钯-离子液体/钛硅复合氧化物催化剂的合及在胺羰化中的应用

长期以来 ,工业上一直使用光气合成法生产异氰酸酯类化合物 ,极易造成环境污染和人员伤害 ,因此研究无光气且环境友好的新工艺已引起广泛关注 .就经济角度考虑 ,由硝基类化合物进行还原羰化1～ 4 ] 或胺类化合物进行氧化羰化 5～ 13] 制备异氰酸酯比较有利 ,但是存在金属配合物催化剂的还原失活等问题14 ,15] .室温离子液体作为一种具有特殊催化性能和可调控溶解能力的新型溶剂和反应介质已用于有机反应中 16 ] ,但将其作为反应介质的含氮化合物进行羰化研究尚未见报道 .本文将离子液体应用于以硅酸四乙酯 ( TEOS)和钛酸四丁酯 ( TBO…

Preparation of TiOy-SiOx Immobilized Pd-BMImCl Catalysts and Their Application in Carbonylation of Amines

A highly efficient Pd\|BMImCl/TiO\-\%y\%\|SiO\-\%x\% catalyst system synthesized through sol\|gel method from palladium complex, ionic liquid, titanate and silicate esters was found for the oxidative carbonylation of amines. The catalyst efficiency was much higher than that reported in previous papers and the TOF number reached to 10 372 when catalyst 0.05%Pd\|4.6%BMImCl/TiO\-\%y\%\|SiO\-\%x\% was used. The usability of ionic liquid was the key point for preparation of this catalyst system because of its high dissolvability to palladium complex and affording appropriate micro\|environment for the reaction. The synergism among palladium complex, ionic liquid, titanate and silicate was the main reason for the high catalytic activity of the catalyst system. BET, AES and XRD were used to characterized the catalysts in detail.