聚合物/凹凸棒石纳米复合材料制备与性能
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摘要
凹凸棒石(ATT)是一种一维棒状硅酸盐矿物,表面极性强易团聚,在与聚合物加工过程中易破碎,这限制了它的应用。本文采用如下两种方法对ATT进行有机改性,提高ATT在聚合物中的相容性:1)硅烷偶联剂(KH570)改性ATT,并用聚烯烃弹性体(POE)包覆ATT制备母粒;2)机械共混过程中,甲苯-2,4-二异氰酸酯(TDI)原位反应改性ATT。
首先采用熔融共混法制备聚丙烯(PP)/ATT二元复合材料及PP/ATT/POE三元复合材料,考察了POE/ATT母粒协同增强聚丙烯(PP),系统地研究了复合材料的力学性能、流变性能和结晶性能。力学性能研究结果表明:在PP/ATT二元纳米复合材料中,未改性ATT与ATT-KH570均能提高PP的拉伸强度,但是在相同凹凸棒石含量下,PP/ATT-KH570复合材料的拉伸性能提高更明显;未改性ATT未能提高PP的冲击强度,而PP/ATT-KH570的冲击强度则随着ATT-KH570含量提高先增加后降低,并在ATT-KH570含量为1%时达到最大值。在PP/ATT-KH570/POE三元纳米复合材料中,当固定PP/ATT-KH570比例为100/5时,POE含量达到5%,复合材料冲击强度为8.91KJ/m~2,与未加POE体系相比提高了21.10%;当POE含量增加到15%时,复合材料冲击强度提高了44.80%,并且其拉伸强度基本得到保持,说明POE和ATT-KH570对PP具有明显的协同增韧增强效果。流变性能测试表明,在低的剪切速率下,ATT-KH570对复合材料的流动性能有较好的改善。DSC分析结果表明,POE和ATT-KH570均能有效地促进PP结晶,并且ATT-KH570/POE母粒对PP具有更有效的协同异相成核促进作用。
论文进一步通过机械共混的方法TDI原位改性ATT,以聚甲基丙烯酸甲酯(PMMA)为基体,成功制备了PMMA/ATT纳米复合材料。原位改性凹凸棒石在PMMA中分散均匀,纳米粒子的形貌(一维棒状)得到保持,纳米复合材料的力学性能、热性能均有大幅提高。傅里叶红外仪和扫描电镜的结果显示,TDI原位改性的ATT有较高TDI表面接枝率。采用透射电镜(TEM)观察纳米复合材料结构时发现,TDI可使ATT在共混过程中原位表面改性,并使ATT在基体中达到均匀分散。随着原位改性凹凸棒石含量从0到6%变化,复合材料的力学性能先增加后减少,并在3%时拉伸强度达到最大值,比纯PMMA提高了19%,在2%时无缺口冲击强度达到最大值,比纯PMMA提高了31%。当在PMMA中加入2%的原位改性凹凸棒石时,因为ATT阻碍了PMMA的链段运动,使其玻璃化转变温度提高了13.20℃,复合材料失重10%的分解温度较纯PMMA提高了73.47℃。
The attapulgite (ATT) clay is a linear hydrated magnesium aluminum silicate. It is easy to aggregate and fracture during the mechanical mixing, which limites its application in polymer composition. In the present work, two approaches were applied for improving the compatibility between ATT and polymer matrix: firstly, a polyolefin elastomer (POE)/ATT masterbach for polypropylene matrix was prepared, and silane coupling agent KH570 was selected for ATT modification; secondly, an in situ modification of ATT clay by toluene-2,4-di-isocyanate (TDI) was employed, therefore polymethylmethacrylate (PMMA)/ATT nanocomposites were prepared by mechanical mixing.
