A comprehensive study of a less harmful functionalization of multiwalled carbon nanotubes (MWCNT) was performed. The influence of ultrasonic cavitation and solid/liquid interface was indirectly evaluated by statistical characterization of MWCNT aspect ratio and degree of functionalization. MWCNT aspect ratio was determined through hundreds of electron microscopy images. Degree of functionalization of MWCNT was characterized by elemental analysis and thermogravimetry. Distribution of different oxygen-containing functional groups was assessed by potentiometric titration. MWCNT aqueous dispersions were evaluated by electrophoretic mobility and dynamic light scattering. An acid volume over 90% lower than usually reported in literature guaranteed MWCNTs with significantly larger aspect ratio, higher proportion of carboxylic groups and a more negative zeta potential in aqueous suspension. These results can be related to a more localized ultrasonic cavitation in MWCNTs/acid interface for reduced liquid volumes. This distinguished influence of ultrasonic cavitation may be a valuable contribution to more eco-friendly processes with nanomaterials.

The introduction of oxygen groups in carbon nanotubes is considered crucial for many applications. However, there is a lack of controlled functionalization methods which ensure nanotubes with specific property values according to each interest. In this work, acid treatments of multiwalled carbon nanotubes (MWCNTs) employing an optimized ultrasound process with moderate heating and stirring were studied by means of a factorial design. The functionalized nanotubes were characterized by thermogravimetry, elemental analysis, Raman spectroscopy, electron microscopy and water stability tests. Statistic models were fitted for the degree of functionalization and length reduction of MWCNTs. Temperature was identified as a key parameter to produce more functionalized MWCNTs with less structural damage. The properties of the functionalized MWCNTs can be tailored by the choice of parameters exploited in the statistical models developed to enable different end-use requests, such as for polymeric composites or bio-related applications, which is the original contribution of this work.

In this work, Ricinus communis L. press cake waste from biodiesel production was used to produce a versatile reactive material for environmental applications. The biodiesel cake waste was impregnated with FeIII at different concentrations (19-45 wt.%) and treated at 400, 600 and 800 °C. Mössbauer, X-ray diffraction (XRD), thermogravimetric analysis (TG/DTA), scanning electron microscope (SEM), elemental analysis CHN, Raman, potentiometric titration, saturation magnetization and Brunauer-Emmett-Teller (BET) analyses showed that the materials prepared at 400 °C are composed mainly of a graphitic and amorphous carbon containing dispersed magnetite (Fe3O4). At higher temperatures, metallic iron (Fe0) and iron carbide (Fe3C) are the predominant phases well dispersed in the carbon porous structure. These reduced iron species, Fe3O4 and Fe0, are active for the reduction of different hazardous contaminants. Preliminary experiments showed very high activities for the reduction and removal of aqueous CrVI.

Polyurethane/multi-walled carbon nanotube (MWCNT) nanocomposites have been prepared with nanotube concentrations between 0.01 wt% and 1 wt%. MWCNT as-synthesized samples with ~74 nm diameter and ~7 μm length were introduced by solution processing in the polyurethane matrix. Scanning electron microscopy (SEM) images demonstrated good dispersion and adhesion of the CNTs to the polymeric matrix. The C=O stretching band showed evidence of perturbation of the hydrogen interaction between urethanic moieties in the nanocomposites as compared to pure TPU. Differential scanning calorimetry and positron anihilation lifetime spectroscopy measurements allowed the detection of glass transition displacement with carbon nanotube addition. Furthermore, the electrical conductivity of the nanocomposites was significantly increased with the addition of CNT.

The fact that alpha- and beta-chitin adopt different arrays in the solid state is explored to emphasize their different properties and distinct spectral characteristics and X ray diffraction patterns. The methods for their extraction from the biomass in view of the preservation of their native structures and aiming to fulfill the claims of purity and uniformity for potential applications are discussed. The different arrays adopted by alpha- and beta-chitin also result in distinct reactivities toward the deacetylation reaction. Thus, the deacetylation of beta-chitin is more efficient owing to the better accessibility to amide groups due to the lower crystallinity of this polymorph.

A pervaporação, que é um dos processos com membranas empregado em separações seletivas específicas, como misturas azeotrópicas, misturas diluídas e misturas orgânicas, tem despertado um grande interesse nos últimos anos. Neste trabalho foram estudadas a influência de parâmetros, tais como concentração da solução polimérica, tempo de exposição, concentração de aditivo e temperatura de tratamento térmico na preparação de membranas assimétricas de poliacrilonitrila. Em função destes parâmetros, as membranas foram observadas por microscopia eletrônica de varredura (MEV), e determinada a cinética de precipitação em experimentos de transmissão de luz. Os resultados mostram que a precipitação é instantânea. As membranas compostas de poliacrilonitrila, obtidas pelo espalhamento de uma solução diluída de poli(álcool vinílico) sobre as membranas assimétricas de poliacrilonitrila, foram caracterizadas na separação de misturas de água/etanol por pervaporação. Os resultados foram comparados com a membrana comercial da GFT de poli(álcool vinílico)/poliacrilonitrila.

The use of pervaporation membrane separation technique for the selective separation of specific conditions like azeotropic, diluted and organic liquid mixtures, there has been increased interest in recent years. In this work, the influence of parameters like concentration polymeric solution, exposition time, additive concentration and annealing temperature in polyacrylonitrile asymmetric membranes were studied. In function of this parameters, the membranes was observed by scanning electron microscopy (SEM) and precipitation kinetic apparatus. The results showed the instantaneous precipitation mechanism. Poly(vinyl alcohol) diluted solution was casting onto polyacrilonitrile asymmetric membranes and the composite membrane was evaluated in pervaporation experiments. The results were compared with GFT commercial poly(vinyl alcohol)/polyacrylonitrile pervaporation membrane.