Preparation of Pd/MIL-100 by bi-solvent impregnation method and its application in Suzuki-coupling reaction
LI Qian-fan1,2, LI Tie-fu1,2, LIU Ying-ya1,2, SUN Zhi-chao1,2, YU Zhi-quan1,2, WANG Yao1, WANG An-jie1,2
1. School of Chemical Engineering, Dalian University of technology, Dalian 116024, China; 2. State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116024, China
Abstract: MIL-100(Cr) is synthesized through solvothermal method,and used to support Pd nanoparticles through a double-solvent impregnation method to prepare Pd/MIL-100,a supported catalyst.Taking the coupling reaction of bromobenzene and phenylboronic acid to synthesize biphenyl as a model reaction,the effects of solvents,base auxiliary,substrate concentration,temperature as well as catalyst dosage on the catalytic activity of the prepared catalyst in Suzuki coupling reaction are investigated.The conversion rate of bromobenzene reaches 97% and the selectivity of biphenyl exceeds 99% when EtOH/H2O (2∶1) is used as solvent,K2CO3 as base auxiliary,and the reaction has performed for 30 min at 60℃.Moreover,Pd/MIL-100 catalyst shows a good substrate applicability for a series of aryl boronic acids by para- and meta-substituted electron donor groups.Recycling experiments show that Pd/MIL-100 catalyst maintains good catalytic activity and stability after 3 consecutive runs.The deactivation mechanism for the catalyst is analyzed by means of XRD,XPS,ICP and TEM.It is discovered that the migration and aggregation of Pd nanoparticles on the surface of MIL-100 is the main reason for the deactivation.
李千帆, 李铁夫, 刘颖雅, 孙志超, 遇治权, 王瑶, 王安杰. 双溶剂法制备Pd/MIL-100及其催化Suzuki偶联反应的研究[J]. 现代化工, 2023, 43(2): 86-91,97.
LI Qian-fan, LI Tie-fu, LIU Ying-ya, SUN Zhi-chao, YU Zhi-quan, WANG Yao, WANG An-jie. Preparation of Pd/MIL-100 by bi-solvent impregnation method and its application in Suzuki-coupling reaction. Modern Chemical Industry, 2023, 43(2): 86-91,97.
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