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.
