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DOE OSTI2025

Thermochemical conversion of waste plastics with coal and biomass to generate value-added products

Co-gasification of waste plastic and waste coal/biomass in steam was investigated to evaluate the effects of operating conditions and low-cost catalyst compositions of coal ash on syngas production and tar mitigation. The results demonstrate the benefits of waste plastic conversion with coal or biomass. A better understanding of these processes will facilitate the development of more accurate kinetic models for industrial-scale chemical recycling.

co-gasification↗

NASA NTRS1996

Effect of CO2 levels on nutrient content of lettuce and radish

Atmospheric carbon-dioxide enrichment is known to affect the yield of lettuce and radish grown in controlled environments, but little is known about CO2 enrichment effects on the chemical composition of lettuce and radish. These crops are useful model systems for a Controlled Ecological Life-Support System (CELSS), largely because of their relatively short production cycles. Lettuce (Lactuca sativa L.) cultivar 'Waldmann's Green' and radish (Raphanus sativus L.) cultivar 'Giant White Globe' were grown both in the field and in controlled environments, where hydroponic nutrient solution, light, and temperature were regulated, and where CO2 levels were controlled at 400, 1000, 5000, or 10,000 ppm. Plants were harvested at maturity, dried, and analyzed for proximate composition (protein, fat, ash, and carbohydrate), total nitrogen (N), nitrate N, free sugars, starch, total dietary fiber, and minerals. Total N, protein N, nonprotein N (NPN), and nitrate N generally increased for radish roots and lettuce leaves when grown under growth chamber conditions compared to field conditions. The nitrate-N level of lettuce leaves, as a percentage of total NPN, decreased with increasing levels of CO2 enrichment. The ash content of radish roots and of radish and lettuce leaves decreased with increasing levels of CO2 enrichment. The levels of certain minerals differed between field- and chamber-grown materials, including changes in the calcium (Ca) and phosphorus (P) contents of radish and lettuce leaves, resulting in reduced Ca/P ratio for chamber-grown materials. The free-sugar contents were similar between the field and chamber-grown lettuce leaves, but total dietary fiber content was much higher in the field-grown plant material. The starch content of growth-chamber lettuce increased with CO2 level.

NASA Discipline Life Support Systems↗

DOE OSTI2011

Understanding Corrosion Mechanisms in Oxy-Fired Systems

Replacing air with oxygen in coal-fired boilers (i.e. oxy-firing) combined with flue gas recirculation is a leading strategy to concentrate CO{sub 2} and assist in carbon capture and sequestration. A significant area of concern is the fireside corrosion with oxy-firing due to the higher CO{sub 2} levels in the combustion gas and potentially higher SO{sub x} and H{sub 2}O levels. In order to investigate this complicated issue, laboratory experiments are being conducted with and without synthetic ash to assess the potential effect of oxy-firing on fireside corrosion rates. The initial results of this project focus on commercial and model Fe-base alloys at 600 C. Without ash, a 50%H{sub 2}O-50%(CO{sub 2}-0.15O{sub 2}) environment was the most aggressive condition, requiring higher Cr contents than 100% H{sub 2}O or Ar-50%CO{sub 2}. With the specimens covered in ash, several gas compositions were examined, including different levels of H{sub 2}O and SO{sub 2} to simulate various oxy-firing strategies. Results also are presented for several laser-clad coating compositions for protecting tubes. An additional task is examining the effect of environment on mechanical properties. Initial work studied Ni-base alloys in steam at 800 C and found little effect of steam on the creep rupture life of alloy 230 but a 35% decrease for alloy 740.

