反应加工制备聚合物/POSS复合材料的结构与性能研究
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摘要
有机/无机纳米复合材料可充分结合有机高分子和无机材料的优点,从而引起人们的广泛关注。多面齐聚倍半硅氧烷(Polyhedral oligomeric silsesquioxane,POSS)是一类重要的纳米尺度的笼型有机-无机杂化分子,其分子式为(RSiO1.5)n,尺寸约为1～3 nm,被认为是“目前可能存在的最小的硅粒子”。由于其特殊的结构与性能,POSS(零维)被认为是和蒙脱土(二维)、碳纳米管(一维)一样最具前景的纳米材料之一,从而成为材料科学研究的热点之一。
目前,POSS已通过化学共聚和物理共混的方法被广泛引入聚合物中。本论文采用反应加工的方法制备聚合物/POSS复合材料,并研究聚合物POSS复合材料的结构和性能。论文研究主要包括三部分:(1)环氧化环己基POSS(epoxy-POSS)扩链聚对苯二甲酸丁二醇酯(PBT)的结构与性能研究;(2)反应共混制备聚丙烯(PP)/八乙烯基POSS(OvPOSS)复合材料的结构与性能研究;(3)马来酸酐接枝PP(MA-g-PP)反应增容PP/八氨基苯基POSS(OapPOSS)复合材料的结构与性能研究。
(1)Epoxy-POSS扩链PBT的结构与性能研究
通过反应挤出的方法制备了epoxy-POSS扩链的PBT。epoxy-POSS扩链后PBT的特性粘数增加,羧基含量降低,熔体流动指数(MFI)降低。当epoxy-POSS含量从0 %增加到2 %时,特性粘数从1.1 dL/g增加到1.7 dL/g,羧基含量从21.6 eq/106g降低到7.0 eq/106g,MFI从30 g/10min降低到7 g/10min。并且机械性能改善,加工热稳定性提高,吸水率降低,有利于PBT的储存、加工和应用。
(2)反应共混制备PP/ OvPOSS复合材料的结构与性能研究
在过氧化二异丙苯(DCP)作用下通过反应共混的方法制备了PP/OvPOSS复合材料,并研究其结构与性能。随着DCP或OvPOSS含量增加,OvPOSS接枝率增加。采用X-射线衍射(XRD)、示差扫描量热法(DSC)、旋转流变等方法研究了不同的加工方法(物理共混和反应共混)制备的PP/OvPOSS复合材料的结构与性能。物理共混时OvPOSS在含量低于2 %时完全分散在PP基体中,含量超过2 %时OvPOSS开始聚集、结晶。以分子状态分散的OvPOSS分子起到PPβ晶成核剂的作用,促进PPβ晶的形成。反应共混后OvPOSS与PP相容性提高,分散更均匀,PP的β晶型消失。反应共混PP/OvPOSS复合材料机械性能比物理共混的综合更好,在OvPOSS含量为2 %时机械性能最佳。DCP用量0.1 %,OvPOSS用量2 %时,复合材料的弯曲模量和冲击强度比纯PP分别提高约20 %和50 %。PP/OvPOSS复合材料的热分解温度低于纯PP,但反应共混复合材料和OvPOSS-g-PP的热稳定性高于物理共混复合材料。OvPOSS加入后材料热释放速率和质量损失速率降低,提高材料阻燃性。
利用旋转流变、熔体流动指数等方法研究了PP/OvPOSS复合材料的流变行为。结果表明物理共混PP/OvPOSS复合材料的粘度随OvPOSS含量增加先降低后增加。反应共混复合材料的粘度在低频区粘度随OvPOSS含量增加而显著增加,在OvPOSS含量高于1 %时表现出明显的凝胶行为。反应共混PP/OvPOSS复合材料的Han图、Cole-Cole图和van Gurp-Palmen图也发生明显偏移。这一现象表明OvPOSS接枝到PP链段上之后由于OvPOSS与PP之间强的粒子-基体相互作用,抑制PP链段运动,出现明显的凝胶行为。而在物理共混时粒子-基体相互作用和粒子-粒子相互作用都很弱,OvPOSS含量为10 %时也不出现凝胶现象。
利用DSC研究了PP/OvPOSS复合材料的等温和非等温结晶动力学。物理共混时OvPOSS对PP非等温结晶时的结晶峰温度(Tp)影响不大;反应共混复合材料和OvPOSS-g-PP的Tp显著提高,并且OvPOSS含量对Tp影响不大,表明复合材料中聚集的OvPOSS晶体对PP成核作用并不明显,而少量OvPOSS接枝到PP上就具有显著的成核作用,进一步增加接枝的OvPOSS含量对PP结晶行为影响不大。Avrami方程能够描述PP和不同体系的PP/OvPOSS复合材料的等温结晶动力学。OvPOSS对PP起到异相成核的作用,影响了PP成核机理和成核过程,促进PP结晶,折叠链表面自由能σe降低。反应共混复合材料结晶速度更快,σe更低。用Ozawa方程、Ozawa和Avrami组合方程研究PP/OvPOSS复合材料的非等温结晶动力学,结果发现Ozawa方程不适合这个体系,而利用Ozawa和Avrami组合方程则能很好的描述。并利用Kissinger和Takhor方程计算非等温结晶过程活化能(ΔE),发现物理共混和反应共混PP/OvPOSS复合材料的ΔE值略高于PP。
