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Nanostructured Functionalised Niobium Oxide as Chemoselective Catalyst for Acetalation of Glucose

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Abstract

Developing a chemoselective catalyst for the acetalation of biomass-derived glucose to alkyl glycosides has been recognised as an emerging field due to its wide range of applications. The present study focuses on synthesising sulfate functionalised niobium oxide-based (NbOx-DS) catalyst to introduce medium/strong acidic sites that contribute to the catalytic activity towards glucose acetalation, which has not been explored previously. The nanosized NbOx-D is prepared via a precipitation approach using niobium chloride and diethylamine as a precursor and precipitating agent, respectively. The sulfate groups incorporated NbOx-DS gives a good yield of ethyl glucosides (60%) with excellent selectivity (97%) in ethanol. On the other hand, the sulfate groups incorporated into the commercial niobium oxide (NbOx-CS) exhibits poor catalytic activity, yielding 6% ethyl glucoside with a low selectivity (8%). FTIR analysis corroborates the incorporation of sulfate groups in the NbOx-DS matrix, unlike NbOx-CS. XRD pattern of NbOx-DS shows a lower angle shift of a peak to 23.5° compared to parent NbOx-D (24.32°), indicating lattice expansion due to the incorporation of sulfate groups, and no such a shift in the case of NbOx-CS is observed. NH3-temperature programmed desorption (NH3-TPD) reveals that NbOx-DS possess a 2.1-fold higher number of acidic sites than NbOx-D, whereas NbOx-CS possess a negligible number of acidic sites, indicating the significance of the synthesis procedure of NbOx-D for efficient incorporation of sulfate groups. NbOx-DS displays recyclability for at least three runs with minor loss in the activity. In a nutshell, the current study reflects that NbOx-DS obtained via precipitation followed by sulfate groups incorporation increases the medium/strong acidic sites, which contributes significantly to enhancing the ethyl glucoside selectivity (97%).

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Acknowledgements

SK, KS and SS would like to acknowledge the Department of Biotechnology, Government of India, for providing the infrastructural facilities through the Center of Innovative and Applied Bioprocessing for executing the research work. SK and XZ gratefully thank Chemical and Process Engineering, University of Strathclyde, Glasgow, United Kingdom, for allowing access to facilities for performing R&D activities. SK and XZ also thank Civil and Environmental Engineering, University of Strathclyde, for allowing access to HPLC. SK gratefully thank the Newton Bhabha PhD placement program, British Council for fellowship and financial support to carry out this research work and also thankful to Energy Research Centre, Panjab University, Chandigarh, for PhD registration. KS is grateful to the University Grants Commission, New Delhi, India, for providing a Junior Research Fellowship and Indian Institute of Science Education and Research (IISER) Mohali for PhD enrolment.

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The funding was provided by Newton Bhabha Fund Ph.D Placement Program(Grant No. 655339901) (Sahil Kumar).

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Correspondence to Shunmugavel Saravanamurugan, Xiaolei Zhang or Sushil Kumar Kansal.

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Kumar, S., Saini, K., Saravanamurugan, S. et al. Nanostructured Functionalised Niobium Oxide as Chemoselective Catalyst for Acetalation of Glucose. Top Catal 65, 1994–2004 (2022). https://doi.org/10.1007/s11244-022-01738-8

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