Among biopolymers, thermoplastic starch (TPS) is a good candidate to obtain biomaterials because of its natural origin, biodegradable character, and processability. Exposure to ultraviolet (UV) radiation causes significant degradation of starch-based materials, inducing photooxidative reactions which result in breaking of polymer chains, production of free radical, and reduction of molar mass. These changes produce a deterioration of TPS mechanical properties, leading to useless materials after an unpredictable time. In this work, changes induced on TPS by UV radiation, analyzing structural properties and mechanical behavior, are studied. TPS was obtained through thermo-mechanical processing of native corn starch in the presence of water (45 % w/w) and glycerol (30 % w/w) as plasticizers. Films were obtained by thermocompression and, before testing, specimens were conditioned to reduce material fragility. Photodegradation process was performed by exposing TPS to 264 h UV radiation in a weathering test chamber. Specimen's weight loss was determined gravimetrically. Chemical changes were studied by Fourier Transform Infrared Spectroscopy (FTIR) and morphological modifications were analyzed by Scanning Electron Microscopy (SEM). Reduction of weight average molar mass was measured by Static Light Scattering (SLS). Changes in mechanical properties were studied from tensile tests. After 96 h exposure, TPS specimens presented a weight reduction of 4-6%, mainly attributed to plasticizers lost by evaporation. SEM observations showed that UV radiation induced morphological changes on TPS, evidenced by an increment of specimens cracking. By FTIR, it was detected the presence of an additional band located at 1726 cm -1 in samples submitted to UV radiation, attributed to the formation of -C=O groups. Weight average molar mass of native starch was in the order of 107 g mol -1 . TPS exposure to UV radiation decreased significantly its molar mass, confirming molecular degradation of the biopolymer. When TPS was exposed during 48 h, it was detected a considerable decrease in elongation at break values (~ 85%), indicating that TPS flexibility was reduced. On the other hand, after 48 h exposure, TPS elastic modulus was 55 times higher than those of the unexposed specimens, evidencing an increase in material rigidity. TPS maximum tensile strength was also increased by UV light, with an increment of ~ 400% after 48 h exposure. Results revealed that starch-based materials can be degraded by exposure to UV radiation, modifying their microstructure and mechanical performance.
Polyhydroxybutyrate (PHB) is one of the few biopolymers that can be processed at industrial scale. Nevertheless, PHB applications in film form are limited, mainly due to the high biopolymer crystallinity and its narrow thermal processing window. In this work, it was studied the effect of glycerol tributyrate (GTB) incorporation as plasticizer, in addition to Irganox® 1010 (I) as phenolic antioxidant on the processability and final properties of PHB-based films. PHB was melt processed in the presence of GTB (5-30 %w/w, PHB basis) and Irganox® (0.3 %w/w, PHB basis) and films were obtained by thermo-compression. PHB films without the plasticizer and the antioxidant were used as control sample. Thermal properties of films demonstrated that PHB thermal processing window was increased due to a synergistic effect of both additives. Improvement can be attributed to changes in the crystalline structure corroborated by X-ray Diffraction (XRD) and Differential Scanning Calorimetry (DSC). Oxygen Transmission Rate (OTR) of PHB films increased in the presence of GTB and Irganox due to the crystalline changes induced by both additives.
Poly(3-hydroxybutyrate), PHB, is a hydrophobic biopolymer with good mechanical and barrier properties. However, neat PHB is a semicrystalline polymer with a relative high degree of crystallinity and poor film properties. In this work, this biopolymer was plasticized with glycerol tributyrate and functionalized with copper (II) sulfate, allowing us to obtain biodegradable antimicrobial flexible films. Films with the minimum inhibitory concentration (MIC) of copper (II) sulfate presented a higher roughness than neat PHB films. The presence of plasticizer significantly improved the copper sulfate diffusion process, which was evidenced by a greater inhibition halo for plasticized materials compared to unplasticized ones, at the same salt concentration. Plasticized PHB with 2.5% copper (II) sulfate inhibited both Gram-positive (Staphylococcus aureus) and Gram-negative (Pseudomona aeruginosa) bacteria, as determined by the bacterial inhibition halo. In addition, neat PHB films and PHB containing copper (II) sulfate did not show in vitro cytotoxicity in the L-929 cell line. Thus, plasticized PHB functionalized with copper (II) sulfate can be used as biodegradable antimicrobial flexible films for different applications.
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