20 FOSSIL-FUELED POWER PLANTS↗

DOE OSTI2012

Environmentally-friendly animal litter

An animal litter composition including geopolymerized ash particulates having a network of repeating aluminum-silicon units is described herein. Generally, the animal litter is made from a quantity of a pozzolanic ash mixed with a sufficient quantity of water and an alkaline activator to initiate a geopolymerization reaction that forms geopolymerized ash. After the geopolymerized ash is formed, it is dried, broken into particulates, and sieved to a desired size. These geopolymerized ash particulates are used to make a non-clumping or clumping animal litter. Odor control is accomplished with the addition of a urease inhibitor, pH buffer, an odor eliminating agent, and/or fragrance.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Impact of biomass ash content on biocomposite properties

Owing to its low cost and sustainable nature, lignocellulosic biomass has been utilized for reinforcing polymers, but it is crucial to understand the impact of high-ash concentrations in biomass on composite strength and processing. Biomass is not only desirable for biofuel production but could also have a strong market, if high-ash biomass is acceptable, for biocomposites. In this work, natural fibers (switchgrass and corn stover) were used to reinforce polylactic acid (PLA) to produce biocomposites. Natural fibers were pretreated to obtain fibers that contain different percentages of ash. The mechanical properties (such as Young's modulus, tensile strength, failure strain, storage modulus) of corn stover/PLA composites remained largely unaffected by the ash concentration of the biomass fibers, despite the large range of ash contents (2.2–11.9 wt%). Furthermore, the tensile strengths of switchgrass/PLA composites were slightly negatively affected by the ash concentration of the switchgrass fibers (0.7–2.1 wt%). Both the switchgrass/PLA and the corn stover/PLA composites exhibited a high-enough tensile strength (49–57 MPa) and suitable complex viscosity (2.0–7.0 kPa·s at the frequency of 3.2 rad/s). They are expected to be 3D-printable through an extrusion-based additive manufacturing process.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Influence of the composition of cement kiln dust on its interaction with fly ash and slag

Cement kiln dust (CKD), a by-product of the cement industry, contains significant amounts of alkali, free lime, chloride and sulfate. Wide variation reported in the chemical composition of CKDs limits their potential application as a sustainable binder component in concrete. In the current study, the performance of two different CKDs as components in a novel binder is evaluated. Several binders are developed by blending CKDs with fly ash or slag. Binders with 70% CKD were prepared at a water-to-binder ratio of 0.4, and heat-cured at 75 °C to accelerate the strength development. The hydration progress was monitored using X-ray diffraction, and morphological examination was performed using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Ettringite and calcium aluminosilicate hydrate (C-A-S-H) were identified as the main hydration products in the hardened binder system. Strength development of CKD-based binder was found to be significantly influenced by its free lime and sulfate contents. -- Highlights: •Interaction of cement kiln dust with fly ash and slag was explored. •CKD with higher free lime and sulfate content increased the strength of binder. •C-S-H like reaction gel with fibrillar morphology is observed in CKD-based binders.

36 MATERIALS SCIENCE↗

DOE OSTI2022

CFD-DEM Modeling of Autothermal Pyrolysis of Corn Stover with a Coupled Particle- and Reactor-Scale Framework

Autothermal operation of fast pyrolysis is an efficient process-intensification technique wherein exothermic oxidation reactions are used to overcome the heat-transfer bottleneck of conventional pyrolysis. The development of accurate, reliable modeling toolsets is imperative to generating a deeper understanding of biomass autothermal pyrolysis systems to support scale-up and industrial deployment. This modeling effort describes the development of single-particle and reactor models which incorporate detailed reaction schemes and simultaneous exothermic oxidation reactions. The particle-scale model was parameterized for corn stover feedstock with particle morphology, density, ash content, and biopolymer composition, all of which impact the emergent conversion characteristics during pyrolysis. Results were then used to parameterize a reactor-scale autothermal pyrolysis model, which was developed using a coarse-grained computational fluid dynamic-discrete element method. The simulation results compared well with experimental results, with the predicted bio-oil, light gas, and biochar yield within 3.0 wt% of the experimental yields. Further analyses were performed to test the influence of equivalence ratio, biomass injection position, and particle size distribution on autothermal pyrolysis. The analysis of the physio-chemical properties of the fluid and solid phase inside the reactor and at the reactor outlet help reveal important process interactions of autothermal pyrolysis.

