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DOE OSTI2021

Wet Waste Hydrothermal Liquefaction and Biocrude Upgrading to Hydrocarbon Fuels: 2020 State of Technology

Data from Pacific Northwest National Laboratory’s conversion hydrothermal liquefaction (HTL) program for wet waste was used to update the pathway techno-economic analysis (TEA) for the fiscal year 2020 State of Technology (2020 SOT). The modeled fuel blendstock MFSP for the 2020 SOT is estimated at $4.50/GGE (with ammonia stripping of the AP), a reduction of $0.61/GGE, or 12%, relative to the 2019 SOT (Snowden-Swan et al. 2020). Progress in the HTL area includes increased reactor LHSV from 3.6 to 4.0 and a newly designed staged approach for the sludge pumping and heating, resulting in a 1 cent and 26 cent reduction in modeled MFSP, respectively. The newly designed heat exchanger configuration is less material and capital intensive than the previous SOT, and provides a system design that is more scalable with regard to practical fabrication limitations. Further improvements may be possible with the use of core inserts to enhance tube velocity and heat transfer rates. Biocrude hydrotreating research progress improved weight hourly space velocity (WHSV) from 0.67 to 0.72 hr-1 in the guard bed and from 0.39 to 1.02 hr-1 in the main hydrotreating bed, a 7% and 162% improvement, respectively. Hydrotreating performance was not sacrificed at the higher throughput rates and catalyst activity remained stable over the run. The demonstrated increase in WHSVs reduced the modeled MFSP by $0.34/GGE.

20 FOSSIL-FUELED POWER PLANTS↗

DOE OSTI2018

Plutonium environmental chemistry: mechanisms for the surface-mediated reduction of Pu(v/vi)

In recent decades, interest in plutonium mobility has increased significantly due to the need of the United States, as well as other nations, to deal with commercial spent nuclear fuel, nuclear weapons disarmament, and the remediation of locations contaminated by nuclear weapons testing and production. Although there is a global consensus that geologic disposal is the safest existing approach to dealing with spent nuclear fuel and high-level nuclear waste, only a few nations are moving towards implementing a geologic repository due to technical and political barriers. Understanding the factors that affect the mobility of plutonium in the subsurface environment is critical to support the development of such repositories. The importance of redox chemistry in determining plutonium mobility cannot be understated. While Pu(IV) is generally assumed to be immobile in the subsurface environment due to sorption or precipitation, Pu(V) tends to be mobile due to its relatively low effective charge and weak complex formation. This review highlights one particularly important aspect of plutonium behaviour at the mineral–water interface—the concept of surface-mediated reduction, which describes the reduction of plutonium on a mineral surface. It provides a conceptual model for and evidence supporting or refuting each proposed mechanism for surface-mediated reduction including (i) radiolysis at the mineral surface, (ii) electron transfer via ferrous iron or manganese in the mineral structure, (iii) electron shuttling due to the semiconducting properties of the mineral, (iv) disproportionation of Pu(V), (v) facilitation by proton exchange sites, (vi) stabilisation of Pu(IV) due to the increased concentration gradient within the electrical double layer, and (vii) a Nernstian favourability of Pu(IV) surface complexes and colloids. It also provides new perspectives on future research directions.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2018

A path for lignin valorization via additive manufacturing of high-performance sustainable composites with enhanced 3D printability