Polypropylene(PP)/ATT-KH570/POE ternary composites and PP/ATT-KH570 binary composites were prepared by melt blending method, and were systemically investigated, in particular for its mechanical properties, rheological and crystallizing behavior. It was found that both of ATT-KH570 and ATT without modification were able to significantly the tensile strength (σt) of PP, and ATT-KH570 exhibited a higher reinforcement efficiency due to the better dispersion and interfacial bonding. The impact strength of PP/ATT-KH570 was higher than that of neat PP and increased with the addition of ATT-KH570 content from 0 to 1 wt%. However, ATT without modification had a negative effect on the impact strength. For the PP/POE/ATT-KH570 ternary composites, The mechanical property characterization showed that at a fixed weight ratio of ATT-KH570 and PP (5/100), the content of POE dominantly affected the impact strength of the composites. When the content of POE was 5%, the impact strength of composites reached 8.91KJ/m~2 which has around 21.10% enhancement over that of the composites wihtout POE. When the content of POE was increased to 15% , a 44.8% enhancement for the impact strength was observed. More importantly, no tensile strength of PP was sacrificed with the addtion of ATT and POE, which might be attributed to the synergistic effect of these two modifiers. From the rheological curves, we found that the addition of ATT-KH570 obviously decreased the melt fluidity of composites at low shear rate. In addition, POE and ATT-KH570 were effective in promoting the crystallization of PP by the analysis of DSC.
A novel in-situ modification of ATT by toluene-2,4-di-isocyanate using mechanical mixing with polymethylmethacrylate (PMMA) was exploited. As a consequence, PMMA/organo-modified ATT nanocomposites were prepared, which provided prominent improvements in strength, toughness and thermal stability. High grafting efficiency of TDI on ATT surface was confirmed by FTIR spectra and SEM observations. The uniform dispersion and rod-like texture of in-situ modified ATT nanorods in the PMMA which was clearly visible in the TEM micrographes, influenced the mechanical and thermal properties of the nanocomposites. The tensile strength of nanocomposites first increased and then decreased with the in-situ modified ATT concentration ranging from 0 to 6.0%, and reached the maximum value at 3.0%. For the impact strengh, PMMA/in-situ modified ATT with 2.0% ATT had the maximum value which showed around 31% enhancement than that of pure PMMA. The chain mobility of PMMA was significantly inhibited by the uniformly dispersed fibrous nanoparticles, leading a 13.20℃increase in the glass transition temperature of PMMA/in-situ modified ATT nanocomposite containing 2.0% ATT. The thermal stability of the nanocomposites was enhanced by the presence of ATT. For example, 10% mass loss temperature of PMMA/in-situ modified ATT was 73.47℃higher than that of pristine PMMA.
首先采用熔融共混法制备聚丙烯(PP)/ATT二元复合材料及PP/ATT/POE三元复合材料,考察了POE/ATT母粒协同增强聚丙烯(PP),系统地研究了复合材料的力学性能、流变性能和结晶性能。力学性能研究结果表明:在PP/ATT二元纳米复合材料中,未改性ATT与ATT-KH570均能提高PP的拉伸强度,但是在相同凹凸棒石含量下,PP/ATT-KH570复合材料的拉伸性能提高更明显;未改性ATT未能提高PP的冲击强度,而PP/ATT-KH570的冲击强度则随着ATT-KH570含量提高先增加后降低,并在ATT-KH570含量为1%时达到最大值。在PP/ATT-KH570/POE三元纳米复合材料中,当固定PP/ATT-KH570比例为100/5时,POE含量达到5%,复合材料冲击强度为8.91KJ/m~2,与未加POE体系相比提高了21.10%;当POE含量增加到15%时,复合材料冲击强度提高了44.80%,并且其拉伸强度基本得到保持,说明POE和ATT-KH570对PP具有明显的协同增韧增强效果。流变性能测试表明,在低的剪切速率下,ATT-KH570对复合材料的流动性能有较好的改善。DSC分析结果表明,POE和ATT-KH570均能有效地促进PP结晶,并且ATT-KH570/POE母粒对PP具有更有效的协同异相成核促进作用。
论文进一步通过机械共混的方法TDI原位改性ATT,以聚甲基丙烯酸甲酯(PMMA)为基体,成功制备了PMMA/ATT纳米复合材料。原位改性凹凸棒石在PMMA中分散均匀,纳米粒子的形貌(一维棒状)得到保持,纳米复合材料的力学性能、热性能均有大幅提高。傅里叶红外仪和扫描电镜的结果显示,TDI原位改性的ATT有较高TDI表面接枝率。采用透射电镜(TEM)观察纳米复合材料结构时发现,TDI可使ATT在共混过程中原位表面改性,并使ATT在基体中达到均匀分散。随着原位改性凹凸棒石含量从0到6%变化,复合材料的力学性能先增加后减少,并在3%时拉伸强度达到最大值,比纯PMMA提高了19%,在2%时无缺口冲击强度达到最大值,比纯PMMA提高了31%。当在PMMA中加入2%的原位改性凹凸棒石时,因为ATT阻碍了PMMA的链段运动,使其玻璃化转变温度提高了13.20℃,复合材料失重10%的分解温度较纯PMMA提高了73.47℃。
The attapulgite (ATT) clay is a linear hydrated magnesium aluminum silicate. It is easy to aggregate and fracture during the mechanical mixing, which limites its application in polymer composition. In the present work, two approaches were applied for improving the compatibility between ATT and polymer matrix: firstly, a polyolefin elastomer (POE)/ATT masterbach for polypropylene matrix was prepared, and silane coupling agent KH570 was selected for ATT modification; secondly, an in situ modification of ATT clay by toluene-2,4-di-isocyanate (TDI) was employed, therefore polymethylmethacrylate (PMMA)/ATT nanocomposites were prepared by mechanical mixing.
