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DOE OSTI2020

Experimental Investigation on Separation Behavior of Heavy-Oil Emulsion for Polymer Flooding on Alaska North Slope

The first-ever field pilot on Alaska North Slope (ANS) to validate using polymer floods for heavy-oil enhanced oil recovery is currently ongoing. One of the major concerns of the operator is the effect of polymer on oil/water-separation efficiency after polymer breakthrough. This work investigates the influence of polymer on the separation behavior of heavy-oil emulsions and evaluates the performance of emulsion breakers (EBs). In this study, two types of heavy-oil emulsions were prepared and tested at 20 and 50% water cut (WC), respectively. The bottle test method was used in the experiments, in which the separated water volume with time, the separated water quality, and the volume fraction of phases were recorded. Results showed that polymer accelerated the oil/water separation acting as an emulsion inhibitor at 20% WC but tended to impede the water separation at 50% WC. Regardless of WC, polymer resulted in poor water quality and the formation of a stable intermediate oil in water (o/w) emulsion, because of the increased viscosity of the water phase. The performance of EBs showed a complex dependency on the WC, the type of demulsifier and dosage, and the polymer concentration. Despite the varied conditions encountered in the heavy-oil/water/polymer/demulsifier system, a compound EB achieved satisfactory demulsification performance, showing the highest potential for deployment in the current ANS polymer flooding pilot. Here, we systematically studied the potential influence of polymer breakthrough on the separation behavior of heavy-oil emulsion on ANS for the first time. The findings of this study will provide practical guidance in advance for produced fluid treatment of the ongoing first-ever polymer flooding pilot on ANS.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

Atomically Precise Membranes for the Separation of Gases

Industrial separations require enormous amounts of energy, accounting for approximately half the industrial energy use and 10–15% of the total energy consumption. Distillation alone accounts for about half the energy demand for industrial separations. If these processes could be replaced by an energy-efficient membrane separation process, this energy demand could be reduced by 90%. However, although some membrane processes have made inroads into thermal distillation, for membrane-based separations to replace the distillation process to a far more significant and practical level, new membranes with higher robustness, selectivity, and flux still need be developed. In this membrane development program, we leveraged Temple University’s prior work in spiroligomers to develop robust membrane structures. These structures can be formed into atomically precise pores by controlling the chemical synthesis and the oligomer building blocks to first build precisely controlled macrocycles and then subsequently crosslinking these macrocycles to produce a membrane. Furthermore, through the highly controllable chemistry of our molecular building blocks, not only can we integrate pores with highly controllable and reproducible size and morphology, but we can also target internal functionalization. By using a range of scalable membrane synthesis approaches, combined with control of each and every pores internal chemistry and molecular conformation we can achieve membrane structures that can display the ultimate in high selectivity and permeance. The Mainstream-Temple University membranes can be designed to achieve ultra-selective separations based on the key factors of molecular size, shape, and functionality. In our approach to fabricate scalable atomically precise membranes, we used our molecular Lego nanostructures. We demonstrated an approach to create atomically precise pores within the membrane with pores that are the dimensions of the molecule we are trying to separate. Moreover, in addition to controlling the morphology of the membrane structure by controlling the size of every pore, we can also decorate every pore with precisely targeted and placed functional groups. These accurately placed functional groups can provide selective binding to molecules and provide enhanced selectivity via a facilitated transport mechanism. In Phase II, the Mainstream-Temple University team demonstrated the scalable synthesis of oligomers and the ability to control the pore internal and external functionality, or chemistry, to allow the fabrication of a thin-film membrane. The initial steps of the spiroligomer synthesis to produce the two key bis-amino enantiomer building blocks were scaled from the gram scale to the kilogram scale, obtaining 25 kg of the materials by transferring the procedure to a toll manufacturer. Finally, we successfully optimized the fabrication of these macrocycles into robust membranes. We successfully transitioned from a laboratory based, hard-to-scale Langmuir trough synthesis to a highly scalable, roll-to-roll applicable, interfacial polymerization process. During this Phase II program, we established a platform of atomically precise membranes where our highly controllable, atomically precise macrocycles served as a scaffold with precisely and uniformly controlled pores. Furthermore, this layer can be tailored to accommodate a diverse range of functional groups, which both further controlled the pore size to enhance the sieving effect as well as imparting precisely controlled targeted selectivity through biomimetic molecular interactions. In this Phase II, we established and scaled up a platform approach to both tune the pore size and chemistry as well as scale it to produce membranes that can be applied to a wide range of industries. In future development, the project team expects to scale up both the macrocycle building block production and interfacial polymerization process to produce the atomically precise membrane with targeted pore sizes and pore chemistries.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Development of Carbon Molecular Sieves Hollow Fiber Membranes based on Polybenzimidazole Doped with Polyprotic Acids with Superior H 2 /CO 2 Separation Properties (Final Report)

