PP/mica复合材料界面增强作用及机理研究
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摘要
通过反应挤出接枝物，并以这种接枝物作为界面改性剂增容PP/mica复合体系，制备出了综合性能优良PP/mica复合材料。
首先通过单螺杆反应挤出接枝物，研究了单体用量和引发剂用量对接枝物接枝率的影响；为了抑制接枝物制备过程中的降解，在PP-g-AA和PP-g-MAH接枝体系中引入了St单体，进行多单体熔融接枝PP，比较了PSA和PP-g-AA流动性的差别；用化学滴定法和红外测试(FTIR)表征了接枝物的接枝率；对PP和PP-g-AA进行了非等温结晶动力学分析，分析了PP-g-AA的结构和带有的极性基团对PP结晶行为的影响。
在PP/mica复合材料的制备过程中，研究了不同云母品种、接枝物品种以及不同云母含量、接枝物含量和接枝物的接枝率对复合体系力学性能的影响；通过两种接枝物共用作为复合体系界面改性剂，结果发现体系综合性能有较大幅度提高；研究了接枝聚丙烯和硅烷偶联剂对PP/mica体系改性效果，分析了偶联剂用量，接枝物用量对体系力学性能的影响，并探讨了硅烷偶联剂和接枝物对体系改性的协同作用；研究了PP/PP-g-AA/mica复合材料的结晶性能，研究发现PP-g-AA，mica都对PP具有成核作用。通过SEM分析得到了更多的经接枝物处理后PP/mica体系的界面信息。
通过上述的研究，我们可以获得接枝物作为PP/mica复合材料界面改性剂时复合材料界面的一些信息。我们用改性后的接枝物来作为界面改性剂，制备PP/mica复合材料，通过分析，我们可以更多地了解接枝物作为界面改性剂的作用机理。
为了提高复合体系的冲击性能，研究了PP/EPDM/mica体系，比较了云母和EPDM对聚丙烯性能影响的不同，确定了云母和EPDM的最佳用量。同时比较了PP-g-MAH和(PP/EPDM)-g-MAH改性效果的差别。
最后研究了云母填充β型聚丙烯体系，比较了云母填充α、β型聚丙烯的力学性能，结果发现体系中加入PP-g-MAH界面改性剂时，β型体系力学性能优于α型。同时通过WAXD(广角X衍射)分析了云母和PP-g-MAH加入对β型聚丙烯晶型、晶体结构参数如微晶尺寸等的影响。发现云母的加入使PP微晶尺寸有所增加，聚丙烯的晶胞参数的变小，而PP-g-MAH作用基本相反，PP-g-MAH不利于β型聚丙烯的形成，但利于云母的取向，从而利于力学强度的提高。
In this thesis, polypropylene(PP)/mica composites were prepared by molten process, with graft copolymers by reactive extrusion as interfacial modifier.
For the preparation and performance of the graft copolymer, the effect of the dosage of monomer AA and catalyzer DCP on the graft ratio of PP-g-AA was discussed, and multi-monomer melt grafting on PP was studied, it was found that the addition of styrene monomer reduced the degradation of PP. The chemical titration and the FTIR were used on the evidence of the graft ratio. Nonisothermal crystallization kinetics of PP and PP-g-AA was analyzed, the result indicated that PP-g-AA could hasten the nucleation of polypropylene and accelerate crystallization rate of polypropylene, and lead to lower degree of crystallization than that of PP..
The further researches on the preparation of PP/mica composite were done. Firstly, the effect of the different kind of mica and graft copolymer on the performance of PP/mica composites was analyzed, the effect of the content of mica and graft copolymer and the graft ratio of graft copolymer was investigated, and PP/mica composite with good mechanical properties could be prepared by the addition of PP-g-AA and PP-g-MAH together into the composite systems. The crystallization behavior and structures of PP/PP-g-AA/Mica composites were studied by differential scanning calorimetry (DSC) and wide angle X ray diffraction (WAXD), and the results indicated that mica and PP-g-AA have nucleation on PP, and the content of mica, the content and graft ratio of PP-g-AA have effect on the crystallization of polypropylene. Secondly, the effect of the grafted polypropylene and silane coupling agent on the PP/mica system was studied, it was found that there existed the coordinate action between the grafted polypropylene and silane coupling agent. Thirdly, by the analyse of SEM testing, we knew more about the interface of PP/mica composites which had treated by graft. Finally, the systems of PP/EPDM/mica were studied, in order to improving the impact properties of PP/mica composites. The effect of mica and EPDM on the properties of polypropylenes was investigated, and the most appropriate content of EPDM and mica was ascertained, comparing the effect of (PP/EPDM)-g-MAH on systems with that of PP-g-MAH.
From the above-mentioned researches, we got hold of some information about the interface behavior of PP/mica composites when the graft copolymer is used as the reagent that can improve the interfacial performance of composites. Based on that, we did some tests about the change of graft copolymer, and the other PP/mica composites were made and studied, so more information could be concluded about the mechanism and action of graft copolymer that was used to improve the interface of PP/mica composites.
Finally, the system of mica filled β crystalline form PP was investigated. If PP-g-MAH was used, the mechanical properties of mica filled β crystalline form PP were increased, comparing with those of mica filled a crystalline form PP. By the analysis of wide angle X-ray diffraction, the effect of mica and PP-g-MAH on the βcrystalline form, the parameter of crystalloid configuration, and microcrystal size was obtained. The microcrystal size of polypropylene was increased, the crystal cell parameter of which was diminished, when mica was appended. On the very reverse, PP-g-MAH was appended. PP-g-MAH was not good for the form of β crystalline form polypropylene, but was good for the orientation of mica and the improvement of the mechanical properties.
