Microfibers are important to several areas of human lifestyle, and the knowledge about their physicochemical characteristics allows for proposing new technological applications. The in natura microfiber of Ochroma pyramidale fruit (IN sample) and its extracted pulp (PU sample) were evaluated by X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR) and Thermogravimetry and Differential Scanning Calorimetry (TG/dTG and DSC). Microfibers were composed mainly of (68 ± 1)% holocellulose, (35.8 ± 0.1)% cellulose, (32 ± 3)% lignin and (3.7 ± 0.3)% extractives. The XRD pattern of the PU sample revealed that the mercerization process resulted in the change of the cellulose crystal structure from Iα type (triclinic) to type II (monoclinic). The SEM technique showed that the IN sample presented regular cylindrical/hollow-shaped wire-like microfibers with diameters ranging from 5 µm to 25 µm. However, the mercerization process changed their natural morphology. A significant change in the FTIR spectra after the removal of hemicellulose and lignin components was observed: weak bands at 1739 cm⁻¹ (C=O stretching of lignin and hemicellulose fractions), 1463 cm⁻¹ (CH₃ of lignin) and 1246 cm⁻¹ (C-O of lignin) were still observed in the PU sample, indicating that the lignin was not completely removed due to the natural difficulty of isolating pure cellulose. The TG/dTG and DSC evaluation revealed a temperature increase of the second thermal event (starting at 235 °C) in the PU sample, which was assigned to the cellulose and residual hemicellulose degradation. Then, this work aimed to disseminate and characterize a microfiber with unusual characteristics still little explored by the scientific community, as well as its cellulosic pulp, providing information that may be useful in its application in different industries, enabling the positive development of new biocompatible, renewable and sustainable materials.

Poly(p-anisidine) (PPA) is a polyaniline derivative presenting a methoxy (–OCH₃) group at the para position of the phenyl ring. Considering the important role of conjugated polymers in novel technological applications, a systematic, combined experimental and theoretical investigation was performed to obtain more insight into the crystallization process of PPA. Conventional oxidative polymerization of p-anisidine monomer was based on a central composite rotational design (CCRD). The effects of the concentration of the monomer, ammonium persulfate (APS), and HCl on the percentage of crystallinity were considered. Several experimental techniques such as X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), multifractal analysis, Nuclear Magnetic Resonance (¹³C NMR), Fourier-transform Infrared spectroscopy (FTIR), and complex impedance spectroscopy analysis, in addition to Density Functional Theory (DFT), were employed to perform a systematic investigation of PPA. The experimental treatments resulted in different crystal structures with a percentage of crystallinity ranging from (29.2 ± 0.6)% (PPA1_HT) to (55.1 ± 0.2)% (PPA16_HT-HH). A broad halo in the PPA16_HT-HH pattern from 2θ = 10.0–30.0° suggested a reduced crystallinity. Needle and globular-particle morphologies were observed in both samples; the needle morphology might have been related to the crystalline contribution. A multifractal analysis showed that the PPA surface became more complex when the crystallinity was reduced. The proposed molecular structures of PPA were supported by the high-resolution ¹³C NMR results, allowing us to access the percentage of head-to-tail (HT) and head-to-head (HH) molecular structures. When comparing the calculated and experimental FTIR spectra, the most pronounced changes were observed in ν(C–H), ν(N–H), ν(C–O), and ν(C–N–C) due to the influence of counterions on the polymer backbone as well as the different mechanisms of polymerization. Finally, a significant difference in the electrical conductivity was observed in the range of 1.00 × 10⁻⁹ S.cm⁻¹ and 3.90 × 10⁻¹⁴ S.cm⁻¹, respectively, for PPA1_HT and PPA16_HT-HH.

Poly(o-methoxyaniline) emeraldine-salt form (ES-POMA) was chemically synthesized using hydrochloric acid and subjected to a heat treatment (HT) process for 1 h at 100 °C (TT₁₀₀) and 200 °C (TT₂₀₀). The HT process promoted a progressive decrease in crystallinity. The Le Bail method revealed a decomposition from tetrameric to trimeric-folded chains after the HT process. The unheated POMA-ES presented a globular vesicular morphology with varied micrometric sizes. The heat treatment promoted a reduction in these globular structures, increasing the non-crystalline phase. The boundary length (S) and connectivity/Euler feature (χ) parameters were calculated from the SEM images, revealing that ES-POMA presented a wide distribution of heights. The TT₁₀₀ and TT₂₀₀ presented a narrow boundary distribution, suggesting smoother surfaces with smaller height variations. The UV-VIS analysis revealed that the transition at 343 nm (nonlocal π → π*) was more intense in the TT₂₀₀ due to the electronic delocalization, which resulted from the reduced polymer chain caused by the HT process. In addition to the loss of conjugation, counter ion withdrawal reduced the ion-chain interaction, decreasing the local electron density. This result shows the influence of the chlorine counter ions on the peaks position related to the HOMO → LUMO transition, since the π → polaron transition occurs due to the creation of the energy states due to the presence of counter ions. Finally, the electrical conductivity decreased after the HT process from 1.4 × 10⁻⁴ S.cm⁻¹ to 2.4 × 10⁻⁶ S.cm⁻¹ as result of the polymer deprotonation/degradation. Thus, this paper proposed a systematic evaluation of the POMA molecular structure and crystallite size and shape after heat treatment.

The development of conjugated polymer-based nanocomposites by adding metallic particles into the polymerization medium allows the proposition of novel materials presenting improved electrical and optical properties. Polyaniline Emeraldine-salt form (ES–PANI) has been extensively studied due to its controllable electrical conductivity and oxidation states. On the other hand, tungsten oxide (WO₃) and its di-hydrated phases, such as WO₃·2H₂O, have been reported as important materials in photocatalysis and sensors. Herein, the WO₃·2H₂O phase was directly obtained during the in-situ polymerization of aniline hydrochloride from metallic tungsten (W), allowing the formation of hybrid nanocomposites based on its full oxidation into WO₃·2H₂O. The developed ES–PANI–WO₃·2H₂O nanocomposites were successfully characterized using experimental techniques combined with Density Functional Theory (DFT). The formation of WO₃·2H₂O was clearly verified after two hours of synthesis (PW₂ nanocomposite), allowing the confirmation of purely physical interaction between matrix and reinforcement. As a result, increased electrical conductivity was verified in the PW₂ nanocomposite: the DFT calculations revealed a charge transfer from the p-orbitals of the polymeric phase to the d-orbitals of the oxide phase, resulting in higher conductivity when compared to the pure ES–PANI.

Drying is a crucial step in ensuring the quality of teas, as it can alter their chemical composition and organoleptic characteristics. In the present study, we examined the effects of different drying temperatures (ranging from 60 to 90°C) using hot air drying (HAD) on Theobroma speciosum flowers concerning drying kinetics, color, digestibility, and antioxidant capacity. From the obtained curves, we analyzed the physical aspects of T. speciosum, along with the moisture loss throughout the process, and the impact of different temperatures. This revealed that the Midilli mathematical model was the most suitable, where a set of equations was used to predict the analysis method’s behavior. The results demonstrated that drying at 60°C was more effective in terms of drying rates, diffusivity, and bioactive compound content, making it a promising option for the pre-treatment of T. speciosum flower tea.