Louisville, KY, United States
Louisville, KY, United States

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Gupta M.,Advanced Energy Materials, LLC | Gupta M.,University of Louisville | Gupta M.,Rice University | He J.,Advanced Energy Materials, LLC | And 6 more authors.
Applied Catalysis B: Environmental | Year: 2016

Here, we report high performance catalysts designed using nanowire supports. Specifically, nickel clusters supported on Zinc Oxide (ZnO) nanowires and γ-alumina found to be highly active for ultra-deep desulfurization and aromatic hydrogenation of diesel. They were also found to be highly active for ultra-deep desulfurization of gasoline and kerosene. The catalysts reduced sulfur from diesel, gasoline, and kerosene fuels containing sulfur as high as approximately 200 ppm to less than 1 ppm with sustained activity over testing periods of 100-150 h. The feed contained some of the most difficult to remove sulfur compounds such as 4-methyldibenzothiophene (MDBT), 4,6-dimethyldibenzothiophene (DMDBT). In addition to activity towards ultra-deep desulfurization, these catalysts have shown to be active towards saturate/hydrogenate aromatics in diesel at moderate reaction conditions (30 bar, 290°C, and LHSV 2.2 h-1). The active catalytic site was determined to be a super Ni rich NixZny phase which seemed to remain essentially sulfur free during the reaction. The regenerated catalyst showed reasonable activity toward desulfurization of gasoline. © 2015 Elsevier B.V. All rights reserved.


Kumar V.,University of Louisville | Kim J.H.,University of Louisville | Kim J.H.,Advanced Energy Materials, LLC | Jasinski J.B.,University of Louisville | And 3 more authors.
Crystal Growth and Design | Year: 2011

We report a new ultrafast (reaction time on the scale of a minute) gas-phase method for synthesizing highly crystalline titanate phase nanowires (NWs) using oxidation of either Ti metal (foils or powders) or spherical TiO2 powders with an atmospheric pressure microwave plasma. In this method, alkali metal compounds of Li, Na, and K are shown to form molten alloys of alkali metal-Ti-O during plasma exposure. Bulk nucleation and subsequent basal growth of the resulting nuclei from the molten alkali metal-Ti-O resulted in the respective titanate NWs. The current state-of-the-art methods involve long reaction time scales (∼1 day) for synthesis of TiO2 NWs. © 2011 American Chemical Society.


Petzold F.G.,University of Louisville | Petzold F.G.,Süd-Chemie, Inc. | Jasinski J.,University of Louisville | Clark E.L.,University of Louisville | And 6 more authors.
Catalysis Today | Year: 2012

A novel catalyst with deep hydrodesulfurization (HDS) capabilities was tested with the aim of producing ultra-low sulfur diesel oil. The catalyst consisted of a zinc oxide nanowire (ZnO NW)/alumina carrier impregnated with nickel (Ni) as the active phase. Based on the concept of reactive adsorption, it was hypothesized that enhanced metal-support interactions and short diffusion paths between Ni and ZnO NWs could lead to improved activity and sulfur uptake capacity. Long ZnO NWs (10-15 μm) were produced in bulk quantities using an atmospheric plasma jet reactor. In situ heating studies of Ni impregnated ZnO NW samples revealed better Ni dispersion, greater Ni-support interaction, and smaller Ni particle sizes when compared to a support comprised spherical ZnO nanoparticles (NPs). The reactive adsorbent was tested for on-stream sulfur uptake with model diesel oil spiked with difficult-to-remove organic sulfur species. The data indicated high activity for deep de-sulfurization in the initial stages but the catalyst deactivated via coking after 16 h. The coking appears to be due to cracking of aromatic species present in the model oil in the absence of adsorbed surface hydrogen. The initial activity of the catalyst with modest composition of nickel loading indicated the potential utility of the catalyst system involving ZnO NWs as support. © 2012 Elsevier B.V.


