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Preparation and characterization of polystyrene/TiO_2 core-shell nanospheres via suspension technique

机译:悬浮技术的制备与表征聚苯乙烯/ TiO_2核 - 壳纳米球

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In the present work, at first, nano-TiO_2 particles in anatase form were effectively surface modified via reacting with NCO groups of 4,4'-methylenediphenyl disocyanate (MDI). Secondly, a solution of azobisisobutyronitrile (AIBN) (0.1 g) in inhibitor-free styrene (10 g) was poured into a 150 mL flask containing poly (vinyl alcohol) (PVA) suspending agent (0.1 g) in deionized water (60 mL) under N_2 flow, while stirring. The reaction mixture was then heated to 80°C, and stirred for another 1 h. Next, it was divided to two portions; one for the synthesis of pure PS, and the other for the synthesis of PS/TiO_2 nanocomposites. Each aqueous portion was individually mixed with dichloromethane in a separating funnel. For PS/TiO_2 nanocomposites, the organic phase was charged with nano-TiO_2 particles (MDI-treated and/or untreated) (0.05 g), and then fully homogenized using ultrasonic homogenizer. Methanol non solvent was eventually used to precipitate the products. All samples involving pure PS, PS/surface modified TiO_2 nanocomposite, and PS/surface unmodified TiO_2 nanocomposite were thoroughly washed, filtered, and dried in vacuum at 50°C for 12 h. From SEM images a core-shell relation could be clearly detected between the nano-TiO_2 particles and PS matrix. Meanwhile, the surface modified TiO_2 was dispersed into the PS matrix with better homogeneity compared to that of unmodified one. Undoubtedly, beside the surface modification factor, PVA suspending agent as an effective nanosized particle stabilizer, too, played a basic role in this high homogeneity. Also, FT-IR and XRD analyses led to promising results.
机译:在目前的工作中,首先,纳米的TiO_2在锐钛矿型的颗粒有效地进行表面通过与4,4'-亚甲基disocyanate(MDI)的NCO基团反应改性。其次,偶氮二异丁腈(AIBN)(0.1克)在不含抑制剂的苯乙烯(10克)中的溶液倒入一个150毫升烧瓶含聚(乙烯醇)(PVA)在去离子水(悬浮剂(0.1克)60毫升)N_2下流动,同时搅拌。然后将反应混合物加热至80℃,并再搅拌1个小时。接着,它被划分到两个部分;一个用于纯PS的合成,以及另一个用于PS /纳米复合材料的TiO_2的合成。各水相部分分别与在分液漏斗二氯甲烷混合。对于PS /纳米复合材料的TiO_2,将有机相加入纳米颗粒的TiO_2(MDI处理的和/或未经处理的)(0.05克),并且然后使用超声波均化器充分均化。最终使用甲醇非溶剂以沉淀产品。所有涉及纯PS样本,PS /表面改性的TiO_2纳米复合材料,和PS /表面未改性的纳米复合材料的TiO_2彻底洗涤,过滤,并在50℃下12小时真空干燥。从SEM图像可以在纳米颗粒的TiO_2和PS基质之间清楚地检测的核 - 壳关系。同时,表面改性的TiO_2分散到具有更好的均匀性的PS基质相比,未经修饰的一种制成。无疑,表面改性因子旁,PVA悬浮剂作为有效纳米颗粒稳定剂也是如此,在这种高均匀性方面发挥了基本的作用。另外,FT-IR和XRD分析导致了可喜的成果。

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