微波法制备五甲基环戊二烯铑及催化苯乙炔聚合  

Preparation of Pentamethylcyclopentadiene Rhodium by Microwave Irradiation and Its Application in Polymerization of Phenylacetylene

作　　者：张钰艳 贾宏葛 韩笑 董少波 张明宇 王成龙 石佳 徐晨曦 张循海 Zhang Yuyan;Jia Hongge;Han Xiao;Dong Shaobo;Zhang Mingyu;Wang Chenglong;Shi Jia;Xu Chenxi;Zhang Xunhai(College of Materials Science and Engineering,Heilongjiang Provinces Key Laboratory of Polymeric Composite Material,Qiqihar University,Qiqihar,Heilongjiang 161006,China)

机构地区：[1]齐齐哈尔大学材料科学与工程学院黑龙江省聚合物基复合材料重点实验室,黑龙江齐齐哈尔161006

出　　处：《化学世界》2021年第12期753-756,共4页Chemical World

基　　金：黑龙江省自然科学基金(No.LH2019B032);黑龙江省省属高等学校基本科研业务费科研(No.135309503)资助项目。

摘　　要：随着催化剂产业的发展,茂金属催化剂受到了很大的关注,而传统水浴加热法制备茂金属催化剂存在收率低、合成费时等问题,因此寻找新的制备工艺迫在眉睫,而微波由于其效率高、节能环保、节省时间等优点已经成为当代研究的热点。以[Rh(cod)Cl]_(2)(cod=1,5-环辛二烯)与五甲基环戊二烯为原料,通过微波法制备了具有夹心结构的[Cp^(*methyl) RhCl]_(2)(μ_(2)-Cl)_(2),通过核磁共振、异核单量子关系谱(HSQC)及红外光谱(IR)等对其结构进行了表征。对产物进行催化效果测试结果表明,微波化学法制备催化剂与传统的水浴加热合成法制备的催化剂相比,节省了反应时间、提高了催化剂的收率。With the development of catalyst industry,metallocene catalyst has been paid great attention.The traditional water bath heating method of the preparation of metallocene catalyst has problems,such as low yield and time-consuming synthesis,so that it is urgent to develop a new preparation process.Microwave has become a popular contemporary research topic due to its high efficiency,energy saving and time saving advantages.[Cp^(*methyl) RhCl]_(2)(μ_(2)-Cl)_(2)with a sandwich structure was prepared for the first time by microwave method using[Rh(cod)Cl]_(2)(cod=1,5-cyclooctadiene)and pentamethylcyclopentadiene as raw materials.The structures were characterized by Nuclear Magnetic Resonance,infrared spectroscopy(IR),and heteronuclear single quantum coherence(HSQC)spectra.The products were tested for catalytic effect.The results showed that in comparison with the traditional water bath heating,the reaction using microwave can not only save the reaction time,but also improve the yield of catalyst.

关 键 词：微波法 茂基 铑 配位 催化剂 

分 类 号：O643.36[理学—物理化学]