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DOE OSTI2011

Advanced Nanostructured Molecular Sieves for Energy Efficient Industrial Separations

Due to the very small relative volatility difference between propane and propylene, current propane/propylene separation by distillation requires very tall distillation towers (150-250 theoretical plates) and large reflux ratios (up to 15), which is considered to be the most energy consuming large-scale separation process. Adsorptive separation processes are widely considered to be more energy-efficient alternatives to distillation. However, slow diffusion kinetics/mass transport rate through the adsorbent bed often limits the performance of such processes, so further improvements are possible if intra-particle mass transfer rates can be improved. Rive Technology, Inc. is developing and commercializing its proprietary mesoporous zeolite technology for catalysis and separation. With well-controlled intracrystalline mesoporosity, diffusion kinetics through such mesoporous zeolite based catalysts is much improved relative to conventional zeolites, leading to significantly better product selectivity. This 'proof-of-principle' project (DE-EE0003470) is intended to demonstrate that Rive mesoporous zeolite technology can be extended and applied in adsorptive propane/propylene separation and lead to significant energy saving compared to the current distillation process. In this project, the mesoporous zeolite Y synthesis technology was successfully extended to X and A zeolites that are more relevant to adsorbent applications. Mesoporosity was introduced to zeolite X and A for the first time while maintaining adequate adsorption capacity. Zeolite adsorbents were tested for liquid phase separation performance using a pulse flow test unit and the test results show that the separation selectivity of the mesoporous zeolite adsorbent is much closer to optimal for a Simulated Moving Bed (SMB) separation process and the enhanced mesoporosity lead to >100% increase of overall mass transport rate for propane and propylene. These improvements will significantly improve the performance of an adsorptive separation unit for propane/propylene separation compared with traditional zeolite adsorbents. The enhanced transport will allow for more efficient utilization of a given adsorbent inventory by reducing process cycle time, allowing a faster production rate with a fixed amount of adsorbent or smaller adsorbent inventory at a fixed production rate. Smaller adsorbent inventory would also lead to significant savings in the capital cost due to smaller footprint of the equipment. Energy consumption calculation, based on the pulse test results for rived NaX zeolite adsorbent, of a hypothetical moderate-scale SMB propane/propylene separation plant that processes 6000 BPSD refinery grade propylene (70% propylene) will consume about 60-80% less energy (both re-boiler and condenser duties) compared to a C3 splitter that process the same amount of feed. This energy saving also translates to a reduction of 30,000-35,000 tons of CO 2 emission per year at this moderate processing rate. The enhancement of mass transport achievable by introduction of controlled mesoporosity to the zeolite also opens the door for the technology to be applied to several other adsorption separation processes such as the separation of xylene isomers by SMB, small- and large scale production of O 2 /N 2 from air by pressure swing adsorption, the separation of CO 2 from natural gas at natural gas wellheads, and the purification of ultra-high purity H 2 from the off gas produced by steam-methane-reforming.

03 NATURAL GAS↗

DOE OSTI2021

Center for Gas Separations (CGS)

The total energy consumption in the U.S. has been rising steadily for decades, and it currently amounts to ~98,000 TBtu/yr, with approximately 30% of this total attributable to the industrial sector. Reasonable estimates indicate that 45–55% of total industry energy consumption derives from chemical separations, and for example, over 120 TBtu/yr alone is used in carrying out olefin/paraffin separations via energy-intensive cryogenic distillation. Therefore, the pursuit of new, even radically different approaches to some of the most energy-intensive industrial separations processes is an imperative scientific pursuit for reducing energy consumption toward a more sustainable future. Adsorbent and membrane-based separations can require a fraction of the energy needed for distillation methods, and as such are considered promising solutions for balancing increasing energy demand in the U.S. with the need for a massive reduction in energy consumption. Although considerable research effort has been devoted to the design of materials capable of carrying out various gas separations, usually operating through size-selective, chemisorptive, or physisorptive mechanisms, it remains a great challenge to design materials that function adequately for real-world applications. Indeed, the chemical and physical differences between molecules in gas mixtures of interest are often small, and therefore it is necessary, through the use of nanoscience and synthetic chemistry, to engineer unprecedented molecular-level control in adsorbate–adsorbent interactions. The overarching mission of the Center for Gas Separations (CGS) was to discover fundamental innovations that have the potential to dramatically reduce the energy associated with critical gas separations. In particular, the CGS developed novel synthetic routes, guided by molecular chemistry principles, as well as advanced characterization and computational methods, that have enabled the discovery of new materials and membranes tailor-made to exhibit exceptional performance for a range of gas separations processes, as required in the clean use of fossil fuels and in reducing CO 2 emissions from industry. A challenge of this magnitude required the collaboration and synergy of a large team of researchers with expertise in materials synthesis, characterization, and computations. During the 11-year project period, the CGS created a range of new materials within the family of highly-tunable, porous solids known as metal–organic frameworks (MOFs). These new frameworks demonstrate novel mechanisms for key industrial gas separations, including revolutionary new cooperative adsorption processes that enable low-energy CO 2 and CO capture, and are capable of efficiently separating olefins from paraffins, O 2 from air, and the shape-selective separation of alkane isomers. In addition, the CGS developed new strategies for incorporating these materials into composite membranes toward highly efficient and selective membrane-based separations. As a testament to the success of the CGS, two start-up companies, Mosaic Materials,4 Inc. and Flux Technology, Inc., grew out of these research efforts, and these companies are seeking to commercialize MOF and composite membranes materials for key separations in industry, including large-scale CO 2 capture and hydrocarbon separations, respectively. Another company, framergy, Inc., licensed IP resulting from CGS research toward the commercialization of adsorbents for various energy-relevant applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Porous Organic Cage Membranes for Molecular Gas Separations (Final Technical Report for DE-SC0021357)