The goal of this project was to develop a highly efficient membrane-based process to capture CO 2 from coal-derived syngas with 95% CO 2 purity, achieving the cost of electricity (COE) 30% below the baseline capture approaches (i.e., Selexol process) when coupled with the advancement in other areas of the power generation facility. Our core approach is based on high-permeance hollow fiber membranes (HFMs) with superior H 2 /CO 2 separation properties at the syngas process conditions, which can then be further utilized to design membrane reactors for process intensification of H 2 production and purification and CO 2 capture. Three organizations with complementary skills collaborated to achieve the goal, including the University at Buffalo (UB), Los Alamos National Laboratory (LANL), and Trimeric Corporation (Trimeric). We formulated logical steps to bring the membrane technology from Technology Readiness Level (TRL) 3 (Experimental proof of concept) to TRL 4 (Laboratory scale validation in relevant environment). During the budget period (BP) 1, we screened various polymeric materials and identified polybenzimidazole doped with inorganic polyprotic acids as the desirable platform. The acid doping increases the H 2 /CO 2 selectivity, and the sequential carbonization increases H 2 permeability while retaining the high selectivity. By manipulating the acid type and doping level and the carbonization temperature, we demonstrated advanced carbon molecular sieving (CMS) materials with H 2 permeability of above 200 Barrer (1 Barrer = 10 -10 cm 3 (STP) cm cm -2 s -2 cmHg -1 ) and H 2 /CO 2 selectivity of above 40 at 200-300°C with simulated syngas containing CO and water vapor. For example, the PBI-(H 3 PO 4 ) 0.11 carbonized at 700 °C exhibits H 2 permeability of 200 Barrer and H 2 /CO 2 selectivity of 60 at 200 °C, and H 2 permeability of 240 Barrer and H 2 /CO 2 selectivity of 54 at 225 °C, which meets the targeted properties and surpasses Robeson’s upper bound. During the BP2, we focused on the conversion of the advanced CMS materials to stable HFMs. Membranes with H 2 permeance of 1,090 GPU (1 GPU = 10 -6 cm 3 (STP) cm -2 s -2 cmHg -1 ) and H 2 /CO 2 selectivity of 57 at 300 °C were successfully fabricated. The effects of temperature, gas compositions, pressure, and time on the separation properties were systematically investigated. Pencil modules were continuously evaluated for 219 h (dry pure gas) and 669 h (dry simulated syngas) and showed initial decline in permeance and increased H 2 /CO 2 selectivity over time, ultimately achieving a steady state stable value, indicating that the ageing phenomena in the nanoporous structures of the membranes during the test. Membrane reactors were fabricated based on the CMS membranes and evaluated for water-gas shift (WGS) reaction. The use of membranes slightly improves the conversion of the CO. However, parametric tests of the membrane reactors at various temperatures and flow rates need to be conducted, as well as the membranes with improved separation performance. We performed a sensitivity analysis on the impact of H 2 /CO 2 selectivity on the COE based on a hybrid process of a membrane unit and cryogenic unit developed by Membrane Technology and Research, Inc. (MTR). Three H 2 /CO 2 selectivity (40, 60, and 15) cases were developed and compared with the baseline capture process (Case B5B) provided by the DOE report. Increasing the membrane H 2 /CO 2 selectivity reduces COE, but the rate of the decrease of COE also diminishes. The COE values for H 2 /CO 2 selectivities of 40 and 60 were nearly the same. As the H 2 /CO 2 selectivity increases, the inert recycling decreases, leading to smaller equipment, less auxiliary power requirements, and less heating, cooling, and refrigeration duty. The refrigeration system used to liquefy the CO 2 is the most expensive piece of equipment and consumes the most electricity within the CO 2 capture process. Increasing the CO 2 concentration in the recycle stream would improve the economics of the process by reducing the refrigeration duty requirement of the unit and also allow for higher liquefaction temperatures. The high H 2 -selective membrane developed by our team may be applicable in other separation processes where lower pressure H 2 retains value. Typically, hydrogen retains its pressure when it is separated from syngas components. Residual components may be used as low-quality fuel and then vented to the atmosphere. Applications might include control of H 2 /CO ratios or mitigation of the water gas shift reaction by CO 2 recycling to the feed of a gasifier or steam methane reformer. To summarize, we have developed industrial HFMs with the best H 2 /CO 2 separation performance reported in the literature. The membranes demonstrate stability with simulated syngas and show great potential for membrane reactors for WGS reactions, lowering the cost of blue H 2 production.

