite (alpha-Fe2O3) sextet whose peaks are skewed toward zero velocity. Skewing is consistent with Al(3+) for Fe(3+) substitution and structural H2O and/or /OH. The grey color of the spherules implies specular hematite. Whole-rock powder X-ray diffraction spectra are dominated by peaks from smectite and the hydroxy sulfate mineral natroalunite as alteration products and plagioclase feldspar that was present in the precursor basaltic tephra. Whether spherule formation proceeded directly from basaltic material in one event (dissolution of basaltic material and precipitation of hematite spherules) or whether spherule formation required more than one event (formation of Fe-bearing sulfate rock and subsequent hydrolysis to hematite) is not currently constrained. By analogy, a formation pathway for the hematite spherules in sulfate-rich outcrops at Meridiani Planum on Mars (the Burns formation) is aqueous alteration of basaltic precursor material under acid-sulfate conditions. Although hydrothermal conditions are present on Mauna Kea, such conditions may not be required for spherule formation on Mars if the time interval for hydrolysis at lower temperatures is sufficiently long.

Morris, R. V.↗

The Formation of Fe/Mg Smectite Under Mildly Acidic Conditions on Early Mars

The detection of Fe/Mg smectites and carbonate in Noachian and early Hesperian terrain of Mars has been used to suggest that neutral to mildly alkaline conditions prevailed during the early history of Mars. However, if early Mars was neutral to moderately alkaline with a denser CO2 atmosphere than today, then large carbonates deposits should be more widely detected in Noachian terrain. The critical question is: Why have so few carbonate deposits been detected compared to Fe/Mg smectites? We suggest that Fe/Mg smectites on early Mars formed under mildly acidic conditions, which would inhibit the extensive formation of carbonate deposits. The goal of this work is to evaluate the formation of Fe/Mg smectites under mildly acidic conditions. The stability of smectites under mildly acidic conditions is attributed to elevated Fe/Mg activities that inhibit smectite dissolution. Beidelite and saponite have been shown to form from hydrothermal alteration of basaltic glass at pH 3.5-4.0 in seawater solutions. Nontronite is also known to be stable in mildly acidic systems associated with mafic and ultramafic rock. Nontronite was shown to form in acid sulfate soils in the Bangkok Plain, Thailand due to oxidation of Fe-sulfides that transformed saponite to nontronite. Smectite is known to transform to kaolinite in naturally acid soils due to selective leaching of Mg. However, if Mg removal is limited, then based on equilibrium relationships, the dissolution of smectite should be minimized. If Fe and Mg solution activities are sufficiently high, such as might be found in a low water/rock ratio system that is poorly drained, smectite could form and remain stable under mildly acidic conditions on Mars. The sources of mild acidity on early Mars includes elevated atmospheric CO2 levels, Fe-hydrolysis reactions, and the presence of volcanic SO2 aerosols. Equilibrium calculations dictate that water equilibrated with an early Mars CO2 atmosphere at 1 to 4 bar yields a pH of 3.6 to 3.9. Fe hydrolysis reactions on Mars is another source of protons that would have contributed to acidity. The presence of SO2 from volcanic processes could also have contributed to geochemical acidification. These sources of acidity competed with base-forming cations that resulted in mildly acidic solutions that were not favorable for carbonate formation but may have allowed for Fe/Mg smectite formation. Noachian to early Hesperian Mars could have been mildly acidic, allowing Fe/Mg smectite formation but preventing widespread carbonate deposition. This paradigm shift from an early Mars that was neutral-alkaline to mildly acidic may possibly explain why there is a disparity between the occurrence of carbonate and Fe/Mg smectites. Potential microbiological activity would not be eliminated under a mildly acidic Mars; however, there could be tighter constraints as to the type and species of microbiology that could exist.

