Al_2O_3负载钯催化剂的制备及催化Suzuki偶联反应的研究

采用浸渍-还原法制备三氧化二铝负载钯催化剂（Pd/Al2O3）,通过ICP-AES、XRD、XPS等分析手段对催化剂的结构和组成进行了表征。考察了溶剂、溶剂与水的比例、碱的种类、反应温度以及反应时间等反应条件对上述制备的催化剂催化Suzuki偶联反应的影响,筛选出最适宜的反应条件。实验结果表明,在1mmol对溴苯乙酮,1.5mmol苯硼酸,2mmol碳酸钾,乙醇∶水=6∶6,反应温度为60℃,反应时间为60min,催化剂加入量为3.5×10-3mmol钯的反应条件下,Suzuki反应收率可达97%以上。

Preparation of Al2O3 Supported Palladium Catalyst and Its Research on Suzuki Coupling Reaction

Al_2O_3 supported palladium catalysts （Pd/Al_2O_3） were prepared via the impregnation-reduction method. The structure and composition of above-prepared catalysts were characterized by X-ray diffraction（XRD）, inductively coupled plasma-atomic emission spectrometry（ICP-AES）and X-ray photoelectron spectroscopy （XPS）. The influences of reaction conditions, suchas species of solvents and the bases, the ratio of the solvents to water, the reaction temperature and time on Suzuki coupling reaction over Pd/Al_2O_3 were investigated. The optimal conditions were confirmed through the results of Suzuki coupling reaction as follows： K2CO3 was 2mmol, ethanol/H2Owas 6/6, Pd adding amount was 3.5x10^-3mmol and the temperature was 60℃, and the reaction yield for lh could reach more than 97%.