Here, we report the manufacture of printable, sustainable polymer systems to address global challenges associated with high-volume utilization of lignin, an industrial waste from biomass feedstock. By analyzing a common three-dimensional printing process—fused-deposition modeling—and correlating the printing-process features to properties of materials such as acrylonitrile-butadiene-styrene (ABS) and nylon, we devised a first-of-its-kind, high-performance class of printable renewable composites containing 40 to 60 weight % (wt %) lignin. An ABS analog made by integrating lignin into nitrile-butadiene rubber needs the presence of a styrenic polymer to avoid filament buckling during printing. However, lignin-modified nylon composites containing 40 to 60 wt % sinapyl alcohol–rich, melt-stable lignin exhibit enhanced stiffness and tensile strength at room temperature, while—unexpectedly—demonstrating a reduced viscosity in the melt. Further, incorporation of 4 to 16 wt % discontinuous carbon fibers enhances mechanical stiffness and printing speed, as the thermal conductivity of the carbon fibers facilitates heat transfer and thinning of the melt. We found that the presence of lignin and carbon fibers retards nylon crystallization, leading to low-melting imperfect crystals that allow good printability at lower temperatures without lignin degradation.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Recovery Act: Hydroelectric Facility Improvement Project - Replacement of Current Mechanical Seal System with Rope Packing System

On January 27, 2010 the City of North Little Rock, Arkansas received notification of the awarding of a Department of Energy (DOE) grant totaling $450,000 in funding from the American Recovery and Reinvestment Act (ARRA) under the Project Title: Recovery Act: Hydroelectric Facility Improvement Project – Automated Intake Clearing Equipment and Materials Management. The purpose of the grant was for improvements to be made at the City’s hydroelectric generating facility located on the Arkansas River. Improvements were to be made through the installation of an intake maintenance device (IMD) and the purchase of a large capacity wood grinder. The wood grinder was purchased in order to receive the tree limbs, tree trunks, and other organic debris that collects at the intake of the plant during high flow. The wood grinder eliminates the periodic burning of the waste material that is cleared from the intake and reduces any additional air pollution to the area. The resulting organic mulch has been made available to the public at no charge. Design discussion and planning began immediately and the wood grinder was purchased in July of 2010 and immediately put to work mulching debris that was gathered regularly from the intake of the facility. The mulch is currently available to the public for free. A large majority of the design process was spent in discussion with the Corps of Engineers to obtain approval for drawings, documents, and permits that were required in order to make changes to the structure of the powerhouse. In April of 2011, the City’s Project Engineer, who had overseen the application, resigned and left the City’s employ. A new Systems Mechanical Engineer was hired and tasked with overseeing the project. The transfer of responsibility led to a re-examination of the original assumptions and research upon which the grant proposal was based. At that point, the project went under review and a trip was booked for July 2011 to visit facilities that currently had an IMD installed. This further study of facilities revealed that the implementation of the project as originally described, while proving the benefits described in the original grant application, would likely intensify sand intake. Increased sand intake would lead to an increase in required shutdowns for maintenance and more rapid depreciation of key equipment which would result in a loss of generation capacity. A better solution to the problem, one that continued to meet the criteria for the original grant and ARRA standards, was developed. A supporting day trip was planned to visit other facilities located on the Arkansas River to determine how they were coping with the same strong amounts of sand, silt, and debris. Upon returning from the trip to other Arkansas River facilities it was extremely clear what direction to go in order to most efficiently address the issue of generator capacity and efficiency. Of the plants visited on the Arkansas River, every one of them was running what is called a rope packing shaft sealing system as opposed to mechanical shaft seals, which the facility was running. Rope packing is a time proven sealing method that has been around for centuries. It has proved to perform very well in dirty water situations just like that of the Arkansas River. In April of 2012 a scope change proposal was submitted to the DOE for approval. In August of 2012 the City received word that the change of scope had been approved. Plans were immediately set in motion to begin the conversion from mechanical seals to a packing box at the facility. Contractors arrived on October 1st, 2012 and the project team began unwatering the unit for disassembly. The seal conversion was completed on February 29th, 2013 with start-up of the unit. Further testing and adjusting was done throughout the first two weeks of March.