(3)MA-g-PP反应增容PP/OapPOSS复合材料的结构与性能研究
制备了OapPOSS,以MA-g-PP为增容剂,研究OapPOSS填充PP的结构与性能。MA-g-PP可以与OapPOSS中氨基反应,MA-g-PP加入到PP/OapPOSS复合材料中可提高PP与OapPOSS的相容性,OapPOSS粒子粒径明显降低,材料机械性能改善。对PP/OapPOSS复合材料,Tp随着OapPOSS含量增加而降低。然而对于PP/ MA-g-PP/OapPOSS复合材料,Tp随着OapPOSS含量增加而增加,表明OapPOSS加入抑制PP成核,而加入MA-g-PP后成核作用大于抑制作用,促进了PP结晶。PP/OapPOSS的η*高于纯PP并且随着OapPOSS含量增加而增加,然而PP/ MA-g-PP /OapPOSS的η*在OapPOSS含量为5 %时达到最大值并且低于相同OapPOSS含量时PP/OapPOSS体系。这可能是由于MA-g-PP与OapPOSS反应后包覆在OapPOSS表面,降低了OapPOSS的粒子-粒子相互作用,同时粒子间滑移更容易,导致粘度降低。
本论文的主要创新之处:
目前POSS主要通过化学共聚或物理共混的方法引入聚合物基体中,采用反应加工的方法制备聚合物/POSS复合材料的研究较少,本论文主要采用反应加工的方法将POSS引入聚合物基体中,改善聚合物的性能。与物理共混方法相比,反应共混后材料的机械性能改善,流变性能、热性能等均有所改变。
(1)研究了一种环氧化环己基POSS通过反应挤出来扩链PBT的方法。该方法扩链PBT的熔体粘度显著增加,凝胶含量低,热稳定性好,吸水性低,更利于PBT的储存、加工及应用。
(2)首次采用反应共混的方法制备了OvPOSS接枝PP,研究了物理共混和反应共混这两种不同加工方法对PP/OvPOSS复合材料的结构与性能的影响。反应共混方法制备PP/OvPOSS复合材料中OvPOSS与PP的相容性改善,OvPOSS粒子的对PP结晶的成核作用更显著,并且材料机械性能优于物理共混复合材料。反应共混方法工艺简单、生产周期短、无需复杂的分离提纯和溶剂回收等后处理过程,为制备聚合物/POSS复合材料提供了一种新的方法。
(3)对比研究了反应共混和物理共混法制备PP/OvPOSS复合材料的动态流变行为,进一步探讨了复合材料内部结构-性能之间的相互关系。反应共混复合材料在OvPOSS含量高于1 %时在低频区出现明显的凝胶行为,而物理共混复合材料在OvPOSS含量为10 %时也不出现凝胶行为。通过比较POSS与聚合物之间相互作用解释了这两种不同加工方法时材料流变行为的差异,可以为研究其他聚合物/填料复合材料结构-性能之间的相互关系提供参考。
(4)采用MA-g-PP反应增容了PP/OapPOSS复合材料。MA-g-PP可与OapPOSS中氨基反应,增加了PP与OapPOSS的相容性,改善了复合材料的机械性能。为选择合适的POSS填充聚合物、改善聚合物性能提供了一种新方法。
Organic-inorganic nanocomposites have drawn great attention due to their excel combination of properties of organic polymers and with inorganic systems. Polyhedral oligermeric silsesquioxane (POSS) is a kind of important organic-inorganic hybrid molecular with a formula of (RSiO1.5)n. Nanostructured POSS molecular, with the diameter of 1~3 nm, is thought as“the smallest possible particles of silica”. Due to its special structure and properties, POSS (0-D) can be thought as one of the most promising nanofillers which including clay layered silicates (2-D), single and multi-wall carbon nanotubes (1-D), and has drawn great interest.
