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Pd catalysts supported on hydrogen titanate nanotubes for Suzuki-Miyaura cross-coupling reactions
Catalysis Today ( IF 5.2 ) Pub Date : 2017-10-16 , DOI: 10.1016/j.cattod.2017.10.015
Mark E. Martínez-Klimov , Patricia Hernández-Hipólito , Marcos Martínez-García , Tatiana E. Klimova

Palladium catalysts supported on hydrogen titanate nanotubes (HTN) were prepared by impregnation of palladium(II) acetate, characterized by N2 physisorption, powder X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy and tested in the Suzuki-Miyaura cross-coupling reactions between 4-bromobenzaldehyde and phenylboronic acid (reaction 1) or 4-hydroxyphenylboronic acid (reaction 2). The aim of this work was to determine the activity of these catalysts in the Suzuki-Miyaura reactions and the possibility of their reusing in several catalytic cycles. The results showed that 3.6 wt.% of Pd was the optimum metal loading in the Pd(x)/HTN catalysts. The Pd(3.6)/HTN catalyst resulted in 97 and 88% yields of biphenyl products in the cross-coupling reactions 1 and 2, respectively, and its activity decreased by about 10% after five catalytic cycles. This deactivation was attributed to different reasons: an amount of the catalyst was lost during its separation by filtration after each catalytic cycle, Pd leaching, the presence of organic and inorganic species on the spent catalyst’s surface acting as poisons, as well as the agglomeration of palladium species.



中文翻译:

钛酸氢纳米管上负载的Pd催化剂用于Suzuki-Miyaura交叉偶联反应

通过浸渍乙酸钯(II)制备了负载在钛酸氢纳米管(HTN)上的钯催化剂,其特征在于N 2物理吸附,粉末X射线衍射,扫描电子显微镜,高分辨率透射电子显微镜并在Suzuki-Miyaura中进行了测试4-溴苯甲醛与苯基硼酸(反应1)或4-羟基苯基硼酸(反应2)之间的交叉偶联反应。这项工作的目的是确定这些催化剂在Suzuki-Miyaura反应中的活性以及在多个催化循环中重复使用这些催化剂的可能性。结果表明,Pd中x的最佳金属负载量为3.6 wt。%。)/ HTN催化剂。Pd(3.6)/ HTN催化剂在交叉偶联反应1和2中分别产生97%和88%的联苯产物收率,并且在五个催化循环后,其活性降低了约10%。这种失活归因于不同的原因:在每个催化循环后,过滤过程中催化剂的分离损失了一定数量的催化剂,Pd浸出,废催化剂表面上有机物和无机物作为毒物的存在,以及催化剂的结块。钯种。

更新日期:2017-10-16
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