原位构建纳米分散相制备高性能弹性体复合材料的研究
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摘要
如何获得填料均一分散的聚合物纳米复合材料一直是学术界和工业界的重要难题。近些年来,原位分散技术逐渐发展成为制备高分散聚合物纳米复合材料的重要手段,继而成为了聚合物纳米复合材料领域的研究热点之一。本论文基于原位法制备聚合物纳米复合材料这一技术手段,对甲基丙烯酸锌(ZDMA)在橡胶基体的过氧化物硫化过程中的原位聚合反应行为进行了详细的跟踪研究,并对所制备的ZDMA增强橡胶纳米复合材料的结构和性能进行了系统的讨论。此外,本论文首次提出并探索研究了一种新型原位反应,即利用对乙烯基苯磺酸钠(NaSS)的原位聚合／接枝反应制备质子交换膜材料的工艺方法。
本论文第三章对ZDMA在HNBR基体过氧化物硫化过程中的原位聚合反应行为进行了详细的跟踪研究。研究结果表明,ZDMA的初始分散粒径对其原位聚合行为有着重要影响,硫化胶中存在的大量微米分散相为发生原位反应的ZDMA;另外,本研究首次发现并证明了ZDMA在原位反应过程中除发生“溶解-扩散-原位聚合”而生成纳米离子簇相分离结构之外,还存在有另一种新的反应行为,即扩散受限的ZDMA颗粒能够在过氧化物自由基的引发下发生固相本体聚合反应而直接从结晶态转变为无定形态,在硫化胶基体中产生大量不同于离子簇结构的特殊微米(甚至纳米)分散相；上述大量微米分散相的存在将导致HNRB/ZDMA硫化胶的离子键交联密度显著减小,力学强度下降。
论文第四章研究了硫化温度对HNBR/ZDMA复合材料结构与性能的影响。研究结果表明,随硫化温度升高,ZDMA的原位聚合接枝率降低,ZDMA固相本体聚合所产生的特殊分散相的尺寸和数量逐渐增加,离子键交联密度减小,最终导致HNBR/ZDMA复合材料的物理机械性能均有不同程度的降低。此外,本工作还从“溶解-扩散”的角度提出了硫化温度对ZDMA原位聚合反应可能存在的影响机理。
在论文第五章中,我们利用氧化锌与甲基丙烯酸在胶料混炼过程中原位中和反应的方法制备了HNBR/N115/ZDMA纳米复合材料,重点研究了ZDMA的原位生成量以及过氧化物DCP的用量对上述纳米复合材料基本力学性能、磨耗性能、动态切割性能和动态压缩疲劳性能的影响,并对其相关机理进行了讨论。研究结果发现,复合材料的阿克隆磨耗性能随ZDMA原位生成量的增加逐渐提高,而DIN磨耗性能反而逐渐降低,由磨耗面形貌所反映出的磨耗机理与复合材料磨耗性能的变化有着较好的相关性；随ZDMA原位生成量的增加,复合材料的动态切割性能先逐渐提高后保持基本稳定,动态压缩疲劳温升逐渐增大,动态压缩永久变形逐渐减小；当ZDMA用量为30phr时,复合材料的动态切割性能、动态压缩疲劳温升和动态压缩永久变形均随DCP用量的增加而逐渐降低。
在本论文第六章中,我们通过并用HNBR与ZSC的方法制备了HNBR/ZSC/CB复合材料,详细考察了HNBR与ZSC的共混比、DCP用量、芳纶短纤维以及炭黑种类对上述复合材料性能的影响。研究结果发现,随ZSC共混比例的增加,HNBR/ZSC/N220复合材料的力学强度逐渐提高,滚动压缩量和生热量逐渐减小；ZSC的用量对复合材料的裤型撕裂行为有着重要影响,且当HNBR/ZSC共混比为70/30时复合材料有着最好的动态切割性能。此外,通过对比发现,与增加DCP用量相比,在HNBR/ZSC/N220体系中加入芳纶短纤维能够在更好的降低其滚动压缩生热的同时,保持较高的裤型撕裂强度。对于含有芳纶短纤维的复合材料体系,填充大粒径、低结构的炭黑能够达到进一步降低其滚动压缩生热的目的,但此时复合材料的裤型撕裂强度和动态切割性能将有所下降。
本论文第七章对利用NaSS在HNBR基体过氧化物硫化过程中的原位聚合／接枝反应制备质子交换膜材料这一方法进行了探索研究,并且详细讨论了HNBR基体的饱和度以及NaSS和过氧化物D25用量对所制备的质子交换膜材料的结构和性能的影响。研究结果表明,NaSS能够在HNBR基体的过氧化物硫化过程中发生原位聚合反应并接枝于HNBR分子链上,NaSS的原位聚合／接枝反应与HNBR的过氧化物硫化过程基本同步发生；硫化后的HNBR基体中存在有大量纳米尺寸的poly-NaSS离子簇相分离结构；接枝的-S03H在最终得到的质子交换膜中有着非常均匀的分布。当NaSS用量高于70phr时,所得质子交换膜的质子电导率能够达到0.01S-cm-1的数量级,并且其甲醇渗透率远低于Nafion212。所制备的以HNBR2010L为基体的质子交换膜材料的IEC、吸水率、质子电导率和甲醇渗透率随D25用量的增加而逐渐减小。几乎所有以HNBR2020L为基体的质子交换膜有着比Nafion212更高的选择性,并且其在直接甲醇燃料电池的使用温度下具有较好的热稳定性。
