PP和PBS基无机纳米复合材料的制备及性能研究
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摘要
聚丙烯材料具有原料来源丰富、价格低廉、性能优良、电绝缘性和化学稳定性好，且易于加工成型的优点，已经被广泛应用于工业、农业、医疗卫生、包装和日常生活等各个领域中，因而也是世界高分子材料中用量最大、增长速度最快的一类产品。聚丁二酸丁二醇酯作为一类典型的生物降解脂肪族聚酯，由于其综合性能优异，性价比合理而备受青睐，成为脂肪族聚酯中发展最快的品种之一。聚丙烯虽然被公认为是最有可能达到工业化和商品化的可生物降解高分子材料，但是其本身在结晶与力学性能方面存在一定局限性，可通过加入其它聚合物、填料及相容剂，达到改善材料性能的目的。聚合物共混合材料研究和应用得到了学术界与工业界的广泛关注和迅速发展。
（1）以聚丙烯接枝马来酸酐（PP-g-MAH）作为界面增容剂，用表面经过硅烷偶联剂处理的硫酸钙晶须，对聚丙烯增强增韧，研究PP-g-MAH增容剂和稀土β成核剂对聚丙烯复合材料结晶、熔融行为和力学性能影响。结果表明：硫酸钙晶须具有一定的诱导β-晶型的异相成核作用，使聚丙烯结晶温度提高和结晶速率增加。PP-g-MAH提高了结晶温度和晶须成核能力，降低了β-晶型含量，不利于β-晶型生成，并改善了树脂与晶须的界面性能，提高了拉伸强度和冲击性能。稀土β成核剂具有很强的诱导形成β-晶型异相成核效应，有效提高了复合材料的冲击性能。动力学分析表明聚丙烯非等温结晶动力学可以用莫志深描述，结晶度相同的情况下，复合材料需要的冷却速率显著小于纯基体。复合材料的组成与降温冷却速率是熔融行为与结晶形态的决定因素。
（2）采用镁盐晶须对聚丙烯硅烷增强增韧，镁盐晶须以硅烷偶联剂表面处理，聚丙烯接枝马来酸酐（PP-g-MAH）作为界面增容剂，研究镁盐晶须和增容剂PP-g-MAH对聚丙烯复合材料的结晶行为、熔融行为和力学性能的影响。结果表明：镁盐晶须具有明显的诱导β晶型成核效应，对PP有一定的增强增韧作用，增容剂PP-g-MAH改善了PP与晶须的界面性能，提高了拉伸强度和冲击强度；PP-g-MAH进一步促进了晶须成核作用，但明显抑制了β晶型的生成。等温结晶动力学分析表明遵循Avrami模型，基于Lauritzen-Hoffman成核理论分析，随着镁盐晶须和增容剂的加入，表面自由能σe呈明显下降趋势，表明镁盐晶须填料的加入降低了产生新界面需要的功，加快了结晶速率。非等温结晶的成核活性分析、结晶活化能分析和有效活化能垒分析都得到类似的结果，镁盐晶须和增容剂的加入降低了活化能，增加了成核活性。
（3）采用Mg-Al水滑石（HT）为聚丁二酸丁二醇酯的改性剂。首先制备聚丁二酸丁二醇酯（PBS），再分别制备不同HT掺量的纳米复合材料混合物，之后对其各项性能指标进行了测试研究。把不同HT纳米粒子含量的纳米复合材料与纯PBS的各项性能指标进行对比，同时对相关机理进行探讨，通过对实验样品的TEM和SEM分析及测试表明HT纳米粒子能够在PBS基体中良好分散，随着HT掺量增加结晶速率逐渐增长，HT纳米粒子对PBS结晶速率增加效果显著。说明HT对PBS基体结晶有异相成核作用，同时促进PBS结晶，但又对PBS的结晶机制和结晶结构没有影响。用Jeziorny、Ozawa和莫志深法分析非等温结晶过程，发现莫志深提出的将Avrami和Ozawa方程联立的方法很好的描述PBS及其纳米复合体系的非等温结晶动力学。加入HT使得PBS成核密度增加，球晶尺寸细化；由于Mg和Al离子对PBS的酯键热分解有催化作用使得PBS的热稳定性有所下降，复合材料的力学性能均有所提高。
（4）通过溶液复合制备了聚丁二酸丁二醇酯（PBS）/氨基笼型低聚倍半硅氧烷（POSS）纳米复合材料，并研究了POSS的加入对其微观结构、晶体结构、结晶行为、球晶形态和球晶生长速率、力学性能和热稳定性等方面的影响。扫描电镜观察POSS能够均匀纳米级地分散在PBS基体中，呈现良好的界面作用。X-射线衍射仪测试表明加入POSS不影响基体PBS的晶型，且POSS在基体中以晶体形态存在。差示扫描量热测试显示加入POSS反而降低了非等温结晶温度，延长了等温结晶时间，表明POSS的成核能力非常有限，且POSS的加入阻碍了PBS链段的运动，偏光显微镜观察POSS降低了PBS的球晶生长速率。力学性能测试表明POSS提高了PBS的杨氏模量和储能模量，增强效果不显著，降低了PBS断裂伸长率，提高了PBS的玻璃化转变温度。POSS分解温度低于PBS，但不影响基体PBS的热稳定性。综上实验结果分析：POSS分子上的氨基与PBS链段上的羰基形成较强的分子间氢键作用，以及POSS的笼型结构起物理交联点作用在PBS/POSS纳米复合材料中形成三维网络结构，是POSS影响PBS结晶行为和力学性能的主要原因。
Isotactic polypropylene (iPP), as one of the commodity plastics, has been used in manyareas such as packaging, households, and automotives, for its low price, excellentperformance, good electrical insulation and chemical stability, and ease of processing. IPP isa kind of typical biological aliphatic polyester for its degradability, and has a high growthrate. Poly(butylene succinate)(PBS) is one of the most promising materials for theproduction of high-performance, environment-friendly and biodegradable. It