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Selective Catalytic Oxidation of Ammonia to Nitric Oxide Via Chemical Looping

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Selective Catalytic Oxidation of Ammonia to Nitric Oxide Via Chemical Looping Selective catalytic oxidation of ammonia to nitric oxide via chemical looping Chongyan Ruan CAS Key Laboratory of Science and Technology on Applied Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China Xijun Wang University of Science and Technology of China https://orcid.org/0000-0001-9155-7653 Chaojie Wang CAS Key Laboratory of Science and Technology on Applied Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China Lin Li Dalian Institute of Chemical Physics Jian Lin Dalian Institute of Chemical Physics Xiao Yan Liu Chinese Academy of Sciences https://orcid.org/0000-0003-2694-2306 Fanxing Li North Carolina State University https://orcid.org/0000-0002-6757-1874 Xiaodong Wang ( [email protected] ) Dalian Institute of Chemical Physics Article Keywords: alternative ammonia oxidation, nitric acid production, chemical looping Posted Date: April 15th, 2021 DOI: https://doi.org/10.21203/rs.3.rs-350833/v1 License: This work is licensed under a Creative Commons Attribution 4.0 International License. Read Full License Selective catalytic oxidation of ammonia to nitric oxide via chemical looping Chongyan Ruan1,2,4, Xijun Wang2,4, Chaojie Wang1,3, Lin Li 1, Jian Lin1, Xiaoyan Liu1, Fanxing Li*2 and Xiaodong Wang*1 Selective oxidation of ammonia to nitric oxide (NO) over platinum-group metal alloy gauzes is the crucial step for nitric acid production, a century-old yet greenhouse gas and capital intensive process in chemical industry. Therefore, developing alternative ammonia oxidation technologies with low environmental impacts and reduced catalyst cost are of significant importance. Herein, we proposed and demonstrated, for the first time, a novel chemical looping ammonia oxidation (CLAO) catalyst and process to replace the costly noble metal catalysts and to reduce greenhouse gas emission. The proposed CLAO process exhibited near complete NH3 conversion and exceptional NO selectivity (99.8%) o with negligible N2O production, using nonprecious V2O5 redox catalyst at a temperature up to 300 C lower than the existing appraoch. Operando spectroscopy techniques complemented with density functional theory calculations point towards a modified, temporally separated Mars-van Krevelen mechanism featuring a reversible V5+/V4+ redox cycle. The V=O sites are suggested to be the catalytically active center leading to the formation of the oxidation products. Meanwhile, both V=O and doubly coordinated oxygen (V-OII-V) participate in the hydrogen transfer process. The outstanding performance is attributed to the low activation energies for the successive hydrogen abstraction (1.06 eV), facile NO formation (0.03 eV) as well as the easy regeneration of V=O species. Our results highlight a transformational CLAO process in extending the chemical looping strategy to producing base chemicals in a sustainable and cost-effective manner. Catalytic oxidation of ammonia to NO is the core reaction for NH3 were supplied at feed and permeate side of the membran e producing nitric acid, one of the top-ten bulk chemicals by reactor separately.3,15 Pérez Ramírez et al. demonstrated that, by annual consumption (over 100 million tons per year) and widely exploiting Ca- and Sr-substituted lanthanum ferrite membran es applied in the manufacturing of fertilizers, nylon, dyes, and for the high-temperature NH3 oxidation, high NO selectivit ies 1-3 explosives, among others. Since the early 20th century, the (92-98 %) can be attained with NH3 conversion ranges between 3 Ostwald process (4NH3 + 5O2 → 4NO + 6H2O), which utiliz es 80-95 %. However, the stability of the oxygen ionic transport Pt-Rh alloy (5-10% Rh) gauzes as the catalysts for ammonia membranes are often impaired by cation segregation and/or oxidation at high temperatures (800-950 oC) and pressures (up to physical degradat ion. Therefore, it is imperative to research into 1,4-9 12 atm), has been the industrial standard. The NO yield can new intensified processes for NH3 oxidation. reach 90−98 % depending on the operation parameters, One method towards process intensification is chemical rendering it one of the most efficient catalytic reactions .1 looping, whereby oxidation reactions are decoupled into two- However, Pt loss through volatilization (0.05-0.3 g per ton of step, spatially separated cyclic redox processes.20-23 Chemica l nitric acid produced) at high-temperature and strongly oxidiz in g looping is a new frontier for producing valuable chemicals in a atmosphere results in significant catalytic performance decay s clean and efficient manner,24-28 and has been demonstrated for and high operating costs.1,6,7 Moreover, nitric acid production is processing methane,28-35 biofuels,36,37 syngas,38,39 coal and 22,40,41 the largest source of the greenhouse gas N2O in the chemica l carbonaceous feedstocks with low cost, reduced emissions 10 industry (125 million tons CO2-equiv per year). The above and higher energy efficiency. Herein, we proposed and