Defective sites assisted N-containing NbOx catalyzed xylose dehydration to furfural

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Kumar, Sahil and Saini, Kanika and Ali, Hadi and Kumar Kansal, Sushil and Zhang, Xiaolei and Saravanamurugan, Shunmugavel (2025) Defective sites assisted N-containing NbOx catalyzed xylose dehydration to furfural. ChemistrySelect, 10 (23). e01787. ISSN 2365-6549 (https://doi.org/10.1002/slct.202501787)

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Abstract

Doping of heteroatoms such as N into a solid metal oxide matrix as catalysts becomes an attractive approach due to the changes in the inherent catalytic properties of the material, offering alternatives to traditional mineral acids-catalyzed reactions in industries. With regard to this, N-doped niobium oxide (NbOx-D) using diethylamine was synthesized, and its catalytic activity was studied for xylose dehydration to furfural. The changes in the catalytic and characteristic properties of NbOx-D, compared with NbOx-D-400 (treated under an O2 atmosphere to remove N species), were studied using various techniques. XRD and Raman analyses confirmed the structural changes in NbOx-D due to N incorporation, based on peak shifting compared to NbOx. O2-temperature programmed desorption (O2-TPD) of NbOx-D exhibited a 1.3-fold higher number of oxygen vacancies due to N incorporation in the lattice of NbOx compared to NbOx-D-400. NH3-TPD and diffuse reflectance infrared Fourier transform (DRIFT) spectroscopic analysis corroborated the higher strength of acidic sites (Lewis and Brønsted) in NbOx-D compared to NbOx-D-400. Besides, anionic nitrogen (γ-N), based on N1s X-ray photoelectron (XPS) spectroscopy, played a key role in the catalytic transformation of xylose to FUR, which was substantiated by the poisoning study with pyrrole (to inhibit the basic sites in NbOx-D) during the reaction. NbOx-D showed a FUR production rate of 49.8 µmolm−2 h−1, which was 1.6-fold higher than NbOx-D-400 (31.1 µmolm−2 h−1). The NbOx-D showed a higher catalytic activity, giving a higher FUR yield (51%) compared to commercial NbOx (<10%) under identical reaction conditions.

ORCID iDs

Kumar, Sahil, Saini, Kanika, Ali, Hadi, Kumar Kansal, Sushil, Zhang, Xiaolei ORCID logoORCID: https://orcid.org/0000-0001-9415-3136 and Saravanamurugan, Shunmugavel;
CORE (COnnecting REpositories)