13 HYDRO ENERGY↗

DOE OSTI2020

Feedback on Forty-year Long Clean-up Operations of a Contaminated Soil for Environmental Purpose - 20026

One of the CEA facilities in France is the place of miscellaneous mapping and clean-up operations since the 1980's. The final purpose of the conducted work deals with the environmental remediation of the building. In France, the absence of a regulatory framework for the management of sites polluted by radioactive substances, especially as the lack of release thresholds, has led to develop different approaches of soil radiological characterization. The geostatistical approach is part of them. Preliminary investigations are an unavoidable step prior to clearance and remediation. First, historical analysis enables to define site perimeters to investigate as well as to precisely locate expected contaminated parts. For radioactive pollutants, the media (water, soil, air) and transfer routes participate in the definition of the investigation perimeter and thus also need to be identified through a geological study. At the same time, functional analysis leads to choose the best measurement means which could provide useful information when combined with visual inspection. An equipment well adapted to easy-to-measure radionuclides as gamma emitters, such as gamma probe or on-site gamma spectrometry, is usually selected as a non-destructive assay. Coupled with spatial positions, processed on-site radiological data can be mapped. Data processing consists in mapping and kriging before a geostatistical analysis in order to identify the zones of interest to be targeted. Selected zones are not only linked to high level count rates but also to low level ones so that a pollution-free reference is known in the area. This data processing also enables to categorize waste types according to their origin and contamination levels. An expected volume of different waste then follows as well as the waste characterization equipments. In-depth investigations, e.g. core drillings and samplings, naturally ensue to aim at remediation optimization through the assessment of environmental impact. After clean-up operations, non-destructive assays as well as destructive samplings enable to check the effective clearance. Following this methodology in the present remediation work, results of the first non-destructive assay campaign highlighted a long-lived transuranic radionuclides contamination in the concrete flagstone. Successive non-destructive assays were then performed in the defined zones of interest. Count rates measured with a surface probe were first mapped. The best localization of destructive assays, i.e. core drillings at a 1 meter depth, came from this surface mapping followed by a geostatistical analysis. The concrete flagstone was totally removed. Then, the depth of soil to remove under the flagstone was optimized from the results of radiological activities measured in core drillings samples. A new surface mapping was then drawn after this partial soil excavation. The sand and demolition rubble samples, homogeneously constituted from the flagstone fragments, were analyzed by gamma spectrometry. Meanwhile, waste drums and other containers were also measured by gamma spectrometry and passive neutron measurement devices. All these results have brought miscellaneous pieces of information. In this context, major issues appear in terms of physical constraints such as the premises tininess as well as of soil sampling techniques and in terms of measurement performances assessment and the representativeness of homogeneous samples. The choice of radiological soil and waste characterization devices is described in the light of enhanced performances by keeping in mind radiation protection requirements and a willing to always optimize waste categories (very low level waste) and volume. The improvement of the characterization methods appears through this forty-year long work while sharing the feedback of encountered difficulties. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2021

Characterization of Infrequent Samples from the Concentration, Storage, and Transfer Facility: H-Area Diversion Box 7 (HDB-7) Sump Sample: December 2021 Sample

In December 2021, SRR-E sent an ~250 mL sample identified as HDB-7 from an H-Area diversion box sump to SRNL for analysis. The sample was clear and colorless and free from any solids. SRNL analysis indicated that the sample contained 2.97E+05 dpm/mL Cs-137, 3.74E+05 dpm/mL total beta activity, 1.04E+03 dpm/mL beta activity following cesium removal, and below detectable levels of alpha activity and alpha activity following cesium removal. In addition, the pH of the sample was 7.32, free hydroxide concentration was 2.09E-07 M, and the density was 0.991 g/mL.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2012

The Mercury Resistance Operon: From an Origin in a Geothermal Environment to an Efficient Detoxification Machine