To achieve homogenous dispersion of a nanophase in polymeric matrix is both scientifically challenging and industrially important for fabricating polymeric nanocomposites. In recent years, the use of in situ techniques to obtain an ultrafine dispersed nanophase in a polymeric matrix has emerged as one of the most attractive fields in polymer science in creating high-performance polymeric nanocomposites. In this paper, based on the in situ technique, we detailed investigated the in situ reaction behavior of ZDMA in HNBR matrix as well as the structure and properties of the prepared ZDMA reinforced HNBR nanocomposites. Moreover, this work firstly put forward a novel environment-friendly route to prepare proton exchange membranes (PEM) for direct methanol fuel cell (DMFC) via the in situ reaction and grafting of sodium4-styrene sulfonate (NaSS) to HNBR during peroxide curing.
The third chapter studied the in situ polymerization behavior of ZDMA during the peroxide curing of HNBR matrix. The results showed that the diameter of the original dispersed ZDMA in HNBR matrix has a significant effect on its in situ polymerization behavior, and the large amount of micron-sized dispersions in the vulcanizate was verified to be the reacted ZDMA. Furthermore, the microstructure of the remaining micron-sized (even nano-sized) dispersions in the cured HNBR/ZDMA was verified for the first time, and a new mechanism for in situ polymerization of ZDMA, i.e., the solid bulk polymerization initialized onto the surface of "dissolve-diffusion" limited ZDMA particles, was put forward. The mciron-sized dispersions generated by the solid bulk polymerization of undiffused ZDMA particles resulted in the decrease of the ionic cross-linking density and mechanical strength of the HNRB/ZDMA vulcanizate.
The fourth chapter studied the influence of curing temperature on the structure and properties of HNBR reinforced by in situ polymerization of ZDMA. The results showed that, with the increase of curing temperature, the in situ grafting ratio of ZDMA and the ionic cross-linking density decreased, and both the number and diameter of the micron-sized dispersions generated by the solid bulk polymerization of ZDMA obviously increased, finally resulting in the dramatic decrease of the mechanical properties of the HNBR/ZDMA nanocomposite. Moreover, a possible mechanism for the influence of curing temperature on "dissolve-diffusion" of ZDMA particles was put forward, which can well explain the phenomenon in this work.
