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Role of porosity on silica immobilized palladium complexes as recyclable catalysts in the methoxycarbonylation of 1-hexene
Microporous and Mesoporous Materials ( IF 5.2 ) Pub Date : 2024-03-16 , DOI: 10.1016/j.micromeso.2024.113092
Saphan O. Akiri , Benjamin Heider , Stefan Lach , Ch. Ziegler , Wolfgang Kleist , Stephen O. Ojwach

Immobilization of the palladium complex [Pd()Cl] (), where = N,N'E,N,N'E)-N,N'-(3-(3-(triethoxysilyl)propyl)pentane-2,4-diylidene)dianiline, on MCM-41 and SBA-15 supports at 100 °C and Pd loading of 10% afforded the respective materials [@MCM-41] ( and [@SBA15] in moderate yields. Calcination temperatures of 150 °C and 200 °C using SBA-15 support gave the corresponding compounds and respectively, while using MCM-41 support and Pd loadings of 5% afforded compound . The characterization of the new materials was achieved by using FT-IR for functional group analyses, ICP-OES, TEM and SEM-EDX and XPS for surface morphology, elemental composition, particle size distribution and oxidation status respectively, PXRD for crystallinity and N physisorption measurements for surface area and porosity determinations. All the immobilized materials (–) formed active catalysts in the methoxycarbonylation of 1-hexene with moderate catalytic activities (TON of 372) to afford mainly linear esters. The catalytic activities of the materials depended on the nature of support and their physical properties and was largely controlled by their porosity. The SBA-15 supported catalysts, which displayed larger pore sizes, were generally more active than those of supported on MCM-41. The supported catalysts were recycled five times with minimum reduction in catalytic activities.

中文翻译:

二氧化硅固定钯配合物的孔隙率作为可回收催化剂在 1-己烯甲氧基羰基化反应中的作用

钯络合物 [Pd()Cl] () 的固定化,其中 = N,N'E,N,N'E)-N,N'-(3-(3-(三乙氧基甲硅烷基)丙基)戊烷-2,4 -二亚基)二苯胺,在 100 °C 和 10% Pd 负载量的 MCM-41 和 SBA-15 载体上,以中等产率提供相应的材料 [@MCM-41](和 [@SBA15])。煅烧温度为 150 °C使用 SBA-15 载体在 200 °C 和 200 °C 下分别得到相应的化合物 和 ,而使用 MCM-41 载体和 5% 的 Pd 负载量则得到相应的化合物。通过使用 FT-IR 进行官能团分析、ICP 来实现新材料的表征。 -OES、TEM 和 SEM-EDX 和 XPS 分别用于表面形貌、元素组成、粒度分布和氧化状态,PXRD 用于结晶度,N 物理吸附测量用于表面积和孔隙率测定。所有固定材料 (-) 均形成活性催化剂。 1-己烯的甲氧基羰基化反应具有中等催化活性(TON为372),主要生成直链酯。材料的催化活性取决于载体的性质及其物理性质,并且很大程度上受其孔隙率控制。 SBA-15 负载型催化剂具有较大的孔径,通常比 MCM-41 负载型催化剂的活性更高。负载型催化剂可循环使用五次,催化活性的降低最小。
更新日期:2024-03-16
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