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Waste valorization of spent wastewater nanoadsorbents is a promising route toward achieving circular economy guidelines. In this study, the residual of layered double hydroxide (LDH) can be used as an electrocatalyst in direct methanol fuel cells as a novel approach. The Co\u2013Ni\u2013Zn\u2013Fe LDH was prepared by the co-precipitation method followed by the adsorption of methyl orange (MO).\u00a0Moreover, the spent adsorbent was calcined at different temperatures (200, 400, and 600\u00a0\u00b0C) to be converted to the corresponding mixed metal oxides (MMO). The prepared samples were characterized using XRD, FTIR, HRTEM, zeta potential, and hydrodynamic size measurements. The spent adsorbent was tested as an electro-catalyst for direct methanol electro-oxidation. The spent LDH\/MO adsorbent showed a maximum current density of 6.66\u00a0mA\/cm<jats:sup>2<\/jats:sup> at a 50\u00a0mV\/s scan rate and a 1\u00a0M methanol concentration. The spent MMO\/MO adsorbent showed a maximum current density of 8.40\u00a0mA\/cm<jats:sup>2<\/jats:sup> at a 200\u00a0\u00b0C calcination temperature, 50\u00a0mV\/s scan rate, and a 3\u00a0M methanol concentration. Both samples show reasonable stability over time, as indicated by the chronoamperometric response. Further nanoengineering of used nanoadsorbents could be a promising path to repurposing these wastes as electro-oxidation catalysts.\n<\/jats:p>","DOI":"10.1038\/s41598-022-23798-2","type":"journal-article","created":{"date-parts":[[2022,11,11]],"date-time":"2022-11-11T19:03:34Z","timestamp":1668193414000},"update-policy":"https:\/\/doi.org\/10.1007\/springer_crossmark_policy","source":"Crossref","is-referenced-by-count":30,"title":["Valorization of spent double substituted Co\u2013Ni\u2013Zn\u2013Fe LDH wastewater nanoadsorbent as methanol electro-oxidation catalyst"],"prefix":"10.1038","volume":"12","author":[{"given":"Rehab","family":"Mahmoud","sequence":"first","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hamdy F. M.","family":"Mohamed","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Sarah H. 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