has particularlyattracted more commercial interests because of its significant properties, including meltprocessability, thermal and chemical resistance, and biodegradability. However, its softnessand low gas-barrier properties have restricted further applications of PBS. Therefore, addingother polymers, fillers, and the compatibilizing agent can improve the material properties.Up to now, the research and application of nanocomposites have attracted enormous interestsin academia and industry.
(1) Polypropylene-graft-maleic anhydride (PP-g-MAH) is used as interfacecompatibilizing agent, and the surface of calcium sulphate whisker is treated with silanecoupling agent to reinforce and toughen polypropylene. The effects of compatibilizerPP-g-MAH and rare earth β-phase nucleating agent have been studied systematically toknow the influence of crystallization, melting behavior and mechanical properties onpolypropylene/calcium sulfate whisker composites. It is found that the calcium sulfatewhisker has a heterogeneous nucleation effect on the polymer matrix and induced theformation of β-crystal, thus increases the peak crystallization temperature and the overallrate of crystallization of PP. PP-g-MAH content improves the interfacial compatibility andtensile strength, which also enhance the nucleation activity of the whisker in the PP matrix,and suppress the formation of β-iPP. The results shows that rare earth β-phase nucleatingagent resulted in dominant β-PP and improved the strength effectively. The analysis of the crystallization process shows that the Mo model can describe the kinetics data ofnonisothermal crystallization successfully. To achieve the identical degree of crystallinity,the composites need a lower cooling rate than pure PP. The results shows that the crystallinestructure and melting behavior of the composites depend on their component and coolingrate. Lower cooling rate is favorable for the formation of β-crystals.
(2) Crystallization behavior of isotactic polypropylene (iPP)/magnesium salt whisker(MSW) composites modified by compatibilizer PP-g-MAH is studied under both isothermaland nonisothermal conditions. It is observed that the addition of MSW affected thecrystallization rate and melting behavior of iPP/MSW composites remarkably. The additionof MSW and/or PP-g-MAH has strong nucleation activity and accelerates the nucleation rateand the overall crystallization rate. Analysis of the isothermal crystallization shows that theAvrami model successfully described the crystallization process.