首先通过单螺杆反应挤出接枝物，研究了单体用量和引发剂用量对接枝物接枝率的影响；为了抑制接枝物制备过程中的降解，在PP-g-AA和PP-g-MAH接枝体系中引入了St单体，进行多单体熔融接枝PP，比较了PSA和PP-g-AA流动性的差别；用化学滴定法和红外测试(FTIR)表征了接枝物的接枝率；对PP和PP-g-AA进行了非等温结晶动力学分析，分析了PP-g-AA的结构和带有的极性基团对PP结晶行为的影响。
在PP/mica复合材料的制备过程中，研究了不同云母品种、接枝物品种以及不同云母含量、接枝物含量和接枝物的接枝率对复合体系力学性能的影响；通过两种接枝物共用作为复合体系界面改性剂，结果发现体系综合性能有较大幅度提高；研究了接枝聚丙烯和硅烷偶联剂对PP/mica体系改性效果，分析了偶联剂用量，接枝物用量对体系力学性能的影响，并探讨了硅烷偶联剂和接枝物对体系改性的协同作用；研究了PP/PP-g-AA/mica复合材料的结晶性能，研究发现PP-g-AA，mica都对PP具有成核作用。通过SEM分析得到了更多的经接枝物处理后PP/mica体系的界面信息。
通过上述的研究，我们可以获得接枝物作为PP/mica复合材料界面改性剂时复合材料界面的一些信息。我们用改性后的接枝物来作为界面改性剂，制备PP/mica复合材料，通过分析，我们可以更多地了解接枝物作为界面改性剂的作用机理。
为了提高复合体系的冲击性能，研究了PP/EPDM/mica体系，比较了云母和EPDM对聚丙烯性能影响的不同，确定了云母和EPDM的最佳用量。同时比较了PP-g-MAH和(PP/EPDM)-g-MAH改性效果的差别。
最后研究了云母填充β型聚丙烯体系，比较了云母填充α、β型聚丙烯的力学性能，结果发现体系中加入PP-g-MAH界面改性剂时，β型体系力学性能优于α型。同时通过WAXD(广角X衍射)分析了云母和PP-g-MAH加入对β型聚丙烯晶型、晶体结构参数如微晶尺寸等的影响。发现云母的加入使PP微晶尺寸有所增加，聚丙烯的晶胞参数的变小，而PP-g-MAH作用基本相反，PP-g-MAH不利于β型聚丙烯的形成，但利于云母的取向，从而利于力学强度的提高。
In this thesis, polypropylene(PP)/mica composites were prepared by molten process, with graft copolymers by reactive extrusion as interfacial modifier.
For the preparation and performance of the graft copolymer, the effect of the dosage of monomer AA and catalyzer DCP on the graft ratio of PP-g-AA was discussed, and multi-monomer melt grafting on PP was studied, it was found that the addition of styrene monomer reduced the degradation of PP. The chemical titration and the FTIR were used on the evidence of the graft ratio. Nonisothermal crystallization kinetics of PP and PP-g-AA was analyzed, the result indicated that PP-g-AA could hasten the nucleation of polypropylene and accelerate crystallization rate of polypropylene, and lead to lower degree of crystallization than that of PP..
The further researches on the preparation of PP/mica composite were done. Firstly, the effect of the different kind of mica and graft copolymer on the performance of PP/mica composites was analyzed, the effect of the content of mica and graft copolymer and the graft ratio of graft copolymer was investigated, and PP/mica composite with good mechanical properties could be prepared by the addition of PP-g-AA and PP-g-MAH together into the composite systems. The crystallization behavior and structures of PP/PP-g-AA/Mica composites were studied by differential scanning calorimetry (DSC) and wide angle X ray diffraction (WAXD), and the results indicated that mica and PP-g-AA have nucleation on PP, and the content of mica, the content and graft ratio of PP-g-AA have effect on the crystallization of polypropylene. Secondly, the effect of the grafted polypropylene and silane coupling agent on the PP/mica system was studied, it was found that there existed the coordinate action between the grafted polypropylene and silane coupling agent. Thirdly, by the analyse of SEM testing, we knew more about the interface of PP/mica composites which had treated by graft. Finally, the systems of PP/EPDM/mica were studied, in order to improving the impact properties of PP/mica composites. The effect of mica and EPDM on the properties of polypropylenes was investigated, and the most appropriate content of EPDM and mica was ascertained, comparing the effect of (PP/EPDM)-g-MAH on systems with that of PP-g-MAH.
From the above-mentioned researches, we got hold of some information about the interface behavior of PP/mica composites when the graft copolymer is used as the reagent that can improve the interfacial performance of composites. Based on that, we did some tests about the change of graft copolymer, and the other PP/mica composites were made and studied, so more information could be concluded about the mechanism and action of graft copolymer that was used to improve the interface of PP/mica composites.
Finally, the system of mica filled β crystalline form PP was investigated. If PP-g-MAH was used, the mechanical properties of mica filled β crystalline form PP were increased, comparing with those of mica filled a crystalline form PP. By the analysis of wide angle X-ray diffraction, the effect of mica and PP-g-MAH on the βcrystalline form, the parameter of crystalloid configuration, and microcrystal size was obtained. The microcrystal size of polypropylene was increased, the crystal cell parameter of which was diminished, when mica was appended. On the very reverse, PP-g-MAH was appended. PP-g-MAH was not good for the form of β crystalline form polypropylene, but was good for the orientation of mica and the improvement of the mechanical properties.
引文
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