SBA-15负载钯催化剂的制备及其在超临界二氧化碳介质中催化Suzuki偶联反应的研究  

Preparation and application of SBA-15-supported palladium catalyst for Suzuki coupling reactions in supercritical carbon dioxide

作　　者：张涛[1] 冯秀娟[1] 颜美[1] 包明[1] 

机构地区：[1]大连理工大学精细化工国家重点实验室,辽宁大连116012

出　　处：《分子科学学报》2008年第1期1-5,共5页Journal of Molecular Science

基　　金：国家自然科学基金资助项目(20603005)

摘　　要：采用3-巯丙基三甲氧基硅烷为内表面修饰剂,三甲氧基苯基硅烷为外表面修饰剂,合成了内外表面被修饰的介孔分子筛SBA-15,并制备了负载钯催化剂.应用X射线粉末衍射仪(XRD),傅立叶红外光谱仪(FT-IR),紫外可见光谱仪,扫描(SEM)、透射(TEM)电子显微镜等仪器对材料结构进行了表征.考察了负载钯催化剂在超临界二氧化碳介质中催化Suzuki偶联反应的活性,结果表明:制得的负载钯催化剂稳定、活性高;以四丁基乙酸胺为碱,对溴硝基苯与苯硼酸在90℃下反应48 h,得到71%收率的对硝基联苯.The external and internal surfaces of mesoporous silicate SBA-15 were modified by trimethoxyphenylsilane and mercaptopropyl trimethoxysilane, respectively, and then the SBA-15-supported palladium catalyst was obtained by treatment of the SBA-15 in a THF solution of Pd（AcO）2. The structures of the modified SBA-15 and SBA-15-Pd were characterized by XRD, FT-IR, UV, SEM, and TEM. The model coupling reaction of 1-bromo-4-nitrobenzene with phenylboronic acid proceeded smoothly in the presence of SBA-15-Pd catalyst and （ n-Bu）4NOAc in supercritical carbon dioxide at 90 ℃ for 48 h to give biaryl in 71% yield,which indicated that the SBA-15-Pd was very stable could be used in supercritical carbon dioxide with high catalytic activity.

关 键 词：SBA-15 SUZUKI 偶联反应 超临界二氧化碳 

分 类 号：O614[理学—无机化学]