Mercuric mercury (Hg[II]) is a highly toxic and mobile element that is likely to have had a pronounced and adverse effect on biology since Earth’s oxygenation ~2.4 billion years ago due to its high affinity for protein sulfhydryl groups, which upon binding destabilize protein structure and decrease enzyme activity, resulting in a decreased organismal fitness. The central enzyme in the microbial mercury detoxification system is the mercuric reductase (MerA) protein, which catalyzes the reduction of Hg(II) to volatile Hg(0). In addition to MerA, mer operons encode for proteins involved in regulation, Hg binding, and organomercury degradation. Mer-mediated approaches have had broad applications in the bioremediation of mercury-contaminated environments and industrial waste streams. Here, we examine the composition of 272 individual mer operons and quantitatively map the distribution of mer-encoded functions on both taxonomic SSU rRNA gene and MerA phylogenies. The results indicate an origin and early evolution of MerA among thermophilic bacteria and an overall increase in the complexity of mer operons through evolutionary time, suggesting continual gene recruitment and evolution leading to an improved efficiency and functional potential of the Mer detoxification system. Consistent with a positive relationship between the evolutionary history and topology of MerA and SSU rRNA gene phylogenies (Mantel R = 0.81, p < 0.01), the distribution of the majority of mer functions, when mapped on these phylograms, indicates an overall tendency to inherit mer-encoded functions through vertical descent. However, individual mer functions display evidence of a variable degree of vertical inheritance, with several genes exhibiting strong evidence for acquisition via lateral gene transfer and/or gene loss. Collectively, these data suggest that (i) mer has evolved from a simple system in geothermal environments to a widely distributed and more complex and efficient detoxification system, and (ii) merA is a suitable biomarker for examining the functional diversity of Hg detoxification and for predicting the composition of mer operons in natural environments.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2020

Independent Verification Plan for Clearance of Real Property of the Operation Roller Coaster Sites

The U.S. Department of Energy (DOE) is pursuing release of the Operation Roller Coaster sites under DOE O 458.1, “Radiation Protection of the Public and the Environment.” The requirements for clearance and release of property under DOE O 458.1 are implemented when DOE intends to facilitate transfer of responsibility or control of real property from DOE. DOE O 458.1 prescribes that all radiological monitoring or surveys performed in support of clearance of property must use methods such as the Multi-Agency Radiation Survey and Site Investigation Manual (MARSSIM) method or other methods approved by DOE. DOE O 458.1 requires an Independent Verification for the clearance of real property. This Independent Verification Plan outlines the process for validating the method and implementation of the MARRSIM process for release of the Operation Roller Coaster sites.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2012

Changing the Rules on Fuel Export at Sellafield's First Fuel Storage Pond - 12065

The Pile Fuel Storage Pond (PFSP) was built in 1949/50 to receive, store and de-can fuel and isotopes from the Windscale Piles. Following closure of the Piles in 1957, plant operations were scaled down until fuel processing eventually ceased in 1962. The facility has held an inventory of metal fuel both from the Piles and from other programmes since that time. The pond is currently undergoing remediation and removal of the fuel is a key step in that process, unfortunately the fuel export infrastructure on the plant is no longer functional and due to the size and limited lifting capability, the plant is not compatible with today's large volume heavy export flasks. The baseline scheme for the plant is to package fuel into a small capacity flask and transfer it to another facility for treatment and repackaging into a flask compatible with other facilities on site. Due to programme priorities the repackaging facility is not available to do this work for several years causing a delay to the work. In an effort accelerate the programme the Metal Fuel Pilot Project (MFPP) was initiated to challenge the norms for fuel transfer and develop a new methodology for transferring the fuel. In developing a transfer scheme the team had to overcome challenges associated with unknown fuel condition, transfers outside of bulk containment, pyro-phoricity and oxidisation hazards as well as developing remote control and recovery systems for equipment not designed for this purpose. A combination of novel engineering and enhanced operational controls were developed which resulted in the successful export of the first fuel to leave the Pile Fuel Storage Pond in over 40 years. The learning from the pilot project is now being considered by the main project team to see how the new methodology can be applied to the full inventory of the pond. (author)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2012

Groundwater Treatment at the Fernald Preserve: Status and Path Forward for the Water Treatment Facility - 12320