This proposal aims at demonstrating the development of a novel family of membranes, composed of porous organic cages (POC) which offer the possibility of displaying high separation performance for challenging molecular gas separations relevant to natural gas purification, and olefin/paraffin separation. The proposed POCs synthesized in membrane form will display the most desirable properties of polymers (facile processability and flexibility) and inorganic materials (hierarchically ordered pores with molecular sieving properties) leading to highly selective and permeable membranes. POCs should display distinctive structural, compositional, adsorption and transport properties than those of conventional porous materials, opening the doors for a new research direction in membrane science, and gas separations. Our preliminary results demonstrate the feasibility of preparing POC crystals with controlled size, and continuous POC membranes with remarkable high permeances, and separation ability for CO 2 /CH 4 , N 2 /CH 4 and C 3 H 6 /C 3 H 8 separations serving as a solid foundation for our proposed work. Fundamentally, this proposal aims at elucidating separation mechanisms of different gas mixtures related to natural gas composition, and olefin/paraffin separation over porous organic cage membranes. The proposed research will result in fundamental understanding of adsorption and transport properties of industrially relevant gas molecules through novel microporous membranes, and may lead to the development of a cost effective membrane technology for natural gas purification, and olefin/paraffin separation surpassing the conventional benchmark technology distillation. Furthermore, we aim at demonstrating selective water transport through POC membranes, which can be positively impactful in numerous industrial applications in which water is present. The ability to fabricate thin, chemically and mechanically stable POC membranes for societal relevant gas separations constitute a new and distinctive direction in membrane science. Our proposed work aims at addressing some of the challenges recognized in the Research Agenda for Transforming Separation Science . Specifically: (a) advancing understanding of complex mixtures on separation performance; (b) exploring thermodynamic and kinetic mechanisms through the elucidation of separation mechanisms, and (c) study potential stability issues of the membranes to be assessed by evaluating the long term membrane stability and performance at various temperatures and pressures. The team is uniquely qualified to execute the proposed work. The PI has solid expertise in the rational molecular engineering design of porous crystalline membranes for molecular gas separations. The PNNL collaborator has extensive experience in the synthesis, characterization, and functional applications of microporous crystals, with particular emphasis on gas adsorption.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2002

Experimental Investigation of Separated and Transitional Boundary Layers Under Low-Pressure Turbine Airfoil Conditions

Modern low-pressure turbine airfoils are subject to increasingly stronger pressure gradients as designers impose higher loading in an effort to improve efficiency and to reduce part count. The adverse pressure gradients on the suction side of these airfoils can lead to boundary-layer separation, particularly under cruise conditions. Separation bubbles, notably those which fail to reattach, can result in a significant degradation of engine efficiency. Accurate prediction of separation and reattachment is hence crucial to improved turbine design. This requires an improved understanding of the transition flow physics. Transition may begin before or after separation, depending on the Reynolds number and other flow conditions, has a strong influence on subsequent reattachment, and may even eliminate separation. Further complicating the problem are the high free-stream turbulence levels in a real engine environment, the strong pressure gradients along the airfoils, the curvature of the airfoils, and the unsteadiness associated with wake passing from upstream stages. Because of the complicated flow situation, transition in these devices can take many paths that can coexist, vary in importance, and possibly also interact, at different locations and instances in time. The present work was carried out in an attempt to systematically sort out some of these issues. Detailed velocity measurements were made along a flat plate subject to the same nominal dimensionless pressure gradient as the suction side of a modern low-pressure turbine airfoil ('Pak-B'). The Reynolds number based on wetted plate length and nominal exit velocity, Re, was varied from 50;000 to 300; 000, covering cruise to takeoff conditions. Low, 0.2%, and high, 7%, inlet free-stream turbulence intensities were set using passive grids. These turbulence levels correspond to about 0.2% and 2.5% turbulence intensity in the test section when normalized with the exit velocity. The Reynolds number and free-stream turbulence level do not have a significant effect on the location of boundary-layer separation unless they are high enough to induce transition upstream of separation. The location and extent of the transition zone, in contrast, depend strongly on Re and TI. The beginning of reattachment closely follows the onset of transition. Under low free-stream turbulence conditions the boundary layer is laminar at separation and then begins to exhibit fluctuations in a finite frequency band in the shear layer over the separation bubble. These fluctuations are due to instability waves. The fluctuations grow in magnitude, higher harmonics are generated, and finally lead to a breakdown to turbulence. Transition begins in the shear layer, but quickly spreads to the near wall region and causes the boundary layer to reattach. The transition is rapid and the resulting turbulence contains a full range of high and low frequencies. Under high free-stream turbulence conditions, slowly growing low-frequency fluctuations are induced in the pretransitional boundary layer by the free-stream. The separation bubbles are considerably thinner than in the low TI cases, resulting in thinner boundary layers at the end of the test wall. At Re=50,000 and 100,000, the pre-transitional boundary layer separates at about the same location as in the low TI cases. Transition occurs through a bypass mode, begins upstream of the corresponding low-TI location, and proceeds in a manner similar to that of an attached boundary layer. Under high TI at Re=200,000 and 300,000, transition begins before separation. The boundary layer may separate, but if it does the separation bubble is very short and does not significantly affect the downstream development of the boundary layer. A comparison is made to previous work in a simulated cascade.

