Microflow reactor synthesis of palladium nanoparticles stabilized with poly(benzyl ether) dendron ligands
Microflow reactor synthesis of palladium nanoparticles stabilized with poly(benzyl ether) dendron ligands
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DOI：
10.1007/s11051-009-9645-7
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发表时间：
2010-03
影响因子：
2.5
通讯作者：
K. Torigoe;Yohsuke Watanabe;T. Endo;K. Sakai;H. Sakai;M. Abe
中科院分区：
文献类型：
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作者：
K. Torigoe;Yohsuke Watanabe;T. Endo;K. Sakai;H. Sakai;M. Abe
在一个简单的玻璃毛细管微流反应器系统中，以聚苄基醚树枝状配体（PBEDGn-NH 2，n= 1-3）为稳定剂，乙酸钯（Pd（OAc）2）在二苯醚中热分解合成了钯纳米粒子。考察了流体动力学参数（毛细管直径、线性流速、体积流速和反应温度）和浓度（前驱体和稳定剂）对粒径的影响。颗粒尺寸可以通过改变线性流速和温度以及配体/前体浓度比来控制。对于不同的毛细管直径（150-320 μm），当线性流速保持恒定时，体积流速不影响粒度。与分批系统不同，在该微反应器系统中，当配体与金属前体的摩尔比在1至5的范围内时，在低配体浓度下产生较小的颗粒。作为微反应器合成的另一个特征，Pd前体的浓度可以增加（高达27 mM），同时保持恒定的粒度（3.1 ± 0.2 nm）和良好的单分散性，而在分批系统中，随着前体浓度的增加，观察到粒度的显著增加和加宽。
A simple glass capillary microflow reactor system has been applied for the synthesis of palladium nanoparticles by thermal decomposition of palladium acetate (Pd(OAc)2) in diphenyl ether in the presence of poly(benzyl ether) dendron ligands (PBED Gn-NH2,n= 1–3) as a stabilizer. Effect of hydrodynamic parameters (capillary diameter, linear flow rate, volume flow rate, and reaction temperature) and concentrations (precursor and stabilizer) on the particle size was investigated. The particle size can be controlled by varying linear flow rate and temperature as well as ligand/precursor concentration ratio. Volume flow rate does not affect the particle size when the linear flow rate is held constant for different capillary diameters (150–320 μm). Unlike batch systems, in this microreactor system, smaller particles are produced at low ligand concentrations when the molar ratio of the ligand to metal precursor ranged from 1 to 5. As another characteristic of the microreactor synthesis, the concentration of the Pd precursor can be increased (up to 27 mM) with maintaining a constant particle size (3.1 ± 0.2 nm) and a good monodispersity, while in the batch system a significant increase and broadening in the particle size are observed with increasing precursor concentration.