20 FOSSIL-FUELED POWER PLANTS↗

DOE OSTI2023

Toward a Photomagnetic Mechanism for f-element separations (Final Technical Report)

The intent behind this proposal was to evaluate magnetic field effects of rare-earth ions on radical pairs. Rare-earth ions are notoriously challenging to separate based on similar thermodynamic characteristics (e.g. solubility) or ion radius, whereas magnetism varies starkly from rare-earth to rare-earth, even when ions are immediately adjacent on the periodic table. Magnetism could be a useful property then for separations, but a mechanism that is effective and selective for magnetic characteristics must be produced. A reactive mechanism for separations could likewise be interesting for selective separations, if a magnetic handle for such a separation could be defined. This proposal sought to understand a specific reactive, magnetic handle for a reactive separations scheme by creating proof of concept model complexes that place rare earths in proximity to photochemically active functional groups.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

The Effect of Acceleration on the Separation Force in Constrained-Surface Stereolithography

Constrained-surface-based stereolithography has recently attracted much attention from both academic and industrial communities. Despite numerous experimental, numerical and theoretical efforts, the fundamental need to reduce the separation force between the newly cured part and constrained surface has not yet been completely solved. In this paper, we develop a fluid dynamics approach, proposed in our previous work, to theoretically model the separation force in 3D printing of a cylindrical part for flat and patterned windows. We demonstrate the possibility of separation force reduction with an accelerated movement of the printing platform. In particular, we investigate behaviors of transient parameter, its reduction rate, and separation force reduction with respect to elevation speed and time. The proposed approach involves deceleration and acceleration stages and allows to achieve the force reduction for the entire printing process. Finally, we provide implicit analytical solutions for time moments when switching between the stages can be done without noticeable increase of separation force and explicit expression for separation force in case of patterned window.

Gritsenko, Dmitry (ORCID:0000000248181512)↗

NASA NTRS1972

Booster recovery following premature space shuttle stage separation

Abort criteria necessary to satisfy space shuttle program requirements to include intact vehicle abort capability are discussed. Intact abort implies the ability of the booster and orbiter to separate and both continue flight to a safe landing, with a full payload aboard the orbiter. Obviously, the requirement to separate early along the ascent trajectory presupposes critical operational problems that are probably booster problems and may preclude booster recovery. On the other hand, some critical problems while mated can become manageable when separated and should result in full booster recovery. All critical orbiter problems fall into this category; since stage separation without orbiter thrust is a capability of some separation system concepts, booster stage recovery following separation is a requirement.

Hurley, M. J.↗

NASA NTRS1973

Prediction of fluctuating pressure environments associated with plume-induced separated flow fields

The separated flow environment induced by underexpanded rocket plumes during boost phase of rocket vehicles has been investigated. A simple semi-empirical model for predicting the extent of separation was developed. This model offers considerable computational economy as compared to other schemes reported in the literature, and has been shown to be in good agreement with limited flight data. The unsteady pressure field in plume-induced separated regions was investigated. It was found that fluctuations differed from those for a rigid flare only at low frequencies. The major difference between plume-induced separation and flare-induced separation was shown to be an increase in shock oscillation distance for the plume case. The prediction schemes were applied to PRR shuttle launch configuration. It was found that fluctuating pressures from plume-induced separation are not as severe as for other fluctuating environments at the critical flight condition of maximum dynamic pressure.

