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首页> 外文期刊>Journal of Materials Chemistry, A. Materials for energy and sustainability >Water compatible Pd nanoparticle catalysts supported on microporous polymers: their controllable microstructure and extremely low Pd-leaching behaviour
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Water compatible Pd nanoparticle catalysts supported on microporous polymers: their controllable microstructure and extremely low Pd-leaching behaviour

机译：负载在微孔聚合物上的与水相容的Pd纳米颗粒催化剂：可控的微观结构和极低的Pd浸出行为

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This paper reports on fabrication of water-compatible palladium nanoparticle (PdNP) catalysts supported on microporous polymers, which show high activity and extremely low Pd leaching behaviour in the usage for carbon cross-coupling reactions. The supported PdNP catalysts were fabricated by utilizing the polymerization-induced phase separation (PIPS) method. An outstanding point of the present study is to use a small molecule ligand monomer (D-m) based on A/,/V-dimethyl ethylenediamine, instead of the PAMAM dendrimer-based monomer used previously having integrated ligand sites. When D-m that had been complexed with Pd~(2+) was copolymerized with excess 1,6-hexanediol dimethacrylate (HX) in the PIPS setup, a highly active catalytic polymer (D-HX) having extremely low Pd leaching characteristics was successfully obtained. The TEM images of D-HX revealed that the created PdlMPs were small with a diameter of mainly ca. 5,0 nm. Catalytic performances of D-HX were investigated for a heterogeneous Suzuki-Miyaura reaction in water. In the presence of 10~(-2) molar equiv. of the polymer, the reaction efficiently proceeded at 80 °C and gave the desired product in ca. 90% yield after 2 h. D-HX could be easily recovered by simple filtration and reused with only a minimal loss of activity. Intriguingly, the hot filtration test indicated that nearly no Pd species was thermally released from D-HX, which is in large contrast with the results of other polymers tested herein leading to a lot of Pd leaching. Through this study, it was demonstrated that the microscopic structure of the polymer supports could be well-controlled by changing the structure of monomers and it was closely related to the Pd leaching behaviour of the present heterogeneous catalysis systems.
机译：本文报道了在微孔聚合物上负载的水相容性钯纳米粒子（PdNP）催化剂的制备，该催化剂在用于碳交叉偶联反应中显示出高活性和极低的Pd浸出行为。利用聚合诱导相分离（PIPS）方法制备了负载型PdNP催化剂。本研究的突出点是使用基于A /，V-二甲基乙二胺的小分子配体单体（D-m），而不是以前使用的具有集成配体位点的基于PAMAM树枝状聚合物的单体。当在PIPS装置中将已与Pd〜（2+）络合的Dm与过量的1,6-己二醇二甲基丙烯酸酯（HX）共聚时，成功获得了具有极低Pd浸出特性的高活性催化聚合物（D-HX）。 。 D-HX的TEM图像表明，所创建的PdlMPs很小，直径主要为ca。 5,0海里研究了D-HX在水中的非均相铃木-宫浦反应的催化性能。在10〜（-2）摩尔当量的存在下在约80℃下，反应有效地进行，并在约2℃得到所需产物。 2小时后产率为90％。 D-HX可以通过简单的过滤很容易地回收，并且只需很少的活性损失就可以重复使用。有趣的是，热过滤测试表明几乎没有Pd物质从D-HX中热释放，这与本文测试的其他聚合物的结果形成了鲜明的对比，导致大量Pd浸出。通过这项研究，证明了通过改变单体的结构可以很好地控制聚合物载体的微观结构，并且它与当前非均相催化体系的Pd浸出行为密切相关。

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