Operating a water treatment facility at the Fernald Preserve in Cincinnati, Ohio-to support groundwater remediation and other wastewater treatment needs-has become increasingly unnecessary. The Fernald Preserve became a U.S. Department of Energy Office of Legacy Management (LM) site in November 2006, once most of the Comprehensive Environmental Response, Compensation, and Liability Act environmental remediation and site restoration had been completed. Groundwater remediation is anticipated to continue beyond 2020. A portion of the wastewater treatment facility that operated during the CERCLA cleanup continued to operate after the site was transferred to LM, to support the remaining groundwater remediation effort. The treatment facility handles the site's remaining water treatment needs (for groundwater, storm water, and wastewater) as necessary, to ensure that uranium discharge limits specified in the Operable Unit 5 Record of Decision are met. As anticipated, the need to treat groundwater to meet uranium discharge limits has greatly diminished over the last several years. Data indicate that the groundwater treatment facility is no longer needed to support the ongoing aquifer remediation effort. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

A Process with Decoupled Absorber Kinetics and Solvent Regeneration through Membrane Dewatering and In-Column Heat Transfer (Final Report)

This report summarizes the work conducted on project DE-FE0031604 where University of Kentucky Center for Applied Energy (UK CAER) has validated its intensified CO 2 capture process through substantial enhancements to the kinetics of the absorption process and energy reductions by absorber temperature profile modification, dewatering and heat integration technologies for achieving significant capital and operating cost reductions. To address DOE’s objective of improving post-combustion CO 2 capture technology and reducing associated cost, UK CAER employed an intensified process which combined three key aspects targeted at overcoming inherent limitations or barriers in the conventional CO 2 capture and desorption process. The process designed to be independent of the type of solvent used, included (1) the use of 3-D printed two-channel structured packing material to control the temperature profile and increase the CO 2 absorption rate in the absorber, (2) a zeolite membrane dewatering unit for dewatering of the carbon-rich solvent to decouple solvent concentration needs for CO 2 absorption and desorption, and (3) a rich-split feed with two-phase flow heat transfer prior to the stripper that provided a secondary point of vapor generation to provide energy savings in steam extraction and solvent regeneration. The project was executed over two budget periods. This involved testing of individual process components which included the advanced heat transfer packing and the dewatering membrane on UK CAER’s 30 liter per minute (L/min) CO 2 (3” Column) capture bench unit with simulated flue gas in the first budget period. Subsequent scaled-up testing of these components together with the split-feed configuration were also tested in UK CAER’s 0.1 MWth CO 2 capture unit with coal-derived flue gas in the second-budget period. Long term studies were done during this period to assess process and solvent performance over extended duration. Project partners Lawrence Livermore National Laboratory (LLNL) and Media & Process Technology (MPT) led the development efforts for the advanced packing material and dewatering membrane respectively. Data from the long term testing was used as input for an environmental, health and safety (EH&S) assessment for the process and scaled technology performed by ALL4 LLC. Trimeric Corporation also completed a techno-economic analysis (TEA) for the UK CAER technology which was compared to the DOE reference Case B12B. Tests on the 3” column capture unit showed that the advanced heat transfer packing could be used to lower the bulge temperature in the absorber, and this was also proven in the scaled testing in the 0.1 MWth CO 2 capture unit. The bulge temperature could be lowered by >10 °C, changing the temperature profile in the absorber, and showed potential to enhance absorption with the ability to tailor the profile to provide conditions suitable for a solvent’s properties and kinetics. Conditions for short term evaluation of a 19” zeolite dewatering membrane on the 3” column capture unit yielded desirable fluxes and sustained rejection rates of >80%. However, for the scaled testing of six membrane modules consisting of 21 parts of 31-inch-long membrane tubes in each bundle (surface area 0.3 m 2 ), over a more extended duration, similar rejection rates could not be achieved. With the split-feed of the rich stream to the stripper, improved heat recovery minimized waste heat exiting the top of the stripper. The stripper exhaust temperatures could be reduced by >10 °C; reducing the amount of water vaporization contributed to lowering the regeneration energy by ~ 15%. The energy benefit could be sustained from the long term monitoring of the solvent performance. The solvent properties were not significantly impacted over the long-term operations. The benefits of the UK CAER process demonstrated experimentally were mostly validated from the TEA comparing a commercial scale application of the technology to DOE reference Case B12B. The cost of CO 2 capture for the UK CAER technology was estimated to be ~$34.97/tonne of CO 2 captured; a reduction of 23% compared to Case B12B. The increase in cost of electricity was also shown to be 16% lower than that of Case B12B. The total parasitic demand was also shown to be 11% lower. The key drivers for the benefits are a result of the process intensification approaches employed in the UK CAER technology for enhanced solvent performance, effective heat recovery and improved energy performance. The EH&S assessment did not find any major environmental concerns or barriers to the full scale implementation of the technology.