Grant
Agency: National Science Foundation | Branch: | Program: SBIR | Phase: Phase I | Award Amount: 150.00K | Year: 2013

This Small Business Innovation Research (SBIR) Phase I project proposes to demonstrate the feasibility of a new type of advanced hydrodesulfurization (HDS) catalyst for deep desulfurization purposes. Specifically, metal nanoparticles supported on zinc oxide nanowires are proposed for creating higher performance, reactive adsorbent type HDS catalysts. HDS is a process used for the removal of sulfur from hydrocarbon fuels. In this process, fuels are treated with hydrogen gas in the presence of a catalyst. The environmental regulations are continuously pushing down the sulfur levels allowed in transportation fuels and will continue to lower the limits much below 10 ppm in future. Also, low sulfur concentrations are desirable for various fuel cell and refinery technologies where presence of small amounts of sulfur can poison the catalysts. The current, traditional HDS catalysts are efficient in removing the sulfur to levels down to around 20 ppm and leaves behind difficult-to-remove thiophenic sulfur compounds. In this project, an advanced catalyst and a scalable and cost-effective manufacturing is proposed that can accomplish deep desulfurization for lowering sulfur levels down well below 5 ppm. The broader/ commercial potential of this project will be improved air quality and energy/cost savings for the nation from improved durability of fuel cell and several refining technologies. The project's other outcome will also include new manufacturing technologies for advanced catalyst materials which is crucial for both the nation and the state of Kentucky to be globally competitive in terms of energy technologies. The catalyst materials using ZnO nanowire supports will also find applications beyond deep hydro-desulfurization such as C1-C4 alcohol production using syngas, and steam reforming of methanol. The market size for the proposed catalysts is estimated to exceed $1B considering the number of application areas.


Grant
Agency: National Science Foundation | Branch: | Program: SBIR | Phase: Phase II | Award Amount: 743.05K | Year: 2014

The broader impact/commercial potential of this Small Business Innovation Research (SBIR) Phase II project is in removing sulfur compounds from various fuels such as diesel, gasoline and mixture of refined fuels known as transmix. It is critically important to reduce sulfur levels below 10 ppm as the emissions from transportation vehicles can cause acid rain and associated undesired effects. Sulfur removal from fuels is even more critical for implementation of fuel cell technologies due to fuel reformer catalyst poisoning at sulfur levels as low as 1 ppm or below. Finally, there is a need for sulfur-tolerant catalysts and sulfur removal processes in value added chemical production using bio-derived and fossil derived fuels. The global market for hydro-desulfurization catalysts in the transportation fuel segment is estimated at over $1B and growing fast. The company's proposed catalyst could address a market size of $150-200M/yr or more. It may find additional applications in commercial markets in ultra-low sulfur diesel, fuel reformer technology and sulfur tolerant catalysts. The development of a scalable manufacturing method for advanced materials undertaken in this project will contribute to U.S. competitiveness and strengthen Cleantech and energy sectors in the state of KY. This project addresses the development of high performance catalysts needed for the removal of sulfur from hydrocarbon fuels. However, sulfur removal at concentrations below 50 ppm is difficult due to the presence of hetero-cyclic thiophenic species. During Phase I, the company developed a catalyst product and demonstrated its performance in terms of ultra-deep hydrodesulfurization activity, reducing sulfur levels from 200 ppm to much lower than 1 ppm in a variety of fuels. Phase II studies will allow optimization of the catalysts for hydrodesulfurization activity and mechanical properties. Catalysts with bi-functional activity toward aromatics hydrogenation and hydrodesulfurization will reduce several process steps, thereby reducing the costs involved in hydroprocessing of fuels. Phase II studies will enable development of a process for scalable production of nanowires. The fundamental insight from the performance can be extended toward designing various high performance catalysts using nanowire supports. Some beneficial effects using nanowire supports include unique active metal/support interactions; single crystal surfaces for uniform morphologies for active metals and their alloys and management of active sites. Specifically, in the case of hydrodesulfurization, nanowire supports provided an easier diffusion pathway for sulfur transfer to maintain active metal sites for desulfurization activity.


