Easily scalable synthesis of Ni nanosols suitable for the hydrogenation of 4-nitrophenol to p-aminophenol under mild condition
Easily scalable synthesis of Ni nanosols suitable for the hydrogenation of 4-nitrophenol to p-aminophenol under mild condition
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DOI：
10.1016/j.cej.2012.11.013
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发表时间：
2013-01-15
影响因子：
15.1
通讯作者：
Sanson, A.
中科院分区：
文献类型：
--
作者：
Blosi, M.;Albonetti, S.;Sanson, A.
采用微波辅助多元醇法合成了尺寸在80 ~ 200 nm之间的镍纳米粒子。该反应在二元螯合剂体系（聚乙烯吡咯烷酮PVP和十二烷基胺DDA）存在下在二甘醇（DEG）中在200 ℃下进行，以获得稳定且高度浓缩的纳米溶胶，其比例被仔细优化。制备稳定的悬浮液具有改善固体氧化物燃料电池（SOFC）阳极层性能的前景，其中金属用作催化剂。研究了不同反应时间对最终产物的影响，可以确定反应路径，该反应路径在10 min后形成结晶的乙醇酸镍，20 min后完全变成结晶的金属镍。通过XRD，TG-DTA，FT-IR，TEM对所得Ni纳米颗粒进行了表征。以NaBH_4为探针，研究了4-硝基苯酚（4-NP）加氢合成对氨基苯酚（4-AP）的反应，并通过循环伏安法计算了其电化学活性表面积（A（ECSA）），对其催化活性和电化学活性进行了初步测试。(C)2012 Elsevier B. V.保留所有权利。
Ni nanoparticles with a dimension ranging between 80 and 200 nm were synthesized by a microwave-assisted polyol route. The reaction was carried out at 200 degrees C in diethylenglycol (DEG) in the presence of a binary chelating agent system (polyvinylpyrrolidone PVP and dodecylamine DDA), in order to obtain stable and highly concentrated nanosols whose ratio was carefully optimized. Stable suspensions were produced with the future prospect of improving the performance of the anodic layer in solid oxide fuel cells (SOFCs), in which the metal is employed as catalyst. Studying the influence of different reaction times on the final product, it was possible to identify the reaction path that goes through the formation, after 10 min, of crystalline Ni-glycolate that turns completely into crystalline Ni metal after 20 min. The as obtained Ni nanoparticles were characterized by XRD, TG-DTA, FT-IR, TEM. Preliminary tests on their catalytic and electrochemical activities were carried out by studying the hydrogenation of 4-nitrophenol (4-NP) to p-aminophenol (4-AP) in the presence of NaBH4 as probe reaction and by calculating the electrochemically active surface area (A(ECSA)) with cyclic voltammetry. (C) 2012 Elsevier B.V. All rights reserved.