20 FOSSIL-FUELED POWER PLANTS↗

DOE OSTI2015

Moving to Sustainable Metals: Multifunctional Ligands in Catalytic, Outer Sphere C-H, N-H and O-H Activation

Much of our work during this grant period has emphasized green chemistry and sustainability. For example, we were able to convert glycerine, a waste byproduct of biodiesel production, into lactic acid, a compound with numerous applications, notably in the food and cosmetics industry, as well as being a source material for a biodegradable plastic. This work required a catalyst, that ceases to work after a certain lapse of time. We were able to identify the way in which this deactivation occurs by identifying some of the metal catalyst deactivation products. These proved to be multimetallic clusters containing up to six metals and up to 14 hydrogen atoms. Both the catalytic reaction itself and the deactivation structures are novel and unexpected. We have previously proposed that nitrogen heterocycles could be good energy carriers in a low CO 2 future world. In another part of our study, we found catalysts for introduction of hydrogen, an energy carrier that is hard to store, into nitrogen heterocycles. The mechanism of this process proved to be unusual in that the catalyst transfers the H 2 to the heterocycle in the form of H + and H - , first transferring the H + and only then the H - . In a third area of study, some of our compounds, originally prepared for DOE catalysis purposes, also proved useful in hydrocarbon oxidation and in water oxidation. The latter is important in solar-to-fuel work, because, by analogy with natural photosynthesis, the goal of the Yale Solar Group of four PIs is to convert sunlight to hydrogen and oxygen, which requires water splitting catalysts. The catalysts that proved useful mediate the latter reaction: water oxidation to oxygen. In a more technical study, we developed methods for distinguishing the case where catalysis is mediated by a soluble catalyst from cases where catalysis arises from a deposit of finely divided solid. One particular application involved electrocatalysis, where catalysis is driven by application of a voltage to electrodes dipped in the reactant mixture. We measured the mass increase of an electrode as material is deposited, and were able to see how this process is affected by the voltage supplied to the electrode. Our work continues to be well cited and we often receive requests for information or samples from fellow researchers.

08 HYDROGEN↗

NASA NTRS2010

Design and Preliminary Thermal Performance of the Mars Science Laboratory Rover Heat Exchangers

