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插层型偶氮二甲酰胺/蒙脱土纳米复合材料的研制

The Study of the Intercalated Azodicarbonamide-Montmorillonite Nanocomposites

【作者】 王丽

【导师】 郭灿雄;

【作者基本信息】 北京化工大学 , 应用化学, 2009, 硕士

【摘要】 本文根据蒙脱土的特性,以二甲基亚砜(DMSO)/H2O为复合分散剂,通过对实验条件的摸索,采用溶液插层法,成功将偶氮二甲酰胺(AC)插层进入了蒙脱土(MMT)的纳米层间,制备得到了新型的插层型纳米复合发泡剂AC-MMT。并采用X射线衍射(XRD)、固体核磁共振(NMR)、傅里叶红外光谱(FT-IR)、热重(TG)和差示扫描量热法(DSC)等手段对新材料进行了表征分析。各表征结果证明AC插入了MMT层间,并与蒙脱土层板内羟基发生了氢键作用。XRD结果表明插层后,蒙脱土的层板间距由1.25nm增加至1.90nm;在固体核磁谱中,13C的化学位移从159.4ppm向低场移动至161.2ppm;红外谱图中AC的羰基吸收峰从1728cm-1红移至1688cm-1,-NH2的伸缩振动和弯曲振动吸收分别从3332cm-1,3182cm-1和1486cm-1蓝移至3397cm-1,3305cm-1和1509cm-1。此外一个新的吸收峰出现在3208cm-1,这可能是由于-NH2与MMT内羟基形成了弱的氢键作用,进一步证实了AC成功插层进入了蒙脱土层间。AC-MMT的TG-DSC表征结果,说明新复合材料中有机物的含量为30.8%,且AC-MMT的热分解温度比纯AC的分解温度提高。此外,研究了制备条件对插层结果的影响,得到了制备AC-MMT的最佳条件:pH=9,温度为60℃,复合分散剂DMSO/H2O中含水量为40%。

【Abstract】 Based on the properties of MMT, the novel intercalated nanocomposite AC-MMT was prepared by intercalating azodicarbonamide (AC) into the nano layers of MMT by solution intercalation method in the DMSO/H2O dispersant solvent. The nanocomposite was characterized by means of XRD, solid state NMR, FT-IR and TG-DSC. The results suggested that AC was intercalated into the nano layers of MMT and hydrogen bond was formed between the NH2 of AC and the inner hydroxyls of MMT. The intercalation of AC was confirmed by the increase in basal spacing of montmorillonite from 1.25 to 1.90 run. The 13C chemical shift of the carbonyl of AC-MMT was shifted from 159.4 ppm in AC to 161.2 ppm after the intercalation. In IR spectra, the characteristic carbonyl absorption band of AC was shifted from 1728 to 1688 cm-1. The strentching and bending vibrations of -NH2 were shifted from 3332cm-1, 3182cm-1 and 1486cm-1 to 3397cm-1, 3305cm-1 and 1509cm-1 separately. A new absorption was observed at 3208cm-1, which was due to the hydrogen bond between -NH2 and the hydroxyl of MMT. These further confirmed that AC was intercalated into the nano layers of MMT. The decomposition temperatures were higher than those of pure AC and the amount of intercalated organic substance was 30.8%. In addition, the optimized condition of preparing AC-MMT was pH=9, 60℃and 40% water content in DMSO/H2O dispersant solvent.

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