新型负载络合配体BDPPEDAEPA-TiO_2/ZrO_2及其钯催化剂的制备和表征  

The Preparation and Characterization of New Type of Support Complex Ligands ZBDPPEDAEPA/TiO_2

作　　者：陈文山[1,2] 傅相锴[1,2] 王强[1,2] 马学兵[1,2] 

机构地区：[1]西南师范大学化学化工学院 [2]西南师范大学应用化学研究所,重庆400715

出　　处：《西南师范大学学报（自然科学版）》2005年第3期500-504,共5页Journal of Southwest China Normal University(Natural Science Edition)

基　　金：重庆市重点攻关资助项目(20006213).

摘　　要：在TiO2或ZrO2粉末存在下用N,N双二苯膦甲基乙二胺N乙基膦酸BDPPEDAEPA,NAH2PO4与ZrOCl2反应,制得了包膜在TiO2或ZrO2表面的(N,N双二苯膦甲基乙二胺N乙基膦酸磷酸氢)锆负载络合配体ZBDP PEDAEPA/TiO2Ⅱa和ZBDPPEDAEPA/ZrO2Ⅱb及其相应的钯催化剂ZBDPPEDAEPA Pd/TiO2Ⅲa,ZBDPPE DAEPA Pd/ZrO2Ⅲb.用IR,TG DSC,XPS和粒径分析进行了表征.Ⅱa的表面属于混合磷酸双金属盐固载型配体,包膜前后钛白粉TiO2与配体Ⅱa的平均粒径增加约0.1μm,平均包膜厚度约为50nm.这可能就是相应的钯催化剂活性高的主要原因.At the present of TiO_2 or ZrO_2 powders, the support complexe ligands ZBDPPEDA EPA/TiO_2Ⅱa and ZBDPPEDAEPA/ZrO_2 Ⅱb which were TiO_2 or ZrO_2 powder coated with zirconium [N, N-bis(diphenylphosphinomethyl)-ethylenediamine-N'-ethylphophonate-phosphate] were prepared with the reaction of N, N-bis(diphenylphosphinomethyl)-ethylenediamine-N'-ethylphophonic acid BDPP EDAEPA, NAH_2PO_4 and ZrOCl_2, and their corresponding palladium catalysts ZBDPPEDAEPA-Pd/TiO_2 Ⅲa and ZBDPPEDAEPA-Pd/ ZrO_2 Ⅲb were also prepared. All the support complexes ligands and corresponding palladium catalysts were characterized by means of IR, TG-DSC, XPS and particle grading analysis. The surface of the Ⅱa particle is made of double-metal (phosphonate-phosphate) solid ligands. The average particle size of Ⅱa is increased about 0.1 μm compared with the Titanium White TiO_2 coated before the reaction. That means the average thickness coated on the ligands Ⅱa is near to 50 nm. This may be the main reasons of activity for the palladium catalyst Ⅲa higher than Ⅲb.

关 键 词：N N-双二苯膦甲基-乙二胺-N′-乙基膦酸 (N N双二苯膦甲基乙二胺-N′-乙基膦酸-磷酸氢)锆 二氧化钛 包膜 粒径分析 

分 类 号：O643.32[理学—物理化学]