In the fifth chapter, we prepared ZDMA reinforced HNBR/N115composites through the neutralization of ZnO and MAA during mixing process and studied the effect of ZDMA and DCP content on the wear (Akron and DIN), cutting and chipping and dynamic compression fatigue behaviors of the prepared composites. The results showed that, with increasing the content of ZDMA, the Akron abrasion resistance of HNBR/N115/ZDMA composite increased while the DIN abrasion resistance decreased, and there was good correlation between the wear properties of the composites and the morphology of their abraded surfaces. Besides, with the increase of ZDMA content, the cutting and chipping properties of the composites firstly enhanced and then remained almost constant, the dynamic compression heat buildup increased and the compression permanent set gradually decreased. When the content of ZDMA is30phr, the cutting and chipping loss, dynamic compression heat buildup and permanent set decreased with increasing the content of DCP.
In the sixth chapter, we prepared ZDMA reinforced HNBR/CB composites by blending the HNBR and ZSC, and studied the effect of HNBR/ZSC blend ratio, DCP content, aramid short fiber and the types of carbon black on the properties of the prepared composites. The results showed that, with increasing the blend ratio of ZSC, the mechanical strength of the HNBR/ZSC/N220composites increased remarkably, and the rolling compression heat buildup gradually decreased. The blend ratio of HNBR/ZSC had a significant effect on the tear behavior of the composites. The best cutting and chipping resistance of the composite was achieved when the blend ratio of HNBR/ZSC was70/30. Besides, compared with increasing the content of DCP, compounding the aramid short fiber into the HNBR/ZSC/N220system was a better choice to decrease the rolling compression, heat buildup and keep relative high tear strength. The rolling compression heat buildup of the composites can be further decreased through mixing the carbon black with higher diameter and lower structural; however, it caused the decrease of the tear strength and cutting and chipping properties.
The seventh chapter explored a novel route to prepare PEM for DMFC application via in situ reaction and grafting of NaSS in HNBR matrix during peroxide curing, and detailed studied the effect of the saturation of HNBR and the content of NaSS and peroxide D25on structure and properties of the prepared PEM. The results showed that NaSS can take place in situ reaction during the peroxide curing of HNBR matrix and graft into the HNBR molecular chains. The in situ reaction and grafting of NaSS was proved to occur along with the peroxide curing of HNBR matrix. A large amount of nano-sized ionic clusters can be observed in the HNBR/NaSS vulcanizates, and the distribution of sulfonic acid groups in the prepared PEM was verified to be quite uniform. The proton conductivity of the prepared PEM can reach the order of0.01S·cm-1with much lower methanol permeability than Nafion212. The IEC, water uptake, proton conductivity and methanol permeability of HNBR2010L based PEM decreased with the content of peroxide D25. Almost all HNBR2020L based membranes had higher selectivity compared to commercial Nafion212, and they can also be thermally stable for DMFC application.
