Abstract: Lignin is natural and renewable polymer, the second most abundant on Earth. Properly used it can reduce synthetic and oil based materials in addition to contributing to the biodegradable systems. In this work, the kraft lignin was subjected to gamma radiation at absorbed doses of 30, 60, and 90 KGy in order to increase the interaction with “Poly(butylene adipate-co-terephthalate) (PBAT)/Poly(lactic acid) (PLA)” blend (Ecovio®). PBAT/PLA/lignin blends with 10% of the weight of lignin were produced by extrusion using twin-screw extruder and characterized by Fourier transform infrared spectroscopy (FTIR), Differential scanning calorimetry (DSC), and Field emission scanning electron microscopy (FE-SEM). FTIR spectra showed partial miscibility between PBAT/PLA and lignin, most due to the hydrogen bond between PBAT/PLA carbonyl and lignin hydroxyl, being intensified in irradiated lignin compounds. As evidenced on DSC scans, in PBAT/PLA/irradiated lignin the crystallization peak was shifted to lower temperatures and the crystallization rate decreased. Crystallization kinetics was modeled using Pseudo Avrami, and isoconversional models of Friedman and Vyazovkin. Pseudo-Avrami displayed linearity deviation at beginning and crystallization ending due to the nucleation and secondary crystallization, while from Friedman and Vyazovkin the activation energy (Ea) was higher for PBAT/PLA/irradiated lignin 30 KGy, characterizing crystallization with higher energy consumption. FE-SEM images showed better dispersion and miscibility in PBAT/PLA/irradiated lignin. The results indicate that the irradiation of Kraft lignin promotes miscibility and compatibility of PBAT/PLA/lignin.

Palavras-Chave: crystallization; polymers; calorimetry; irradiation; kinetics

BARROS, JANETTY J.P.; SOARES, CARLOS P.; MOURA, ESPERIDIANA A.B. de; WELLEN, RENATE M.R. Enhanced miscibility of PBAT/PLA/lignin upon γ-irradiation and effects on the non-isothermal crystallization. Journal of Applied Polymer Science, v. 139, n. 45, p. 1-18, 2022. DOI: 10.1002/app.53124. Disponível em: http://repositorio.ipen.br/handle/123456789/33423. Acesso em: $DATA.

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Abstract: Many studies report that nanocomposites obtained by dispersion of a small amount nanofiller into the polymer have remarkable improvements achieved in the mechanical and physical properties. However, in order to achieve this great improvement in properties, it is necessary that the nanofillers be dispersed homogeneously into the polymeric matrix. Often this dispersion is difficult to achieve due to the high interfacial energy of the nanoparticles present. This study reports the effect of gamma irradiation induced graft of glycidyl methacrylate (GMA) onto the surface of TiO2 and Clay nanofillers to improve their dispersion into the EVA matrix. The physical and mechanical properties of Ethylene-vinyl acetate copolymer (EVA) flexible films with these nanoparticles were studied. EVA nanocomposite with adding of the different amount of TiO2 and modified montmorillonite clay grafted and un-grafted with glycidyl methacrylate (GMA) using gamma irradiation have been prepared by melt extrusion. The nanocomposite flexible films were produced using a flat die extrusion process. The PGMA-grafted nanofillers were characterized by XRD and TEM analysis. The flexible films were characterized by Tensile tests, ATR–FTIR, UV–VIS, XRD, TG, and FE-SEM analysis to understand the nature of the interaction between the nanofillers and EVA matrix. The results showed that the addition of PGMA-grafted TiO2 and Clay nanofillers into EVA matrix improved the bonding between the nanofillers and matrix. It was also found that the PGMA-grafted nanofillers could be well dispersed into an EVA matrix in contrast to that of un-grafted. The tensile strength and modulus of the resulting EVA/TiO2-PGMA enhanced in comparison to that of un-grafted TiO2. The EVA/Clay-PGMA had slightly decreased tensile strength comparable to that of EVA/Clay but had considerably improved elastic modulus. In addition, the flexible films based on TiO2 exhibited high UV–Vis light absorption with energy gap shifted to the visible region. The results demonstrated that TiO2 and Clay nanofillers grafted with GMA by gamma radiation can be used to prepare EVA flexible films with improved bonding between the nanofillers and matrix and, consequently, enhanced properties for food and cosmetic packaging application.

Palavras-Chave: dispersions; films; gamma radiation; irradiation; methacrylates; nanocomposites; physical properties; polymerization; titanium oxides; x-ray diffraction

BARTOLOMEI, SUELLEN S.; SANTANA, JULYANA G.; DIAZ, FRANCISCO R.V.; KAVAKLI, PINAR A.; GUVEN, OLGUN; MOURA, ESPERIDIANA A.B. Investigation of the effect of titanium dioxide and clay grafted with glycidyl methacrylate by gamma radiation on the properties of EVA flexible films. Radiation Physics and Chemistry, v. 169, p. 1-9, 2020. DOI: 10.1016/j.radphyschem.2018.08.022. Disponível em: http://repositorio.ipen.br/handle/123456789/31073. Acesso em: $DATA.

