重氮化制备钯(0)催化剂及其用于合成芳香胺研究

以2,3-二氨基萘为配体,K_2PdCl_4为金属前驱体,经重氮化制备出一种Pd(0)纳米催化剂(Pd-NPs),其结构经TEM、 XPS、 XRD、 EA和ICP-OES表征,并将催化剂应用于芳香醛类化合物直接还原胺化反应中.在常温常压下以苯甲醛为底物,水为溶剂,H_2为还原剂,探究了胺源、溶剂pH、催化剂用量、反应时间等变量对芳香伯胺产率的影响.实验结果表明芳香伯胺产率高达99%,且该催化剂能多次使用而不失活.

Study on Preparation of Palladium (0) Catalyst by Diazotization and its Application in Synthesis of Aromatic Amines

A nano-catalyst (Pd-NPs) was prepared by diazotization using 2,3-diaminonaphthalene as the ligand and K2PdCl4 as the metal precursor. Its structure was characterized by TEM, XPS, XRD, EA and ICP-OES. Then the catalyst was used in the direct reductive amination reaction of aromatic aldehyde compounds. Using benzaldehyde as substrate, water as solvent and H2 as reducing agent under normal temperature and pressure, the influence of variables such as amine source, the solvent pH, the amount of catalyst, and the reaction time were investigated. The results showed that the yield of aromatic primary amines was up to 99%. The catalyst could be used for many times without deactivation.