Sutter, Brad↗

Strategies for Stabilizing Nitrogenous Compounds in ECLSS Wastewater: Top-Down System Design and Unit Operation Selection with Focus on Bio-Regenerative Processes for Short and Long Term Scenarios

Water recycling and eventual nutrient recovery is crucial for surviving in or past low earth orbit. New approaches and syste.m architecture considerations need to be addressed to meet current and future system requirements. This paper proposes a flexible system architecture that breaks down pretreatment , steps into discrete areas where multiple unit operations can be considered. An overview focusing on the urea and ammonia conversion steps allows an analysis on each process's strengths and weaknesses and synergy with upstream and downstream processing. Process technologies to be covered include chemical pretreatment, biological urea hydrolysis, chemical urea hydrolysis, combined nitrification-denitrification, nitrate nitrification, anammox denitrification, and regenerative ammonia absorption through struvite formation. Biological processes are considered mainly for their ability to both maximize water recovery and to produce nutrients for future plant systems. Unit operations can be considered for traditional equivalent system mass requirements in the near term or what they can provide downstream in the form of usable chemicals or nutrients for the long term closed-loop ecological control and life support system. Optimally this would allow a system to meet the former but to support the latter without major modification.

Lunn, Griffin M.↗

Effect of Solution pH and Chloride Concentration on Akaganeite Precipitation: Implications for Akaganeite Formation on Mars

Akaganeite (Beta-FeOOH, chloride-containing Fe(III) (hydr)oxide) has been recently discovered on the surface of Mars by the Mars Science Laboratory Curiosity rover in Yellowknife Bay, Gale Crater, Mars [1] and from orbit by the Mars Reconnaissance Orbiter in Robert Sharp crater and Antoniadi basin [2]. However, the mechanism and aqueous environmental conditions of akaganeite formation (e.g., pH and chloride concentration) remain unknown. We have investigated formation of akaganeite through Fe(III) hydrolysis at variable initial pH and chloride concentrations. The formed Fe(III) precipitates were characterized by instruments similar to instruments on Mars robotic spacecraft. Syntheses were performed through hydrolysis of Fe(III) perchlorate with addition of Na cloride (Fe/Cl ratio between 0.5 and 5) and at initial pH of 1.5, 2, 4, 6 and 8 at 90degC. X-ray diffraction analysis revealed formation of akaganeite alone or in mixture with goethite, hematite and ferrihydrite at all initial pHs and Fe/Cl ratio between 0.5 and 2 while akaganeite precipitated only at pH 1.5 and Fe/Cl greater than2. Chloride content of akaganeite was affected by initial pH and decreased from 20-60 mg/g at pH 1.5 to less than 0.1 mg/g at pH 8. The synthesized akaganeite samples were also characterized by Mössbauer and infrared spectroscopy and volatiles were analysed by thermal and evolved gas analysis. The obtained characterization data will be compared to published data from rover and orbital missions [1-3] to determine martian akaganeite composition, crystallinity and formation conditions.

Peretyazhko, T. A.↗

Titan's Ionospheric Chemistry, Fullerenes, Oxygen, Galactic Cosmic Rays and the Formation of Exobiological Molecules on and Within Its Surfaces and Lakes

