乙交酯、L-丙交酯均聚物及其共聚物的制备和性能研究
发布时间:2018-10-10 11:43
【摘要】:以辛酸亚锡为催化剂、1,4-丁二醇为引发剂,在高温、高真空条件下本体熔融开环聚合制备了聚乙交酯(PGA)、聚L-丙交酯(PLLA)及其不同比例的共聚物(PLGA).通过红外光谱(IR)、核磁共振(1H-NMR)对聚合物的结构进行了表征,用乌氏黏度计、凝胶渗透色谱仪(GPC)、示差扫描量热仪(DSC)、热重分析仪(TGA)、X射线粉末衍射仪(XRD)、流变仪等对聚合物的特性黏数、分子量与分子量分布、热性能、结晶性、流变性能进行了研究.结果表明PLGA和PLLA具有较高的分子量和窄的分子量分布;PGA、PLLA、PLGA均具有较高的热稳定性,随着PLGA中PGA单元的增加,分解温度逐渐升高.直接熔融合成的PGA在各有机溶剂中溶解性都不理想,用二甲基亚砜(DMSO)重结晶后的PGA在六氟异丙醇(HFIP)中的溶解度增大;PGA、PLLA具有较高的结晶度,而PLGA以非晶态存在,DMSO重结晶后的PGA的结晶度降低.PGA、PLLA、PLGA的熔体均是剪切变稀流体,但PGA、PLLA具有较高的储能模量,PLGA具有较高的损耗模量.相对于PGA和PLLA,无规共聚的PLGA易纯化,并且柔性较好,更易加工,因此PLGA是更适宜的生物可降解材料.
[Abstract]:Poly (glycolide) (PGA), poly (L- lactide) (PLLA) and its copolymers (PLGA). Were prepared by bulk melt ring-opening polymerization at high temperature and high vacuum using stannous octanoate as catalyst. The structure of the polymer was characterized by infrared (IR), NMR (1H-NMR). The intrinsic viscosity of the polymer was characterized by Wursonian viscometer, (GPC), differential scanning calorimeter, (TGA) X-ray powder diffractometer, (XRD), rheometer, etc. Molecular weight and molecular weight distribution, thermal properties, crystallization, rheological properties were studied. The results show that both PLGA and PLLA have high molecular weight and narrow molecular weight distribution. The decomposition temperature increases with the increase of PGA units in PLGA. The solubility of PGA synthesized by direct melt synthesis is not ideal in all organic solvents. The solubility of PGA after recrystallization with dimethyl sulfoxide (DMSO) in hexafluoroisopropanol (HFIP) is increased, and that of PGA,PLLA has higher crystallinity. However, the crystallinity of DMSO recrystallized PGA decreases with the existence of PLGA in amorphous state. The melt of PGA,PLLA,PLGA is shear-thinning fluid, but PGA,PLLA has higher storage modulus and PLGA has higher loss modulus. Compared with the random copolymerization of PGA and PLLA, PLGA is easy to purify, flexible and easy to process, so PLGA is a more suitable biodegradable material.
【作者单位】: 山东师范大学化学化工与材料科学学院教育部化学成像功能探针协同创新中心 齐鲁工业大学山东省轻工助剂重点实验室
【基金】:山东省自然科学基金(基金号ZR2013EMM004) 国家级大学生创新计划项目(项目号201101020236)资助
【分类号】:R318.08
[Abstract]:Poly (glycolide) (PGA), poly (L- lactide) (PLLA) and its copolymers (PLGA). Were prepared by bulk melt ring-opening polymerization at high temperature and high vacuum using stannous octanoate as catalyst. The structure of the polymer was characterized by infrared (IR), NMR (1H-NMR). The intrinsic viscosity of the polymer was characterized by Wursonian viscometer, (GPC), differential scanning calorimeter, (TGA) X-ray powder diffractometer, (XRD), rheometer, etc. Molecular weight and molecular weight distribution, thermal properties, crystallization, rheological properties were studied. The results show that both PLGA and PLLA have high molecular weight and narrow molecular weight distribution. The decomposition temperature increases with the increase of PGA units in PLGA. The solubility of PGA synthesized by direct melt synthesis is not ideal in all organic solvents. The solubility of PGA after recrystallization with dimethyl sulfoxide (DMSO) in hexafluoroisopropanol (HFIP) is increased, and that of PGA,PLLA has higher crystallinity. However, the crystallinity of DMSO recrystallized PGA decreases with the existence of PLGA in amorphous state. The melt of PGA,PLLA,PLGA is shear-thinning fluid, but PGA,PLLA has higher storage modulus and PLGA has higher loss modulus. Compared with the random copolymerization of PGA and PLLA, PLGA is easy to purify, flexible and easy to process, so PLGA is a more suitable biodegradable material.
【作者单位】: 山东师范大学化学化工与材料科学学院教育部化学成像功能探针协同创新中心 齐鲁工业大学山东省轻工助剂重点实验室
【基金】:山东省自然科学基金(基金号ZR2013EMM004) 国家级大学生创新计划项目(项目号201101020236)资助
【分类号】:R318.08
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