Fenaroli, Davide (2012) Sintesi e caratterizzazione di derivati di MWNT come filler per membrane polimeriche. [Laurea specialistica biennale]
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Aim of this thesis is the improvement of carbon nanotubes (CNTs) solubility by covalent exohedral functionalization to be employed as fillers for membrane polymers. The first samples are functionalized through oxidative reaction with cutting and etching procedures, are activated with thionyl chloride and are reacted with (metoxypolyethylen glycol amine and tert-butyl 2-(2-(2 ethylamine)ethoxy)ethyl carbamate). Then, CNTs are also functionalized by addition of the diazonium salts generated from 4-methoxyaniline, pentafluoroaniline, 4-(heptadecafluorooctyl)aniline and 2-(4-aminophenol)propanol) in batch conditions. Moreover the derivatization of CNT with 4-methoxyaniline and isoamilnitrite is implemented in the commercial agitated cell reactor Coflore®. A protocol is developed to compare the degrees of functionalization and the concentrations of functionalized CNTs. This protocol consists on an extraction procedure to separate the soluble derivatives and on the analysis of the supernatant by NIR-Uv-Vis spectroscopy, dynamic light scattering (DLS), thermal gravimetric analysis (TGA) and Raman spectroscopy. Furthermore in this thesis a kinetic analysis of CNT solubility is done in order to study the solubility of CNT and their aggregation as function of the time. The results of this thesis work highlight that the solubility of CNTs in organic and fluorinated solvents (DMF, EtOH, 1,1,2-trichloro-1,2,2-trifluoroethane) can be improved by functionalization depending on the nature of the functional groups reacted and on the initial concentration of the reagents.
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