多尺度有机硅基纳米材料改性聚合物
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摘要
影响聚合物纳米复合材料性能的因素很多,其中纳米粒子在聚合物中的分散和纳米粒子与基体界面处的相互作用强度,以及纳米粒子的形状尺寸等尤为重要。利用不同纳米材料自身的特点,调节其与聚合物基体界面相互作用,进而有针对性去设计和改善相关聚合物,获得高性能的新型聚合物纳米复合材料具有重要的意义。纳米材料的自身特点包括其形状差异如一维管状、二维层状及三维球状或类球状,它们分别具有不同的优势；还包括其表面性质和官能团不同,如表面含有非反应性有机官能团可提高纳米材料与基体的相容性,表面含有反应性官能团能促进纳米材料与聚合物结合更紧密,甚至形成交联网络结构。
(1)苯胺甲基寡聚笼型倍半硅氧烷(ND42-POSS)是表面含有丰富的可反应性胺基官能团的三维纳米粒子,根据其特点,将其选作纳米交联中心,以化学反应的方式引入到苯乙烯-马来酸酐共聚物中。POSS在所制备的复合材料中添加量达30%时仍无宏观相分离现象。扫面电子显微镜和透射电子显微镜可观察到POSS以纳米尺度分散于基体中。DSC结果表明POSS的引入提高了复合材料的玻璃化转变温度,主要是由于体系中交联网络结构的形成限制了聚合物分子链段的运动。DMA结果揭示复合材料在高温下的储能模量显著提高,尤其是当POSS含量较高时(>18%)体系中形成了完整的三维交联网络结构。TGA数据显示复合材料在发生25%和70%热失重的温度均提高,并且材料最终的残炭也有所提高,综合性热能得到较大改善。
(2)乙烯基有机硅纳米微球表面含有丰富的有机官能团,与聚合物具有良好的相容性,我们根据其可在聚合物基体中均分分散又无化学键合作用的特点,将其作为新型纳米材料引入到通用工程塑料聚丙烯和可再生材料聚乳酸中。通过SEM表征证实了乙烯基微球在基体中以单个粒子的形式在两种基体中均匀分散。对于聚丙烯,乙烯基纳米微球的加入除了表现无机纳米粒子的增强作用外,还为复合材料引入了新的能量耗散机制。通过拉伸测试和缺口冲击测试等表征发现,乙烯基纳米微球的加入同时提高了材料强度和韧性,并且复合材料的热稳定性也有所改善。对于聚乳酸,均匀分散于基体中的乙烯基纳米微球的加入起到了异相成核剂的作用,促进了聚乳酸结晶度和结晶速度的提高,解决了聚乳酸在应用中结晶慢和结晶度不高的问题。
(3)石墨烯是具有大比表面积的片层结构纳米材料,但是加入到聚合物中时容易发生团聚和叠加。我们用氨乙基氨丙基三甲氧基硅烷对其进行功能化处理,改善了其在有机溶剂和聚合物中的分散。将该功能化石墨烯引入聚乳酸后,复合材料在聚乳酸进入橡胶态后的储能模量大幅提高。例如,质量比0.5%功能化石墨烯的加入使得聚乳酸在Tg附近储能模量的提高超过了一个数量级(从20MPa提高至300MPa)。同时,复合材料的抗热变形能力也显著提高。这主要是由于经功能化处理后,石墨烯在聚乳酸基体中均匀分散,与聚合物分子形成互相穿透的网络结构。
The properties of nanocomposites were affected by several factors. Of which, dispersion of nanoparticles, interactions between nanoparticles and polymer matrix, dimensions of the nanoparticles were particularly important. By considering the features of different nanoparticles and adjusting the interactions between nanofiller and matrix, nanocomposites with high performance could be obtained. Here the features of the nanoparticles mainly contained the dimensions and the surface functional groups. The dimensions of nanoparticles could be one dimensional nanomaterials like nanotubes, two dimensional nanomaterials like clay or graphene and three dimensional nanomaterials like silica or POSS. The surface functional groups of nanoparticles could be reactive or non-reactive. Research on the interaction of the nanoparticle dimensions and the interactions between nanofiller and matrix could be of great significance.