Recently, POSS has been widely introduced into polymers by chemical copolymerization or physical blending. In this study, polymer/POSS composites were prepared through reactive processing method and their structure and properties were studied. There are three parts in this study: (1) The study on structure and properties of epoxycyclohexyl POSS (epoxy-POSS) chain-extended poly(butylene terephthalate) (PBT), (2) The study on structure and properties of octavinyl POSS (OvPOSS) grafted polypropylene (PP) by reactive blending, (3) The study on structure and properties of maleic anhydride-grafted PP (MA-g-PP) reactive compatibilized PP/octaaminophenyl polyhedral oligomeric silsesquioxane (OapPOSS) composites.
(1) The study on structure and properties of epoxy-POSS chain-extended PBT
Epoxy-POSS chain-extended PBT was prepared by reactive extrusion. The epoxy-POSS chain-extended PBT has higher intrinsic viscosity, lower carboxyl content and melt flow index (MFI) than PBT. PBT had an intrinsic viscosity of 1.1 dL/g, carboxy1 content of 21.6 eq/106g and MFI of 30 g/10min, but the PBT chain-extended with 2 wt% epoxy-POSS had an intrinsic viscosity of 1.7 dL/g, carboxy1 content less than 7 eq/106g and MFI of 7 g/10min. The chain-extended PBT has also improved mechanical properties and thermal properties, indicating it is favorable for storage, processing and application.
(2) The study on structure and properties of OvPOSS grafted PP by reactive blending
The OvPOSS grafted PP was prepared by reactive blending in the presence of dicumyl peroxide (DCP), and the structure and properties of PP/OvPOSS composites were studied. The graft ratio of OvPOSS increased with the increase of DCP or OvPOSS content. The structure and properties of PP/OvPOSS composites prepared by two different processing methods (physical blending and reactive blending) were studied by X-ray diffraction (XRD), differential scanning calorimetry (DSC) and rheological test, respectively. For the physical blending composites, POSS molecules can completely dissolve in PP matrix at OvPOSS content lower than 2 %, and aggregate to crystal with further increasing OvPOSS content. And the dissolved OvPOSS molecules can act asβ-form crystalline nucleating agents. While for the reactive blending composites, OvPOSS had good compatibility and dispersion in PP matrix. Theβ-form crystal disappeared. The reactive blending composites have better mechanical properties than the physical blending ones, and have the best mechanical properties at 2 % OvPOSS content. The impact strength and flexural modulus of PP filled with 2 % POSS and 0.1 % DCP are about 50 % and 20 % higher than that of pure PP, respectively. PP/OvPOSS composites have lower degradation temperature than PP, and the reactive blending composites have better thermal stability than that of the physical blending ones. The heat release rate and mass loss rate decreased when
OvPOSS was added.
The rheological behavior of physical and reactive blending composites was compared by using oscillatory rheological measurements and melt flow index. It was found that the viscosity of physical blending composites drops at lower OvPOSS content (0.5~1 wt %) and thereafter increases with increasing OvPOSS content. While the viscosity of the reactive blending composites increases with increasing OvPOSS content and the composites display a solid-like rheological behavior at low frequency region when POSS content is higher than 1 wt %. The deviation of reactive blending composites from the scaling log G′-log G″of linear polymer in Han plot, upturning at high viscosity in Cole-Cole plot and from van Gurp-Palmen plot are related to the gelation behavior when OvPOSS was grafted to PP chains..
