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Preparation of polypropylene/Mg–Al layered double hydroxides nanocomposites through wet pan-milling: formation of a second-staging structure in LDHs intercalates

机译:通过湿盘磨制备聚丙烯/ Mg-Al层状双氢氧化物纳米复合材料:LDHs插层中形成第二阶段结构

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In this paper, polypropylene/MgAl-layered double hydroxide nanocomposites were in situ prepared by using a novel solid state shear milling (S3M) technology without use of any compatibilizer and any prior organic treatment of raw LDHs. The obtained composite powders and nanocomposites were characterized using X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. The results show that under the very strong shear force field of pan-milling, the anion-exchange reaction of CO32?-LDHs with sodium dodecyl sulfate (SDS) can be realized under non-acidic conditions. In addition, the in situ modification of LDHs with SDS and the co-intercalation of PP macromolecular chains into LDH interlayers were found to be completed in one process in aqueous medium. XRD results demonstrate that there are two types of layered structures in the prepared PP/LDHs co-powders and the occurrence of the transformation from layered structure I to II with increasing milling cycles and SDS loading. Staging is proposed to illustrate the anion-exchange reaction of intercalation of the SDS anion into CO32?-LDH layers and the corresponding transformation, showing the second stage intermediate corresponding to layered structure I and the first stage product corresponding to structure II. Both XRD analysis and TEM observation show the formation of exfoliated LDH layers at low LDH loading and concomitant intercalated/exfoliated LDH layers at high LDH loading in the prepared PP/LDHs nanocomposites. The dynamic mechanical properties and crystallization behavior of the obtained nanocomposites were also investigated using dynamic mechanical analysis (DMA) and differential scanning calorimetry (DSC), respectively.
机译:本文采用新型固态剪切研磨法(S 3 M)原位制备聚丙烯/ MgAl层状双氢氧化物纳米复合材料。技术,无需使用任何增容剂,也无需事先对原始LDH进行有机处理。分别使用X射线衍射(XRD),傅立叶变换红外光谱(FT-IR),扫描电子显微镜(SEM)和透射电子显微镜(TEM)对获得的复合粉末和纳米复合材料进行表征。结果表明,在很强的碾磨剪切力场下,CO 3 2?的阴离子交换反应具有十二烷基硫酸钠(SDS)的 -LDHs可以在非酸性条件下实现。另外,发现LDHs用SDS的原位修饰和PP大分子链共插入LDH中间层中的过程是在水性介质中的一个过程中完成的。 XRD结果表明,制备的PP / LDHs共粉中存在两种类型的层状结构,并且随着研磨周期和SDS负载的增加,发生了从层状结构I到II的转变。提出了分期来说明SDS阴离子嵌入CO 3 2? -中的阴离子交换反应LDH层和相应的转换,显示对应于分层结构I的第二阶段中间体和对应于结构II的第一阶段产物。 XRD分析和TEM观察均表明,在制备的PP / LDHs纳米复合材料中,低LDH负载下剥落的LDH层的形成以及高LDH负载下伴随的嵌入/剥落的LDH层。还分别使用动态力学分析(DMA)和差示扫描量热法(DSC)研究了获得的纳米复合材料的动态力学性能和结晶行为。

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