Solvent-free mechanochemical synthesis of catalytically active nanomaterials Elisabete Alegria 1,2 , Ana P.C. Ribeiro 1 , Maximilian N. Kopylovich 1 , Armando J.L. Pombeiro 1 1 Chemical Engineering Departament, ISEL, Instituto Politécnico de Lisboa, Portugal 2 Centro de Química Estrutural, Complexo I, Instituto Superior Técnico, Universidade de Lisboa, Portugal Design and synthesis of micro- and nanoscale materials with specific morphologies still face challenges due to their wide range of applications in nanotechnology. In this view, mechanochemical and similar dry synthetic methods can be particularly interesting since they can exclude solvation and surface effects, which can significantly influence and hinder the preparation of new dispersed nano- and micro-scale materials. A simple and clean mechanochemical synthesis at room temperature was employed to prepare 3d metal-based dispersed composites with different ratios of components using simple metal salts/oxides and multi-walled carbon nanotubes (CNT) or graphene oxide (GO) additives. The thus prepared composite materials were characterized by XPS, SEM, FEGSEM, EDX, and TEM techniques. XPS analysis revealed no metal redox change upon ball milling treatment. The heterometallic dispersed catalysts were screened for the peroxidative oxidation of alcohols and alkanes, under mild conditions. Parameters such as size, type and the number of milling balls, and reaction time (milling time) are evaluated. The influence of multi-walled carbon nanotubes (CNTs) and graphene oxide (GO) as additives are tested for the reinforcement of the catalytic performance. A comparison with traditional wet synthetic approaches will be discussed to highlight the advantages of mechanochemistry and its high energy efficiency. This work was supported by the Fundação para a Ciência e Tecnologia, Portugal, through project 2022.02069. PTDC and from the Instituto Politécnico de Lisboa for the IPL/2022/MMOF4CO2_ISEL_project. References 1. M.N. Kopylovich, A.P.C. Ribeiro, E.C.B.A. Alegria, “Mechanochemical Activation and Catalysis”, in Noncovalent Interactions in Catalysis, edited by Kamran T. Mahmudov, Maximilian N. Kopylovich, M Fatima C. Guedes da Silva, Armando J.L. Pombeiro, RSC, 2019, Ch. 25, 548-563 (ISBN 978-1-78801-468-7). 2. E.C.B.A., Alegria, E. Fontolan, A.P.C. Ribeiro, M.N. Kopylovich, C. Domingos, A.M. Ferraria, R. Bertani, A.M.B. Rego, A.J.L. Pombeiro, Mater.Today Chem. 5 (2017) 52. 3. Fontolan, E.C.B.A. Alegria, A.P.C. Ribeiro, M.N. Kopylovich, R. Bertani, A.J.L. Pombeiro, Inorg. Chim. Acta 455 (2017) 653. 4. A.P.C. Ribeiro, E. Fontolan, E.C.B.A. Alegria, M.N. Kopylovich, R. Bertani, A.J.L. Pombeiro, J. Molec. Catal, A: Chem. 426 (2017) 557.
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