| 氨基硫脲纤维素负载钯配合物的制备及其对Heck反应的催化性能 |
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| 引用本文： | 许英,蔡永红,崔元臣,李金金.氨基硫脲纤维素负载钯配合物的制备及其对Heck反应的催化性能[J].石油化工,2008,37(4):328. |
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| 作者姓名： | 许英 蔡永红 崔元臣 李金金 |
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| 作者单位： | 河南大学,化学化工学院,河南,开封,475001 |
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| 基金项目： | 河南省自然科学基金资助项目(611020500) |
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| 摘 要： | 通过较简单的方法合成了氨基硫脲纤维素负载钯配合物(CC-TSC-Pd)催化剂,并利用X射线光电子能谱、热重-差热分析等手段对其进行了表征。该催化剂在室温至240℃内热稳定性很好,在低温、空气氛围、水溶剂中能有效催化丙烯酸或苯乙烯与芳基碘(或带取代基的芳基碘)的Heck反应,立体选择性地生成反式肉桂酸(或带取代基的反式肉桂酸)或1,2-二苯乙烯,在110℃下反应5～6h,产物的收率在90.0%以上。CC-TSC-Pd催化剂具有较好的重复使用性能,连续使用5次,反式肉桂酸的收率仍可达76.3%。CC-TSC-Pd催化剂中起催化作用的是金属态的钯。
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| 关 键 词： | 氨基硫脲纤维素 钯配合物 负载型催化剂 Heck反应 丙烯酸 苯乙烯 芳基碘 |
Synthesis of Thiosemicarbazide Cellulose Supported Palladium Complex and Its Catalytic Behavior in Heck Reaction |
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| Xu Ying,Cai Yonghong,Cui Yuanchen,Li Jinjin.Synthesis of Thiosemicarbazide Cellulose Supported Palladium Complex and Its Catalytic Behavior in Heck Reaction[J].Petrochemical Technology,2008,37(4):328. |
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| Authors: | Xu Ying Cai Yonghong Cui Yuanchen Li Jinjin |
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| Affiliation: | Xu Ying,Cai Yonghong,Cui Yuanchen,Li Jinjin(College of Chemistry , Chemical Engineering,Henan University,Kaifeng Henan 475001,China) |
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| Abstract: | Thiosemicarbazide cellulose supported palladium complex was synthesized by simple method and characterized by XPS and TG-DTA.The complex has good thermal stability in range of room temperature to 240 ℃ and is an efficient catalyst for Heck reaction of acrylic acid or styrene with aryl iodide(or substitued aryl iodides)at low temperatures,water as solvent and in air atmosphere.The trans-cinnamic acid(or substitued trans-cinnamic acid)or 1,2-stilbene is stereoselectively obtained with high yield(more than 90.0%) at 110 ℃ for reaction time about 5-6 h.Thiosemicarbazide cellulose supported palladium complex can be separated from the reaction mixture easily and reused for several cycles.The trans-cinnamic acid yield can be maintained at about 76.3% after the catalyst has been run for 5 times.Metallic Pd species are the active center. |
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| Keywords: | theiosemizidcarbae cellulose palladium complex supported catalyst Heck reaction acrylic acid styrene aryl iodide |
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