Hultgren, Lennart S.↗

NASA NTRS2002

Regaining Lost Separation in a Piloted Simulation of Autonomous Aircraft Operations

NASA is currently investigating a new concept of operations for the National Airspace System, designed to improve capacity while maintaining or improving current levels of safety. This concept, known as Distributed Air/Ground Traffic Management (DAG-TM), allows appropriately equipped autonomous aircraft to maneuver freely for flight optimization while resolving conflicts with other traffic and staying out of special use airspace and hazardous weather. While Airborne Separation Assurance System (ASAS) tools would normally allow pilots to resolve conflicts before they become hazardous, evaluation of system performance in sudden, near-term conflicts is needed in order to determine concept feasibility. If an acceptable safety level can be demonstrated in these situations, then operations may be conducted with lower separation minimums. An experiment was conducted in NASA Langley s Air Traffic Operations Lab to address issues associated with resolving near-term conflicts and the potential use of lower separation minimums. Sixteen commercial airline pilots flew a total of 32 traffic scenarios that required them to use prototype ASAS tools to resolve close range pop-up conflicts. Required separation standards were set at either 3 or 5 NM lateral spacing, with 1000 ft vertical separation being used for both cases. Reducing the lateral separation from 5 to 3 NM did not appear to increase operational risk, as indicated by the proximity to the intruder aircraft. Pilots performed better when they followed tactical guidance cues provided by ASAS than when they didn't follow the guidance. As air-air separation concepts are evolved, further studies will consider integration issues between ASAS and existing Airborne Collision Avoidance Systems (ACAS).These types of non-normal events will require the ASAS to provide effective alerts and resolutions prior to the time that an Airborne Collision Avoidance System (ACAS) would give a Resolution Advisory (RA). When an RA is issued, a pilot must take immediate action in order to avoid a potential near miss. The Traffic Alert and Collision Avoidance System (TCAS) II currently functions as an ACAS aboard commercial aircraft. Depending on the own aircraft s altitude, TCAS only issues RA s 15-35 seconds prior to the Closest Point of Approach (CPA). Prior to an RA, DAG-TM pilots operating autonomous aircraft must rely solely on ASAS for resolution guidance. An additional area of DAG-TM concept feasibility relates to a potential reduction in separation standards. Lower separation standards are likely needed in order to improve NAS efficiency and capacity. Current separation minimums are based in large part on the capabilities of older radar systems. Safety assessments are needed to determine the feasibility of reduced separation minimums. They will give strong consideration to surveillance system performance, including accuracy, integrity, and availability. Candidate surveillance systems include Automatic Dependent Surveillance-Broadcast (ADS-B) and multi-lateration systems. Considering studies done for Reduced Vertical Separation Minimums (RVSM) operations, it is likely that flight technical errors will also be considered. In addition to a thorough evaluation of surveillance system performance, a potential decision to lower the separation standards should also take operational considerations into account. An ASAS Safety Assessment study identified improper maneuvering in response to a conflict (due to ambiguous or improper resolution commands or a pilot s failure to comply with the resolution) as a potential safety risk. If near-term conflicts with lower separation minimums were determined to be more challenging for pilots, the severity of these risks could be even greater.

