RT Journal Article T1 Improving sustainability of cellulose nanofibrils production: FTIR spectroscopy for online control of the synthesis of recyclable magnetic TEMPO catalyst A1 Xu, Hongyu A1 Balea Martín, Ana A1 Merayo, Noemí A1 Martínez, Ainhoa A1 Negro Álvarez, Carlos Manuel AB 2,2,6,6-tetramethylpiperidine-N-oxyl (TEMPO) and its derivatives are well-established catalysts for various oxidation processes, despite its hazardous nature, causing harm to aquatic ecosystems. Thus, the reuse of TEMPO with a sustained high activity has gained significant importance for its industrial application, which has led to the development of supported TEMPO catalyst. In this context, the efficiency of the support process acquires high relevance. Therefore, this research is aimed at the improvement of the TEMPO supported on silica magnetically modified with Fe3O4 through the application of an online Fourier transform infrared spectroscopy (FTIR) probe to monitor its synthesis. FTIR effectively controlled the synthesis of supported TEMPO, by tracking online the concentration of 3-aminopropyltriethoxysilane (APTES) and tetraethyl orthosilicate (TEOS). Additionally, the presence of Fe3O4 particles in the core of the catalyst allowed its convenient recovery and subsequent reuse. Furthermore, the supported TEMPO catalyst was successfully applied in the oxidation of cellulose to produce nano/microfibrils. The carboxyl groups of the initial untreated cellulose increase from 0.05 mmol/g to 0.68 mmol/g with the supported TEMPO catalyst in presence of sodium hypochlorite and sodium bromide at 50 °C PB Elsevier SN 2666-8939 YR 2024 FD 2024-06 LK https://hdl.handle.net/20.500.14352/105194 UL https://hdl.handle.net/20.500.14352/105194 LA eng NO Xu, H.; Balea, A.; Merayo, N.; Martínez, A.; Negro, C. Improving Sustainability of Cellulose Nanofibrils Production: FTIR Spectroscopy for Online Control of the Synthesis of Recyclable Magnetic TEMPO Catalyst. Carbohydrate Polymer Technologies and Applications 2024, 7, 100417. https://doi.org/10.1016/j.carpta.2023.100417 NO 2024 Acuerdo transformativo financiado por la CRUE NO Ministerio de Ciencia e Innovación (España) NO Comunidad de Madrid DS Docta Complutense RD 21 jul 2025