We discuss the formation of aerosols within Titan's thermosphere-ionosphere and the different chemical pathways. Negative ion measurements by the Cassini Plasma Spectrometer (CAPS) Electron Spectrometer (ELS) give evidence for formation of unsaturated anion carbon chains, while positive ion measurements of the Cassini Ion Neutral Mass Spectrometer (INMS) indicate formation of more aromatic cation hydrocarbons. There is presently no direct observational evidence for large neutral molecule growth in Titan's thermosphere-ionosphere. The hydrocarbon cations are expected to form Polycyclic Aromatic Hydrocarbons (PAHs), those with the addition of nitrogen being called PAHNs. We theorize anion carbon chains can eventually become long enough to fold into fullerene C60,70 carbon shells, of various charge states. Based on laboratory data the fullerenes can trap incoming O+ magnetospheric ions that have relatively high energy collisions with the fullerenes and, once trapped, protect the oxygen atom from Titan's reducing thermosphere-ionosphere. The fullerenes can form into larger onion fullerenes and condense into larger embryo aerosols (i.e., m/q (mass-to-charge ratio) greater than 10,000 amu/q (atomic mass unit-to-charge ratio) anions as observed by CAPS/ELS) eventually falling onto Titan's surface and precipitating to the bottom of its hydrocarbon lakes. Molecule production composed of H, C, N is known to occur in Titan's atmosphere with energy input from the magnetosphere, solar UV (ultraviolet), and deep-penetrating irradiation from galactic cosmic rays (GCR). Space radiation effects by GCR irradiation of Titan's surface and lakes can lead to the manufacture of exobiological molecules with oxygen as the new ingredient. We have developed a model of galactic cosmic ray irradiation of Titan's atmosphere, surface, subsurface and bottoms of Titan lakes. GCR would provide further energy for processing of the aerosols into more complex organic forms such as tholins and precursor molecules for amino acids. A second process called hydrolysis then converts the precursor molecules into amino acids. Hydrolysis is provided via meteor impacts with size greater than 10 kilometers and cryovolcanism both which can produce liquid water on Titan's surface for episodic periods more than several 100 to 1000 years. Our model shows that GCR secondary particles can penetrate ~100 meters below the ice surface (including the bottom of Titan's less dense hydrocarbon lakes ~150-meter depths) and produce chemically significant dosages over very long timescales ~450 million years. The GCR model is combined with laboratory data from experiments in which dry methyl ices were irradiated to doses producing prebiotic amino acids such as glycine. The model calculations show glycine can form to ~2.5 parts-per-billion levels near the surface after ~450 million years of GCR proton irradiation and potentially to 5 parts-per-billion if heavy-ion GCRs up through Fe are included. If such molecules were detected, this would not only confirm this model but indicate that life forms different from ours may not be required.

Edward C. Sittler Jr↗

Titan's Ionospheric Chemistry, Fullerenes, Oxygen, Galactic Cosmic Rays and the Formation of Exobiological Molecules on and within its Surfaces and Lakes

We discuss the formation of aerosols within Titan's thermosphere-ionosphere and the different chemical pathways. Negative ion measurements by the Cassini Plasma Spectrometer (CAPS) Electron Spectrometer (ELS) give evidence for formation of unsaturated anion carbon chains, while positive ion measurements of the Cassini Ion Neutral Mass Spectrometer (INMS) indicate formation of more aromatic cation hydrocarbons. There is presently no direct observational evidence for large neutral molecule growth in Titan's thermosphere-ionosphere. The hydrocarbon cations are expected to form Polycyclic Aromatic Hydrocarbons (PAH), those with the addition of nitrogen being called PAHNs. We theorize anion carbon chains can eventually become long enough to fold into fullerene C(60,70) carbon shells, of various charge states. Based on laboratory data the fullerenes can trap incoming O(sup +) magnetospheric ions that have relatively high energy collisions with the fullerenes and, once trapped, protect the oxygen atom from Titan's reducing thermosphere-ionosphere. The fullerenes can form into larger onion fullerenes and condense into larger embryo aerosols (i.e., m/q > 10,000 amu/q anions as observed by CAPS/ELS) eventually falling onto Titan's surface and precipitating to the bottom of its hydrocarbon lakes. Molecule production composed of H, C, N is known to occur in Titan's atmosphere with energy input from the magnetosphere, solar UV, and deeppenetrating irradiation from galactic cosmic rays (GCR). Space radiation effects by GCR irradiation of Titan's surface and lakes can lead to the manufacture of exobiological molecules with oxygen as the new ingredient. We have developed a model of galactic cosmic ray irradiation of Titan's atmosphere, surface, subsurface and bottoms of Titan lakes. GCR would provide further energy for processing of the aerosols into more complex organic forms such as tholins and precursor molecules for amino acids. A second process called hydrolysis then converts the precursor molecules into amino acids. Hydrolysis is provided via meteor impacts with size > 10 km and cryovolcanism both which can produce liquid water on Titan's surface for episodic periods > several 100 to 1000 years. Our model shows that GCR secondary particles can penetrate ~ 100 m below the ice surface (including the bottom of Titan's less dense hydrocarbon lakes ~ 150 m depths) and produce chemically significant dosages over very long timescales ~ 450 Myrs. The GCR model is combined with laboratory data from experiments in which dry methyl ices were irradiated to doses producing prebiotic amino acids such as glycine. The model calculations show glycine can form to ~ 2.5 ppb levels near the surface after ~450 Myrs of GCR proton irradiation and potentially to 5 ppb if heavy-ion GCRs up through Fe are included. If such molecules were detected, this would not only confirm this model but indicate that life forms different from ours may not be required.