Barhydt, Richard↗

NASA NTRS2007

Active-Adaptive Control of Inlet Separation Using Supersonic Microjets

Flow separation in internal and external flows generally results in a significant degradation in aircraft performance. For internal flows, such as inlets and transmission ducts in aircraft propulsion systems, separation is undesirable as it reduces the overall system performance. The aim of this research has been to understand the nature of separation and more importantly, to explore techniques to actively control it. In this research, we extended our investigation of active separation control (under a previous NASA grant) where we explored the use of microjets for the control of boundary layer separation. The geometry used for the initial study was a simple diverging Stratford ramp, equipped with arrays of microjets. These early results clearly show that the activation of microjets eliminated flow separation. Furthermore, the velocity-field measurements, using PIV, also demonstrate that the gain in momentum due to the elimination of separation is at least an order of magnitude larger (two orders of magnitude larger in most cases) than the momentum injected by the microjets and is accomplished with very little mass flow through the microjets. Based on our initial promising results this research was continued under the present grant, using a more flexible model. This model allows for the magnitude and extent of separation as well as the microjet parameters to be independently varied. The results, using this model were even more encouraging and demonstrated that microjet control completely eliminated significant regions of flow separation over a wide range of conditions with almost negligible mass flow. Detailed studies of the flowfield and its response to microjets were further examined using 3-component PIV and unsteady pressure measurements, among others. As the results presented this report will show, microjets were successfully used to control the separation of a much larger extent and magnitude than demonstrated in our earlier experiments. In fact, using the appropriate combination of control parameters (microjet, location, angle and pressure) separation was completely eliminated for the largest separated flowfield we could generate with the present model. Separation control also resulted in a significant reduction in the unsteady pressures in the flow where the unsteady pressure field was found to be directly responsive to the state of the flow above the surface. Hence, our study indicates that the unsteady pressure signature is a strong candidate for a flow state sensor , which can be used to estimate the location, magnitude and other properties of the separated flowfield. Once better understood and properly utilized, this behavior can be of significant practical importance for developing and implementing online control.

Alvi, Farrukh S.↗

DOE OSTI2022

Methodology for assessing the maximum potential impact of separations opportunities in industrial processes

Separation technologies currently used in U.S. manufacturing industries are estimated to account for more than 20% of plant energy consumption. However, accurately determining the impact of new separation technology solutions can sometimes be difficult, especially when evaluating a slate of new candidate separation technologies, each of which has its own separation performance, energy demand, and capital cost. In these cases, a typical approach is to assess each new separation technology by collecting performance and cost information and then using that information to develop a techno-economic analysis to identify overall benefits. While this approach is thorough, it can be time consuming and can hinder reaching a critical understanding of the potential of a given separation challenge, especially when there is no known solution. To address these issues, we developed an assessment methodology, using industrial screening processes, that can be used to better understand the potential impacts of addressing a given separation challenge. This paper presents an overview of our separation challenge stream assessment methodology. The methodology involves defining an “ideal” separator and deriving the associated minimum separation energy. The “ideal” separator represents the most optimistic outlook of a given opportunity so the maximum impact from existing and not-yet-developed solutions can be assessed. Using established biorefinery models, we applied the methodology to 10 different separation challenge streams from two different biomass conversion platforms to identify the type of information that can be obtained. Three of the ten challenge streams assessed had maximum possible cost savings predictions >20%, and associated reductions in process energy carbon intensity ranging from 0 to 54%. Two streams had cost and energy savings potential that were < 5%. Some of the opportunity drivers from the various assessments include higher product yields, reduction or elimination of downstream equipment, new co-products, and cost savings associated with raw materials and energy consumption. The information from these assessments can help guide the selection or development of new separation technology solutions based on the various potential factors that drive the projected benefits.

09 BIOMASS FUELS↗

NASA NTRS2021

Separation at Crossing Waypoints Under Wind Uncertainty in Urban Air Mobility

To enable high-density operations in major metropolitan areas, urban air mobility networks are anticipated to have air traffic management with higher levels of autonomy. To ensure that this type of autonomy is feasible, one of the critical steps from a safety and efficiency perspective is understanding various factors that affect the spatial separation between airborne flights and ensure that these factors can be managed. In terms of separation assurance and scheduling, an important real-world concern is that future states of aircraft cannot be perfectly predicted. The focus of this research paper is to understand how these prediction errors affect separation and scheduling services and to explore mitigation strategies to handle these errors. In this research, we have simulated these types of uncertainty by adding wind-prediction errors to trajectory predictions for separation. With these wind-prediction errors, we decompose the problem into two separate questions. First, using both simulation and analytical methods, we look at conflict-detection-only scenarios to understand how the wind errors affect required minimum temporal separation between crossing flights to ensure a specific spatial separation. Next, we study how trajectory errors effect conflict resolution, and we explore different combinations of scheduling and separation assurance to mitigate the effects of uncertainty between crossing flights. The conflict resolution algorithm aims to minimize necessary temporal separation between crossing flights under uncertainty, still ensuring safety-critical spatial separation. In summary, this research suggests that the required minimum temporal separation at a crossing waypoint is dependent on factors such as inbound crossing angle, the relative angle between wind direction and bearing of each route, wind magnitude, wind magnitude uncertainty, nominal cruise airspeed of aircraft, and look-ahead time of the conflict detection algorithm. This research also suggests that different combinations of scheduling and separation have different qualitative results. Using a combination of strategic, flow-based scheduling, tactical scheduling at crossings, speed control near crossing points, and separation management leads to a system that is insensitive to trajectory prediction errors with high throughput and flexibility for aircraft away from shared resources.