(3) Biodegradable poly(butylene succinate)(PBS) and layered double hydroxide (HT)nanocomposites are prepared. By means of TEM and SEM,conclusions are drawed: HTnanoparticles dispersed well in PBS, PBS crystallization rate has been improved with theaddition of the HT nanoparticles greatly. HT nanoparticles in the PBS/HT nanocompositeshave heterogeneous nucleation effect on crystallization of PBS matrix, through experimentalresults of DSC, and the results show that the crystallization rate increases with the growth ofthe HT content, and the HT nanoparticles act as the heterogeneous nucleation agents topromote the crystallization process. Adding HT to PBS material can not greatly change themechanism of nucleation and crystal growth morphology. Furthermore, The non-isothermalcrystallization processes is analyzed by methods of Jeziorny, Ozawa and Mo, and found thatthe method proposed by Mo could successfully analyze the non-isothermal crystallizationkinetics of PBS and its nanocomposites. The experimental results of POM show that thespherulitic morphologies did not change, but the spherulite size of PBS and itsnanocomposites decreases with the addition of HT nanoparticles.
(4) Poly(butylene succinate)(PBS) and aminopropylisobutyl polyhedral oligomericsilsesquioxanes (POSS) nanocomposites are prepared by solution-casting method. The effects of POSS on the microstructure, crystal structure, crystallization behavior, spheruliticmorphology and spherulite grow rate, mechanical properties, and thermal stability ofPBS/POSS nanocomposites are investigated with various techniques. Scanning electronmicroscope measurements reveals that POSS particles are well-dispersed uniformly on thenanoscale in the PBS matrix and has a good interfacial interaction with PBS chains.Wide-angle X-ray diffraction patterns shows that the POSS molecules are able to crystallizein PBS matrix, but do not affect the crystalline structure of PBS matrix. Differential scanningcalorimetry results indicate that the incorporation of POSS particles into PBS matrix,unexpectedly, decrease the crystallization temperature during nonisothermal meltcrystallization and prolong the crystallization time during isothermal crystallization. Thenucleation effect of such POSS on the crystallization of PBS is extraordinary limited;furthermore, it hinders the motion of PBS chains and decelerated the spherulite growth rate,as confirmed by polarized optical microscopy. Mechanical properties are evaluated byInstron and dynamic mechanical analysis. The Young’s modules and storage modules of thenanocomposites are enhanced relative to PBS by the addition of POSS, however, the tensilestrength is not much improved and the elongation at break is reduced in the nanocomposites.Glass transition temperature (Tg) of the PBS/POSS nanocomposites increased slightly withincreasing POSS content, which indicated that the molecular mobility of amorphous PBSchains is constrained in the nanocomposites. The above results indicate that the retardedcrystallization of PBS and the effect of mechanical properties of the nanocomposites in thepresence of POSS are ascribed the stronger hydrogen-bonding interactions between thePOSS molecules and the PBS matrix as well as the network formation based on the POSSphysical crosslinking points in the PBS/POSS nanocomposites.
