An efficient Suzuki cross-coupling reaction under continuous flow conditions was developed utilizing an immobilized solid supported catalyst consisting of bimetallic nickel–palladium nanoparticles (Ni–Pd/MWCNTs). In this process, the reactants can be continuously pumped into a catalyst bed at a high flow rate of 0.6 mL/min and the temperature of 130 °C while the Suzuki products are recovered in high steady-state yields for prolonged continuous processing. The catalyst was prepared by mechanical shaking of the appropriate nickel and palladium salts using ball-mill energy without the requirement of any solvent or reducing agent. This straightforward, facile, and simple method allows for bulk production of Ni–Pd/MWCNTs nanoparticles with a small particle size ideal for application in continuous flow cross-coupling catalysis. The as-prepared catalyst mostly contains nickel (7.9%) with a very small amount of palladium (0.81%) according to ICP-OES analysis. This remarkable immobilized catalyst can be used several times for different Suzuki reactions with a minimum loss of reactivity and no detectable leaching of the metal nanoparticles. Notably, by modifying the groups on both aryl halides and phenylboronic acids, the method provides access to a diverse array of the Suzuki products in flow with high steady-state yield, making it suitable for applications in industrial and pharmaceutical scales. Moreover, several spectroscopic techniques were employed to identify the structure and composition of the as-prepared Ni–Pd/MWCNTs nanoparticles before and after the reaction in flow such as transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), BET surface area (physisorption), and FTIR spectroscopy.

中文翻译：

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多壁碳纳米管上负载的双金属镍-钯纳米颗粒用于连续流中的 Suzuki 交叉偶联反应


利用由双金属镍-钯纳米颗粒 （Ni-Pd/MWCNTs） 组成的固定化固体负载催化剂，开发了一种在连续流动条件下的高效 Suzuki 交叉偶联反应。在该工艺中，反应物可以以 0.6 mL/min 的高流速和 130 °C 的温度连续泵入催化剂床，同时以高稳态产率回收 Suzuki 产品，以进行长时间的连续加工。催化剂是通过使用球磨机能量机械振荡适当的镍盐和钯盐来制备的，无需任何溶剂或还原剂。这种简单明了的方法允许批量生产小粒径的 Ni-Pd/MWCNTs 纳米颗粒，非常适合连续流交叉偶联催化。根据 ICP-OES 分析，所制备的催化剂主要含有镍 （7.9%） 和极少量的钯 （0.81%）。这种卓越的固定化催化剂可以多次用于不同的 Suzuki 反应，反应性损失最小，并且金属纳米颗粒没有可检测的浸出。值得注意的是，通过修饰芳基卤化物和苯硼酸上的基团，该方法以高稳态产率获得流动中的各种 Suzuki 产品，使其适用于工业和制药规模的应用。此外，采用多种光谱技术来识别所制备的 Ni-Pd/MWCNTs 纳米颗粒在流动反应前后的结构和组成，例如透射电子显微镜 （TEM）、X 射线衍射 （XRD）、X 射线光电子能谱 （XPS）、热重分析 （TGA）、BET 表面积（物理吸附）和 FTIR 光谱。