Abstract

Herein, a novel ball milling-pyrolysis strategy was proposed for preparing a highly dispersed Ni3Fe nanoalloy catalyst (Ni3Fe@NC) used for 5-hydroxymethylfurfural (HMF) electro-oxidation reaction. The Ni3Fe@NC delivered a high current density of 100 mA cm−2 at a low potential of 1.467 V vs RHE, with a HMF conversion rate of over 99.6 %, 2,5-furan dicarboxylic acid (FDCA) selectivity of 97.1 % and a Faraday efficiency of 96.7 %. Theoretical calculations, in-situ EIS, quasi-in-situ XRD and XPS demonstrated that Fe-doping optimizes the electronic structure of Ni3Fe@NC and regulates its d-band center, which not only promoted the reconstruction of Ni3Fe@NC to form high-oxidation-activity Ni2+δ and Ni3+δ species but also reduced the reaction barrier of the key rate-determining step (*5-Hydroxymethyl-2-furancarboxylic acid (HMFCA)→*5-formyl-2-furancarboxylic acid (FFCA)) during HMFOR. Based on this interesting work, we provided a facile macroscopic preparation strategy on highly dispersed nanoalloy catalyst for efficient electro-oxidation of HMF.

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