（1）以聚丙烯接枝马来酸酐（PP-g-MAH）作为界面增容剂，用表面经过硅烷偶联剂处理的硫酸钙晶须，对聚丙烯增强增韧，研究PP-g-MAH增容剂和稀土β成核剂对聚丙烯复合材料结晶、熔融行为和力学性能影响。结果表明：硫酸钙晶须具有一定的诱导β-晶型的异相成核作用，使聚丙烯结晶温度提高和结晶速率增加。PP-g-MAH提高了结晶温度和晶须成核能力，降低了β-晶型含量，不利于β-晶型生成，并改善了树脂与晶须的界面性能，提高了拉伸强度和冲击性能。稀土β成核剂具有很强的诱导形成β-晶型异相成核效应，有效提高了复合材料的冲击性能。动力学分析表明聚丙烯非等温结晶动力学可以用莫志深描述，结晶度相同的情况下，复合材料需要的冷却速率显著小于纯基体。复合材料的组成与降温冷却速率是熔融行为与结晶形态的决定因素。
（2）采用镁盐晶须对聚丙烯硅烷增强增韧，镁盐晶须以硅烷偶联剂表面处理，聚丙烯接枝马来酸酐（PP-g-MAH）作为界面增容剂，研究镁盐晶须和增容剂PP-g-MAH对聚丙烯复合材料的结晶行为、熔融行为和力学性能的影响。结果表明：镁盐晶须具有明显的诱导β晶型成核效应，对PP有一定的增强增韧作用，增容剂PP-g-MAH改善了PP与晶须的界面性能，提高了拉伸强度和冲击强度；PP-g-MAH进一步促进了晶须成核作用，但明显抑制了β晶型的生成。等温结晶动力学分析表明遵循Avrami模型，基于Lauritzen-Hoffman成核理论分析，随着镁盐晶须和增容剂的加入，表面自由能σe呈明显下降趋势，表明镁盐晶须填料的加入降低了产生新界面需要的功，加快了结晶速率。非等温结晶的成核活性分析、结晶活化能分析和有效活化能垒分析都得到类似的结果，镁盐晶须和增容剂的加入降低了活化能，增加了成核活性。
（3）采用Mg-Al水滑石（HT）为聚丁二酸丁二醇酯的改性剂。首先制备聚丁二酸丁二醇酯（PBS），再分别制备不同HT掺量的纳米复合材料混合物，之后对其各项性能指标进行了测试研究。把不同HT纳米粒子含量的纳米复合材料与纯PBS的各项性能指标进行对比，同时对相关机理进行探讨，通过对实验样品的TEM和SEM分析及测试表明HT纳米粒子能够在PBS基体中良好分散，随着HT掺量增加结晶速率逐渐增长，HT纳米粒子对PBS结晶速率增加效果显著。说明HT对PBS基体结晶有异相成核作用，同时促进PBS结晶，但又对PBS的结晶机制和结晶结构没有影响。用Jeziorny、Ozawa和莫志深法分析非等温结晶过程，发现莫志深提出的将Avrami和Ozawa方程联立的方法很好的描述PBS及其纳米复合体系的非等温结晶动力学。加入HT使得PBS成核密度增加，球晶尺寸细化；由于Mg和Al离子对PBS的酯键热分解有催化作用使得PBS的热稳定性有所下降，复合材料的力学性能均有所提高。
（4）通过溶液复合制备了聚丁二酸丁二醇酯（PBS）/氨基笼型低聚倍半硅氧烷（POSS）纳米复合材料，并研究了POSS的加入对其微观结构、晶体结构、结晶行为、球晶形态和球晶生长速率、力学性能和热稳定性等方面的影响。扫描电镜观察POSS能够均匀纳米级地分散在PBS基体中，呈现良好的界面作用。X-射线衍射仪测试表明加入POSS不影响基体PBS的晶型，且POSS在基体中以晶体形态存在。差示扫描量热测试显示加入POSS反而降低了非等温结晶温度，延长了等温结晶时间，表明POSS的成核能力非常有限，且POSS的加入阻碍了PBS链段的运动，偏光显微镜观察POSS降低了PBS的球晶生长速率。力学性能测试表明POSS提高了PBS的杨氏模量和储能模量，增强效果不显著，降低了PBS断裂伸长率，提高了PBS的玻璃化转变温度。POSS分解温度低于PBS，但不影响基体PBS的热稳定性。综上实验结果分析：POSS分子上的氨基与PBS链段上的羰基形成较强的分子间氢键作用，以及POSS的笼型结构起物理交联点作用在PBS/POSS纳米复合材料中形成三维网络结构，是POSS影响PBS结晶行为和力学性能的主要原因。
Isotactic polypropylene (iPP), as one of the commodity plastics, has been used in manyareas such as packaging, households, and automotives, for its low price, excellentperformance, good electrical insulation and chemical stability, and ease of processing. IPP isa kind of typical biological aliphatic polyester for its degradability, and has a high growthrate. Poly(butylene succinate)(PBS) is one of the most promising materials for theproduction of high-performance, environment-friendly and biodegradable. It has particularlyattracted more commercial interests because of its significant properties, including meltprocessability, thermal and chemical resistance, and biodegradability. However, its softnessand low gas-barrier properties have restricted further applications of PBS. Therefore, addingother polymers, fillers, and the compatibilizing agent can improve the material properties.Up to now, the research and application of nanocomposites have attracted enormous interestsin academia and industry.