BIOMASS FUELS,INORGANIC, ORGANIC, PHYSICAL, AND AN↗

DOE OSTI2020

Distribution of rare earth elements in fly ash derived from the combustion of Illinois Basin coals

This study examined rare earth element (REE) trends for Illinois Basin coal-sourced fly ashes, with the goal of understanding the elemental composition and resource potential for various fly ash fractions. Illinois Basin coals have a high volatile C through A bituminous rank with a moderate ash content (slightly>12% ash (dry basis)), about 3% sulfur, and, in general, lower concentrations of hazardous and other trace elements than many Central Appalachian coals. Fly ash from the combustion of Illinois Basin coals tends to have a high Fe 2 O 3 content owing to the amount of pyrite in the feed coals. The rare earth element (REE) concentrations in Illinois Basin coal-sourced fly ashes are less than that for fly ashes from the combustion of Central Appalachian coals. The Upper continental crust-corrected fly ashes show an H-type enrichment, a positive Eu N /Eu N * , and, in some cases, a sharp Gd peak. For comparison, a suite of fly ashes from the combustion of a blend of eastern Kentucky coals had an H-type enrichment, a positive Eu N /Eu N * , but only a minimal Gd peak. In contrast, fly ash from the combustion of the Fire Clay coal, a REE-rich coal, had a negative Eu N /Eu N * and a sharp Gd peak. Finally, these results highlight the importance of feed coal composition on trace element contents of respective combustion fly ash fractions and also the unique REE enrichment patterns of the Illinois Basin fly ashes relative to the better studied fly ashes of eastern Kentucky and Central Appalachia.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2010

Synthesis of zeolite from Italian coal fly ash: Differences in crystallization temperature using seawater instead of distilled water

In this study Italian coal fly ash was converted into several types of zeolite in laboratory experiments with temperatures of crystallization ranging from 35 up to 90 deg. C. Distilled and seawater were used during the hydrothermal synthesis process in separate experiments, after a pre-treatment fusion with NaOH. The results indicate that zeolites could be formed from different kind of Italian coal fly ash at low temperature of crystallization using both distilled and seawater. SEM data and the powder patterns of X-ray diffraction analysis show that faujasite, zeolite ZK-5 and sodalite were synthesized when using both distilled and seawater; zeolite A crystallized only using distilled water. In particular the experiments indicate that the synthesis of zeolite X and zeolite ZK-5 takes place at lower temperatures when using seawater (35 and 45 deg. C, respectively). The formation of sodalite is always competitive with zeolite X which shows a metastable behaviour at higher temperatures (70-90 deg. C). The chemical composition of the fly ash source could be responsible of the differences on the starting time of synthesized zeolite with distilled water, in any case our data show that the formation of specific zeolites takes place always at lower temperatures when using seawater.

36 MATERIALS SCIENCE↗

NASA NTRS1982

Time variations of aerosols in the stratosphere following Mount St. Helens eruptions

Samples of stratospheric aerosols collected with U-2 aircraft for several months following the first three major eruptions of Mount St. Helens were analyzed for ash and liquid acid content. Ash grain sizes and compositions vary depending on collection altitude, location within the drifting cloud, and days following their injection. s computers Size distributions of ash particles vary with altitude. Generally small particles are depleted more rapidly at low altitudes (12 km) than at higher altitudes (17-18 km). Although samples collected 1 day after the first eruption of May 18, 1980, were dry, flow marks on the aircraft indicated parts of the cloud contained heavy acid concentrations. Indeed, all other samples obtained within 1 to 4 days after later eruptions (May 25 and June 12, 1980) were covered with copious amounts of liquid acid. Proportions of liquid to ash varied considerably depending on sampling location and cloud age. Because the acid-coated ash globules were large, they rapidly fell from the stratosphere until, by late June 1980, only a residue of acid droplets remained. Size distributions and concentrations of these droplets varied considerably.