urban air mobility↗

NASA NTRS2021

Separation at Crossing Waypoints Under Wind Uncertainty in Urban Air Mobility

urban air mobility↗

DOE OSTI2016

Enhanced separation of rare earth elements

Industrial rare earth separation processes utilize PC88A, a phosphonic acid ligand, for solvent extraction separations. The separation factors of the individual rare earths, the equipment requirements, and chemical usage for these flowsheets are well characterized. Alternative ligands such as Cyanex® 572 and the associated flowsheets are being investigated at the pilot scale level to determine if significant improvements to the current separation processes can be realized. These improvements are identified as higher separation factors, reduced stage requirements, or reduced chemical consumption. Any of these improvements can significantly affect the costs associated with these challenging separation proccesses. A mid/heavy rare earth element (REE) separations flowsheet was developed and tested for each ligand in a 30 stage mixer-settler circuit to compare the separation performance of PC88A and Cyanex® 572. The ligand-metal complex strength of Cyanex® 572 provides efficient extraction of REE while significantly reducing the strip acid requirements. Reductions in chemical consumption have a significant impact on process economics for REE separations. Partitioning results summarized Table 1 indicate that Cyanex® 572 offers the same separation performance as PC88A while reducing acid consumption by 30% in the strip section for the mid/heavy REE separation. Flowsheet Effluent Compositions PC88A Cyanex® 572 Raffinate Mid REE Heavy REE 99.40% 0.60% 99.40% 0.60% Rich Mid REE Heavy REE 2.20% 97.80% 0.80% 99.20% Liquor Strip Acid Required 3.4 M 2.3 M Table 1 – Flowsheet results comparing separation performance of PC88A and Cyanex® 572 for a mid/heavy REE separation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2012

Sulfur Hexafluoride Treatment of Used Nuclear Fuel to Enhance Separations

Reactive Gas Recycling (RGR) technology development has been initiated at Savannah River National Laboratory (SRNL), with a stretch-goal to develop a fully dry recycling technology for Used Nuclear Fuel (UNF). This approach is attractive due to the potential of targeted gas-phase treatment steps to reduce footprint and secondary waste volumes associated with separations relying primarily on traditional technologies, so long as the fluorinators employed in the reaction are recycled for use in the reactors or are optimized for conversion of fluorinator reactant. The developed fluorination via SF 6 , similar to the case for other fluorinators such as NF 3 , can be used to address multiple fuel forms and downstream cycles including continued processing for LWR via fluorination or incorporation into a aqueous process (e.g. modified FLUOREX) or for subsequent pyro treatment to be used in advanced gas reactor designs such metal- or gas-cooled reactors. This report details the most recent experimental results on the reaction of SF 6 with various fission product surrogate materials in the form of oxides and metals, including uranium oxides using a high-temperature DTA apparatus capable of temperatures in excess of 1000°C. The experimental results indicate that the majority of the fission products form stable solid fluorides and sulfides, while a subset of the fission products form volatile fluorides such as molybdenum fluoride and niobium fluoride, as predicted thermodynamically. Additional kinetic analysis has been performed on additional fission products. A key result is the verification that SF 6 requires high temperatures for direct fluorination and subsequent volatilization of uranium oxides to UF 6 , and thus is well positioned as a head-end treatment for other separations technologies, such as the volatilization of uranium oxide by NF 3 as reported by colleagues at PNNL, advanced pyrochemical separations or traditional full recycle approaches. Based on current results of the research at SRNL on SF 6 fluoride volatility for UNF separations, SF 6 treatment renders all anticipated volatile fluorides studied to be volatile, and all non-volatile fluorides studied to be non-volatile, with the notable exception of uranium oxides. This offers an excellent opportunity to use this as a head-end separations treatment process because: 1. SF 6 can be used to remove volatile fluorides from a UNF matrix while leaving behind uranium oxides. Therefore an agent such as NF 3 should be able to very cleanly separate a pure UF 6 stream, leaving compounds in the bottoms such as PuF 4 , SrF 2 and CsF after the UNF matrix has been pre-treated with SF 6 . 2. Due to the fact that the uranium oxide is not separated in the volatilization step upon direct contact with SF 6 at moderately high temperatures (≤ 1000°C), this fluoride approach may be well-suited for head-end processing for Gen IV reactor designs where the LWR is treated as a fuel stock, and it is not desired to separate the uranium from plutonium, but it is desired to separate many of the volatile fission products. 3. It is likely that removal of the volatile fission products from the uranium oxide should simplify both traditional and next generation pyroprocessing techniques. 4. SF 6 treatment to remove volatile fission products, with or without treatment with additional fluorinators, could be used to simplify the separations of traditional aqueous processes in similar fashion to the FLUOREX process. Further research should be conducted to determine the separations efficiency of a combined SF 6 /NF 3 separations approach which could be used as a stand-alone separations technology or a head-end process.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1988