The challenging range of proposed landing sites for the Mars Science Laboratory Rover requires a rover thermal management system that is capable of keeping temperatures controlled across a wide variety of environmental conditions. On the Martian surface where temperatures can be as cold as -123 degrees Centigrade and as warm as 38 degrees Centigrade, the Rover relies upon a Mechanically Pumped Fluid Loop (MPFL) and external radiators to maintain the temperature of sensitive electronics and science instruments within a -40 degrees Centigrade to 50 degrees Centigrade range. The MPFL also manages significant waste heat generated from the Rover power source, known as the Multi Mission Radioisotope Thermoelectric Generator (MMRTG). The MMRTG produces 110 Watts of electrical power while generating waste heat equivalent to approximately 2000 Watts. Two similar Heat Exchanger (HX) assemblies were designed to both acquire the heat from the MMRTG and radiate waste heat from the onboard electronics to the surrounding Martian environment. Heat acquisition is accomplished on the interior surface of each HX while heat rejection is accomplished on the exterior surface of each HX. Since these two surfaces need to be at very different temperatures in order for the MPFL to perform efficiently, they need to be thermally isolated from one another. The HXs were therefore designed for high in-plane thermal conductivity and extremely low through-thickness thermal conductivity by using aerogel as an insulator inside composite honeycomb sandwich panels. A complex assembly of hand welded and uniquely bent aluminum tubes are bonded onto the HX panels and were specifically designed to be easily mated and demated to the rest of the Rover Heat Recovery and Rejection System (RHRS) in order to ease the integration effort. During the cruise phase to Mars, the HX assemblies serve the additional function of transferring heat from the Rover MPFL to the separate Cruise Stage MPFL so that heat generated deep inside the Rover can be dissipated via the Cruise Stage radiators. Significant fabrication challenges had to be overcome in order to make the HX design a reality. The cruise phase thermal performance of the Rover HXs was verified in the cruise phase system level thermal vacuum test that was performed at JPL in January of 2009. The Rover HXs were modeled in I-DEAS TMG and predictions are compared to actual data from the test.

Heat Rejection System↗

DOE OSTI2024

Active species in chloroaluminate ionic liquids catalyzing low-temperature polyolefin deconstruction

Abstract Chloroaluminate ionic liquids selectively transform (waste) polyolefins into gasoline-range alkanes through tandem cracking-alkylation at temperatures below 100 °C. Further improvement of this process necessitates a deep understanding of the nature of the catalytically active species and the correlated performance in the catalyzing critical reactions for the tandem polyolefin deconstruction with isoalkanes at low temperatures. Here, we address this requirement by determining the nuclearity of the chloroaluminate ions and their interactions with reaction intermediates, combining in situ 27 Al magic-angle spinning nuclear magnetic resonance spectroscopy, in situ Raman spectroscopy, Al K-edge X-ray absorption near edge structure spectroscopy, and catalytic activity measurement. Cracking and alkylation are facilitated by carbenium ions initiated by AlCl 3 - tert -butyl chloride (TBC) adducts, which are formed by the dissociation of Al 2 Cl 7 − in the presence of TBC. The carbenium ions activate the alkane polymer strands and advance the alkylation cycle through multiple hydride transfer reactions. In situ 1 H NMR and operando infrared spectroscopy demonstrate that the cracking and alkylation processes occur synchronously; alkenes formed during cracking are rapidly incorporated into the carbenium ion-mediated alkylation cycle. The conclusions are further supported by ab initio molecular dynamics simulations coupled with an enhanced sampling method, and model experiments using n-hexadecane as a feed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Physical Modeling of Coupled Thermohydraulic Behavior of Compacted MX80 Bentonite during Heating

Abstract This paper describes a tank-scale test setup and experimental methodology used to investigate coupled heat transfer and water flow processes during heating of compacted MX80 bentonite to high temperatures. Specifically, a temperature of 200°C was maintained by a cylindrical heating element at the center of a compacted bentonite layer containing an array of temperature, dielectric, and relative humidity sensors. In addition to providing an evaluation of the spatiotemporal variations in temperature, relative humidity, degree of saturation, and global volume, the coupled thermohydraulic properties of the bentonite were assessed. A wetting front was initially observed to move away from the central heater, followed by a drying process until reaching thermohydraulic equilibrium. The soil–water retention curve (SWRC) of the bentonite followed a wetting scanning path before following the primary drying path exhibiting a shift in water retention with elevated temperature. Results from the tank-scale test can be used for validation of numerical simulations of drying processes in the engineered barrier system of a high-level radioactive waste geological disposal repository and confirm that a temperature-dependent hysteretic SWRC with scanning paths is required to accurately capture the bentonite response.

