几种生物降解多相多组分高分子材料的制备、形态、结构与性能研究
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摘要
生物降解高分子材料由于其环境友好的特性而得到研究者们的青睐。但是,由于价格高、力学性能差以及加工窗口窄等缺点,可生物降解高分子材料的应用受到严重限制。因此,对现已工业化的生物降解高分子材料进行改性是一个非常重要且有意义的研究课题。
本论文采用共混与复合两种方法,利用组分之间的氢键相互作用力,设计制备了一系列相容的结晶/非晶共混物,以及分散性良好的粘土纳米复合材料。采用差示扫描量热仪(DSC)、偏光显微镜(POM)、热失重分析仪(TGA)、广角X光衍射仪(WAXD)、小角X光散射仪(SAXS)、透射电镜(TEM)和动态力学分析仪(DMA)对不同共混物/复合体系的相容性、结晶行为以及复合体系的形态、结晶行为与性能进行了研究。
1.结晶/非晶共混物相容性与结晶行为
采用溶液涂膜法制备了一系列结晶/非晶共混物,研究了聚丁二酸/己二酸丁二醇酯(PBSA)/聚对羟基苯乙烯(PVPh)、酚氧树脂(phenoxy)共混物,聚羟基丁酸酯-羟基戊酸酯共聚物(PHBV)/酚醛树酯(phenolic)共混物,聚丁二酸丁二醇酯(PBSU)/单宁酸(TA)共混物相容性,以及非晶组分含量对结晶组分结晶行为的影响规律。单一组成依赖的玻璃化温度以及Nishi-Wang方程中聚合物相互作用参数均表明上述体系为相容体系。非晶组分的加入阻碍了结晶组分的成核与结晶,改变了结晶组分在相同温度下的球晶形态,但是并未改变其结晶机理与晶体结构。PBSA/phenoxy共混物的总结晶速率显著大于PBSA/PVPh共混物。所得相容的结晶/非晶共混物,在等温结晶后,仍然能够长满视野。研究发现PVPh与TA均己分别扩散至PBSA与PBSU的片晶之间。不同的是,PVPh加入会使得PBSA的片晶厚度略有增加,而TA不改变PBSU的片晶厚度。
2.聚对苯二甲酸/己二酸丁二醇酯(PBAT)/粘土C30B纳米复合材料结构与性能的研究
采用溶液超声复合的方法制备了不同C30B含量的PBAT/C30B纳米复合材料。实验结果表明：在C30B含量小于等于5 wt%时,C30B剥离于PBAT基体中；在C30B含量达到8 wt%时,插层与剥离并存。C30B在PBAT非等温结晶的过程中,充当成核剂的作用。当加入5 wt%的C30B时,复合材料成核活性最高。C30B的加入大幅度增加复合材料中PBAT的结晶速率。研究还发现：C30B的加入并未改变PBAT的结晶结构,也未明显改变PBAT的绝对结晶度。C30B加入没有明显改变PBAT的热稳定性,但是大幅提高了PBAT的储能模量E'。
In recent years, conventional plastics have been widely used which caused severe environmental problems. Therefore, biodegradable polymers have received more and more attention because of the environmental benign property. However, the application of the biodegradable polymers has been badly limited because of the relatively higher price, narrower processing window and poorer mechanical properties. The modificaition of industrial biodegradable polymer is a meaningful project and of great importance.
The polymer blending and nanocompounding with solution casting method were employed in this work. According to the special interaction between two neat components, a series of miscible crystalline/amorphous polymer blends and compatible organolclay nanocomposites were prepared. The influence of compositions, processing conditions to the morphology and crystallization was studied. It will be usefull in designing the polymer blend or composite materials with comprehensive properties.
1. The miscibility and crystallization behavior of crystalline/amorphous polymer blends
Four miscible crystalline/amorphous polymer blends have been prepared by solution-casting method. The single composition dependent glass transition temperature and the negative polymer-polymer interaction parameter indicate the complete miscibility of the polymer blends. The influence of the addition of amorphous polymer on the crystallization behavior and microstructure of crystalline polymer was also studied. The overall crystallization rates of crystalline polymer decrease with increasing crystallization temperature and the amorphous content in the blends; however, the crystallization mechanism of crystalline polymer does not change in the blends. The microstructural parameters, including the long period, thickness of crystalline phase and thickness of amorphous phase, change with increasing the amorphous content.
2. Poly(butylene adipate-co-terephthalate) (PBAT)/organo-modified montmorillonite nanocomposites
Biodegradable PBAT/C30B intercalated and exfoliated nanocomposites were fabricated by solution casting method to study the effect of clay loadings on the crystallization behavior, thermal stability, and dynamical mechanical properties of PBAT in the PBAT/C30B nanocomposites. X-ray diffraction and transmission electron microscopy results indicate the formation of exfoliated nanocomposites at low clay loadings less than 5 wt% and the mixture of exfoliated and intercalated nanocomposite at 8 wt% clay content throughout the PBAT matrix. Nonisothermal melt crystallization studies indicate that C30B enhances the crystallization of PBAT apparently due to the heterogeneous nucleation effect. Moreover, an attempt has been made to study the influence of the presence of C30B and its contents on the nucleation activity of PBAT quantitatively in the PBAT/C30B nanocomposites. It is also found that the thermal stability of PBAT decreases slightly in the nanocomposites. However, the storage modulus of PBAT increases apparently with increasing the C30B loadings in the PBAT/C30B nanocomposites.
