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    Scaling-Up an Aqueous Self-Degassing Electrochemically Mediated ATRP in Dispersion for the Preparation of Cellulose-Polymer Composites and Films

    Year: 2022

    Journal: Polymers, Volume 14, NOV

    Authors: De Bon, Francesco; Azevedo, Ines M.; Ribeiro, Diana C. M.; Rebelo, Rafael C.; Coelho, Jorge F. J.; Serra, Armenio C.

    Organizations: FCT-Fundacao para a Ciencia e a Tecnologia (Portuguese Foundation for Science and Technology) [PTDC/EQUEQU/2686/2020, POCI-01-0145-FEDER-029742]; FEDER-European Regional Development Fund through the COMPETE Programme; National Funds through FCT-Fundacao para a Ciencia e a Tecnologia (Portuguese Foundation for Science and Technology) [REEQ/481/QUI/2006, RECI/QEQ-QFI/0168/2012, CENTRO-07CT62-FEDER-002012]; Rede Nacional de Ressonancia Magnetica Nuclear (RNRMN); FEDER funds through the program COMPETE-Programa Operacional Factores de Competitividade; FCT-Fundacao para a Ciencia e a Tecnologia [UIDB/00285/2020, LA/P/0012/2020]

    Keywords: eATRP; self-degassing; polyacrylamides; cellulose; scale-up

    Electrochemically mediated atom transfer radical polymerization (eATRP) is developed in dispersion conditions to assist the preparation of cellulose-based films. Self-degassing conditions are achieved by the addition of sodium pyruvate (SP) as a ROS scavenger, while an aluminum counter electrode provides a simplified and more cost-effective electrochemical setup. Different polyacrylamides were grown on a model cellulose substrate which was previously esterified with 2-bromoisobutyrate (-BriB), serving as initiator groups. Small-scale polymerizations (15 mL) provided optimized conditions to pursue the scale-up up to 1000 mL (scale-up factor similar to 67). Cellulose-poly(N-isopropylacrylamide) was then chosen to prepare the tunable, thermoresponsive, solvent-free, and flexible films through a dissolution/regeneration method. The produced films were characterized by Fourier-transform infrared (FTIR), scanning electron microscopy (SEM), dynamic scanning calorimetry (DSC), and thermogravimetric analysis (TGA).
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