Unsteady three-dimensional flow separation

A concise mathematical framework is constructed to study the topology of steady 3-D separated flows of an incompressible, or a compressible viscous fluid. Flow separation is defined by the existence of a stream surface which intersects with the body surface. The line of separation is itself a skin-friction line. Flow separation is classified as being either regular or singular, depending respectively on whether the line of separation contains only a finite number of singular points or is a singular line of the skin-friction field. The special cases of 2-D and axisymmetric flow separation are shown to be of singular type. In regular separation it is shown that a line of separation originates from a saddle point of separation of the skin-friction field and ends at nodal points of separation. Unsteady flow separation is defined relative to a coordinate system fixed to the body surface. It is shown that separation of an unsteady 3-D incompressible viscous flow at time t, when viewed from such a frame of reference, is topologically the same as that of the fictitious steady flow obtained by freezing the unsteady flow at the instant t. Examples are given showing effects of various forms of flow unsteadiness on flow separation.

Hui, W. H.↗

NASA NTRS1996

Separator Materials Used in Secondary Alkaline Batteries Characterized and Evaluated

Nickel-cadmium (Ni/Cd) and nickel-hydrogen (Ni/H2) secondary alkaline batteries are vital to aerospace applications. Battery performance and cycle life are significantly affected by the type of separators used in those batteries. A team from NASA Lewis Research Center's Electrochemical Technology Branch developed standardized testing procedures to characterize and evaluate new and existing separator materials to improve performance and cycle life of secondary alkaline batteries. Battery separators must function as good electronic insulators and as efficient electrolyte reservoirs. At present, new types of organic and inorganic separator materials are being developed for Ni/Cd and Ni/H2 batteries. The separator material previously used in the NASA standard Ni/Cd was Pellon 2505, a 100-percent nylon-6 polymer that must be treated with zinc chloride (ZnCl2) to bond the fibers. Because of stricter Environmental Protection Agency regulation of ZnCl2 emissions, the battery community has been searching for new separators to replace Pellon 2505. As of today, two candidate separator materials have been identified; however, neither of the two materials have performed as well as Pellon 2505. The separator test procedures that were devised at Lewis are being implemented to expedite the search for new battery separators. The new test procedures, which are being carried out in the Separator Laboratory at Lewis, have been designed to guarantee accurate evaluations of the properties that are critical for sustaining proper battery operation. These properties include physical and chemical stability, chemical purity, gas permeability, electrolyte retention and distribution, uniformity, porosity, and area resistivity. A manual containing a detailed description of 12 separator test procedures has been drafted and will be used by the battery community to evaluate candidate separator materials for specific applications. These standardized procedures will allow for consistent, uniform, and reliable results that will ensure that separator materials have the desired properties for long life and good performance in secondary alkaline cells.

Source record↗

NASA NTRS2009

Detection of Subsurface Material Separation in Shuttle Orbiter Slip-Side Joggle Region of the Wing Leading Edge using Infrared Imaging Data from Arc Jet Tests

The objective of the present study was to determine whether infrared imaging (IR) surface temperature data obtained during arc-jet tests of Space Shuttle Orbiter s reinforced carbon-carbon (RCC) wing leading edge panel slip-side joggle region could be used to detect presence of subsurface material separation, and if so, to determine when separation occurs during the simulated entry profile. Recent thermostructural studies have indicated thermally induced interlaminar normal stress concentrations at the substrate/coating interface in the curved joggle region can result in local subsurface material separation, with the separation predicted to occur during approach to peak heating during reentry. The present study was an attempt to determine experimentally when subsurface material separations occur. A simplified thermal model of a flat RCC panel with subsurface material separation was developed and used to infer general surface temperature trends due to the presence of subsurface material separation. IR data from previously conducted arc-jet tests on three test specimens were analyzed: one without subsurface material separation either pre or post test, one with pre test separation, and one with separation developing during test. The simplified thermal model trend predictions along with comparison of experimental IR data of the three test specimens were used to successfully infer material separation from the arc-jet test data. Furthermore, for the test specimen that had developed subsurface material separation during the arc-jet tests, the initiation of separation appeared to occur during the ramp up to the peak heating condition, where test specimen temperature went from 2500 to 2800 F.