Grant
Agency: NSF | Branch: Standard Grant | Program: | Phase: | Award Amount: 180.00K | Year: 2013

This Small Business Innovation Research (SBIR) Phase I project proposes to demonstrate the feasibility of a new type of advanced hydrodesulfurization (HDS) catalyst for deep desulfurization purposes. Specifically, metal nanoparticles supported on zinc oxide nanowires are proposed for creating higher performance, reactive adsorbent type HDS catalysts. HDS is a process used for the removal of sulfur from hydrocarbon fuels. In this process, fuels are treated with hydrogen gas in the presence of a catalyst. The environmental regulations are continuously pushing down the sulfur levels allowed in transportation fuels and will continue to lower the limits much below 10 ppm in future. Also, low sulfur concentrations are desirable for various fuel cell and refinery technologies where presence of small amounts of sulfur can poison the catalysts. The current, traditional HDS catalysts are efficient in removing the sulfur to levels down to around 20 ppm and leaves behind difficult-to-remove thiophenic sulfur compounds. In this project, an advanced catalyst and a scalable and cost-effective manufacturing is proposed that can accomplish deep desulfurization for lowering sulfur levels down well below 5 ppm.

The broader/ commercial potential of this project will be improved air quality and energy/cost savings for the nation from improved durability of fuel cell and several refining technologies. The projects other outcome will also include new manufacturing technologies for advanced catalyst materials which is crucial for both the nation and the state of Kentucky to be globally competitive in terms of energy technologies. The catalyst materials using ZnO nanowire supports will also find applications beyond deep hydro-desulfurization such as C1-C4 alcohol production using syngas, and steam reforming of methanol. The market size for the proposed catalysts is estimated to exceed $1B considering the number of application areas.


Grant
Agency: NSF | Branch: Standard Grant | Program: | Phase: SMALL BUSINESS PHASE II | Award Amount: 891.66K | Year: 2014

The broader impact/commercial potential of this Small Business Innovation Research (SBIR) Phase II project is in removing sulfur compounds from various fuels such as diesel, gasoline and mixture of refined fuels known as transmix. It is critically important to reduce sulfur levels below 10 ppm as the emissions from transportation vehicles can cause acid rain and associated undesired effects. Sulfur removal from fuels is even more critical for implementation of fuel cell technologies due to fuel reformer catalyst poisoning at sulfur levels as low as 1 ppm or below. Finally, there is a need for sulfur-tolerant catalysts and sulfur removal processes in value added chemical production using bio-derived and fossil derived fuels. The global market for hydro-desulfurization catalysts in the transportation fuel segment is estimated at over $1B and growing fast. The companys proposed catalyst could address a market size of $150-200M/yr or more. It may find additional applications in commercial markets in ultra-low sulfur diesel, fuel reformer technology and sulfur tolerant catalysts. The development of a scalable manufacturing method for advanced materials undertaken in this project will contribute to U.S. competitiveness and strengthen Cleantech and energy sectors in the state of KY.



This project addresses the development of high performance catalysts needed for the removal of sulfur from hydrocarbon fuels. However, sulfur removal at concentrations below 50 ppm is difficult due to the presence of hetero-cyclic thiophenic species. During Phase I, the company developed a catalyst product and demonstrated its performance in terms of ultra-deep hydrodesulfurization activity, reducing sulfur levels from 200 ppm to much lower than 1 ppm in a variety of fuels. Phase II studies will allow optimization of the catalysts for hydrodesulfurization activity and mechanical properties. Catalysts with bi-functional activity toward aromatics hydrogenation and hydrodesulfurization will reduce several process steps, thereby reducing the costs involved in hydroprocessing of fuels. Phase II studies will enable development of a process for scalable production of nanowires. The fundamental insight from the performance can be extended toward designing various high performance catalysts using nanowire supports. Some beneficial effects using nanowire supports include unique active metal/support interactions; single crystal surfaces for uniform morphologies for active metals and their alloys and management of active sites. Specifically, in the case of hydrodesulfurization, nanowire supports provided an easier diffusion pathway for sulfur transfer to maintain active metal sites for desulfurization activity.


