以甲基丙烯酸甲酯(MMA)、丙烯酸丁酯(BA)及蒙脱土(MMT)为主要原料,使用悬浮聚合法制备聚合物(甲基丙烯酸甲酯.共聚-丙烯酸丁酯)/蒙脱土纳米复合微球。采用红外光谱(FTIR)、X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电镜(TEM)对所制备的复合材料微观结构进行了表征;通过热重分析(TGA)对复合材料的热稳定性进行了研究。探讨了蒙脱土含量对复合材料热稳定性及膨胀性能的影响。结果表明,聚合物/MMT纳米复合微球(蒙脱土含量为3%(质量分数))表面光滑且颗粒间团聚现象对比于纯聚合物微球明显改善,平均粒径在60~120μm;XRD分析得出钠基蒙脱土的层间距为1.21nm,十六烷基三甲基溴化铵(CTAB)离子交换改性后的有机蒙脱土层间距为1.88nm,聚合物/MMT复合材料的层间距约为3.53nm,这与TEM分析相符;纯共聚物最大质量损失温度为482℃,当蒙脱土含量为3%时,聚合物/MMT复合材料最大质量损失温度提高到505℃;在本实验条件下,纯聚合物微球在水中最后膨胀率约为250%,聚合物/MMT纳米复合微球(MMT3%)在水中最后膨胀率约为125%。岩心封堵率效果测试表明,纳米聚合物复合微球具有良好的运移能力和深部封堵性能。
The poly (MMA-co-BA)/MMT nanocomposite microspheres were prepared by suspension polymerization of methyl methacrylate ( MMA), butyl acrylate (BA) and montmorillonite (MMT). The microstructure of the composites was characterized by fourier transform infrared spectroscopy (FFIR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The thermal stability of the composites was studied by thermo-gravimetric analysis (TGA). The effect of the load- ing of MMT on the thermal stability and swelling rate of the composites was discussed. The results showed that the average volume size of the polymer/MMT composite microspheres (3.0% (mass fraction) MMT loading) was in the range of 60 to 120 μm and the polymer/MMT nanocomposite microspheres were smoother and less agglomerated than that of the pure copolymer microspheres. XRD analysis showed that the interlayer spacing was 1.21 nm for Na-MMT, 1.88 nm for CTAB-MMT and about 3.53 nm for polymer/MMT nanocomposites which was consistent with TEM results. The maximum decomposed temperature was 482 ℃ for the pure copolymer and 505 ℃ for polymer/MMT nanocomposites with montmorillonite 3%. The final swelling rate of the pure polymer microspheres was about 250% in deionized water and the final swelling rate of the polymer/MMT nanocomposite microspheres ( MMT 3% ) was about 125%. Tests of microspheres' plugging showed that nanocomposite microspheres had good migration ability and deep flooding performance in the sand tube core.