This study evaluates the properties of chitosan (CS) membranes modified with different percentages (0.5%, 3%, and 5% w/w) of a graphene-based material. Graphene oxide (GO) and reduced graphene oxide (RGO) were obtained by the chemical exfoliation of graphite and thermal reduction. Then, they were characterized by electrical conductivity measurements, FESEM, XRD, AFM, and Raman spectroscopy. The composites’ morphology was evaluated by FESEM. The degree of swelling over a 48 h period and mass loss behavior in phosphate-buffered saline solution for up to 70 days were also studied. The hydrophilicity of the CS and CS/graphene nanocomposites was examined by water contact angle. The graphene materials showed small stacks (6-8 sheets) with low defect density and nanoscale thickness (1.3-5.9 nm). The dispersion of the graphene material in the CS matrix significantly decreased the degree of swelling (460%) but did not modify the hydrolytic degradation process and the hydrophilicity of membranes.
This work aimed to produce graphene oxide with few graphene layers, a low number of defects, good conductivity and reasonable amount of oxygen, adequate for use as filler in polymeric composites. Two starting materials were evaluated: expanded graphite and graphite flakes. The method of oxidation used was the Staudenmaier one, which was tested over different lengths of time. No appreciable differences were found among the oxidation times and so the lowest oxidation time (24 h) was chosen as the most adequate. An investigation was also conducted into suitable temperatures for the reduction of graphite oxide. A temperature of 1000 ºC gave the best results, allowing a good quality material with few defects to be obtained. The reduction was also evaluated under inert and normal atmosphere. The best results were obtained when the least modified material, e. g., graphite flakes, was used as a starting material, oxidized for 24h and reduced at 1000 ºC for 30 s in a quartz ampoule under a normal atmosphere.
A new titanium catalyst easily synthesized from ethylmaltol bidentate chelator ligand was studied in homogeneous and heterogeneous ethylene polymerization. The dichlorobis(3-hydroxy-2-ethyl-4-pyrone)titanium(IV) complex was characterized by 1H and 13C NMR (nuclear magnetic resonance), UV-Vis and elemental analysis. Theoretical study by density functional theory (DFT) showed that the complex chlorines exhibit cis configuration, which is important for the activity in olefin polymerization. The complex was supported by two methods, direct impregnation or methylaluminoxane (MAO) pre-treatment, in five mesoporous supports: MCM-41 (micro and nano), SBA-15 and also the corresponding modified Al species. All the catalytic systems were active in ethylene polymerization and the catalytic activity was strongly influenced by the method of immobilization of the catalyst and the type of support.
Polyethylene/carbon nanotubes, PE/NTC, nanocomposites were synthesized by in situ polymerization for comparison with polyethylene/graphene nanosheets, PE/NG, nanocomposites obtained in the same conditions. The nanocomposites of polyethylene/NTC were obtained with good catalytic activities and were characterized by DSC and TEM. The nanocomposites with NG showed better thermal stability than with NTC, however, no significant differences in dynamic mechanical properties were found. In the electrical conductivity study, PE/NTC nanocomposites reached conductivities of semiconductor materials at lower content of filler than PE/NG nanocomposites.
Nanocompósitos de polietileno/nanotubos de carbono foram sintetizados através da polimerização in situ para serem comparados com nanocompósitos de polietileno/nanolâminas de grafeno, obtidos nas mesmas condições. Os nanocompósitos de polietileno/NTC foram obtidos com boas atividades catalíticas e foram caracterizados por DSC e MET. Os nanocompósitos com NG apresentaram melhor estabilidade térmica que os de NTC, porem não houve diferenças significativas nas propriedades dinâmico-mecânicas. No estudo da condutividade elétrica os nanocompósitos PE/NTC atingiram condutividades de materiais semicondutores com menor teor de nanocarga que os de PE/NG.