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Ceramic Membrane Enhanced Two-Stage Hydrothermal Liquefaction for Simultaneous Biofuels and Biochemicals from Liquid Wastes
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Scalable Bottom-Up Synthesis of Nanoporous Hexagonal Boron Nitride ( h -BN) for Large-Area Atomically Thin Ceramic Membranes
Nanopores embedded within monolayer hexagonal boron nitride (h-BN) offer possibilities of creating atomically thin ceramic membranes with unique combinations of high permeance (atomic thinness), high selectivity (via molecular sieving), increased thermal stability, and superior chemical resistance. However, fabricating size-selective nanopores in monolayer h-BN via scalable top-down processes remains nontrivial due to its chemical inertness, and characterizing nanopore size distribution over a large area remains extremely challenging. Here, we demonstrate a facile and scalable approach of exploiting the chemical vapor deposition (CVD) process temperature to enable direct incorporation of subnanometer/nanoscale pores into the monolayer h-BN lattice, in combination with manufacturing compatible polymer casting to fabricate centimeter-scale nanoporous atomically thin ceramic membranes. We leverage diffusive transport of analytes including size-selective Ficoll sieving to characterize subnanometer-scale and nanoscale defects that manifest as pores in centimeter-scale h-BN membranes, overcoming previous limitations in large-area characterization of nanoscale defects in h-BN. Our approach opens a new frontier to advance atomically thin membranes to 2D ceramic materials, such as h-BN via facile and direct formation of nanopores, for size-selective separations.
Electrocatalytically Upgrading Methane to Benzene in a Highly Compacted Microchannel Protonic Ceramic Membrane Reactor
This project aims to develop highly compacted microchannel protonic ceramic membrane reactors (HCM-PCMRs) for efficient and cost-effective methane dehydrogenation to aromatics (MDA, e.g., benzene). The integration of single-atom catalysis, electrocatalysis, membrane catalysis, membrane separation, and advanced manufacturing is designed to fulfill this goal. This project's success will ultimately develop a new cost-effective, efficient, and highly compacted infrastructure technology to address the flare and venting issue during oil and gas operations and other gas-to-liquid technologies. The key objectives for the three budget periods (BPs) are as follows.
Ceramic Membrane Solar Desal: Pilot System Design and Full-Scale System Techno-Economic Analysis (CRADA Final Report)
This work is conducted in support of the American Made Challenges Solar Prize. The current scope addresses the Design portion of the overall prize competition. This team, led by the University of Connecticut, will design a solar powered, pilot scale, ceramic-based membrane distillation system that can operate on high salinity waters and propose that design for construction in the Test phase of the Prize competition.
CFA-17-12798: Nanostructured Ceramic Membranes for Enhanced Tritium Management
This project focuses on the novel use of interfacial hydrated layers in ionic conducting ceramic materials for tritiated water (HTO) adsorption and recovery. Low-temperature water adsorption properties of nanoscale structured ceramics combined with hydrogen isotope exchange in their hydrated layers could provide a low-cost and transformative avenue to address tritium management challenges.
Textured ceramic membranes for desilting and deoiling of produced water in the Permian Basin
Oil production in the Permian Basin gives rise to large volumes of produced water contaminated by silt, emulsified oil, and additives used for enhanced oil recovery. There is intense interest in the design of membrane modules as sustainable alternatives for produced water treatment to enable the reuse of produced water for agricultural applications, injection into aquifers, and redeployment in oil recovery. Here, we report a hierarchically textured cement-based membrane exhibiting orthogonal wettability, specifically, superhydrophilic and underwater superoleophobic characteristics. The in situ formation of ettringite needles accompanied by embedding of glass spheres imbues multiscale texturation to stainless-steel mesh membranes, enabling the separation of silt and oil from produced water at high flux rates (1600 L h -1 ∙m -2 , at ca. 2.7 bar). Oil concentration is reduced as low as 1 ppb with an overall separation efficiency of 99.7% in singlepass filtration. The membranes show outstanding mechanical resilience and retention of performance across multiple cycles.
Evolution of Copper Electrodes Fabricated by Electroless Plating on BaZr0.7Ce0.2Y0.1O3-δ Proton-Conducting Ceramic Membrane: From Deposition to Testing in Methane
We investigated copper electrodes deposited onto a BaZr0.7Ce0.2Y0.1O3-δ (BZCY72) proton-conducting membrane via a novel electroless plating method, which resulted in significantly improved performance when compared to a traditional painted copper electrode. The increased performance was examined with a multiscale multitechnique characterization method including time-of-flight secondary-ion mass spectroscopy (TOF-SIMS), transmission electron microscopy (TEM), scanning spreading-resistance microscopy (SSRM), and atom-probe tomography (APT). Through this method, we observed that a palladium catalyst layer alloys with the copper electrode. We also explored the nature of a non-coking-induced carbon-rich phase that may be involved with the improved performance of the electrode.
