Throughput Optimization of Molybdenum Carbide Nanoparticle Catalysts in a Continuous Flow Reactor Using Design of Experiments

Journal Article · 09 February 2022 · ACS Applied Nano Materials

DOI:https://doi.org/10.1021/acsanm.1c02916· OSTI ID:1855583

Karadaghi, Lanja R.; Madani, Majed S.; Williamson, Emily M.; To, Anh T.; Habas, Susan E. ; Baddour, Frederick G. ; Schaidle, Joshua A. ; Ruddy, Daniel A. ; Brutchey, Richard L.; Malmstadt, Noah

Transition metal carbides (TMCs) have attracted significant attention because of their applications toward a wide range of catalytic transformations. However, the practicality of their synthesis is still limited because of the harsh conditions in which most TMCs are prepared. Recently, a solution-phase synthesis of phase-pure a-MoC1-x nanoparticles was presented. While this synthetic route yielded nanoparticles with exceptional catalytic performance, the reaction parameter space was not explored, and catalyst throughput was not optimized for scale-up. Continuous flow platforms coupled with statistical design of experiments (DoE) can provide a powerful method for understanding the reaction parameter space for optimizations. Here, we demonstrate the use of statistical DoE in tandem with response surface methodology for a parametric screening analysis to optimize the throughput of a MoC1-x nanoparticle synthesis utilizing a millifluidic flow reactor. A full factorial design was implemented to evaluate four input variables (reaction temperature, flow rate, solvent fraction of oleylamine, and precursor concentration) that carry statistically significant effects on three responses (throughput, residence time, and isolated yield). A Doehlert matrix was implemented to investigate each significant variable at a higher number of levels to optimize throughput. Our results give a nonintuitive set of experimental conditions that resulted in an optimized throughput of 2.2 g h-1. This translates to a 50-fold increase in throughput compared to the previously reported batch method. The catalytic performance of the MoC1-x nanoparticles produced under optimized throughput was demonstrated in the CO2 hydrogenation reaction. This DoE screening analysis and throughput optimization of MoC1-x synthesis open the door to an increased feasibility for scale-up.

• Research Organization: National Renewable Energy Lab. (NREL), Golden, CO (United States)
• Sponsoring Organization: USDOE Office of Energy Efficiency and Renewable Energy (EERE), Sustainable Transportation Office. Bioenergy Technologies Office
• DOE Contract Number: AC36-08GO28308
• OSTI ID: 1855583
• Report Number(s): NREL/JA-5100-80300; MainId:42503; UUID:8643063b-468b-4cf9-ad4a-08b87ee30322; MainAdminID:64056
• Journal Information: ACS Applied Nano Materials, Vol. 5, Issue 2
• Country of Publication: United States
• Language: English

Related Subjects

INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY,NANOSCIENCE AND NANOTECHNOLOGY
design of experiments
millifluidic flow reactor
molybdenum carbide
nanoparticles
response surface methodology