本论文第三章对ZDMA在HNBR基体过氧化物硫化过程中的原位聚合反应行为进行了详细的跟踪研究。研究结果表明,ZDMA的初始分散粒径对其原位聚合行为有着重要影响,硫化胶中存在的大量微米分散相为发生原位反应的ZDMA;另外,本研究首次发现并证明了ZDMA在原位反应过程中除发生“溶解-扩散-原位聚合”而生成纳米离子簇相分离结构之外,还存在有另一种新的反应行为,即扩散受限的ZDMA颗粒能够在过氧化物自由基的引发下发生固相本体聚合反应而直接从结晶态转变为无定形态,在硫化胶基体中产生大量不同于离子簇结构的特殊微米(甚至纳米)分散相；上述大量微米分散相的存在将导致HNRB/ZDMA硫化胶的离子键交联密度显著减小,力学强度下降。
论文第四章研究了硫化温度对HNBR/ZDMA复合材料结构与性能的影响。研究结果表明,随硫化温度升高,ZDMA的原位聚合接枝率降低,ZDMA固相本体聚合所产生的特殊分散相的尺寸和数量逐渐增加,离子键交联密度减小,最终导致HNBR/ZDMA复合材料的物理机械性能均有不同程度的降低。此外,本工作还从“溶解-扩散”的角度提出了硫化温度对ZDMA原位聚合反应可能存在的影响机理。
在论文第五章中,我们利用氧化锌与甲基丙烯酸在胶料混炼过程中原位中和反应的方法制备了HNBR/N115/ZDMA纳米复合材料,重点研究了ZDMA的原位生成量以及过氧化物DCP的用量对上述纳米复合材料基本力学性能、磨耗性能、动态切割性能和动态压缩疲劳性能的影响,并对其相关机理进行了讨论。研究结果发现,复合材料的阿克隆磨耗性能随ZDMA原位生成量的增加逐渐提高,而DIN磨耗性能反而逐渐降低,由磨耗面形貌所反映出的磨耗机理与复合材料磨耗性能的变化有着较好的相关性；随ZDMA原位生成量的增加,复合材料的动态切割性能先逐渐提高后保持基本稳定,动态压缩疲劳温升逐渐增大,动态压缩永久变形逐渐减小；当ZDMA用量为30phr时,复合材料的动态切割性能、动态压缩疲劳温升和动态压缩永久变形均随DCP用量的增加而逐渐降低。
在本论文第六章中,我们通过并用HNBR与ZSC的方法制备了HNBR/ZSC/CB复合材料,详细考察了HNBR与ZSC的共混比、DCP用量、芳纶短纤维以及炭黑种类对上述复合材料性能的影响。研究结果发现,随ZSC共混比例的增加,HNBR/ZSC/N220复合材料的力学强度逐渐提高,滚动压缩量和生热量逐渐减小；ZSC的用量对复合材料的裤型撕裂行为有着重要影响,且当HNBR/ZSC共混比为70/30时复合材料有着最好的动态切割性能。此外,通过对比发现,与增加DCP用量相比,在HNBR/ZSC/N220体系中加入芳纶短纤维能够在更好的降低其滚动压缩生热的同时,保持较高的裤型撕裂强度。对于含有芳纶短纤维的复合材料体系,填充大粒径、低结构的炭黑能够达到进一步降低其滚动压缩生热的目的,但此时复合材料的裤型撕裂强度和动态切割性能将有所下降。
本论文第七章对利用NaSS在HNBR基体过氧化物硫化过程中的原位聚合／接枝反应制备质子交换膜材料这一方法进行了探索研究,并且详细讨论了HNBR基体的饱和度以及NaSS和过氧化物D25用量对所制备的质子交换膜材料的结构和性能的影响。研究结果表明,NaSS能够在HNBR基体的过氧化物硫化过程中发生原位聚合反应并接枝于HNBR分子链上,NaSS的原位聚合／接枝反应与HNBR的过氧化物硫化过程基本同步发生；硫化后的HNBR基体中存在有大量纳米尺寸的poly-NaSS离子簇相分离结构；接枝的-S03H在最终得到的质子交换膜中有着非常均匀的分布。当NaSS用量高于70phr时,所得质子交换膜的质子电导率能够达到0.01S-cm-1的数量级,并且其甲醇渗透率远低于Nafion212。所制备的以HNBR2010L为基体的质子交换膜材料的IEC、吸水率、质子电导率和甲醇渗透率随D25用量的增加而逐渐减小。几乎所有以HNBR2020L为基体的质子交换膜有着比Nafion212更高的选择性,并且其在直接甲醇燃料电池的使用温度下具有较好的热稳定性。
To achieve homogenous dispersion of a nanophase in polymeric matrix is both scientifically challenging and industrially important for fabricating polymeric nanocomposites. In recent years, the use of in situ techniques to obtain an ultrafine dispersed nanophase in a polymeric matrix has emerged as one of the most attractive fields in polymer science in creating high-performance polymeric nanocomposites. In this paper, based on the in situ technique, we detailed investigated the in situ reaction behavior of ZDMA in HNBR matrix as well as the structure and properties of the prepared ZDMA reinforced HNBR nanocomposites. Moreover, this work firstly put forward a novel environment-friendly route to prepare proton exchange membranes (PEM) for direct methanol fuel cell (DMFC) via the in situ reaction and grafting of sodium4-styrene sulfonate (NaSS) to HNBR during peroxide curing.