An Industrial Membrane System Suitable for Distributed Used Oil Re-refining
Under this SBIR project, Media and Process Technology Inc (MPT) has achieved ~60% cost reduction and system foot print of its ceramic membrane product, which leads to successful commercialization of its industrial ceramic membrane process to large scale applications. Ceramic membrane is known for its rugged materials and performance reliability; however, it has been limited in niche applications due to its cost and footprint. The low-cost ceramic membrane thus developed under this project has been field tested successfully in our semi-works production facility for used oil re-refining. Our membrane subsystem of our re-refining production capacity was tripled through the installation of this low-cost high packing density of ceramic membranes. In addition, we have successfully field tested/demonstrated with a pilot unit in two large scale applications for refinery FCC slurry upgrading and decoker/amine scrubber wastewater treatment. Commercialization of these two applications in oil refineries are currently actively pursued by our commercialization partner. With regard to the membrane product sales, we have produced >500 m 2 ceramic membranes for two full-scale installations for industrial oil/water separations in 2017, which is equivalent to ~50% of the annual US ceramic membrane market size. We will continue to push our low-cost high packing density ceramic membrane developed from this project for large scale applications, which are not currently occupied by existing ceramic membranes.
High temperature steam separation membrane
Ceramic proton-conducting oxide membranes are described herein, which are useful for separating steam from organic chemicals under process conditions. The membranes have a layered structure, with a dense film of the perovskite over a porous composite substrate comprising the perovskite material and a metallic material (e.g., Ni, Cu, or Pt). The perovskite comprises an ABO 3 -type structure, where “A” is Ba and “B” is a specified combination of Ce, Zr, and Y. The perovskite ceramic materials described herein have an empirical formula of Ba(Ce x Zr 1-x-n Y n )O 3-δ , wherein 0<x<0.8 (e.g., 0.1≤x≤0.7 or 0.2≤x≤0.5); and 0.05≤n≤0.2; and δ=n/2. In some embodiments n is about 0.2. In some other embodiments 0.6≤x≤0.8; and n is about 0.2, such as Ba(Ce 0.7 Zr 0.1 Y 0.2 )O 3-δ , also referred to herein as BCZY712.
Fabrication and analysis of hydroxide/ceramic dual-phase (HCDP) membranes
Ceramic materials show potential to serve as support structures for membranes that can be used to uptake carbon dioxide from high temperature environments, like those found in nuclear flue plants. The porosity of ceramic materials allows for the infilling of those pores with molten hydroxides, that show a natural affinity for absorbing CO 2 from its surroundings. The membranes are easy to produce and were made with thickness of 0.5mm, 1.0mm, and 2.0mm. The membranes were exposed to various conditions after the infilling process and their responses were measured. The percent of hydroxides were measured after the infilled membranes had been in a tube furnace at 400°C, followed by exposure to 30 minutes of CO 2 , and lastly 4 hours of steam. Those tests yielded mole percent hydroxide results of 88.4% ± 4.6%, 68.6% ± 5.1%, and 80.7% ± 4.6%, respectively.
Revolutionizing Methane Transformation with the Dual Production of Aromatics and Electricity in a Protonic Ceramic Electrocatalytic Membrane Reactor
Reducing the energy and carbon intensity of the conventional chemical processing industry can be achieved by electrochemically transforming natural gases into higher-value chemicals with higher efficiency and near-zero emissions. In this work, the direct conversion of methane to aromatics and electricity has been achieved in a protonic ceramic electrocatalytic membrane reactor through the integration of a proton-conducting membrane assembly and a trimetallic Pt–Cu/Mo/ZSM-5 catalyst for the nonoxidative methane dehydro-aromatization reaction. In this integrated system, a remarkable 15.6% single-pass methane conversion with an 11.4% benzene yield has been demonstrated, while a peak power density of 276 mW cm –2 is obtained at 700 °C. The enhanced 15.7% increase in conversion and 16.0% improvement in the yield are observed when compared with the thermochemical process, which is attributed to the shift of reaction equilibrium by the removal of hydrogen through the protonic membrane. Concurrently, the faster H2 removal at a higher electrical current gave rise to a higher methane conversion and benzene yield. Furthermore, the catalyst can be efficiently regenerated by eliminating carbon deposition. A stable cell potential is maintained for 45 h under a constant current load of 0.13 A cm –2 . Lastly, the dual production of aromatics and electricity in the electrocatalytic membrane reactor has been demonstrated to be an attractive approach for decarbonizing chemical processing.
Fe-based ceramic nanocomposite membranes fabricated via e-spinning and vacuum filtration for Cd 2+ ions removal
Here, vacuum filtered and polymer mixed e-spinning membranes (ESPMs) made from or doped with Fe-based nanomaterials were successfully fabricated to remove Cd 2+ ions from a neutral aqueous solution. The used Fe-based nanomaterials including FeOOH precursor Nanowires (NWs), α-Fe 2 O 3 NWs and Fe 3 O 4 nanoparticles (NPs) were synthesized by elevating the hydrothermal reaction temperature from 250 °C to 500 °C or doing post-heating treatment. The adsorption results showed that vacuum filtered membranes (VFMs) overall performed a better Cd 2+ ions removal behavior than e-spinning ones. Among them, VFM made from Fe 3 O 4 NPs has the highest adsorption capacity (qt) with the adsorption amount of Cd 2+ ions reaching about 29.3 mg/g within only 2 min due to the high specific surface area of NPs. Models of pseudo-first-order, pseudo-second-order and intraparticle diffusion were used to study the kinetics of Cd 2+ ions removal process, and a high correlation coefficient (R 2 ) of 0.99 was obtained when pseudo-second-order model was used. It was measured that the equilibrium rate constant of VFM made from Fe 3 O 4 NPs has reached about 0.28 g mg –1 min –1 , much smaller than those of other membranes, which suggested a high Cd 2+ ions removal efficiency.