(1) N-Phenylamino-methyl POSS was three dimensional reactive nanoparticle. Considering the reactivity, it was incorporated to modify the PSMA resin. A series of crosslinked hybrids were prepared using various amounts of POSS as nano-scale crosslink agent. The hybrids showed no macro-phase separation even when the POSS concentration was up to30wt%. HRTEM measurements showed the POSS was nano scale separated in PSMA matrix. DSC results indicated that Tg increased with the addition of POSS. DMA revealed the storage modulus of the hybrids at high temperature was much improved compared with that of neat PSMA, especially with high POSS loadings. TGA revealed the values of Td,25%to Td,70%of the hybrids were increased and the char yields were much improved. The enhanced properties were ascribed to the synergetic effects of PSMA and POSS. Because of the good compatibility between POSS and PSMA, POSS as a crosslinker could be dispersed into PSMA matrix in nano scale. PSMA chains would be restricted by the nano scale crosslinker, and resulted in the great enhancement of mechanical and thermal properties.
(2) The vinyl-silica nanoparticles were three dimensional nanoparticles, which had good compatibility with polymers due to the rich surface organic functional groups. Considering the good dispersion of vinyl-silica nanoparticles in polymers and its non-reactivity, we incorporated the nanofillers into polypropylene (PP) and polylactic acid (PLLA). SEM indicated that vinyl-silica nanoparticles were homogeneously dispersed in both polymers. For PP, Vinyl-silica nanoparticles not only worked as rigid particles, but also brought new energy-dissipating mechanisms for the nanocomposites. Simultaneously improved strength and toughness of the nanocomposites was confirmed by tensile test and notched impact test. Also, the enhanced thermostabilization was proved by TGA measurement. For PLLA, the well dispersed vinyl-silica nanoparticles worked as heterogeneous nucleation agent. The improvements of crystallinity and crystallization rate of PLLA were both confirmed by DSC.
(3) Graphene was a two dimensional nanoparticles with large specific surface area. When composited with polymers, it tended to aggregated. Here we functionalize the graphene with N-(aminoethyl)-aminopropyltrimethoxysilane (KH792) to improve its dispersion in organic solvent and polymer matrix. With the incorporation of the KH792-RGO, the storage modulus of the composite was largely increased in the rubber state.0.5wt%addition of KH792-RGO dramatically increased the storage modulus of PLLA around Tg by one order of magnitude compared with neat PLLA (from20to300MPa). Meanwhile, the heat distortion resistance of PLLA/KH792-RGO was greatly improved as well. Formation of a graphene network in the composites was considered to be the main driving force of the outstanding performance for the nanocomposites.
(1)苯胺甲基寡聚笼型倍半硅氧烷(ND42-POSS)是表面含有丰富的可反应性胺基官能团的三维纳米粒子,根据其特点,将其选作纳米交联中心,以化学反应的方式引入到苯乙烯-马来酸酐共聚物中。POSS在所制备的复合材料中添加量达30%时仍无宏观相分离现象。扫面电子显微镜和透射电子显微镜可观察到POSS以纳米尺度分散于基体中。DSC结果表明POSS的引入提高了复合材料的玻璃化转变温度,主要是由于体系中交联网络结构的形成限制了聚合物分子链段的运动。DMA结果揭示复合材料在高温下的储能模量显著提高,尤其是当POSS含量较高时(>18%)体系中形成了完整的三维交联网络结构。TGA数据显示复合材料在发生25%和70%热失重的温度均提高,并且材料最终的残炭也有所提高,综合性热能得到较大改善。
(2)乙烯基有机硅纳米微球表面含有丰富的有机官能团,与聚合物具有良好的相容性,我们根据其可在聚合物基体中均分分散又无化学键合作用的特点,将其作为新型纳米材料引入到通用工程塑料聚丙烯和可再生材料聚乳酸中。通过SEM表征证实了乙烯基微球在基体中以单个粒子的形式在两种基体中均匀分散。对于聚丙烯,乙烯基纳米微球的加入除了表现无机纳米粒子的增强作用外,还为复合材料引入了新的能量耗散机制。通过拉伸测试和缺口冲击测试等表征发现,乙烯基纳米微球的加入同时提高了材料强度和韧性,并且复合材料的热稳定性也有所改善。对于聚乳酸,均匀分散于基体中的乙烯基纳米微球的加入起到了异相成核剂的作用,促进了聚乳酸结晶度和结晶速度的提高,解决了聚乳酸在应用中结晶慢和结晶度不高的问题。
(3)石墨烯是具有大比表面积的片层结构纳米材料,但是加入到聚合物中时容易发生团聚和叠加。我们用氨乙基氨丙基三甲氧基硅烷对其进行功能化处理,改善了其在有机溶剂和聚合物中的分散。将该功能化石墨烯引入聚乳酸后,复合材料在聚乳酸进入橡胶态后的储能模量大幅提高。例如,质量比0.5%功能化石墨烯的加入使得聚乳酸在Tg附近储能模量的提高超过了一个数量级(从20MPa提高至300MPa)。同时,复合材料的抗热变形能力也显著提高。这主要是由于经功能化处理后,石墨烯在聚乳酸基体中均匀分散,与聚合物分子形成互相穿透的网络结构。
