In order to search nanofiller for controlling release of drugs lamellar α-zirconium phosphate (α-ZrP) was modified with ether-amine oligomer (E-A). Synthesis and chemical modification followed specific reaction conditions and different EA:ZrP ratios. Infrared spectra showed strong interaction between P-OH and NH2 groups. Thermogravimetric curves showed that ether-amine oligomer was incorporated by ZrP. Interlamellar space of α-ZrP increased at least four times indicating intercalation. The relaxometry analysis indicated that α-ZrP molecular mobility changed according to the ether-amine amount. The scanning electron microscopy/energy dispersive analysis revealed the presence of octadecylamine inside the α-ZrP galleries. The results showed that P-OH group (Brønsted acid) and amine group (Brønsted base) reacted to each other, resulting in an ionic bond PO- + 3HN-[-(CH2-CH2-O)m-(CH2-C-H(CH3)-O)n-]. Partially intercalated nanofiller were achieved.

Abstract Nanocomposite based on high density polyethylene (HDPE) and layered zirconium phosphate organically modified with octadecylamine (ZrPOct) was obtained through melt processing. The ZrPOct was synthesized by precipitation and modified by suspension and sonication procedures. The initial and maximum degradation temperatures (Tonset and Tmax) were increased. A slight decrease of crystallinity degree was detected. Reduction of elastic modulus and elongation at break were noticed. The lamellar spacing was increased (3.3 times higher). The storage modulus decreased and low field nuclear magnetic resonance (LFNMR) revealed an increasing of molecular mobility. The presence of octadecylamine enhanced the entrance of HDPE in the ZrPOct galleries. Several characteristics of HDPE were changed indicating that intercalation was successful. All results indicated that partially intercalated and/or exfoliated nanocomposite was achieved.

In this study we investigated the natural weathering of a catalyzed blend of poly(ethylene terephthalate)/polycarbonate PET/PC (80/20wt/wt%). The results were compared to the accelerated photoaging tests. The specimens were characterized by wide angle X-ray diffraction (WAXD), optical microscopy (OM), thermogravimetry (TG/DTG), medium infrared spectroscopy (FT-IR) and stress-strain analysis. The OM analysis revealed the coexistence of at least three phases – one rich in PET (matrix), the other rich in PC (dispersed droplet) and an interfacial region between them, made of PET/PC copolymer (compatibilizing agent) produced in situ. The TG/DTG curves showed that UV radiation acted mainly on the PET-rich phase and the PET/PC copolymer. The OM and TG/DTG results indicated that the degradation of the compatibilizing agent has had a critical effect on the mechanical properties. For both types of aging (natural and accelerated), the PET’s carbonyl index decreased with the exposure time. The FT-IR results corroborated what was seen in the OM images, showing that the PET phase acts as a shield against the PC degradation. Under accelerated aging, the mechanical properties decreased abruptly - mainly the stress-strain at yield and break - due to the degradation of the in situ compatibilizing agent.

A systematic study of solid state polymerization (SSP), concerning the melt extruded blend of poly(ethylene terephthalate)/polycarbonate (catalyzed PET/PC, 80/20 wt %), as a function of temperature range (180-190°C) for a fixed time (6 h) is presented. The materials obtained were evaluated by differential scanning calorimetry (DSC), thermogravimetry/derivative thermogravimetry (TG/DTG), optical microscopy (OM) and intrinsic viscosity (IV) analysis. After SSP, at all reaction temperatures, PET glass transition and heating crystallization temperatures slightly decreased, melting temperature slightly increased, while degree of crystallinity was practically invariable. The DTG curves indicated that, at least, three phases remained. The OM images revealed that the morphology is constituted of a PET matrix and a PC dispersed phase. In the interfacial region we noticed the appearance of structures like bridges linking the matrix and the dispersed domains. These bridges were correlated to the PET/PC block copolymer obtained during blending in the molten state. IV increased for all polymerization temperatures, due to the occurrence of PET chain extension reactions - esterification and transesterification. The IV range for bottle grade PET was achieved.