Isothermal and nonisothermal crystallization behavior was analyzed by DSC test. The crystallize peak temperature (Tp) of physical blending PP/OvPOSS composites is close to that of pure PP and changes little with increasing OvPOSS content. While for the reactive blending composites and OvPOSS-g-PP, Tp is greatly higher than that of PP and changes little with increasing OvPOSS content. It indicates that aggregated OvPOSS crystals have little nucleating effect on PP while grafted OvPOSS has significant nucleating effect and the nucleating effect changes little with increasing the graft ratio of OvPOSS. The Avrami equation was used to study the isothermal crystallization kinetics of PP and PP/OvPOSS composites. The results show that OvPOSS can act as a heterogeneous nucleating agent, especially effective for the reactive blending composites. Addition of OvPOSS accelerates the crystallization of PP, increases the rate of crystallization and decreases the chain folding energy of PP. For the nonisothermal crystallization kinetics of PP/OvPOSS composites, the Ozawa equation is not suitable for these materials while the combination of Avrami and Ozawa equations exhibits great advantages in treating the nonisothermal crystallization kinetics of PP/OvPOSS composites. The activation energies (ΔE) calculated by Kissinger and Takhor methods for the nonisothermal crystallization of phtsical blending and reactive blending PP/OvPOSS composites are slightly higher than PP.
(3) The study on structure and properties of MA-g-PP reactive compatibilized PP/OapPOSS composites.
OapPOSS was prepared and filled to PP and MA-g-PP was selected as compatibilizer. The addition of MA-g-PP could improve the compatibility between PP and OapPOSS, promote a fine dispersion of OapPOSS particles in PP matrix and improve the mechanical properties of PP due to the reaction of amine groups of OapPOSS with maleic anhtydride groups of MA-g-PP. With increasing OapPOSS content, the Tp of PP/OapPOSS composites decreased while that of PP/MA-g-PP/OapPOSS composites increased, indicating OapPOSS could retard the crystallization of PP in PP/OapPOSS composites, while the nucleating effect compensated and overlapped the retardation effects when MA-g-PP was added. For PP/OapPOSS composites,η* increased with increasing OapPOSS content, while theη* of all the PP/MAPP/OapPOSS composites was lower than that of PP /OapPOSS at the same OapPOSS content and reached the maximum at 5 % OapPOSS content. It is probably due to the lower particle-particle interaction and interface slipping when OapPOSS was encapsulated by PP chain when OapPOSS was reacted with MA-g-PP.
The innovations of this dissertation are list as follows:
Recently, POSS has been widely introduced into polymers by chemical copolymerization or physical blending. While there are little reports about PP/POSS composites prepared by reactive processing. In this study, POSS was introduced to polymers to improve the properties of polymers. Compared with PP/POSS composites prepared by physical blending, the reactive blending composites had better mechanical properties. Their rheological behavior and thermal properties were different.
(1) A method of epoxy-POSS chain-extended PBT was investigated. PBT chain extended by this method has higher viscosity, lower gel content, better thermal stability and lower water absorption, which is advantage for storage, processing and application of PBT.
(2) OvPOSS was firstly grafted to PP by reactive blending method. The structure and properties of the composites prepared by the two processing methods (reactive blending and physical blending) was studied. For the reactive blending composites, OvPOSS has goog compatibility and dispersion in PP matrix, significant nucleating effect on the crystallization of PP and improved the mechanical properties of PP. Reactive blending has advantages of simplified technique, short product cycle and no complicated aftertreat including separation, purification and solvent recycle. The properties of reactive blending composites also have better properties than physical blending composites. It provides a new method to prepare polymer/POSS composites.
(3) The rheological behavior of reactive blending and physical blending composites was compared, and the structure-property relationship of composites was discussed. The reactive blending composites display solid-like rheological behavior at low frequency region when OvPOSS content is higher than 1 %, while the physical blending composites do not display solid-like rheological behavior even at 10 % OvPOSS content. The difference of rheological behavior of two different methods was explained by the interaction of POSS and polymer, which can provide the reference for investigating the structure-property relationship of other polymer/fillers composites.