Edward C. Sittler Jr↗

Radiocatalyst for Radiation Protection and Microbial Control

Radiocatalysts are materials that reduce the activation energy required to split water into hydrogen and reactive oxygen species (ROS). They are activated by radiation and can be used to improve the ability of water to act as a radiation barrier. This paper reports the results of an experimental evaluation of a gold radiocatalyst. This work provides a preliminary evaluation of the ability of these types of catalysts to increase the efficiency of water hydrolysis when exposed to different types of radiation (GCR). Although the radiation exposure devices used in this testing were not capable of generating radiation as diverse as is commonly found in space, the testing is useful in evaluating the function of these radiocatalytic nanoparticles when exposed to a a subset of the types of radiation that are found in GCR. The results are relevant to evaluating the use of this material for both space radiation protection and the production of useful byproducts, such as ROS, which can be used to maintain the sterility of stored water supplies. Radiocatalysts are materials typically used in radiation cancer therapy to improve the kill rate of tumors. These nanoparticles can be directly injected into tumors or functionalized to enter tumor cells via the blood stream. When they are exposed to radiation, they produce ROS. ROS are water hydrolysis products such as OH¯, O¯, O3, H2O2. This study used radiocatalytic 1.8 nm gold nanoparticles functionalized with citrate. These nanoparticles were tested through exposure to Xrays, 56Fe particles and gamma rays to demonstrate activity to a variety of radiation sources. The results demonstrate that radiocatalysts can improve the radiation absorption of water by a factor of 3 to 8 and can effectively kill bacteria at radiation levels above 1 Gy.

radiocatalyst radiation protection biocide↗

Limitations in Representation of Physical Processes Prevents Successful Simulation of PM2.5 During KORUS-AQ

High levels of fine particulate matter (PM2.5) pollution in East Asia often exceed local air quality standards. Observations from the Korea United States-Air Quality (KORUS-AQ) field campaign in May and June 2016 showed that development of extreme pollution (haze) occurred through a combination of long-range transport and favorable meteorological conditions that enhanced local production of PM2.5. Atmospheric models often have difficulty simulating PM2.5 chemical composition during haze, which is of concern for the development of successful control measures. We use observations from KORUS-AQ to examine the ability of the GEOS-Chem chemical transport model to simulate PM2.5 composition throughout the campaign and identify the mechanisms driving the pollution event. At the surface, the model underestimates sulfate by -64% but overestimates nitrate by +36%. The largest underestimate in sulfate occurs during the pollution event, where models typically struggle to generate elevated sulfate concentrations due to missing heterogeneous chemistry in aerosol liquid water in the polluted boundary layer. Hourly surface observations show that the model nitrate bias is driven by an overestimation of the nighttime peak. In the model, nitrate formation is limited by the supply of nitric acid, which is biased by +100% against aircraft observations. We hypothesize that this is due to a large missing sink, which we implement here as a factor of five increase in dry deposition. We show that the resulting increased deposition velocity is consistent with observations of total nitrate as a function of photochemical age. The model does not account for factors such as the urban heat island effect or the heterogeneity of the built-up urban landscape resulting in insufficient model turbulence and surface area over the study area that likely results in insufficient dry deposition. Other species such as NH3 could be similarly affected but were not measured during the campaign. Nighttime production of nitrate is driven by NO2 hydrolysis in the model, while observations show that unexpectedly elevated nighttime ozone (not present in the model) should result in N2O5 hydrolysis as the primary pathway. The model is unable to represent nighttime ozone due to an overly rapid collapse of the afternoon mixed layer and excessive titration by NO. We attribute this to missing nighttime heating driving deeper nocturnal mixing that would be expected to occur in a city like Seoul. This urban heating is not considered in air quality models run at large enough scales to treat both local chemistry and long-range transport. Key model failures in simulating nitrate, mainly overestimated daytime nitric acid, incorrect representation of nighttime chemistry, and an overly shallow and insufficiently turbulent nighttime mixed layer, exacerbate the model’s inability to simulate the buildup of PM2.5 during haze pollution. To address the underestimate in sulfate most evident during the haze event, heterogeneous aerosol uptake of SO2 is added to the model which previously only considered aqueous production of sulfate from SO2 in cloud water. Implementing a simple parameterization of this chemistry improves the model abundance of sulfate but degrades the SO2 simulation implying that emissions are underestimated. We find that improving model simulations of sulfate has direct relevance to determining local vs. transboundary contributions to PM2.5. During the haze pollution event, the inclusion of heterogeneous aerosol uptake of SO2 decreases the fraction of PM2.5 attributable to long-range transport from 66% to 54%. Locally-produced sulfate increased from 1% to 25% of locally-produced PM2.5, implying that local emissions controls would have a larger effect than previously thought. However, this additional uptake of SO2 is coupled to the model nitrate prediction which affects the aerosol liquid water abundance and chemistry driving sulfate-nitrate-ammonium partitioning. An additional simulation of the haze pollution with heterogeneous uptake of SO2 to aerosol and simple improvements to the model nitrate simulation results in 30% less sulfate due to 40% less nitrate and aerosol water, and results in an underestimate of sulfate during the haze event. Future studies need to better consider the impact of model physical processes such as dry deposition and nighttime boundary layer mixing on the simulation of nitrate and the effect of improved nitrate simulations on the overall simulation of secondary inorganic aerosol (sulfate+nitrate+ammonium) in East Asia. Foreign emissions are rapidly changing, increasing the need to understand the impact of local emissions on PM2.5 in South Korea to ensure continued air quality improvements.

