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

Lanja Karadaghi, Majed Madani, Emily Williamson, Anh To, Susan Habas, Frederick Baddour, Joshua Schaidle, Daniel Ruddy, Richard Brutchey, Noah Malmstadt

Research output: Contribution to journalArticlepeer-review

10 Scopus Citations


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 α-MoC1-xnanoparticles 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-xnanoparticle 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-xnanoparticles produced under optimized throughput was demonstrated in the CO2hydrogenation reaction. This DoE screening analysis and throughput optimization of MoC1-xsynthesis open the door to an increased feasibility for scale-up.

Original languageAmerican English
Pages (from-to)1966-1975
Number of pages10
JournalACS Applied Nano Materials
Issue number2
StatePublished - 2022

Bibliographical note

Publisher Copyright:
© 2022 American Chemical Society. All rights reserved.

NREL Publication Number

  • NREL/JA-5100-80300


  • design of experiments
  • millifluidic flow reactor
  • molybdenum carbide
  • nanoparticles
  • response surface methodology


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