Daryabeigi, Kamran↗

DOE OSTI2012

Ruthenium Behavior at Phase Separation of Borosilicate Glass-12259

The Rokkasho reprocessing plant (RRP) located in Aomori, Japan, vitrifies high level waste (HLW) into a borosilicate glass. The HLW is generated from the reprocessing of spent fuel and contains ruthenium (Ru) and other platinum group metals (PGMs). Based on the recent consequences after a huge earthquake that occurred in Japan, a hypothetical blackout was postulated for the RRP to address additional safety analysis requirements. During a prolonged blackout, the borosilicate glass could phase separate due to cooling of the glass in the melter. The Ru present in the glass matrix could migrate into separate phases and impact the durability of the borosilicate glass. The durability of the glass is important for quality assurance and performance assessment of the vitrified HLW. A fundamental study was performed at an independent university to understand the impact of a prolonged blackout. Simulated HLW glasses were prepared for the RRP, and the Ru behavior in phase separated glasses was studied. The simulated HLW glasses contained nonradioactive elements and PGMs. The glass compositions were then altered to enhance the formation of the phase-separated glasses when subjected to thermal treatment at 700 deg. C for 24 hours. The synthesized simulated glasses contained 1.1 % Ru by weight as ruthenium dioxide (RuO{sub 2}). A portion of the RuO{sub 2} formed needle-shaped crystals in the glass specimens. After the thermal treatment, the glass specimen had separated into two phases. One of the two phases was a B{sub 2}O{sub 3} rich phase, and the other phase was a SiO{sub 2} rich phase. The majority of the chemical species in the B{sub 2}O{sub 3} rich phase was leached away with the Material Characterization Center-3 (MCC-3) protocol standardized by the Pacific Northwest National Laboratory using an aqueous low-concentrated nitric acid solution, but the leaching of the Ru fraction was very limited; less than 1% of the original Ru content. The Ru leaching was much less than those of the other elements, and the needle-shaped crystals of RuO{sub 2} were observed in the B{sub 2}O{sub 3} rich phase in the specimen after the leaching test. Another experiment was performed using another glass specimen which had been prepared with the same frits, but used reagent RuO{sub 2} of granular shape at lower content (0.0073% by weight as RuO{sub 2}). The leached fractions of elements for the latter specimen increased to almost the same fraction (more than 10% of the original Ru content) as observed for boron and sodium, when the phase separated glass was leached using the MMC-3 protocol with non-acidic de-ionized water. Based on the results of this study, it was concluded that needle-shaped RuO{sub 2} crystals are contained in the B{sub 2}O{sub 3}-rich phase after phase separation of the borosilicate glass after a hypothetical blackout. The leaching fraction for the needle-shaped RuO{sub 2} present in the phase separated glass is much lower than those for boron or sodium. Ruthenium behavior has been studied for a hypothetical loss of cooling in the liquid fed ceramic melter for high level waste by taking into account the phase separation of borosilicate glass. The needle-shaped crystal of ruthenium dioxide after bi-nodal-type phase separation of the borosilicate glass at 700 deg. C migrated into the B{sub 2}O{sub 3} rich phase, but remained without dissolution by an acidic aqueous solution. Additionally, granular ruthenium dioxide can be a morphological form of ruthenium after bimodal-type phase separation of the vitrified high level waste with borosilicate glass media. After the phase separation of the borosilicate glass, the crystal shape of the ruthenium dioxide is either needle-shaped or granular, and the leachable fraction of ruthenium is relatively much lower than those of major components (boron and sodium) in the vitrified borosilicate glass. The fraction of leached ruthenium increased to almost the same fraction as observed for boron and sodium when the phase-separated glass was leached with ultrapure water. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2019

Kr/Xe SeparatioKr/Xe Separation over Metal Organic Framework Membranes

The central thrust of this project is to develop a novel family of continuous membranes, composed of porous crystalline membranes (mainly metal organic frameworks) which offer the possibility of demonstrating high separation performance for Kr/Xe gas mixtures. The specific objectives of the proposed work are: (1) The development of continuous and reproducible MOF membranes on porous tubular supports displaying high Kr permeabilities and high Kr/Xe separation selectivities.(2) Demonstrating the membrane performance long term stability.(3) Establish the basic structure/separation relationships of MOF membranes in Kr/Xe separations, and (4) Demonstrating that membrane synthesis could be amenable to large scale production. We have demonstrated that porous crystalline molecular sieve membranes including metal organic frameworks, zeolites, and alumino phosphates can effectively separate Kr/Xe gas mixtures ate industrially relevant compositions. Specifically, these three compositions correspond to a different family of microporous crystals, namely zeolites (SAPO-34), metal organic frameworks (ZIF-8) and alumino phosphates (AlPO-18). SAPO-34 membranes displayed the best overall separation performance, while AlPO-18 membranes displayed the highest Kr permeances. The key factors affecting the separation selectivity and permeance of these membranes were identified, and decoupled. The presence of rigid micropores with size lying between Kr and Xe atomic sizes, lower Xe/Kr uptakes (adsorption selectivity), and lower concentration of non-selective pores led to the highest observed Kr/Xe separation selectivities among these three microporous crystals, which corresponded to SAPO-34. The Kr permeances for these three microporous crystalline membrane compositions decreased exponentially with membrane thickness. The best membranes separated Kr/Xe gas mixtures with separation selectivities as high as 45 and Kr permeances ~ as high as 1.2 x 10 -7 mol/m 2 s Pa. In addition, SAPO-34 and ZIF-8 membranes were effective in separating Air/Xe mixtures. With separation selectivities as high as 30, and air permeances of 2.3 x 10 -7 mol/m 2 s Pa. Finally, we explore the synthesis in powder form of other potentially suitable porous crystals that if prepared in membrane form could be highly appealing candidates for Kr/Xe and Air/Xe separation. These crystals are porous organic cages which potentially can molecular sieve Kr and air from Xenon based on the unimodal pore sizes lying between the size of the permeant molecules.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2016