The properties of nanocomposites were affected by several factors. Of which, dispersion of nanoparticles, interactions between nanoparticles and polymer matrix, dimensions of the nanoparticles were particularly important. By considering the features of different nanoparticles and adjusting the interactions between nanofiller and matrix, nanocomposites with high performance could be obtained. Here the features of the nanoparticles mainly contained the dimensions and the surface functional groups. The dimensions of nanoparticles could be one dimensional nanomaterials like nanotubes, two dimensional nanomaterials like clay or graphene and three dimensional nanomaterials like silica or POSS. The surface functional groups of nanoparticles could be reactive or non-reactive. Research on the interaction of the nanoparticle dimensions and the interactions between nanofiller and matrix could be of great significance.
(1) N-Phenylamino-methyl POSS was three dimensional reactive nanoparticle. Considering the reactivity, it was incorporated to modify the PSMA resin. A series of crosslinked hybrids were prepared using various amounts of POSS as nano-scale crosslink agent. The hybrids showed no macro-phase separation even when the POSS concentration was up to30wt%. HRTEM measurements showed the POSS was nano scale separated in PSMA matrix. DSC results indicated that Tg increased with the addition of POSS. DMA revealed the storage modulus of the hybrids at high temperature was much improved compared with that of neat PSMA, especially with high POSS loadings. TGA revealed the values of Td,25%to Td,70%of the hybrids were increased and the char yields were much improved. The enhanced properties were ascribed to the synergetic effects of PSMA and POSS. Because of the good compatibility between POSS and PSMA, POSS as a crosslinker could be dispersed into PSMA matrix in nano scale. PSMA chains would be restricted by the nano scale crosslinker, and resulted in the great enhancement of mechanical and thermal properties.
(2) The vinyl-silica nanoparticles were three dimensional nanoparticles, which had good compatibility with polymers due to the rich surface organic functional groups. Considering the good dispersion of vinyl-silica nanoparticles in polymers and its non-reactivity, we incorporated the nanofillers into polypropylene (PP) and polylactic acid (PLLA). SEM indicated that vinyl-silica nanoparticles were homogeneously dispersed in both polymers. For PP, Vinyl-silica nanoparticles not only worked as rigid particles, but also brought new energy-dissipating mechanisms for the nanocomposites. Simultaneously improved strength and toughness of the nanocomposites was confirmed by tensile test and notched impact test. Also, the enhanced thermostabilization was proved by TGA measurement. For PLLA, the well dispersed vinyl-silica nanoparticles worked as heterogeneous nucleation agent. The improvements of crystallinity and crystallization rate of PLLA were both confirmed by DSC.
(3) Graphene was a two dimensional nanoparticles with large specific surface area. When composited with polymers, it tended to aggregated. Here we functionalize the graphene with N-(aminoethyl)-aminopropyltrimethoxysilane (KH792) to improve its dispersion in organic solvent and polymer matrix. With the incorporation of the KH792-RGO, the storage modulus of the composite was largely increased in the rubber state.0.5wt%addition of KH792-RGO dramatically increased the storage modulus of PLLA around Tg by one order of magnitude compared with neat PLLA (from20to300MPa). Meanwhile, the heat distortion resistance of PLLA/KH792-RGO was greatly improved as well. Formation of a graphene network in the composites was considered to be the main driving force of the outstanding performance for the nanocomposites.
引文
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