Farlow, N. H.↗

DOE OSTI2010

Estimating the Heat of Formation of Foodstuffs and Biomass

Calorie estimates for expressing the energy content of food are common, however they are inadequate for the purpose of estimating the chemically defined heat of formation of foodstuffs for two reasons. First, they assume utilization factors by the body.1,2,3 Second, they are usually based on average values for their components. The best way to solve this problem would be to measure the heat of combustion of each material of interest. The heat of formation can then be calculated from the elemental composition and the heats of formation of CO2, H2O, and SO2. However, heats of combustion are not always available. Sometimes elemental analysis only is available, or in other cases, a breakdown into protein, carbohydrates, and lipids. A simple way is needed to calculate the heat of formation from various sorts of data commonly available. This report presents improved correlations for relating the heats of combustion and formation to the elemental composition, moisture content, and ash content. The correlations are also able to calculate heats of combustion of carbohydrates, proteins, and lipids individually, including how they depend on elemental composition. The starting point for these correlations are relationships commonly used to estimate the heat of combustion of fossil fuels, and they have been modified slightly to agree better with the ranges of chemical structures found in foodstuffs and biomass.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Slag Management of Carbon Feedstock Used in Gasification FY17 TCF between Eastman Chemical and NETL (Final Report)

NETL, in collaboration with Eastman Chemical Corp (Kingsport, TN), targeted the joint evaluation and refinement of a slag management program developed by NETL (NETL IP, patent applied for) to control gasifier slag properties formed from ash in individual or combinations of different coal-based carbon feedstock materials and specific slag modifiers used in gasification. Slag forms from mineral or organic-metallic impurities in the carbon feedstock that melt at the high temperatures of gasification, coalescing to form a liquid (slag) that must flow from the gasifier. Slag additives, also known as slag modifiers, are often added to the carbon feedstock to modify the ash chemistry and achieve desired slag flow properties at target temperatures used in gasification. If slag does not flow from a gasifier, its buildup within the gasification chamber will cause either gasifier shutdown to physically remove the slag (consuming time and damaging the protective refractory lining), or the gasification temperature must be increased to lower slag viscosity so it can flow from the gasifier, leading to greater refractory wear/corrosion, along with increased fouling and downstream component wear. Because of these issues, gasification is typically targeted at the lowest temperature possible where slag will flow in a controlled manner (a temperature range called T100 for the lowest temperature, with T250 being the highest temperature where the slag has achieved the desired fluidity). That temperature range also needs to yield a desired syngas composition, highlighting the importance of knowing and being able to control carbon feedstock slag viscosity and the temperature of thermal breakdown of the carbon feedstock. Slag viscosity varies with changes in the gasification chamber temperature, oxygen partial pressure, and slag chemistry. The slag model work with Eastman Chemical targeted predicting and controlling molten coal ash slag behavior at specific gasification conditions. The final goal of the refined model was to develop/refine the NETL slag model so a gasifier operator would be able to predict slag behavior prior to purchasing or using a carbon feedstock and control slag properties once a carbon feedstock is being gasified, allowing a gasifier user to determine what mineral additives or blends of different carbon materials would be needed to achieve desired slag properties at targeted gasification conditions. For a given carbon feedstock and desired gasification condition, the actual gasification cost and slag behavior would be able to be predicted using the slag management program in advance of purchasing or using the carbon feedstock – allowing accurate control of slag ash behavior in real time. As part of the TCF project work with Eastman Chemical, the viscosity of several ash compositions of interest to them would be measured and used to populate the slag model, along with a large database of historical slag temperature, chemistry, and viscosity information they possess – information that would in-crease the predictive accuracy of the slag management model with slag ash chemistry of interest to them. As part of the model evaluation and refinement, the predictive model and its database will be installed on computers at Eastman Chemical and used to manage slag properties in a gasifier during real-time operation of their gasifier. In summary, success of the slag management program at Eastman Chemical would support its use by other gasifier operators to manage slag chemistry and properties over other desired gasification temperature ranges, allowing greater process control and efficiency of their carbon feedstock conversion during gasification.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2025

Composition and Plume Gas Interaction Control Iron Fractional Solubility More Than Particle Size in Volcanic Ash: Implications for Fertilization of the North Atlantic