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Abstract: This study focuses on the preparation and characterization of nanocomposite system with bio-based epoxy resin (Super SAP 100/1000, contains 37% bio-based carbon content) and natural clays including Georgian clay and Brazilian clay. Georgian clay was surface modified using an ultrasound processing in presence of Decalin. Brazilian clay was modified to organophilic bentonite using quaternary ammonium salts. The resulting nano clay particles were characterized using XRD and TEM to confirm the particle size reduction and uniform distribution. The as-fabricated nanocomposites were characterized using flexure, DMA, TMA and TGA. The flexure analysis showed that the modified clay composites have significant improvement in strength (23–38%) and modulus (28–37%). Delayed thermal degradation was observed from TGA analysis which showed that the major degradation temperatures improved from 7°-25°C. DMA and TMA analysis showed improvements in storage moduli (4–6%) and coefficient of thermal expansion (CTE) (6–64%), respectively. The notable improvement in thermal and mechanical properties suggested the effective dispersion and the high degree of polymer particle interaction. The bio based content present in the Super Sap 100/1000 acts as plasticizer resulting in the extensive ductility of the polymer.

Palavras-Chave: nanocomposites; epoxides; clays; mechanical properties; thermal degradation; bentonite; thermomechanical treatments; differential thermal analysis; calorimetry

KODALI, DEEPA; UDDIN, MD-JAMAL; MOURA, ESPERIDIANA A.B.; RANGARI, VIJAK K. Mechanical and thermal properties of modified Georgian and Brazilian clay infused biobased epoxy nanocomposites. Materials Chemistry and Physics, v. 257, 2021. DOI: 10.1016/j.matchemphys.2020.123821. Disponível em: http://200.136.52.105/handle/123456789/31620. Acesso em: $DATA.

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Abstract: The amount of plastic waste generated is causing damage to the environment, such as sea and soil pollution, and one of the alternatives for disposing of polymers is recycling. This work proposes recycling expanded polystyrene using a biodegradable solvent, its plastification with glycerol, and the preparation of the composite with post-consumer recycled gypsum for applications to manufacturing by 3D printing and for finishing materials for construction. Specimen for tensile testing and shore D hardness were prepared by injection process and by 3D printing. In addition, Thermogravimetric (TG), Fourier-transform infrared spectrometry (FTIR), Differential scanning calorimeter, Scanning electron microscope (FESEM) analyses, and flame propagation tests were also carried out. TG and FTIR analyses show that the recycling process did not degrade the material, and the addition of glycerol and gypsum improved the thermal stability of the composite. The mechanical properties of the injected and 3D printed samples with gypsum were similar, due to the dimensional stability of the manufactured filament, which improved the speed and quality of the specimen printing. The increase in ductility and the reduction in the glass transition temperature showed that the recycled expanded polystyrene (RPS) were effectively plasticized with the addition of 2 wt% glycerol, preserving their flame self-extinguishment when subjected to the flame propagation test. Due to these properties, the plasticized RPS can be used to manufacture articles for finishing in civil construction, and the RPS composite can be used to manufacture 3D printed prototypes.

Palavras-Chave: 3d printing; recycling; composite materials; gypsum; polystyrene

BARTOLOMEI, SUELLEN S.; SILVA, FELIPE L.F. da; MOURA, ESPERIDIANA A.B. de; WIEBECK, HELIO. Recycling expanded polystyrene with a biodegradable solvent to manufacture 3D printed prototypes and finishing materials for construction. Journal of Polymers and the Environment, v. 30, n. 9, p. 3701-3717, 2022. DOI: 10.1007/s10924-022-02465-7. Disponível em: http://repositorio.ipen.br/handle/123456789/33227. Acesso em: $DATA.

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Abstract: Graphene and its derivatives, such as graphene oxide (GO), have attracted enormous interest from academia and industry because of its unique electrical, mechanical, and thermal properties, which can lead to enhanced material performance. In the present study, low contents of GO were incorporated into the poly (vinyl alcohol-co-ethylene) (EVOH). First, the GO was prepared by chemical oxidation of graphite employing a modified Hummer's method. The GO content of 0.1–0.3 wt % was incorporated in the EVOH matrix using a twin-screw extruder and extrusion blown film process to prepare flexible films. EVOH/GO film samples were irradiated at 100 kGy, using a 1.5 MeV electron-beam accelerator, at room temperature, in the presence of air. GO was characterized by XRD, ATR-FTIR, FE-SEM, and TEM analysis. XRD patterns of GO show a sharp reflection peak at 2θ = 10° (d001) corresponding to a d-spacing at 8.84 Å, characteristic of GO. The non-irradiated and irradiated samples were characterized by XRD, FEG-SEM, TG, DSC, oxygen transmission rate (OTR), UV/VIS analysis, and tensile tests. EVOH/GO nanocomposite films had an improved oxygen barrier, while also retaining fairly good transparency. As an effect of e-beam irradiation, the thermal, mechanical, and barrier behaviors of the nanocomposite films were even better than non-irradiated film samples, and obviously better than neat EVOH. Thus, the incorporation of low contents of GO followed by e-beam radiation treatment might be an interesting alternative to produce packaging materials based on EVOH with outstanding performance even under very humid conditions.

Palavras-Chave: graphene; oxide minerals; synergism; electron beam fusion reactors; radiations; polyethylenes; tensile properties; morphology

SANTANA, JULYANA G.; AKBULUT, MESHUDE; TEMPERINI, MARCIA L.A.; RANGARI, VIJAY K.; GUVEN, OLGUN; MOURA, ESPERIDIANA. Synergistic effect of e-beam irradiation and graphene oxide incorporation on thermal, mechanical, and barrier properties of poly (ethylene-co-vinyl alcohol) film. Radiation Physics and Chemistry, v. 199, p. 1-10, 2022. DOI: 10.1016/j.radphyschem.2022.110343. Disponível em: http://repositorio.ipen.br/handle/123456789/33467. Acesso em: $DATA.

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