Grant
Agency: National Science Foundation | Branch: | Program: SBIR | Phase: Phase I | Award Amount: 150.00K | Year: 2011

This Small Business Innovation Research (SBIR) Phase I project aims to develop a new method and reactor for continuous and large-scale production of titania and other related metal oxide nanowires. Inexpensive micron scale metal oxide and spherically shaped powders will be converted to nanowires using a plasma oxidation scheme. The fast reaction time (on the order of minutes) of this process will allow the development of a reactor for continuous production of nanowire powders. The broader/commercial impact of this project will be the potential to provide a process and reactor for the production of nanowire-based materials in large volume. Titania and manganese oxide nanowire powders will find commercial applications in lithium-ion batteries for transportation and large-scale storage. Ceria and titania nanowire powders may also be used in catalysis, paints, light-weight and optical composite materials etc.


Grant
Agency: NSF | Branch: Standard Grant | Program: | Phase: | Award Amount: 180.00K | Year: 2011

This Small Business Innovation Research (SBIR) Phase I project aims to develop a new method and reactor for continuous and large-scale production of titania and other related metal oxide nanowires. Inexpensive micron scale metal oxide and spherically shaped powders will be converted to nanowires using a plasma oxidation scheme. The fast reaction time (on the order of minutes) of this process will allow the development of a reactor for continuous production of nanowire powders.

The broader/commercial impact of this project will be the potential to provide a process and reactor for the production of nanowire-based materials in large volume. Titania and manganese oxide nanowire powders will find commercial applications in lithium-ion batteries for transportation and large-scale storage. Ceria and titania nanowire powders may also be used in catalysis, paints, light-weight and optical composite materials etc.


Grant
Agency: Department of Energy | Branch: | Program: SBIR | Phase: Phase I | Award Amount: 150.00K | Year: 2016

This project proposes the development of advanced catalyst technology for ultra-deep hydro-desulfurization and cetane number improvement process for diesel fuel. The proposed process will enhance the cetane number to as high as 58, lower sulfur content and reduce the boiling end-point to obtain a higher-quality diesel fuel. In this project, Advanced Energy Materials, LLC (AdEM) proposes to demonstrate the feasibility of advanced catalyst formulations using lab scale packed bed reactor with diesel and light cycle oil (LCO) feeds obtained from refineries in midwest region. Phase I of the proposed project involves three major components: 1). Demonstrate the feasibility of improving the cetane number of diesel fuel, with catalysts made using the proposed 1-D nanowire-based materials. With the addition of noble metal alloy, the catalysts are anticipated to exhibit at least 8 point of cetane numer enhancement due to the selective ring opening (SRO) hydrogenation activity. It’s also important to verify that AdEM’s catalysts capability for removing sulfur species and increasing cetane number of diesel fuel simultaneously. 2). Investigate the feasibility of hydrodesulfurization performance using “spent” sulfided nanowire-based catalysts. The catalysts should exhibit high sulfur-removal performance and regenerable for 10 cycles and with less than 5% loss of initial performance. 3). Demonstrate scalability of catalyst materials and extrudate production at kilogram necessary for continuous testing at 10-100 gram scale. AdEM has developed a break-through technology for scalable manufacturing of both one-dimensional and two-dimensional nanomaterials, and formulating nanopowders to macroscopic shape catalyst products with high mechanical strength and stability. Potential impact: Sulfur is a natural component of crude oil that is present in gasoline and diesel unless removed. Demand for higher performance diesel engines has resulted in an increase in minimum cetane number required for diesel fuel. The development of advanced catalyst which can remove sulfur to below 15 ppm and improves cetane number simultaneously is attracting considerable attention in recent years due to the new government policies and its global market is growing fast. AdEM’s proposed catalyst and its scalable manufacturing methods can lead to the highly efficient sulfur removal in oil refineries with a substantial energy savings. Summary for Congress: This SBIR project will develop a new class of zinc oxide and titanium dioxide nanowire based selective catalysts for ultra-deep sulfur removal from various fuels; selective ring opening catalysis for significant cetane number improvement, and decreasing the cost of catalyst manufacture. Keywords: Sulfur removal, hydrodesulfurization, cetane number, selective ring opening, nanowire, plasma, kilogram scale production.

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