The third chapter studied the in situ polymerization behavior of ZDMA during the peroxide curing of HNBR matrix. The results showed that the diameter of the original dispersed ZDMA in HNBR matrix has a significant effect on its in situ polymerization behavior, and the large amount of micron-sized dispersions in the vulcanizate was verified to be the reacted ZDMA. Furthermore, the microstructure of the remaining micron-sized (even nano-sized) dispersions in the cured HNBR/ZDMA was verified for the first time, and a new mechanism for in situ polymerization of ZDMA, i.e., the solid bulk polymerization initialized onto the surface of "dissolve-diffusion" limited ZDMA particles, was put forward. The mciron-sized dispersions generated by the solid bulk polymerization of undiffused ZDMA particles resulted in the decrease of the ionic cross-linking density and mechanical strength of the HNRB/ZDMA vulcanizate.
The fourth chapter studied the influence of curing temperature on the structure and properties of HNBR reinforced by in situ polymerization of ZDMA. The results showed that, with the increase of curing temperature, the in situ grafting ratio of ZDMA and the ionic cross-linking density decreased, and both the number and diameter of the micron-sized dispersions generated by the solid bulk polymerization of ZDMA obviously increased, finally resulting in the dramatic decrease of the mechanical properties of the HNBR/ZDMA nanocomposite. Moreover, a possible mechanism for the influence of curing temperature on "dissolve-diffusion" of ZDMA particles was put forward, which can well explain the phenomenon in this work.
In the fifth chapter, we prepared ZDMA reinforced HNBR/N115composites through the neutralization of ZnO and MAA during mixing process and studied the effect of ZDMA and DCP content on the wear (Akron and DIN), cutting and chipping and dynamic compression fatigue behaviors of the prepared composites. The results showed that, with increasing the content of ZDMA, the Akron abrasion resistance of HNBR/N115/ZDMA composite increased while the DIN abrasion resistance decreased, and there was good correlation between the wear properties of the composites and the morphology of their abraded surfaces. Besides, with the increase of ZDMA content, the cutting and chipping properties of the composites firstly enhanced and then remained almost constant, the dynamic compression heat buildup increased and the compression permanent set gradually decreased. When the content of ZDMA is30phr, the cutting and chipping loss, dynamic compression heat buildup and permanent set decreased with increasing the content of DCP.
In the sixth chapter, we prepared ZDMA reinforced HNBR/CB composites by blending the HNBR and ZSC, and studied the effect of HNBR/ZSC blend ratio, DCP content, aramid short fiber and the types of carbon black on the properties of the prepared composites. The results showed that, with increasing the blend ratio of ZSC, the mechanical strength of the HNBR/ZSC/N220composites increased remarkably, and the rolling compression heat buildup gradually decreased. The blend ratio of HNBR/ZSC had a significant effect on the tear behavior of the composites. The best cutting and chipping resistance of the composite was achieved when the blend ratio of HNBR/ZSC was70/30. Besides, compared with increasing the content of DCP, compounding the aramid short fiber into the HNBR/ZSC/N220system was a better choice to decrease the rolling compression, heat buildup and keep relative high tear strength. The rolling compression heat buildup of the composites can be further decreased through mixing the carbon black with higher diameter and lower structural; however, it caused the decrease of the tear strength and cutting and chipping properties.
The seventh chapter explored a novel route to prepare PEM for DMFC application via in situ reaction and grafting of NaSS in HNBR matrix during peroxide curing, and detailed studied the effect of the saturation of HNBR and the content of NaSS and peroxide D25on structure and properties of the prepared PEM. The results showed that NaSS can take place in situ reaction during the peroxide curing of HNBR matrix and graft into the HNBR molecular chains. The in situ reaction and grafting of NaSS was proved to occur along with the peroxide curing of HNBR matrix. A large amount of nano-sized ionic clusters can be observed in the HNBR/NaSS vulcanizates, and the distribution of sulfonic acid groups in the prepared PEM was verified to be quite uniform. The proton conductivity of the prepared PEM can reach the order of0.01S·cm-1with much lower methanol permeability than Nafion212. The IEC, water uptake, proton conductivity and methanol permeability of HNBR2010L based PEM decreased with the content of peroxide D25. Almost all HNBR2020L based membranes had higher selectivity compared to commercial Nafion212, and they can also be thermally stable for DMFC application.
引文
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