(1) Polypropylene-graft-maleic anhydride (PP-g-MAH) is used as interfacecompatibilizing agent, and the surface of calcium sulphate whisker is treated with silanecoupling agent to reinforce and toughen polypropylene. The effects of compatibilizerPP-g-MAH and rare earth β-phase nucleating agent have been studied systematically toknow the influence of crystallization, melting behavior and mechanical properties onpolypropylene/calcium sulfate whisker composites. It is found that the calcium sulfatewhisker has a heterogeneous nucleation effect on the polymer matrix and induced theformation of β-crystal, thus increases the peak crystallization temperature and the overallrate of crystallization of PP. PP-g-MAH content improves the interfacial compatibility andtensile strength, which also enhance the nucleation activity of the whisker in the PP matrix,and suppress the formation of β-iPP. The results shows that rare earth β-phase nucleatingagent resulted in dominant β-PP and improved the strength effectively. The analysis of the crystallization process shows that the Mo model can describe the kinetics data ofnonisothermal crystallization successfully. To achieve the identical degree of crystallinity,the composites need a lower cooling rate than pure PP. The results shows that the crystallinestructure and melting behavior of the composites depend on their component and coolingrate. Lower cooling rate is favorable for the formation of β-crystals.
(2) Crystallization behavior of isotactic polypropylene (iPP)/magnesium salt whisker(MSW) composites modified by compatibilizer PP-g-MAH is studied under both isothermaland nonisothermal conditions. It is observed that the addition of MSW affected thecrystallization rate and melting behavior of iPP/MSW composites remarkably. The additionof MSW and/or PP-g-MAH has strong nucleation activity and accelerates the nucleation rateand the overall crystallization rate. Analysis of the isothermal crystallization shows that theAvrami model successfully described the crystallization process.
(3) Biodegradable poly(butylene succinate)(PBS) and layered double hydroxide (HT)nanocomposites are prepared. By means of TEM and SEM,conclusions are drawed: HTnanoparticles dispersed well in PBS, PBS crystallization rate has been improved with theaddition of the HT nanoparticles greatly. HT nanoparticles in the PBS/HT nanocompositeshave heterogeneous nucleation effect on crystallization of PBS matrix, through experimentalresults of DSC, and the results show that the crystallization rate increases with the growth ofthe HT content, and the HT nanoparticles act as the heterogeneous nucleation agents topromote the crystallization process. Adding HT to PBS material can not greatly change themechanism of nucleation and crystal growth morphology. Furthermore, The non-isothermalcrystallization processes is analyzed by methods of Jeziorny, Ozawa and Mo, and found thatthe method proposed by Mo could successfully analyze the non-isothermal crystallizationkinetics of PBS and its nanocomposites. The experimental results of POM show that thespherulitic morphologies did not change, but the spherulite size of PBS and itsnanocomposites decreases with the addition of HT nanoparticles.
(4) Poly(butylene succinate)(PBS) and aminopropylisobutyl polyhedral oligomericsilsesquioxanes (POSS) nanocomposites are prepared by solution-casting method. The effects of POSS on the microstructure, crystal structure, crystallization behavior, spheruliticmorphology and spherulite grow rate, mechanical properties, and thermal stability ofPBS/POSS nanocomposites are investigated with various techniques. Scanning electronmicroscope measurements reveals that POSS particles are well-dispersed uniformly on thenanoscale in the PBS matrix and has a good interfacial interaction with PBS chains.Wide-angle X-ray diffraction patterns shows that the POSS molecules are able to crystallizein PBS matrix, but do not affect the crystalline structure of PBS matrix. Differential scanningcalorimetry results indicate that the incorporation of POSS particles into PBS matrix,unexpectedly, decrease the crystallization temperature during nonisothermal meltcrystallization and prolong the crystallization time during isothermal crystallization. Thenucleation effect of such POSS on the crystallization of PBS is extraordinary limited;furthermore, it hinders the motion of PBS chains and decelerated the spherulite growth rate,as confirmed by polarized optical microscopy. Mechanical properties are evaluated byInstron and dynamic mechanical analysis. The Young’s modules and storage modules of thenanocomposites are enhanced relative to PBS by the addition of POSS, however, the tensilestrength is not much improved and the elongation at break is reduced in the nanocomposites.Glass transition temperature (Tg) of the PBS/POSS nanocomposites increased slightly withincreasing POSS content, which indicated that the molecular mobility of amorphous PBSchains is constrained in the nanocomposites. The above results indicate that the retardedcrystallization of PBS and the effect of mechanical properties of the nanocomposites in thepresence of POSS are ascribed the stronger hydrogen-bonding interactions between thePOSS molecules and the PBS matrix as well as the network formation based on the POSSphysical crosslinking points in the PBS/POSS nanocomposites.
引文
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