(4) MA-g-PP was selected as reacitve compatibilizer to PP/OapPOSS composites. The addition of MA-g-PP could improve the compatibility between PP and OapPOSS, and improve the mechanical properties of PP due to the reaction of amine groups of OapPOSS with MA-g-PP. It provides a method for choosing suitable formation of POSS filled polymer and studying the structure-properties relationship.
目前,POSS已通过化学共聚和物理共混的方法被广泛引入聚合物中。本论文采用反应加工的方法制备聚合物/POSS复合材料,并研究聚合物POSS复合材料的结构和性能。论文研究主要包括三部分:(1)环氧化环己基POSS(epoxy-POSS)扩链聚对苯二甲酸丁二醇酯(PBT)的结构与性能研究;(2)反应共混制备聚丙烯(PP)/八乙烯基POSS(OvPOSS)复合材料的结构与性能研究;(3)马来酸酐接枝PP(MA-g-PP)反应增容PP/八氨基苯基POSS(OapPOSS)复合材料的结构与性能研究。
(1)Epoxy-POSS扩链PBT的结构与性能研究
通过反应挤出的方法制备了epoxy-POSS扩链的PBT。epoxy-POSS扩链后PBT的特性粘数增加,羧基含量降低,熔体流动指数(MFI)降低。当epoxy-POSS含量从0 %增加到2 %时,特性粘数从1.1 dL/g增加到1.7 dL/g,羧基含量从21.6 eq/106g降低到7.0 eq/106g,MFI从30 g/10min降低到7 g/10min。并且机械性能改善,加工热稳定性提高,吸水率降低,有利于PBT的储存、加工和应用。
(2)反应共混制备PP/ OvPOSS复合材料的结构与性能研究
在过氧化二异丙苯(DCP)作用下通过反应共混的方法制备了PP/OvPOSS复合材料,并研究其结构与性能。随着DCP或OvPOSS含量增加,OvPOSS接枝率增加。采用X-射线衍射(XRD)、示差扫描量热法(DSC)、旋转流变等方法研究了不同的加工方法(物理共混和反应共混)制备的PP/OvPOSS复合材料的结构与性能。物理共混时OvPOSS在含量低于2 %时完全分散在PP基体中,含量超过2 %时OvPOSS开始聚集、结晶。以分子状态分散的OvPOSS分子起到PPβ晶成核剂的作用,促进PPβ晶的形成。反应共混后OvPOSS与PP相容性提高,分散更均匀,PP的β晶型消失。反应共混PP/OvPOSS复合材料机械性能比物理共混的综合更好,在OvPOSS含量为2 %时机械性能最佳。DCP用量0.1 %,OvPOSS用量2 %时,复合材料的弯曲模量和冲击强度比纯PP分别提高约20 %和50 %。PP/OvPOSS复合材料的热分解温度低于纯PP,但反应共混复合材料和OvPOSS-g-PP的热稳定性高于物理共混复合材料。OvPOSS加入后材料热释放速率和质量损失速率降低,提高材料阻燃性。
利用旋转流变、熔体流动指数等方法研究了PP/OvPOSS复合材料的流变行为。结果表明物理共混PP/OvPOSS复合材料的粘度随OvPOSS含量增加先降低后增加。反应共混复合材料的粘度在低频区粘度随OvPOSS含量增加而显著增加,在OvPOSS含量高于1 %时表现出明显的凝胶行为。反应共混PP/OvPOSS复合材料的Han图、Cole-Cole图和van Gurp-Palmen图也发生明显偏移。这一现象表明OvPOSS接枝到PP链段上之后由于OvPOSS与PP之间强的粒子-基体相互作用,抑制PP链段运动,出现明显的凝胶行为。而在物理共混时粒子-基体相互作用和粒子-粒子相互作用都很弱,OvPOSS含量为10 %时也不出现凝胶现象。
利用DSC研究了PP/OvPOSS复合材料的等温和非等温结晶动力学。物理共混时OvPOSS对PP非等温结晶时的结晶峰温度(Tp)影响不大;反应共混复合材料和OvPOSS-g-PP的Tp显著提高,并且OvPOSS含量对Tp影响不大,表明复合材料中聚集的OvPOSS晶体对PP成核作用并不明显,而少量OvPOSS接枝到PP上就具有显著的成核作用,进一步增加接枝的OvPOSS含量对PP结晶行为影响不大。Avrami方程能够描述PP和不同体系的PP/OvPOSS复合材料的等温结晶动力学。OvPOSS对PP起到异相成核的作用,影响了PP成核机理和成核过程,促进PP结晶,折叠链表面自由能σe降低。反应共混复合材料结晶速度更快,σe更低。用Ozawa方程、Ozawa和Avrami组合方程研究PP/OvPOSS复合材料的非等温结晶动力学,结果发现Ozawa方程不适合这个体系,而利用Ozawa和Avrami组合方程则能很好的描述。并利用Kissinger和Takhor方程计算非等温结晶过程活化能(ΔE),发现物理共混和反应共混PP/OvPOSS复合材料的ΔE值略高于PP。
