RESUMO
In this work, poly (vinyl alcohol) (PVA) was employed to produce a Mesoporous Composition of Matter-48 Modified (MCM-48-M or MCM-48-PVA). After surface modification, MCM-48-M was used to produce nanocomposite (NC) films with polycaprolactone (PCL) as a matrix at room temperature. PCL and MCM-48 nanoparticles (NPs) were chosen due to their great biocompatibility and low toxicity. However, MCM-48-M is more compatible with PCL than MCM-48. NC films were sterilized by gamma radiation with a dose of 25 kGy and characterized by experimental techniques to investigate their chemical, mechanical (tensile) and thermal properties. Scanning electron microscopy (SEM) and transmission electronic microscopy (TEM) results indicated that MCM-48-M exhibited a random distribution in the PCL matrix. The PCL chemical structure was preserved in NC films as described by Fourier transform infrared (FT-IR) spectroscopy as well as the tensile and thermal properties of NC films. FT-IR and thermogravimetric analysis (TGA) results showed surface modification. X-ray diffraction (XRD) and differential scanning calorimetry (DSC) showed that crystalline symmetries were preserved and the crystallinity of NC films had small variations in all samples before and after irradiation, respectively. But, our results did not indicate major changes showing that this method is successful for the sterilization of PCL/MCM-48-PVA NC films.
RESUMO
MCM-48 mesoporous support was synthesized with the ionic solid 1-tetradecyl-3-methylimidazolium chloride ([C14MI]Cl) as a structure-directing agent for in situ immobilization of Candida antarctica B (CALB). The MCM-48[C14MI]Cl support showed characteristics of mesoporous material of interest, with a pore size of 20.30 and 73.41 A for the support without and with the enzyme, respectively. The elongation of the carbonic chain of the ionic solid directly influenced the increase in the specific area and pore volume of the material. In addition, the decrease in the specific area and pore volume for support with the enzyme showed the effectiveness of immobilization in situ. It was possible to obtain the ideal levels for the best activities of esterification of the enzyme with optimization of a mathematical model. The optimized variables were 0.31 g of enzyme and 3.35% of ionic solid with a maximum esterification activity of 392.92 U/g and 688% of yield. The support showed residual activity above 50% when stored under refrigeration for 75 days. At 60 and 80 °C, the enzyme immobilized on the support retained more than 80 and 40% of its residual activity, respectively. In addition, the support presented the possibility of reuse for up to 10 cycles with residual activity of approximately 50%. The support synthesized in the present study presents a great industrial opportunity for the immobilization and use of the CALB enzyme.
Assuntos
Enzimas ImobilizadasRESUMO
MCM-41 and MCM-48 with niobium were successfully synthesized using 1-tetradecyl-3-methylimidazolium chloride ([C14MI]Cl) as a structure-directing agent. The best Si/Nb molar ratio was chosen (Si/Nb = 20) and the CALB enzyme was immobilized in situ in the synthesized Nb-MCM. SEM micrographs showed the formation of very regular spherical agglomerates with a diameter between 0.25 and 0.75 µm. The material presented a surface area of 954 and 704 m2/g and a pore volume of 0.321 and 0.286 cm3/g, for Nb-MCM-41 and Nb-MCM-48, respectively. Also, both materials showed a pore size of 2.261 nm. The number of recycles obtained for the CALB enzyme immobilized in Nb-MCM-41 and Nb-MCM-48 was 26 recycles with a residual activity of 49.62% and 16 recycles with a residual activity of 53.01%, respectively. For both materials, enzymatic activity remained stable for 5 months of storage at room temperature and refrigeration. The supports were able to catalyze the esterification reaction at 40, 60, and 80 °C, showing industrial application in reactions that require high temperatures. This methodology allows the preparation of new highly active and selective enzyme catalysts using niobium and [C14MI]Cl. Also, the new materials can provide greater viability in processes, ensuring a longer service life of catalysts. Graphical abstract.