RESUMO
The thermal decomposition and kinetic parameters of four polymers, PN-1, PN-05, PN-01, and PN-005, were determined by thermogravimetry (TGA/DTG) under non-isothermal conditions. N-isopropylacrylamide (NIPA)-based polymers were synthesized by the surfactant-free precipitation polymerization (SFPP) with different concentrations of the anionic initiator potassium persulphate (KPS). Thermogravimetric experiments were carried out in the temperature range of 25-700 °C at four heating rates, 5, 10, 15, and 20 °C min-1, under a nitrogen atmosphere. Poly NIPA (PNIPA) showed three stages of mass loss during the degradation process. The thermal stability of the test material was determined. Activation energy values were estimated using Ozawa, Kissinger, Flynn-Wall-Ozawa (FWO), Kissinger-Akahira-Sunose (KAS), and Friedman (FD) methods.
RESUMO
The aim of the study was to monitor the influence of increasing initiator concentrations on the properties of poly-N-isopropylacrylamide (polyNIPA) nanoparticles obtained via surfactant free precipitation polymerization (SFPP). In all studied systems P-001 to P-1, the same amount of monomer was used, and increasing amounts of potassium persulphate (KPS). The course of each reaction was monitored by measuring the conductivity of the whole system. The resulting composition of products was confirmed by attenuated total reflectance within Fourier transformed infrared spectroscopy (ATR-FTIR) measurements. The hydrodynamic diameters with polydispersity index (PDI) and zeta potential (ZP) were measured in aqueous dispersions of the synthesized polymers in dynamic light scattering (DLS) device (λ = 678 nm), and were found to be for P-1: 20.33 nm (PDI = 0.49) and -7 mV, for P-05: 22.24 nm (PDI = 0.39) and -5 mV, for P-01: 50.14 nm (PDI = 0.49) and -3 mV, for P-005: 62.75 nm (PDI = 0.54) and -3 mV and for P-001: 509.4 nm (PDI = 0.61) and -12 mV at 18 °C, respectively. Initiator concentration affects the size and ZP of particles. The hydrodynamic diameter decreases with initiator concentration increase, whereas the time of the reaction decreases when the initiator concentration increases. This fact is reflected in the observed values of conductivity in the course of the performed reaction. Evaluated volume phase transition temperature in the range of 32 °C enables further research of the nanoparticles as thermosensitive drug carriers.
