重氮化制备钯(0)催化剂及其用于合成芳香胺研究  

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

作　　者：武安奇 刘四新 王桂平 王博[1] WU An-qi;LIU Si-xin;WANG Gui-ping;WANG Bo(College of Chemical Engineering and Technology,Hainan University,Haikou 570228,China;College of Science,Hainan University,Haikou 570228,China;Shandong Shouguang LuQing Petrochemical Co.,LTD,Bohai Chemical Industry Park,Yangkou Town,Slwuguang 262715,China)

机构地区：[1]海南大学化学工程与技术学院,海南海口570228 [2]海南大学理学院,海南海口570228 [3]山东寿光鲁清石化有限公司,山东省寿光市羊口镇渤海化工园,山东寿光262715

出　　处：《分子催化》2021年第1期40-47,I0002,共9页Journal of Molecular Catalysis(China)

基　　金：国家自然科学基金项目(21868011)。

摘　　要：以2,3-二氨基萘为配体,K_(2)PdCl_(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.A nano-catalyst(Pd-NPs) was prepared by diazotization using 2,3-diaminonaphthalene as the ligand and K_(2)PdCl_(4) 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 H_(2) 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.

关 键 词：钯纳米催化剂 重氮化反应 常温常压 芳香伯胺 

分 类 号：O643.32[理学—物理化学]