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镁铝层状双金属氢氧化物作为杀菌剂载体及其表面修饰杂化物的制备与表征
Synthesis and Characterization of Layered Double Hydroxides as Bacteridides Delivery System and Surface Modification Nanohybirds
【作者】 杨衡;
【导师】 全贞兰;
【作者基本信息】 青岛科技大学 , 物理化学, 2009, 硕士
【摘要】 层状双金属氢氧化物(LDHs)是一类带有永久正电荷的新型无机材料,层间存在可交换的阴离子,层间空间可调,可以将药物分子嵌入层间形成药物-LDHs纳米杂化物。LDHs广泛应用于催化剂、抗酸剂、废水处理、抗絮凝剂、药物载体、阴离子交换剂以及流变改性剂等领域。将不能电离、难溶于水的杀菌剂包裹到阴离子表面活性剂的胶束内,分别采用共沉淀法、结构重建法和离子交换法将带负电的胶束嵌入到LDHs层中,合成了两种杀菌剂己唑醇和三唑醇的LDHs杂化物。采用粉末X射线衍射(PXRD)、透射电镜(TEM)和傅里叶变换红外光谱(FT-IR)对杀菌剂-LDHs纳米杂化物进行表征。由X射线衍射图可知杀菌剂-LDHs的层间距比纯LDHs的层间距明显增大,并且003峰向低2θ值移动,说明带负电的胶束将通道内原有的阴离子取代。红外光谱图证明了杀菌剂-LDHs中杀菌剂的存在,成功的合成了杀菌剂-LDHs.紫外-可见分光光度(UV-Vis)检测显示杀菌剂-LDHs具有一定的缓释性能,杀菌剂-LDHs杂化物是一种有潜力的药物缓释系统。CO3-LDHs分别和柠檬酸,萘乙酸,1-羟基环己基甲酸的丙酮溶液反应,进行表面修饰。产物用粉末X射线衍射、傅里叶变换红外光谱和透射电镜进行表征。PXRD谱图显示修饰后的CO3-LDHs层间距没有增大,在红外谱图上可以观察到所修饰剂的特征基团吸收峰。TEM照片显示CO3-LDHs修饰前后粒子尺寸没有改变,修饰后的CO3-LDHs层片连接在一起,说明其表面连接上了修饰剂,证明成功制备了表面修饰的CO3-LDHs.
【Abstract】 LDHs are a family of layered inorganic materials with structurally positively charged layers and interlayer balancing anions. The anions between the interlayer can be exchanged by the other anions and the space can be adjusted. LDHs nanohybirds can be prepared by intercalate anions into interlayer space. LDHs nanocomplexes were widely applied in various aspects such as catalyst, antiacid, waste water treatment, antiflocculant agent, drug carrier, anion exchanger and rheological modification.Two bactericides-LDHs nanocomplexes hexaconazole-LDHs and triadmenol-LDHs were prepared by following procedures: bactericides that were nonionic and difficult to dissolve in water were first incorporated into micelles derived from negatively charged surfactants, and the negatively charged micelles were then intercalated in nanoparticles of LDHs by coprecipitation, ion exchange and reconstruction method respectively. The bactericides-LDHs nanohybirds were characterized by PXRD, TEM and FT-IR. The PXRD patterns indicated that the basal spacing of bactericides-LDHs was obviously larger than pristine LDHs, and 003 peak was shifted to the low 2θvalue, which indicated that the originated anions between the interlayer were replaced by the micelles containing bactericides. The successful synthesis of bactericides-LDHs were also proved by the FT-IR spectra, which indicated the existence of hexaconazole and triadimenol. The bactericides-LDHs were successfully synthesized. UV-Vis results showed that bactericides can be slowly released from the bactericides-LDHs nanohybirds, so bactericides-LDHs are a potential system in the bactericides slow release. CO3-LDHs reacted with citric acid (CA), naphthyl acetic acid (NAA) and 1-hydroxycyclohexane carboxylic acid (HCCA) dissolved in acetone respectively to prepare surface modified LDHs. The resulting complexes were characterized by PXRD, FT-IR and TEM. The results of PXRD patterns indicated that the basal spacing values of modified complexes didn’t change from the pristine CO3-LDHs. The functional groups of organic vibration modes can be observed in the FT-IR spectra. TEM images of modified CO3-LDHs indicated that the size of particals were not varied. But the particals stacked together, which indicated that organism were joined on the surface of CO3-LDHs. The surface modification CO3-LDHs were successfully prepared.
【Key words】 LAYERED DOUBLE HYDROXIDES; BACTERICIDES; HEXACONAZOLE; MICELLES;