Plotkin, K. J.↗

NASA NTRS1977

Space shuttle engineering and operations support. ALT separation reference trajectories for tailcone on orbiter forward and aft CG configurations. Mission planning, mission analysis and software formulation

A preflight analysis of the ALT separation reference trajectories for the tailcone on, forward, and aft cg orbiter configurations is documented. The ALT separation reference trajectories encompass the time from physical separation of the orbiter from the carrier to orbiter attainment of the maximum ALT interface airspeed. The trajectories include post separation roll maneuvers by both vehicles and are generated using the final preflight data base. The trajectories so generated satisfy all known separation design criteria and violate no known constraints. The requirement for this analysis is given along with the specifications, assumptions, and analytical approach used to generate the separation trajectories. The results of the analytical approach are evaluated, and conclusions and recommendations are summarized.

Glenn, G. M.↗

NASA NTRS1979

Improved, low cost inorganic-organic separators for rechargeable silver-zinc batteries

Several flexible, low-cost inorganic-organic separators with performance characteristics and cycle life equal to, or better than, the Lewis Research Center Astropower separator were developed. These new separators can be made on continuous-production equipment at about one-fourth the cost of the Astropower separator produced the same way. In test cells, these new separators demonstrate cycle life improvement, acceptable operating characteristics, and uniform current density. The various separator formulas, test cell construction, and data analysis are described.

Sheibley, D. W.↗

NASA NTRS1982

Separated trailing-edge flow at a transonic Mach number

Results from an experimental investigation of a small-scale separated flow at a sharp trailing edge are presented. The separated flow was a result of sustained adverse pressure gradients. Experiments were carried out at a transonic Mach number, without any shock wave in the flow, and at a high Reynolds number. Measurements include surface pressure distributions, mean velocity, turbulent shear stress, turbulent kinetic energy, and some streamwise turbulence intensity profiles in the region from just upstream of separation to downstream into the near-wake, following wake-closure. The results show noticeable changes in the mean and turbulent quantities in the separated region although the wall adverse pressure gradients are relatively weak. Turbulent normal stress becomes important in the vicinity of separation and in the separated zone with regard to both mean-flow development and turbulence-energy production. The experimental data are used to assess the performance of two boundary-layer calculation methods.

Viswanath, P. R.↗

NASA NTRS1983

Diffusive separation of binary mixtures of CO2-H2 in a sonic-orifice expansion

The separation of binary gas mixtures of carbon dioxide and hydrogen in sonic-orifice-generated free jets is investigated over a source Reynolds number range of 100 to 3000 using the well-known electron beam fluorescence technique. The lighter species, hydrogen, is chosen as the minor species in order to examine the extent of the validity of Sherman's first-order diffusive separation theory for large separation. The diffusive separation of mixtures containing approximately 2, 5, and 20 percent hydrogen in carbon dioxide is investigated by experimentally determining the relative number densities of the two species as a function of centerline axial distance within the free jets. Sherman's diffusive separation theory is applied to the jets using axial Mach number profiles which were a combination of experimental and analytical results for gamma = 1.40 expansions. The gamma = 1.40 expansion is shown to approximate the CO2-H2 expansion quite well, and the calculated separation agrees remarkably well with the experimentally determined values.

Mccay, T. D.↗

NASA NTRS1987

Control of vortical separation on conical bodies

In a variety of aeronautical applications, the flow around conical bodies at incidence is of interest. Such applications include, but are not limited to, highly maneuverable aircraft with delta wings, the aerospace plane and nose portions of spike inlets. The theoretical model used has three parts. First, the single line vortex model is used within the framework of slender body theory, to compute the outer inviscid field for specified separation lines. Next, the three dimensional boundary layer is represented by a momentum equation for the cross flow, analogous to that for a plane boundary layer; a von Karman Pohlhausen approximation is applied to solve this equation. The cross flow separation for both laminar and turbulent layers is determined by matching the pressure at the upper and lower separation points. This iterative procedure yields a unique solution for the separation lines and consequently for the position of the vortices and the vortex lift on the body. Lastly, control of separation is achieved by blowing tangentially from a slot located along a cone generator. It is found that for very small blowing coefficients, the separation can be postponed or suppressedy completely.