本论文采用共混与复合两种方法,利用组分之间的氢键相互作用力,设计制备了一系列相容的结晶/非晶共混物,以及分散性良好的粘土纳米复合材料。采用差示扫描量热仪(DSC)、偏光显微镜(POM)、热失重分析仪(TGA)、广角X光衍射仪(WAXD)、小角X光散射仪(SAXS)、透射电镜(TEM)和动态力学分析仪(DMA)对不同共混物/复合体系的相容性、结晶行为以及复合体系的形态、结晶行为与性能进行了研究。
1.结晶/非晶共混物相容性与结晶行为
采用溶液涂膜法制备了一系列结晶/非晶共混物,研究了聚丁二酸/己二酸丁二醇酯(PBSA)/聚对羟基苯乙烯(PVPh)、酚氧树脂(phenoxy)共混物,聚羟基丁酸酯-羟基戊酸酯共聚物(PHBV)/酚醛树酯(phenolic)共混物,聚丁二酸丁二醇酯(PBSU)/单宁酸(TA)共混物相容性,以及非晶组分含量对结晶组分结晶行为的影响规律。单一组成依赖的玻璃化温度以及Nishi-Wang方程中聚合物相互作用参数均表明上述体系为相容体系。非晶组分的加入阻碍了结晶组分的成核与结晶,改变了结晶组分在相同温度下的球晶形态,但是并未改变其结晶机理与晶体结构。PBSA/phenoxy共混物的总结晶速率显著大于PBSA/PVPh共混物。所得相容的结晶/非晶共混物,在等温结晶后,仍然能够长满视野。研究发现PVPh与TA均己分别扩散至PBSA与PBSU的片晶之间。不同的是,PVPh加入会使得PBSA的片晶厚度略有增加,而TA不改变PBSU的片晶厚度。
2.聚对苯二甲酸/己二酸丁二醇酯(PBAT)/粘土C30B纳米复合材料结构与性能的研究
采用溶液超声复合的方法制备了不同C30B含量的PBAT/C30B纳米复合材料。实验结果表明：在C30B含量小于等于5 wt%时,C30B剥离于PBAT基体中；在C30B含量达到8 wt%时,插层与剥离并存。C30B在PBAT非等温结晶的过程中,充当成核剂的作用。当加入5 wt%的C30B时,复合材料成核活性最高。C30B的加入大幅度增加复合材料中PBAT的结晶速率。研究还发现：C30B的加入并未改变PBAT的结晶结构,也未明显改变PBAT的绝对结晶度。C30B加入没有明显改变PBAT的热稳定性,但是大幅提高了PBAT的储能模量E'。
In recent years, conventional plastics have been widely used which caused severe environmental problems. Therefore, biodegradable polymers have received more and more attention because of the environmental benign property. However, the application of the biodegradable polymers has been badly limited because of the relatively higher price, narrower processing window and poorer mechanical properties. The modificaition of industrial biodegradable polymer is a meaningful project and of great importance.
The polymer blending and nanocompounding with solution casting method were employed in this work. According to the special interaction between two neat components, a series of miscible crystalline/amorphous polymer blends and compatible organolclay nanocomposites were prepared. The influence of compositions, processing conditions to the morphology and crystallization was studied. It will be usefull in designing the polymer blend or composite materials with comprehensive properties.
1. The miscibility and crystallization behavior of crystalline/amorphous polymer blends
Four miscible crystalline/amorphous polymer blends have been prepared by solution-casting method. The single composition dependent glass transition temperature and the negative polymer-polymer interaction parameter indicate the complete miscibility of the polymer blends. The influence of the addition of amorphous polymer on the crystallization behavior and microstructure of crystalline polymer was also studied. The overall crystallization rates of crystalline polymer decrease with increasing crystallization temperature and the amorphous content in the blends; however, the crystallization mechanism of crystalline polymer does not change in the blends. The microstructural parameters, including the long period, thickness of crystalline phase and thickness of amorphous phase, change with increasing the amorphous content.
2. Poly(butylene adipate-co-terephthalate) (PBAT)/organo-modified montmorillonite nanocomposites
Biodegradable PBAT/C30B intercalated and exfoliated nanocomposites were fabricated by solution casting method to study the effect of clay loadings on the crystallization behavior, thermal stability, and dynamical mechanical properties of PBAT in the PBAT/C30B nanocomposites. X-ray diffraction and transmission electron microscopy results indicate the formation of exfoliated nanocomposites at low clay loadings less than 5 wt% and the mixture of exfoliated and intercalated nanocomposite at 8 wt% clay content throughout the PBAT matrix. Nonisothermal melt crystallization studies indicate that C30B enhances the crystallization of PBAT apparently due to the heterogeneous nucleation effect. Moreover, an attempt has been made to study the influence of the presence of C30B and its contents on the nucleation activity of PBAT quantitatively in the PBAT/C30B nanocomposites. It is also found that the thermal stability of PBAT decreases slightly in the nanocomposites. However, the storage modulus of PBAT increases apparently with increasing the C30B loadings in the PBAT/C30B nanocomposites.
引文
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