Hydrogen Isotope Separation from Aqueous Streams using Zeolite Membranes

Efficient separation of heavy hydrogen isotopes {sup 3}H (or T, tritium) and {sup 2}H (or D, deuterium) from {sup 1}H has been a long-standing endeavor in nuclear fuel cycle research and development. For example, tritium (half-life 12.3 years) is a fission product from nuclear plants and is found as tritiated water (HTO) in effluent streams from nuclear installations. Tritium must be concentrated and removed from such aqueous streams for waste storage. The separation of deuterium from deuterated water (HDO) has applications in heavy water production, and can also be used as a nonradioactive simulant in HTO separation research. Several methods have been explored such as ion exchange/adsorption and membrane permeation. Adsorption by molecular sieving materials such as zeolites can separate tritiated water from water with moderate selectivity (HTO/H{sub 2}O separation factor∼1.2-1.4) due to a subtle difference in adsorption characteristics between the two species. However, there remains a requirement for high-selectivity continuous separation of heavy hydrogen isotopes from water. Here we demonstrate new results on the use of zeolite membranes as a potential high-performance, low-cost, radiation-stable candidate for such separations. In zeolite membranes, separation of HTO (or HDO) from water would take place by a combination of adsorption and diffusion characteristics. Here we describe the hydrogen isotope separation properties of silicoaluminophosphate (SAPO-34) membranes synthesized on porous α-alumina supports. D{sub 2}O/H{sub 2}O feed mixtures of realistic compositions are used as a non-radioactive simulant for tritiated water feeds. Our results show promising applications of zeolite membranes for hydrogen isotope separation and recovery. In summary, SAPO-34 membranes were fabricated and investigated to demonstrate their pervaporative separation properties for D{sub 2}O-H{sub 2}O binary systems. These membrane exhibit high selectivity (up to ∼19) for D{sub 2}O and good permeance (> 600 GPU) even at low concentrations of D{sub 2}O in the feed, making them highly interesting candidates for capture of heavy hydrogen isotopes (D and T) from aqueous streams encountered in the nuclear fuel cycle. The mechanism of separation appears to involve both diffusivity and adsorption differences as expected in nanoporous materials, even though detailed identification of their respective contributions is a subject of future work. We also hypothesize that tritiated (T{sub 2}O/H{sub 2}O) mixtures will also show similar performance in relation to the present deuterated mixtures. This is planned to be further investigated through pervaporation measurements. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2005

Rotary Drum Separator and Pump for the Sabatier Carbon Dioxide Reduction System

A trade study conducted in 2001 selected a rotary disk separator as the best candidate to meet the requirements for an International Space Station (ISS) Carbon Dioxide Reduction Assembly (CRA). The selected technology must provide micro-gravity gasfliquid separation and pump the liquid from 10 psia at the gasfliquid interface to 18 psia at the wastewater bus storage tank. The rotary disk concept, which has pedigree in other systems currently being built for installation on the ISS, failed to achieve the required pumping head within the allotted power. The separator discussed in this paper is a new design that was tested to determine compliance with performance requirements in the CRA. The drum separator and pump @SP) design is similar to the Oxygen Generator Assembly (OGA) Rotary Separator Accumulator (RSA) in that it has a rotating assembly inside a stationary housing driven by a integral internal motor. The innovation of the DSP is the drum shaped rotating assembly that acts as the accumulator and also pumps the liquid at much less power than its predecessors. In the CRA application, the separator will rotate at slow speed while accumulating water. Once full, the separator will increase speed to generate sufficient head to pump the water to the wastewater bus. A proof-of- concept (POC) separator has been designed, fabricated and tested to assess the separation efficiency and pumping head of the design. This proof-of-concept item was flown aboard the KC135 to evaluate the effectiveness of the separator in a microgravity environment. This separator design has exceeded all of the performance requirements. The next step in the separator development is to integrate it into the Sabatier Carbon Dioxide Reduction System. This will be done with the Sabatier Engineering Development Unit at the Johnson Space Center.

Holder, Don↗