Deposition of volcanic ash is thought to impact marine biogeochemical cycling by adding soluble iron (Fe) to the surface ocean. The magnitude of this input is a function of the amount of ash deposited, the total Fe content in the ash, and ash‐derived Fe's fractional solubility. However, the relative importance of chemical composition, acidic processing by the volcanic plume, and ash particle size in determining solubility is unclear. We paired an aerosol leach meant to provide an upper limit for fractional Fe solubility with chemical analyses of ash from the Cumbre Vieja (CV) and La Soufrière eruptions, which both impacted the North Atlantic in 2021. Fe in the ash samples is <6% soluble, but Fe fractional solubility in CV ash is approximately triple that of La Soufrière ash. Compared to La Soufrière, a larger proportion of the Fe in CV ash is in silicate rather than oxide minerals, which release more soluble Fe. Elevated levels of surficial fluorine (F) also suggest that CV ash was subjected to a more fluorine‐rich eruption plume and underwent more acidic processing. Particle size does not appear to be a primary control on Fe release. We estimate that the CV eruption had a much larger impact on dissolved Fe (DFe) concentration in the surface ocean than the La Soufrière eruption because of differences in soluble Fe content and particle deposition velocity. These differences may help explain why some eruptions elicit a biological response in the ocean while others do not.

Elliott, Hope E. [Univ. of Miami, FL (United State↗

DOE OSTI2017

Quantitative multiphase model for hydrothermal liquefaction of algal biomass

Here, optimized incorporation of hydrothermal liquefaction (HTL, reaction in water at elevated temperature and pressure) within an integrated biorefinery requires accurate models to predict the quantity and quality of all HTL products. Existing models primarily focus on biocrude product yields with limited consideration for biocrude quality and aqueous, gas, and biochar co-products, and have not been validated with an extensive collection of feedstocks. In this study, HTL experiments (300 °C, 30 min) were conducted using 24 different batches of microalgae feedstocks with distinctive feedstock properties, which resulted in a wide range of biocrude (21.3–54.3 dry weight basis, dw%), aqueous (4.6–31.2 dw%), gas (7.1–35.6 dw%), and biochar (1.3–35.0 dw%) yields. Based on these results, a multiphase component additivity (MCA) model was introduced to predict yields and characteristics of the HTL biocrude product and aqueous, gas, and biochar co-products, with only feedstock biochemical (lipid, protein, carbohydrate, and ash) and elemental (C/H/N) composition as model inputs. Biochemical components were determined to distribute across biocrude product/HTL co-products as follows: lipids to biocrude; proteins to biocrude > aqueous > gas; carbohydrates to gas ≈ biochar > biocrude; and ash to aqueous > biochar. Modeled quality indicators included biocrude C/H/N contents, higher heating value (HHV), and energy recovery (ER); aqueous total organic carbon (TOC) and total nitrogen (TN) contents; and biochar carbon content. The model was validated with HTL data from the literature, the potential to expand the application of this modeling framework to include waste biosolids (e.g., wastewater sludge, manure) was explored, and future research needs for industrial application were identified. Ultimately, the MCA model represents a critical step towards the integration of cultivation models with downstream HTL and biorefinery operations to enable system-level optimization, valorization of co-product streams (e.g., through catalytic hydrothermal gasification and nutrient recovery), and the navigation of tradeoffs across the value chain.

09 BIOMASS FUELS↗

DOE OSTI2012

Microstructural and compositional change of NaOH-activated high calcium fly ash by incorporating Na-aluminate and co-existence of geopolymeric gel and C-S-H(I)

This study explores the reaction products of alkali-activated Class C fly ash-based aluminosilicate samples by means of high-resolution synchrotron X-ray diffraction (HSXRD), scanning electron microscope (SEM), and compressive strength tests to investigate how the readily available aluminum affects the reaction. Class C fly ash-based aluminosilicate raw materials were prepared by incorporating Na-aluminate into the original fly ashes, then alkali-activated by 10 M NaOH solution. Incorporating Na-aluminate reduced the compressive strength of samples, with the reduction magnitude relatively constant regardless of length of curing period. The HSXRD provides evidence of the co-existence of C-S-H with geopolymeric gels and strongly suggests that the C-S-H formed in the current system is C-S-H(I). The back-scattered electron images suggest that the C-S-H(I) phase exists as small grains in a finely intermixed form with geopolymeric gels. Despite providing extra source of aluminum, adding Na-aluminate to the mixes did not decrease the Si/Al ratio of the geopolymeric gel.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Exploring biofiber properties and their influence on biocomposite tensile properties