(3)MA-g-PP反应增容PP/OapPOSS复合材料的结构与性能研究
制备了OapPOSS,以MA-g-PP为增容剂,研究OapPOSS填充PP的结构与性能。MA-g-PP可以与OapPOSS中氨基反应,MA-g-PP加入到PP/OapPOSS复合材料中可提高PP与OapPOSS的相容性,OapPOSS粒子粒径明显降低,材料机械性能改善。对PP/OapPOSS复合材料,Tp随着OapPOSS含量增加而降低。然而对于PP/ MA-g-PP/OapPOSS复合材料,Tp随着OapPOSS含量增加而增加,表明OapPOSS加入抑制PP成核,而加入MA-g-PP后成核作用大于抑制作用,促进了PP结晶。PP/OapPOSS的η*高于纯PP并且随着OapPOSS含量增加而增加,然而PP/ MA-g-PP /OapPOSS的η*在OapPOSS含量为5 %时达到最大值并且低于相同OapPOSS含量时PP/OapPOSS体系。这可能是由于MA-g-PP与OapPOSS反应后包覆在OapPOSS表面,降低了OapPOSS的粒子-粒子相互作用,同时粒子间滑移更容易,导致粘度降低。
本论文的主要创新之处:
目前POSS主要通过化学共聚或物理共混的方法引入聚合物基体中,采用反应加工的方法制备聚合物/POSS复合材料的研究较少,本论文主要采用反应加工的方法将POSS引入聚合物基体中,改善聚合物的性能。与物理共混方法相比,反应共混后材料的机械性能改善,流变性能、热性能等均有所改变。
(1)研究了一种环氧化环己基POSS通过反应挤出来扩链PBT的方法。该方法扩链PBT的熔体粘度显著增加,凝胶含量低,热稳定性好,吸水性低,更利于PBT的储存、加工及应用。
(2)首次采用反应共混的方法制备了OvPOSS接枝PP,研究了物理共混和反应共混这两种不同加工方法对PP/OvPOSS复合材料的结构与性能的影响。反应共混方法制备PP/OvPOSS复合材料中OvPOSS与PP的相容性改善,OvPOSS粒子的对PP结晶的成核作用更显著,并且材料机械性能优于物理共混复合材料。反应共混方法工艺简单、生产周期短、无需复杂的分离提纯和溶剂回收等后处理过程,为制备聚合物/POSS复合材料提供了一种新的方法。
(3)对比研究了反应共混和物理共混法制备PP/OvPOSS复合材料的动态流变行为,进一步探讨了复合材料内部结构-性能之间的相互关系。反应共混复合材料在OvPOSS含量高于1 %时在低频区出现明显的凝胶行为,而物理共混复合材料在OvPOSS含量为10 %时也不出现凝胶行为。通过比较POSS与聚合物之间相互作用解释了这两种不同加工方法时材料流变行为的差异,可以为研究其他聚合物/填料复合材料结构-性能之间的相互关系提供参考。
(4)采用MA-g-PP反应增容了PP/OapPOSS复合材料。MA-g-PP可与OapPOSS中氨基反应,增加了PP与OapPOSS的相容性,改善了复合材料的机械性能。为选择合适的POSS填充聚合物、改善聚合物性能提供了一种新方法。
Organic-inorganic nanocomposites have drawn great attention due to their excel combination of properties of organic polymers and with inorganic systems. Polyhedral oligermeric silsesquioxane (POSS) is a kind of important organic-inorganic hybrid molecular with a formula of (RSiO1.5)n. Nanostructured POSS molecular, with the diameter of 1~3 nm, is thought as“the smallest possible particles of silica”. Due to its special structure and properties, POSS (0-D) can be thought as one of the most promising nanofillers which including clay layered silicates (2-D), single and multi-wall carbon nanotubes (1-D), and has drawn great interest.