Katherine R. Travis↗

Evaluating the Feasibility of Higher Titers and Yields for 2,3-Butanediol Production to Achieve the Biofuel Industry Economic Goal of Under $3.50 GGE

To achieve the economic goal of producing biofuels that can compete with petroleum-based products, we increased titers of 2,3-butanediol (BDO) production. BDO has many advantages over ethanol; including lower toxicity, higher heat of capacity, and is a precursor to various valuable applications. To produce BDO for fuel upgrading, we have genetically modified Zymomonas mobilis (YC-1). Several materials and feed strategies were evaluated to determine the best titer and economic feasibility. Titers from DMR corn stover in a batch process were in the range of 70-80 g/L. The fully hydrolyzed material was easy to work with but suffered from dilution issues. We pushed the concentration of solids to above 25% w/w and were met with numerous challenges. This included an initial sugar concentration above 150 g/L, the high solid concentration altered the oxygen mass transfer rate and affected which products were produced, and the fermentation conditions were not optimal for the enzyme. Despite these challenges, our current results yielded 100 g/L of upgradeable products (70 g/L BDO and 30 g/L acetoin) and 83% fermentation process yield. However, the poor enzymatic hydrolysis yield of 64%, unconverted xylose, and the high acetoin levels warrant further exploration for optimization. Using unhydrolyzed solids as the feed material, we achieved titers in the range of 75-95 g/L BDO. The raw solids feed, though operationally more challenging to work with, proved to be promising as the rate of hydrolysis promoted co-utilization of the sugars. We reached 150 g/L BDO using concentrated DDR liquors under boules and continuous feeding strategies. The clarified liquors showed high titers, high productivity, high yield, and high sugar utilization with little drawback operationally. The target goal of under $3.50 GGE was achieved in several feeding strategies. Scale-up feasibility has also been demonstrated at the 100L scale using both whole slurry and liquor hydrolysates.

BIOMASS FUELS↗

The solubility of thorium in carbonate-bearing solutions at hydrothermal conditions

