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采用一种简单的原位塌陷自组装法利用高锰酸钾(KMnO4)和油酸(OA)在O/W乳液界面上发生的“Baeyer test for unsaturation”反应,用乙醚作为共溶剂来制备氧化锰纳米结构.与之前相比,加入乙醚(EE)最大的优点是减少了反应过程中油酸的用量,大大简化了产品的洗涤过程,降低了制备成本.得到的产品分别用SEM,TEM和XRD进行了表征.产品的形貌和尺寸可以通过调控OA/乙醚体积比,KMnO4/OA物质的量比,油相/水相体积比和反应温度来实现.当OA/乙醚的体积比在10∶0～3∶7之间,KMnO4/OA物质的量比小于1∶1,或油相/水相体积比小于2∶45时,得到的产品形貌为蜂窝状;当OA/乙醚体积比低于3∶7,KMnO4/OA物质的量比大于0.67∶1,或油相/水相体积比大于2∶75时,得到的产品形貌为片状结构;当反应温度从25℃升高到33℃,产品的形貌、结构和尺寸变化不大,继续升高到45℃时,颗粒中的纳米片数量有所减少.依据所得的结果推断反应是通过一个纳米片不断塌陷的过程形成的.
A simple method of in-situ collapse self-assembly was developed using the “Baeyer test for unsaturation” reaction at the O / W emulsion interface with potassium permanganate (KMnO4) and oleic acid (OA) Compared with the former, the biggest advantage of adding diethyl ether (EE) is to reduce the amount of oleic acid during the reaction, greatly simplifying the washing process of the product and reducing the preparation cost.The obtained products were respectively analyzed by SEM, TEM And XRD.The morphology and size of the product can be controlled by the volume ratio of OA / ether, the ratio of KMnO4 / OA, the volume ratio of oil / water phase and the reaction temperature.When the volume ratio of OA / 10: 0 ~ 3: 7, the ratio of KMnO4 / OA is less than 1: 1, or the volume ratio of oil / water is less than 2:45, the product morphology is honeycomb; Less than 3: 7, the ratio of KMnO4 / OA is greater than 0.67: 1, or the volume ratio of oil / water is greater than 2:75, the morphology of the product is flaky. When the reaction temperature rises from 25 ℃ As high as 33 ° C, the morphology, structure and size of the product did not change much, and continue to increase to 45 ° C, the number of nano-particles in the particles decreased The results obtained by a reaction inference process continued collapse nanosheet form.