Recently, POSS has been widely introduced into polymers by chemical copolymerization or physical blending. In this study, polymer/POSS composites were prepared through reactive processing method and their structure and properties were studied. There are three parts in this study: (1) The study on structure and properties of epoxycyclohexyl POSS (epoxy-POSS) chain-extended poly(butylene terephthalate) (PBT), (2) The study on structure and properties of octavinyl POSS (OvPOSS) grafted polypropylene (PP) by reactive blending, (3) The study on structure and properties of maleic anhydride-grafted PP (MA-g-PP) reactive compatibilized PP/octaaminophenyl polyhedral oligomeric silsesquioxane (OapPOSS) composites.
(1) The study on structure and properties of epoxy-POSS chain-extended PBT
Epoxy-POSS chain-extended PBT was prepared by reactive extrusion. The epoxy-POSS chain-extended PBT has higher intrinsic viscosity, lower carboxyl content and melt flow index (MFI) than PBT. PBT had an intrinsic viscosity of 1.1 dL/g, carboxy1 content of 21.6 eq/106g and MFI of 30 g/10min, but the PBT chain-extended with 2 wt% epoxy-POSS had an intrinsic viscosity of 1.7 dL/g, carboxy1 content less than 7 eq/106g and MFI of 7 g/10min. The chain-extended PBT has also improved mechanical properties and thermal properties, indicating it is favorable for storage, processing and application.
(2) The study on structure and properties of OvPOSS grafted PP by reactive blending
The OvPOSS grafted PP was prepared by reactive blending in the presence of dicumyl peroxide (DCP), and the structure and properties of PP/OvPOSS composites were studied. The graft ratio of OvPOSS increased with the increase of DCP or OvPOSS content. The structure and properties of PP/OvPOSS composites prepared by two different processing methods (physical blending and reactive blending) were studied by X-ray diffraction (XRD), differential scanning calorimetry (DSC) and rheological test, respectively. For the physical blending composites, POSS molecules can completely dissolve in PP matrix at OvPOSS content lower than 2 %, and aggregate to crystal with further increasing OvPOSS content. And the dissolved OvPOSS molecules can act asβ-form crystalline nucleating agents. While for the reactive blending composites, OvPOSS had good compatibility and dispersion in PP matrix. Theβ-form crystal disappeared. The reactive blending composites have better mechanical properties than the physical blending ones, and have the best mechanical properties at 2 % OvPOSS content. The impact strength and flexural modulus of PP filled with 2 % POSS and 0.1 % DCP are about 50 % and 20 % higher than that of pure PP, respectively. PP/OvPOSS composites have lower degradation temperature than PP, and the reactive blending composites have better thermal stability than that of the physical blending ones. The heat release rate and mass loss rate decreased when
OvPOSS was added.
The rheological behavior of physical and reactive blending composites was compared by using oscillatory rheological measurements and melt flow index. It was found that the viscosity of physical blending composites drops at lower OvPOSS content (0.5~1 wt %) and thereafter increases with increasing OvPOSS content. While the viscosity of the reactive blending composites increases with increasing OvPOSS content and the composites display a solid-like rheological behavior at low frequency region when POSS content is higher than 1 wt %. The deviation of reactive blending composites from the scaling log G′-log G″of linear polymer in Han plot, upturning at high viscosity in Cole-Cole plot and from van Gurp-Palmen plot are related to the gelation behavior when OvPOSS was grafted to PP chains..