validat ed economic challenges and environmental concern stimulat e the first chemical looping ammonia oxidation (CLAO) process. research towards developing cost-efficient catalysts and new As depicted in Figure 1, during the reduction step, NH3 is processes with favourable NO yield while reducing N2O oxidized by the active lattice oxygen derived from the metal emission. Over the past decades, extensive efforts have been devot ed to replacing noble metal catalysts by transition metal oxides.2,3, 11 - 18 A large number of metal oxide catalysts have claimed promising performance for ammonia oxidation, includin g 17,19 spinels (Co3O4), perovskites (ABO3 where A = Ca, Sr, La 3,12,13,15 and B = Mn, Co, Fe) and K2NiF4 structured oxides 1 (La2BO4 where B = Co, Cu, Ni) . The industrial implement at io n is impeded, however, by the insufficient NO selectivity and rapid catalyst deactivation. For instance, Co3O4 exhibited good activity towards NH3 oxidation with a promising NO selectivit y over 90%.1,17,19 However, the rapid deactivation due to the reduction to less active CoO, despite in the presence of Fig. 1 Schematic of the chemical looping ammonia oxidation (CLAO) considerable excess O2, has impaired its commerci a l process. The red and gray spheres represent metal and oxygen atoms, deployment. Recently, an alternative approach based on oxy gen- respectively. conducting membrane reactor was proposed, where the O2 and 1CAS Key Laboratory of Science and Technology on Applied Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China. 2Department of Chemical and Biomolecular Engineering, North Carolina State University, Raleigh, NC, USA. 3University of Chinese Academy of Sciences, Beijing, 100049, China. 4These authors contributed equally: Chongyan Ruan, Xijun Wang. *e-mail: [email protected]; [email protected] oxide redox catalyst, producing concentrated NO. In the indicated that the reaction involved the reversible reduction of 5+ 4+ subsequent oxidation step, the reduced metal oxide redox V to V , with V=O participated in the oxidation of NH3 via a catalyst is re-oxidiz ed with air, completing the redox cycle. The modified, temporally separated Mars-van Krevelen (MvK) novel CLAO process is potentially advantageous compared to mechanism. The subsequent re-oxidation of vanadium cation to 5+ the conventional co-feed approach where NH3 and air are V with molecular oxygen replenished V=O and completed the introduced simultaneously. First, since CLAO process decoup les catalytic cycle. The facile reaction between V=O and NH3 the reaction into two, the operation parameters can be optimiz ed (activation energy: 16.0 kJ/mol) was responsible for the independently in order to achieve improved performance s. extraordinary NH3 oxidation performance at a relatively low Second, catalyst deactivation could be avoided as the reduced temperature, as substantiated by DFT calculations. catalyst is regenerat ed in each oxidation half cycle. Third, the utilization of lattice oxygen instead of nonselective gaseous oxygen may effectively suppress the formation of undesirabl e Results N2O, thus reducing the greenhouse gas footprint. That last point Redox Performance and Stability. In order to validate the feasibility is that as large quantities of inert N2 (about 3/4 of the total flow of the proposed CLAO process, consecutive redox cycles were carried in a current plant)3 are excluded from the product NO, allow in g out to investigate the product distribution and the overall chemical for a radically intensified process for nitric acid production. looping process efficiency. Fig. 2a illustrates the ammonia conversion The metal oxide redox catalyst functions as the react ive and product distribution over V2O5 as a function of temperature in intermediat e to transport oxygen ions between the cyclic steps. typical chemical looping mode. The corresponding products evolution Hence, the techno-economic viability of the CLAO technology upon NH3 injection are reproduced in Fig. S2a-h, which indicates that is critically dependent upon the redox properties of the met al NO, N2O and N2 were the only N-containing products. While no H2 oxide catalyst. By virtue of the excellent catalytic activity in was observed in the reaction temperature range, with water being the various redox reactions, vanadium oxide catalysts have been only H-containing product that has been condensed out to avoid intensively investigat ed in chemical and environme nt a l interference. As depicted in Fig. 2a, ammonia conversion increases industries, including oxidative dehydrogenation of alkanes , from 78.5% to 97.0% at 300 to 650 oC and plateaus around 97.0% in oxidation of methanol to formaldehyde, mass production of the temperature range of 580 to 650 oC. Meanwhile, the selectivity to 42-48 sulfuric acid, and selective catalytic reduction of NOx. In nitrogen-containing products depends critically upon temperature: N2 o recent studies, V2O5-based redox catalysts have emerged as is the dominate product at low temperature (<500 C), whereas NO attractive candidates for oxidative dehydrogenation of ethane via takes over at high temperature (580-650 oC).
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