Mourtos, Nikos J.↗

NASA NTRS1988

Surface flow visualization of separated flows on the forebody of an F-18 aircraft and wind-tunnel model

A method of in-flight surface flow visualization similar to wind-tunnel-model oil flows is described for cases where photo-chase planes or onboard photography are not practical. This method, used on an F-18 aircraft in flight at high angles of attack, clearly showed surface flow streamlines in the fuselage forebody. Vortex separation and reattachment lines were identified with this method and documented using postflight photography. Surface flow angles measured at the 90 and 270 degrees meridians show excellent agreement with the wind tunnel data for a pointed tangent ogive with an aspect ratio of 3.5. The separation and reattachment line locations were qualitatively similar to the F-18 wind-tunnel-model oil flows but neither the laminar separation bubble nor the boundary-layer transition on the wind tunnel model were evident in the flight surface flows. The separation and reattachment line locations were in fair agreement with the wind tunnel data for the 3.5 ogive. The elliptical forebody shape of the F-18 caused the primary separation lines to move toward the leeward meridian. Little effect of angle of attack on the separation locations was noted for the range reported.

Fisher, David F.↗

NASA NTRS1989

On the Lagrangian description of unsteady boundary layer separation. Part 2: The spinning sphere

A theory to explain the initial stages of unsteady separation was proposed by Van Dommelen and Cowley (1989). This theory is verified for the separation process that occurs at the equatorial plane of a sphere or a spheroid which is impulsively spun around an axis of symmetry. A Lagrangian numerical scheme is developed which gives results in good agreement with Eulerian computations, but which is significantly more accurate. This increased accuracy, and a simpler structure to the solution, also allows verification of the Eulerian structure, including the presence of logarithmic terms. Further, while the Eulerian computations broke down at the first occurrence of separation, it is found that the Lagrangian computation can be continued. It is argued that this separated solution does provide useful insight into the further evolution of the separated flow. A remarkable conclusion is that an unseparated vorticity layer at the wall, a familiar feature in unsteady separation processes, disappears in finite time.

Vandommelen, Leon L.↗

NASA NTRS1989

Computation of Navier-Stokes equations for three-dimensional flow separation

Supersonic flows over a sharp and a flat-faced blunt fin mounted on a flat plate are simulated numerically. Several basic issues involved in the resultant three-dimensional steady flow separation are studied. Using the same number of grid points, different grid spacings are employed to investigate the effects of a grid resolution on the origin of the line of separation. Various shock strengths are used to study the so-called separated and unseparated boundary layer and to establish the existence or absence of secondary separation. The length of separation ahead of the flat-faced blunt fin, bifurcation of a horseshoe vortex, and the accessibility of a closed-type separation are investigated. The usual interpretation of the flow field from previous studies and new interpretations arising from the present simulation are discussed.

Hung, Ching-Mao↗

NASA NTRS1990

Flow separation in shock wave boundary layer interactions at hypersonic speeds

An assessment is presented for the experimental data on separated flow in shock wave turbulent boundary layer interactions at hypersonic and supersonic speeds. The data base consists mainly of two dimensional and axisymmetric interactions in compression corners or cylinder-flares, and externally generated oblique shock interactions with boundary layers over flat plates or cylindrical surfaces. The conditions leading to flow separation and the subsequent changes in the flow empirical correlations for incipient separation are reviewed. The effects of the Mach number, Reynolds number, surface cooling and the methods of detecting separation are discussed. The pertinent experimental data for the separated flow characteristics in separated turbulent boundary layer shock interaction are also presented and discussed.

Hamed, A.↗

NASA NTRS1989

Polymer solution phase separation: Microgravity simulation

In many multicomponent systems, a transition from a single phase of uniform composition to a multiphase state with separated regions of different composition can be induced by changes in temperature and shear. The density difference between the phase and thermal and/or shear gradients within the system results in buoyancy driven convection. These differences affect kinetics of the phase separation if the system has a sufficiently low viscosity. This investigation presents more preliminary developments of a theoretical model in order to describe effects of the buoyancy driven convection in phase separation kinetics. Polymer solutions were employed as model systems because of the ease with which density differences can be systematically varied and because of the importance of phase separation in the processing and properties of polymeric materials. The results indicate that the kinetics of the phase separation can be performed viscometrically using laser light scattering as a principle means of following the process quantitatively. Isopycnic polymer solutions were used to determine the viscosity and density difference limits for polymer phase separation.

Cerny, Lawrence C.↗

NASA NTRS1990

On the Lagrangian description of unsteady boundary-layer separation. II - The spinning sphere

Van Dommelen, Leon L.↗