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机构地区:[1]内蒙古大学化学化工学院,呼和浩特010021
出 处:《应用化学》2004年第9期923-927,共5页Chinese Journal of Applied Chemistry
基 金:国家自然科学基金资助项目 ( 2 0 0 62 0 0 0 4)
摘 要:采用浓H2 SO4 CH3 OH体系作催化剂 ,使单烷基二茂铁、双烷基二茂铁分别与丙酮进行非均相缩合反应 ,用柱层析分离得到了 2 ,2 二 (单烷基二茂铁基 )丙烷和 2 ,2 二 (双烷基二茂铁基 )丙烷 2个系列的化合物。最佳的反应条件为 :物料配比n(烷基二茂铁 )∶n(丙酮 )∶n(浓硫酸 )∶n(甲醇 ) =1∶0 5 5∶2∶6 7,在 80~ 90℃反应4 6h ,用元素分析、FTIR、1HNMR对这些化合物的结构进行了表征 ;测试了这 2个系列化合物的电化学性质及其在固体推进剂中的燃速催化效能 ,结果表明 ,这类化合物的燃速催化效率均随着烷基碳链增长而缓慢下降 ,烷基总碳数相同时 。Non-homogenous condensation of alkylferrocenes with acetone has been carried out in the presence of methyl alcohol and concentrated sulfurric acid. Two series of compounds, 2,2-bis(monoalkylferrocenyl)propanes and 2,2-bis(dialkylferrocenyl)propanes were isolated by column chromatography. It was found the (optimal) conditions were n(alkylferrocene)∶n(acetone)∶n(concentrated sulfuric acid)∶n(methyl (alcohol)=)1∶0.55∶2∶6.7, reaction time 4~6 h, and reaction temperature 80~90 ℃. The structures of these compounds were characterized by elemental analysis, IR, and ^(1)H NMR. The electrochemical properties of these compounds were investigated by cyclic voltammetry. The results indicated that the burning-rate catalytic (efficiency) of the title compounds showed a slow decrease with the increase of the alkyl chain length, and for the alkyl group with same carbon number, the more alkyl groups the stronger the electron repulsion and reducibility, and hense the higher the burning-rate catalytic activity. The effect of the structures, electrochemical properties, and catalytic activity on the burning-rate were also discussed.
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