Thorium mineralization is frequently hosted in carbonate-bearing rocks, and thorium commonly substitutes into the structures of carbonate-bearing minerals that have precipitated from or been modified by hydrothermal fluids. Given this common association, it is reasonable to consider the hypothesis that the presence of carbonate ligands in hydrothermal solutions promotes the transport of Th through the formation of stable aqueous complexes. Our ability to evaluate this hypothesis, however, is hindered by the lack of experimental data for Th-carbonate species at conditions beyond ambient. The low-temperature data indicate that carbonate is a strong complexing agent for Th. In this contribution, we investigate the solubility of Th in carbonate-bearing fluids relevant to natural systems (0.05–0.5 m NaHCO 3 /Na 2 CO 3 ; pH T ~ 7.8–9.8) at elevated temperature (175–250 °C). We demonstrate that, in contrast to the behavior of Th at low temperature, the stability of Th-carbonate complexes is not sufficient for them to predominate at these conditions. Instead, the solubility of Th is governed by hydrolysis reactions. Under the experimental conditions investigated, the predominant hydroxyl complexes are Th(OH) 4 0 and Th(OH) 5 -. Furthermore, thermodynamic formation constants were derived for these species at the temperatures considered in our experiments (log β 4 = 43.34 and 44.31 at 175 and 200 °C, respectively, and log β 5 = 46.15 and 47.9 at 225 and 250 °C, respectively) to permit forward modeling of Th mobility in natural systems. Our study indicates that carbonate ions are unlikely to play a role in transporting Th in hydrothermal fluids. Summarizing the results of this study and our previous studies of the solubility of Th in hydrothermal fluids, we conclude that SO 4 2- is the primary ligand responsible for the hydrothermal transport of Th.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Dihydroxyterephthalate—A Trojan Horse PET Counit for Facile Chemical Recycling

Abstract Here, low‐energy poly(ethylene terephthalate) (PET) chemical recycling in water: PET copolymers with diethyl 2,5‐dihydroxyterephthalate (DHTE) undergo selective hydrolysis at DHTE sites, autocatalyzed by neighboring group participation, is demonstrated. Liberated oligomeric subchains further hydrolyze until only small molecules remain. Poly(ethylene terephthalate‐ stat ‐2,5‐dihydroxyterephthalate) copolymers were synthesized via melt polycondensation and then hydrolyzed in 150–200 °C water with 0–1 wt% ZnCl 2 , or alternatively in simulated sea water. Degradation progress follows pseudo‐first order kinetics. With increasing DHTE loading, the rate constant increases monotonically while the thermal activation barrier decreases. The depolymerization products are ethylene glycol, terephthalic acid, 2,5‐dihydroxyterephthalic acid, and bis(2‐hydroxyethyl) terephthalate dimer, which could be used to regenerate virgin polymer. Composition‐optimized copolymers show a decrease of nearly 50% in the Arrhenius activation energy, suggesting a 6‐order reduction in depolymerization time under ambient conditions compared to that of PET homopolymer. This study provides new insight to the design of polymers for end‐of‐life while maintaining key properties like service temperature and mechanical properties. Moreover, this chemical recycling procedure is more environmentally friendly compared to traditional approaches since water is the only needed material, which is green, sustainable, and cheap.

36 MATERIALS SCIENCE↗

Moving from residual lignocellulosic biomass into high–value products: Outcomes from a long–term international cooperation

Major progress in the bioprocessing of lignocellulose to fuels and value-added chemicals has created the possibility of a low carbon-footprint economy. However, the current complexity and associated costs of lignocellulose conversion result in a higher price for ethanol than for fossil fuels. The cost of cellulosic ethanol production will be lowered by further progress in development of biorefinery technology that produces both ethanol and high-value chemicals with bio-based products that are beginning to penetrate consumer markets in the USA, Brazil, and worldwide. The cost-effectiveness of low carbon-footprint bioproducts will benefit from advances in supplying large amounts of biomass solids to the biorefinery. We describe here outcomes from a successful long-term international cooperation between the Laboratory of Renewable Resources Engineering (LORRE) at Purdue University in the United States and Brazil's Agricultural Research Corporation (EMBRAPA) and Federal University of Sâo Carlos (UFSCar), which has contributed practical pathways to enhance the biorefinery concept. Furthermore, this paper gives an overview of developments that address fundamental knowledge of lignocellulosic biomass pretreatment hydrolysis under optimized operational conditions and bioreactor configurations, and the science and engineering that contributes to the effective production of fuel and ethanol and value-added products from biomass.

