Acta Chim Slov. 2020 Mar;67(1):137-150.
This study aimed to prepare poly (3-hydroxybutyrate-co-3-hydroxyvalerate), biocomposites with incorporating various percentages of calcium carbonate using extrusion processing. Calcium carbonate was synthesized in the absence and presence of poly(vinyl sulfonic acid). The polymorph and morphology of calcium carbonate chanced with the introduction of poly(vinyl sulfonic acid). The rhombohedral calcite was obtained in the absence of poly(vinyl sulfonic acid). Rhombohedral calcite transformed into spherical vaterite with the addition of poly(vinyl sulfonic acid). The influence of filler contents on the properties of poly (3-hydroxybutyrate-co-3-hydroxyvalerate) composites was studied. The structure and properties of poly (3-hydroxybutyrate-co-3-hydroxyvalerate)/ calcium carbonate biocomposites were investigated by XRD, FTIR, TGA, DSC, SEM, OTR and DMA. The nucleation effect of the calcium carbonate on the crystallization of poly (3-hydroxybutyrate-co-3-hydroxyvalerate) was observed in the DSC and XRD measurements by increasing crystallinity of poly (3-hydroxybutyrate-co-3-hydroxyvalerate). It was shown that the variation of the barrier properties of biocomposites was influenced by polymorph and morphology of calcium carbonate. The addition of 0.5 wt% of the rhombohedral calcite and spherical vaterite increased the barrier properties by 25% and 12%, respectively compared to neat polymer. The dynamic mechanical properties of composites based on rhombohedral calcite and spherical vaterite in poly (3-hydroxybutyrate-co-3-hydroxyvalerate) matrix were investigated. The storage modulus increases by adding both particles in the composites over a wide range of temperature (-30 to 150 °C) where the reinforcing effect of calcite and vaterite was confirmed. At the same loading level, rhombohedral calcite led to more increase in the storage modulus, while less increase in storage modulus was observed in the presence of spherical vaterite particles.
本研究旨在使用挤出加工制备掺入不同百分比碳酸钙的聚(3-羟基丁酸酯-共-3-羟基戊酸酯)生物复合材料。碳酸钙是在不存在和存在聚(乙烯基磺酸)的情况下合成的。碳酸钙的多晶型和形态随聚(乙烯基磺酸)的引入而变化。在不存在聚(乙烯基磺酸)的情况下,得到菱面体方解石。加入聚(乙烯基磺酸)后,菱面体方解石转变为球形文石。研究了填充剂含量对聚(3-羟基丁酸酯-共-3-羟基戊酸酯)复合材料性能的影响。通过 XRD、FTIR、TGA、DSC、SEM、OTR 和 DMA 研究了聚(3-羟基丁酸酯-共-3-羟基戊酸酯)/碳酸钙生物复合材料的结构和性能。通过增加聚(3-羟基丁酸酯-共-3-羟基戊酸酯)的结晶度,在 DSC 和 XRD 测量中观察到碳酸钙对聚(3-羟基丁酸酯-共-3-羟基戊酸酯)结晶的成核作用。结果表明,生物复合材料的阻隔性能的变化受碳酸钙的多晶型和形态的影响。与纯聚合物相比,添加 0.5wt%的菱面体方解石和球形文石分别使阻隔性能提高了 25%和 12%。研究了基于菱面体方解石和球形文石的复合材料在聚(3-羟基丁酸酯-共-3-羟基戊酸酯)基质中的动态力学性能。在较宽的温度范围内(-30 至 150°C),复合材料中添加两种颗粒都会使储能模量增加,证实了方解石和文石的增强作用。在相同的负载水平下,菱面体方解石导致储能模量的增加更多,而在存在球形文石颗粒的情况下,储能模量的增加较少。