Engineering↗

DOE OSTI2018

Enhanced photocatalytic treatment of Cr(VI) and phenol by monoclinic BiVO4 with {010}-orientation growth

Highlights: • Removal of Cr(VI) and phenol in wastewater was greatly improved. • The reduction and oxidation processes were enhanced on {010} and {110} facets. • The selective transfer of charge carriers enhanced their separation. - Abstract: Photocatalytic technology has unique advantages in the purification of organic wastewater containing chromium(VI). Simultaneously photodegradation efficiency of Cr(VI) and phenol was significantly enhanced over BiVO{sub 4} with {010}-oriented growth. In this study, the effect of pH values in photoreduction of Cr(VI) and concentrations of phenol in the simultaneous photocatalytic reaction process were systematically analyzed based on characterizations about material physical properties. The results suggested that the enhanced photocatalytic activity over {010}-oriented BiVO{sub 4} was attributed to sufficient utilization of surface junction between {010} and {110}. These junctions achieved higher separation efficiency and selectively transfer of photogenerated charge carriers between two surfaces. Thus the photoreduction of Cr(VI) and photooxidation of phenol can selectively occur on the different crystal surfaces. This study demonstrates the possibility of purification of organic wastewater containing toxic heavy metals such as Cr(VI) using photocatalytic technology and provides new ideas and methods for the design of highly active photocatalytic materials.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2018

Final Technical Report: Imaging a Dry Storage Cask with Cosmic Ray Muons

The goal of this project is to build a scaled prototype system for monitoring used nuclear fuel (UNF) dry storage casks (DSCs) through cosmic ray muon imaging. Such a system will have the capability of verifying the content inside a DSC without opening it. Because of the growth of the nuclear power industry in the U.S. and the policy decision to ban reprocessing of commercial UNF, the used fuel inventory at commercial reactor sites has been increasing. Currently, UNF needs to be moved to independent spent fuel storage installations (ISFSIs), as its inventory approaches the limit on capacity of on-site wet storage. Thereafter, the fuel will be placed in shipping containers to be transferred to a final disposal site. The ISFSIs were initially licensed as temporary facilities for ~20-yr periods. Given the cancellation of the Yucca mountain project and no clear path forward, extended dry-cask storage (~100 yr.) at ISFSIs is very likely. From the point of view of nuclear material protection, accountability and control technologies (MPACT) campaign, it is important to ensure that special nuclear material (SNM) in UNF is not stolen or diverted from civilian facilities for other use during the extended storage.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Biomass-Derived Carbon and Their Composites for Supercapacitor Applications: Sources, Functions, and Mechanisms

Biomass-derived carbons are eco-friendly and sustainable materials, making them ideal for supercapacitors due to their high surface area, excellent conductivity, cost-effectiveness, and environmental benefits. This review provides valuable insights into biomass-derived carbon and modified carbon for supercapacitors, integrating both experimental results and theoretical calculations. This review begins by discussing the origins of biomass-derived carbon in supercapacitors, including plant-based, food waste-derived, animal-origin, and microorganism-generated sources. Then, this review presents strategies to improve the performance of biomass-derived carbon in supercapacitors, including heteroatom doping, surface functionalization, and hybrid composite construction. Furthermore, this review analyzes the functions of biomass-derived carbon in supercapacitors both in its pure form and as modified materials. The review also explores composites derived from biomass-based carbon, including carbon/MXenes, carbon/MOFs, carbon/graphene, carbon/conductive polymers, carbon/transition metal oxides, and carbon/hydroxides, providing a thorough investigation. Most importantly, this review offers an innovative summary and analysis of the role of biomass-derived carbon in supercapacitors through theoretical calculations, concentrating on four key aspects: energy band structure, density of states, electron cloud density, and adsorption energy. Finally, the review concludes the future research directions for biomass carbon-based supercapacitors, including the discovery of novel biomass materials, tailoring surface functional groups, fabricating high-performance composite materials, exploring ion transfer mechanisms, and enhancing practical applications. In summary, this review offers a thorough exploration of the sources, functions, and mechanisms of biomass-derived carbon in supercapacitors, providing valuable insights for future research.

biomass-derived carbon↗