Patil Aniruddha B, Bhanage Bhalchandra M
Department of Chemistry, Institute of Chemical Technology, Autonomous, N. M. Parekh Marg, Matunga, Mumbai 400019, India.
J Nanosci Nanotechnol. 2013 Jul;13(7):5061-8. doi: 10.1166/jnn.2013.7583.
Present work reports a novel one step, greener protocol for the synthesis of starch-stabilized palladium nanoparticles (PdNPs) with an average particle diameter of 30-40 nm. These particles were stable and uniform in size. In present protocol, the concentrated solar energy mediated reduction of palladium chloride was achieved by using citric acid as a reducing agent and starch as a capping agent. UV-Visible spectroscopy, Transmission Electron Microscopy, Field Emission Gun-Scanning Electron Microscopy, Selected Area Electron Diffraction and Electron dispersive X-ray Spectral analysis techniques were used to characterize this starch capped PdNPs. Herein; we are reporting such combination of starch and citric acid in the synthesis of PdNPs for the first time. The catalytic activity of synthesized nanoparticles has been checked for Suzuki and Heck cross coupling reactions. The product yield was confirmed by GC. The products were confirmed using GC-MS analysis and also using GC with the help of authentic standards. Solar energy assisted starch stabilized PdNPs showed excellent activity in the C-C bond formation between aryl halides (I, Br) with phenyl boronic acid and its derivatives. In addition, the catalyst showed good activity in the Heck coupling reaction of C-C bond formation of aryl halides with aromatic alkene. The use of starch, citric acid, water and solar energy makes present protocol greener.
目前的工作报道了一种新颖的一步法、更环保的合成淀粉稳定钯纳米颗粒(PdNPs)的方法,其平均粒径为30-40纳米。这些颗粒尺寸稳定且均匀。在目前的方法中,通过使用柠檬酸作为还原剂和淀粉作为封端剂,实现了浓缩太阳能介导的氯化钯还原。采用紫外可见光谱、透射电子显微镜、场发射枪扫描电子显微镜、选区电子衍射和电子色散X射线光谱分析技术对这种淀粉包覆的PdNPs进行表征。在此,我们首次报道了淀粉和柠檬酸在合成PdNPs中的这种组合。已对合成的纳米颗粒在铃木和赫克交叉偶联反应中的催化活性进行了检测。产物产率通过气相色谱法确认。产物通过气相色谱-质谱联用分析以及借助标准品的气相色谱法进行确认。太阳能辅助淀粉稳定的PdNPs在芳基卤化物(I、Br)与苯硼酸及其衍生物之间的碳-碳键形成中表现出优异的活性。此外,该催化剂在芳基卤化物与芳香烯烃的碳-碳键形成的赫克偶联反应中表现出良好的活性。淀粉、柠檬酸、水和太阳能的使用使目前的方法更环保。