Polypropylene(PP)/ATT-KH570/POE ternary composites and PP/ATT-KH570 binary composites were prepared by melt blending method, and were systemically investigated, in particular for its mechanical properties, rheological and crystallizing behavior. It was found that both of ATT-KH570 and ATT without modification were able to significantly the tensile strength (σt) of PP, and ATT-KH570 exhibited a higher reinforcement efficiency due to the better dispersion and interfacial bonding. The impact strength of PP/ATT-KH570 was higher than that of neat PP and increased with the addition of ATT-KH570 content from 0 to 1 wt%. However, ATT without modification had a negative effect on the impact strength. For the PP/POE/ATT-KH570 ternary composites, The mechanical property characterization showed that at a fixed weight ratio of ATT-KH570 and PP (5/100), the content of POE dominantly affected the impact strength of the composites. When the content of POE was 5%, the impact strength of composites reached 8.91KJ/m~2 which has around 21.10% enhancement over that of the composites wihtout POE. When the content of POE was increased to 15% , a 44.8% enhancement for the impact strength was observed. More importantly, no tensile strength of PP was sacrificed with the addtion of ATT and POE, which might be attributed to the synergistic effect of these two modifiers. From the rheological curves, we found that the addition of ATT-KH570 obviously decreased the melt fluidity of composites at low shear rate. In addition, POE and ATT-KH570 were effective in promoting the crystallization of PP by the analysis of DSC.
A novel in-situ modification of ATT by toluene-2,4-di-isocyanate using mechanical mixing with polymethylmethacrylate (PMMA) was exploited. As a consequence, PMMA/organo-modified ATT nanocomposites were prepared, which provided prominent improvements in strength, toughness and thermal stability. High grafting efficiency of TDI on ATT surface was confirmed by FTIR spectra and SEM observations. The uniform dispersion and rod-like texture of in-situ modified ATT nanorods in the PMMA which was clearly visible in the TEM micrographes, influenced the mechanical and thermal properties of the nanocomposites. The tensile strength of nanocomposites first increased and then decreased with the in-situ modified ATT concentration ranging from 0 to 6.0%, and reached the maximum value at 3.0%. For the impact strengh, PMMA/in-situ modified ATT with 2.0% ATT had the maximum value which showed around 31% enhancement than that of pure PMMA. The chain mobility of PMMA was significantly inhibited by the uniformly dispersed fibrous nanoparticles, leading a 13.20℃increase in the glass transition temperature of PMMA/in-situ modified ATT nanocomposite containing 2.0% ATT. The thermal stability of the nanocomposites was enhanced by the presence of ATT. For example, 10% mass loss temperature of PMMA/in-situ modified ATT was 73.47℃higher than that of pristine PMMA.
引文
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[1] S.C.Tiong, et a1..Mechanical Behavior of Injection Moldedβ-Crystalline Phase Polypropylene [J]. Polym.Eng.Sci.. 1 996, 36(1): 100-105
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[5]王平华,徐国永,宋功品. PP/凹凸棒土纳米复合材料的制备与性能研究[J].工程塑料应用. 2003, 31(12): 12-15.
[6] Pan Yongzheng, Xu Yue, An Li, Lu Hongbin, Yang Yuliang, Chen Wei, Steven Nutt. Hybrid Network Structure and Mechanical Properties of Rodlike Silicate/Cyanate Ester Nanocomposites[J]. Macromolecules. 2008, 41 (23): 9245-9258.
[7] Rahma F, Fellahi S. Performance evaluation of synthesized acrylic acid grafted polypropylene within CaCO3/polypropylene composites[J]. Polymer Composites. 2000, 21(2):175-186.
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