Composites of recycled high density polyethylene (HDPE-R) and coffee dregs (COFD) were elaborated. The blends were made at the proportions of 100-0, 90-10, 80-20, 70-30, 60-40, 50-50 and 40-60% polymer-filler ratio. The materials were evaluated through scanning electron microscopy (SEM), differential scanning calorimetry (DSC), thermogravimetry/derivative thermogravimetry (TGA), and compressive resistance test. The compounding was done using a two-stage co-kneader system extruder, and then cylindrical specimens were injection molded. All composites had a fine dispersion of the COFD into the polymeric matrix. The composites degraded in two steps. The first one was in a temperature lower than the neat HDPE, but higher than the average processing temperature of the polymer. The melting temperature and the degree of crystallinity of the composites resulted similar to the neat HDPE ones. The compressive moduli of the composites resulted similar to the neat polymer one. The results show that these composites have interesting properties as a building material.

In order to study the influence of different sulfonation routes on its thermal and structural properties sulfonated polyaniline (SPAni) was prepared. FT-IR revealed that the formation of PAni salt or ring sulfonation depends on the route. UV-visible spectra pointed out that the level of the PAni protonation was dependent on the sulfonation route. A new approach was given for TG/DTG and DSC results correlating different energy levels with the distinguished sulfonation routes. The TG/DTG degradation steps and the amount of the released material corroborated the structural differences of the polyanilines. For each DSC first regime of heating, a broad and intense peak (from -30 to 250 ºC) with different level of energy was noticed. That peak could be ascribed to the multiple relaxations and breaking of the PAni intra and inter hydrogen bonds after sulfonation.

RelyX TM Unicem, dual-curing self-adhesive resin cement, was tested in order to evaluate the degree of conversion (DC) and Vickers microhardness (VMH). The specimens were prepared into 4 groups (GR). For GR1, the specimens were irradiated with 500 mW.cm-2 during 20 seconds while for GR3 the same intensity was used but the irradiation time was 40 seconds. The GR2 followed the same polymerization mode of the GR1 but a ceramic disk was applied as a light barrier. For the last group, only the chemical polymerization was carried out. The DC and VMH were measured immediately after the irradiation time and again after 24 hours. Dual-polymerization (light and chemical polymerization) showed higher DC and VMH than the chemical polymerization (dark cure). The presence of a ceramic disk did not affect the DC but reduced the VMH. Increasing the exposure to light, the DC remained almost constant whereas the VMH raised slightly indicating that the VMH is quite dependent on the incident energy. Additionally, the powder/liquid portions of the cement were also characterized. The TG showed that the solid fraction was constituted of 96% of inorganic matter and 4% of vinyl-silane, a coupling agent. Regarding the liquid part, it was found that 84% was related to the mixture of monomers. The SEM revealed that the size particle of the inorganic fillers were between 400 and 11.000 nm. Factors such as energy density, size and distribution of inorganic fillers and the low effectiveness of the chemical cure contributed to the low values of the DC and VMH.

New types of copolymers using monomers which form inorganic polymers network (glass-like) and organic networks have been developed, known as ormocers. The aim of this work was to study how a particular dental filling material is degraded when subjected to a caries challenge by using low pH solutions. The supernadants were studied by HPLC to detect the presence of molecules from the resin, while the changes of the material surface were evaluated by contact angle. An organic modified ceromer (ormocer) called Definite® (Degussa ) was tested. Samples were built following manufacturer's instructions. After pH cycles, solutions were injected in a HPLC. The contact angle was obtained using a goniometer after and before the cycles. HPLC results showed material degradation, only detected in acid solutions. Bis-GMA and TEGDMA were detected in Definite® residues. Means and S.D. of contact angle were (p < 0,05): baseline: 85.16° ± 3.90° and after pH cycles: 69.77° ± 7.12°. The authors concluded that an ormocer filling material degraded on a caries simulated environment.