Biofibers serve as effective reinforcements for neat polylactic acid (PLA) in biocomposites, offering an attractive opportunity to decarbonize the manufacturing sector of the United States by displacing fossil-based reinforcement fibers such as carbon fibers. Also, biofiber production can stimulate economic growth in rural economies, fueling sustainable development. PLA resins are commonly compounded with biofibers to create biocomposites suitable for additive manufacturing. PLA-biofiber composites often exhibit better overall material properties than neat (pure) PLA, but the associations between biofiber properties and the material properties of their biocomposites remain largely unexplored. Hence, this research delves into a comprehensive exploration of diverse biofibers, scrutinizing their physical and chemical attributes, including size, shape, ash content and biochemical composition. The study meticulously analyzes the flow properties of each biofiber and elucidates the ultimate tensile strengths and Young's modulus of corresponding biocomposite samples. Noteworthy correlations between biofiber and biocomposite tensile properties are uncovered, shedding light on critical interrelationships. The study introduces an approach employing regression models to predict the ultimate tensile strength and Young's modulus of biocomposites. These models, validated with a cross-validation technique, exhibit remarkable predictive accuracy, particularly in estimating ultimate tensile strength. © 2024 Oak Ridge National Laboratory managed by UT-Battelle, LLC and The Author(s). Polymer International published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Investigation on the fly ash thermal treatment on the performance of Lithium Ferriphosphate (LiFePO{sub 4}) battery

Addition of the fly ash can be used to improve the capacity of LiFePO{sub 4} battery. Fly ash was added in Acethylene Black (AB) as 2% of the total weight of Acetylene Black (AB). The effects of temperature variation and fly ash characteristics were analyzed. Fly ash was prepared by heating at 50, 100, 150, and 250°C in muffle furnace for 5 hours and passed in 200 mesh screen prior to mixing it with other compounds. Lithium Ferriphospat (LiFePO{sub 4}), fly ash, Acethylene Black (AB), Polyvinylidene Fluoride (PVDF) as a binder and N-methyl-2-pyrrolidone (NMP) as a solvent were mixed to be slurry. The slurry were coated, dried and hot pressed to make a cathode film. The performance of battery lithium was examined by eight channel battery analyzer. The composition of the fly ash was examined by X-ray fluorescence spectrometry (XRF) and Fourier Tansform Infrared Spectroscopy (FTIR). The excellent performance was shown in the fly ash addition which were treated by heating at 150°C. The capacity of fly ash added LiFePO{sub 4} battery is 94.373 mAh/g, which is higher than that of without fly ash addition, i.e. 67.998 mAh/g.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Design and scale-up of 3D printed bat houses with biomass-derived polymer composites

Biomass (e.g., pine sawdust, especially high–ash content pine sawdust) is commonly disposed of as waste. Combining biomass with polymers to make composite feedstocks for 3D printing has been explored as a method to reduce or repurpose the biomass waste. Although not all biocomposite properties are known, the wood-based polylactic acid (PLA) composite has promising qualities for applications in ecological settings. In this work, pine wood–PLA composite feedstock was used to 3D print supplemental roost structures for endangered tree-roosting bats, which often face a paucity of suitable naturally occurring roosts. This material combination was selected because it is estimated to degrade faster than the synthetic material systems that are used widely in supplemental bat roosting structures to aid in the conservation of tree roosting bats. The layered, rough surface created by the 3D printing process serves as a surface that bats can grip while roosting. Computer-aided design (CAD) models were generated based on natural roost structures, and a full-size bat house was successfully additively manufactured using a pellet-fed large-scale 3D printing system. The 3D printed hexagon exhibited a tensile strength of 22–23 MPa and a Young’s modulus of 3202–3218 MPa in the x-direction. It has been demonstrated that the 3D printed bat house can be installed on a tree in a stable fashion. This successful demonstration of a bat roost manufactured using a bioderived composite should promote its use in other fish and wildlife structures and broader industrial applications such as construction and automobiles.

3D printing↗