09 BIOMASS FUELS↗

Macroscale Control of Reactivity using 3D Printed Materials with Intrinsic Catalytic Properties

The morphology of heterogeneous catalysts can impact their performance. However, standard manufacturing methods like extrusion or pelleting offer little options for tailoring catalyst shape. Herein, stereolithographic 3D printing is used to produce catalysts with controlled topologies to enhance their performance. A series of magnetic stir-bar compartments (SBC) were 3D printed and tested as catalysts for sucrose hydrolysis. The SBC were printed using acrylic acid (AA) and 1,6-hexanediol diacrylate (HDDA) as acid sites and hydrophobic crosslinking domains, respectively. Variations in the number and tilt direction of the SBC blades produced significant changes in their apparent catalytic activities. These changes resulted from differences in the fraction of active surface effectively interacting with the reactants in solution, as revealed by computational fluid dynamics simulations. Moreover, varying HDDA:AA ratios in SBC regulated reactant-surface interactions to control catalytic activity. Overall, 3D printing catalysts enables quick performance optimization by simultaneously controlling macroscopic structure and molecular composition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Production of xylose enriched hydrolysate from bioenergy sorghum and its conversion to β-carotene using an engineered Saccharomyces cerevisiae

A new bioprocess has been created that allows for producing β-carotene from the xylose portion of bioenergy sorghum. Bioenergy sorghum was pretreated in a pilot-scale continuous hydrothermal reactor followed by disc refining. Xylose was extracted using low-severity dilute acid hydrolysis. A xylose yield of 64.9% (17.4 g/L) was obtained by hydrolyzing at 120 °C for 5 min with 2% sulfuric acid. The xylose-enriched syrup was separated and concentrated to either 32 g xylose/L (medium-concentrated hydrolysate, MCB) or 66 g xylose/L (high-concentrated hydrolysate, HCB). The non- (NCB), medium-, and high-concentrated xylose syrup were neutralized and fermented to β-carotene using Saccharomyces cerevisiae strain SR8B, which had been engineered for xylose utilization and β-carotene production. In HCB, MCB, and NCB cultures, the yeast produced β-carotene titers of 114.50 mg/L, 93.56 mg/L, and 82.50 mg/L, which corresponds to specific yeast biomass productions of 7.32 mg/g DCW, 8.10 mg/g DCW, and 8.29 mg/g DCW, respectively.

09 BIOMASS FUELS↗

Utilization of guaiacol-based deep eutectic solvent for achieving a sustainable biorefinery

This study proposed a renewable deep eutectic solvent (DES) pretreatment using lignin-derived guaiacol as the hydrogen bond donor. The DES showed excellent biomass fractionation efficiency after the incorporation of trace AlCl 3 as the reinforcer, which removed 79.1 % lignin while preserving more than 90 % glucan. The pretreated bamboo exhibited 96.2 % glucan enzymatic hydrolysis yield at only 110 °C. The physicochemical properties of the pretreated solids were comprehensively investigated to explain how the DES fractionation overcame the biomass recalcitrance. The regenerated lignin from the DES pretreatment was also analyzed, which revealed that lignin β-O-4 bond was significantly cleaved. In conclusion, this guaiacol-based DES could greatly contribute to establish a closed-loop biorefinery sequence with high lignin fractionation efficiency and great solvent recyclability.

09 BIOMASS FUELS↗

Biocompatible organosolv fractionation via a novel alkaline lignin-first strategy towards lignocellulose valorization

Simultaneous valorization of both carbohydrate and lignin fractions in lignocellulose remains a great challenge. Herein, a novel lignin-first strategy using triethylene glycol (TEG) under alkaline conditions for effective biomass fractionation producing highly digestible carbohydrates and reactive lignin was developed. Delignification was over 80% and fermentable sugar yields were close to 90% after pretreatment at 90°C. The biocompatibility of TEG allowed direct enzymatic hydrolysis of the solid residue without washing, thus minimizing wastewater generation. Furthermore, the obtained lignin (TEGL) had an uncondensed structure with well-preserved β-O-4 linkage, leading to near-equal aromatic monomer yields compared to cellulolytic enzyme lignin after catalytic-free pyrolysis, demonstrating high valorization potential. Finally, the proposed TEG solvent system is promising for a green and sustainable biorefinery process to achieve the complete utilization of lignocellulose.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