Isothermal and nonisothermal crystallization behavior was analyzed by DSC test. The crystallize peak temperature (Tp) of physical blending PP/OvPOSS composites is close to that of pure PP and changes little with increasing OvPOSS content. While for the reactive blending composites and OvPOSS-g-PP, Tp is greatly higher than that of PP and changes little with increasing OvPOSS content. It indicates that aggregated OvPOSS crystals have little nucleating effect on PP while grafted OvPOSS has significant nucleating effect and the nucleating effect changes little with increasing the graft ratio of OvPOSS. The Avrami equation was used to study the isothermal crystallization kinetics of PP and PP/OvPOSS composites. The results show that OvPOSS can act as a heterogeneous nucleating agent, especially effective for the reactive blending composites. Addition of OvPOSS accelerates the crystallization of PP, increases the rate of crystallization and decreases the chain folding energy of PP. For the nonisothermal crystallization kinetics of PP/OvPOSS composites, the Ozawa equation is not suitable for these materials while the combination of Avrami and Ozawa equations exhibits great advantages in treating the nonisothermal crystallization kinetics of PP/OvPOSS composites. The activation energies (ΔE) calculated by Kissinger and Takhor methods for the nonisothermal crystallization of phtsical blending and reactive blending PP/OvPOSS composites are slightly higher than PP.
(3) The study on structure and properties of MA-g-PP reactive compatibilized PP/OapPOSS composites.
OapPOSS was prepared and filled to PP and MA-g-PP was selected as compatibilizer. The addition of MA-g-PP could improve the compatibility between PP and OapPOSS, promote a fine dispersion of OapPOSS particles in PP matrix and improve the mechanical properties of PP due to the reaction of amine groups of OapPOSS with maleic anhtydride groups of MA-g-PP. With increasing OapPOSS content, the Tp of PP/OapPOSS composites decreased while that of PP/MA-g-PP/OapPOSS composites increased, indicating OapPOSS could retard the crystallization of PP in PP/OapPOSS composites, while the nucleating effect compensated and overlapped the retardation effects when MA-g-PP was added. For PP/OapPOSS composites,η* increased with increasing OapPOSS content, while theη* of all the PP/MAPP/OapPOSS composites was lower than that of PP /OapPOSS at the same OapPOSS content and reached the maximum at 5 % OapPOSS content. It is probably due to the lower particle-particle interaction and interface slipping when OapPOSS was encapsulated by PP chain when OapPOSS was reacted with MA-g-PP.
The innovations of this dissertation are list as follows:
Recently, POSS has been widely introduced into polymers by chemical copolymerization or physical blending. While there are little reports about PP/POSS composites prepared by reactive processing. In this study, POSS was introduced to polymers to improve the properties of polymers. Compared with PP/POSS composites prepared by physical blending, the reactive blending composites had better mechanical properties. Their rheological behavior and thermal properties were different.
(1) A method of epoxy-POSS chain-extended PBT was investigated. PBT chain extended by this method has higher viscosity, lower gel content, better thermal stability and lower water absorption, which is advantage for storage, processing and application of PBT.
(2) OvPOSS was firstly grafted to PP by reactive blending method. The structure and properties of the composites prepared by the two processing methods (reactive blending and physical blending) was studied. For the reactive blending composites, OvPOSS has goog compatibility and dispersion in PP matrix, significant nucleating effect on the crystallization of PP and improved the mechanical properties of PP. Reactive blending has advantages of simplified technique, short product cycle and no complicated aftertreat including separation, purification and solvent recycle. The properties of reactive blending composites also have better properties than physical blending composites. It provides a new method to prepare polymer/POSS composites.
(3) The rheological behavior of reactive blending and physical blending composites was compared, and the structure-property relationship of composites was discussed. The reactive blending composites display solid-like rheological behavior at low frequency region when OvPOSS content is higher than 1 %, while the physical blending composites do not display solid-like rheological behavior even at 10 % OvPOSS content. The difference of rheological behavior of two different methods was explained by the interaction of POSS and polymer, which can provide the reference for investigating the structure-property relationship of other polymer/fillers composites.
(4) MA-g-PP was selected as reacitve compatibilizer to PP/OapPOSS composites. The addition of MA-g-PP could improve the compatibility between PP and OapPOSS, and improve the mechanical properties of PP due to the reaction of amine groups of OapPOSS with MA-g-PP. It provides a method for choosing suitable formation of POSS filled polymer and studying the structure-properties relationship.
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