球壳形3,3′-二氨基-4,4′-氧化偶氮呋咱的限域自组装及热行为研究
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摘要
基于限域自组装技术,采用溶剂非溶剂法制备了一种结构奇异的高品质球壳形3,3′-二氨基-4,4′-氧化偶氮呋咱(DAOAF),研究了不同表面活性剂和搅拌速度对DAOAF晶体形貌的影响,通过扫描电镜(SEM)表征了球壳形DAOAF的形貌,提出其限域自组装的机理:聚乙烯吡咯烷酮(PVP)在水中通过搅拌形成球形胶束,DAOAF晶粒在胶束表面的区域内聚集形成氢键,最终自组装为球壳形DAOAF。利用X射线衍射(XRD)分析了球壳形DAOAF的晶体结构;通过高效液相色谱(HPLC)分析了球壳形DAOAF的纯度;由差示扫描热量法(DSC)研究了其热分解行为。结果表明:在水中加入PVP,搅拌速度控制在280r/min,可获得粒径分布在5～20μm、球壳厚度为8μm、纯度为98.86%、表面光滑且边缘整齐的球壳形DAOAF。相比于原料DAOAF,球壳形DAOAF的热分解表观活化能降低了10.76 kJ/mol。
Based on contained self-assemble technology,spherical shell structure of DAOAF was obtained by a solvent anti-solvent method and the effects of different surfactants and stirring speed on the morphology of DAOAF crystals were studied. SEM was employed to characterize different morphologies of DAOAF and the formation mechanism was discussed. The spherical micelles were formed by proper stirring of PVP in water, then DAOAF crystalline grains aggregated on the surface of the micelles to form hydrogen bonds, finally the grains self-assembled into spherical shell structure. XRD, HPLC and DSC were used to analyze the crystal structure, purity and the thermal decomposition behavior of the product, respectively. The results show that the confined self-assemble spherical shell structure of DAOAF with the particle size distribution of 5～20μm, an average of 8μm thickness, the purity of 98.86%, smooth surface and neat edge can be prepared by adding PVP as a surfactant into water with stirring speed 280 ppm. Compared with raw DAOAF, the apparent activation energy of the as-prepared DAOAF has reduced by 10.76 kJ/mol.
Based on contained self-assemble technology,spherical shell structure of DAOAF was obtained by a solvent anti-solvent method and the effects of different surfactants and stirring speed on the morphology of DAOAF crystals were studied. SEM was employed to characterize different morphologies of DAOAF and the formation mechanism was discussed. The spherical micelles were formed by proper stirring of PVP in water, then DAOAF crystalline grains aggregated on the surface of the micelles to form hydrogen bonds, finally the grains self-assembled into spherical shell structure. XRD, HPLC and DSC were used to analyze the crystal structure, purity and the thermal decomposition behavior of the product, respectively. The results show that the confined self-assemble spherical shell structure of DAOAF with the particle size distribution of 5～20μm, an average of 8μm thickness, the purity of 98.86%, smooth surface and neat edge can be prepared by adding PVP as a surfactant into water with stirring speed 280 ppm. Compared with raw DAOAF, the apparent activation energy of the as-prepared DAOAF has reduced by 10.76 kJ/mol.
引文
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