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双核羧酸钼Mo2(OCOR)4合成的研究

Study on the synthesis of molybdenum(Ⅱ)carboxylates

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【作者】 杨纪民路琼华

【Author】 Yang Jimin Lu Qionghua (Department of Chemistry,East China University of Chemical Technology,Shanghai 200237)

【机构】 华东化工学院化学系华东化工学院化学系 上海200237上海200237

【摘要】 对双核羧酸钼的氧化聚合法进行了考察,优化了合成条件。Mo2(OCOCH34、Mo2(OCOC3H74、Mo2(OCOC4H?)4和 Mo2(OCOC?H5)4的产率分别为57.02%、48.90%、38.90%和67.10%。提出了可能的反应机理。研究发现,使用一定配比的苯与乙醚的混合溶剂且在水解时加铁,有助于 Mo(CO)?产率的提高。Mo(CO)?的产率为43.8%。

【Abstract】 Molybdenum(Ⅱ)carboxylates were synthe-sized from Mo(CO)8 by oxidation-polymerizationin nitrogen atmosphere.All kinds of synthesisconditions were discussed and improved,whichwere favorable to higher yield of molybdenum(Ⅱ)carboxylates.The reaction mechanism of theoxidation-polymerization was also given.Theyields of Mo2(OCOCH34,Mo2(OCOC3H74,Mo2-(OCOC4H94,and Mo2(OCOC6H54 were 57.02%,48.90%,38.90%,and 67.10% respectively.Mo-(CO)6 was the precursor of the molybdenum(Ⅱ)carboxylates.The purpose of this paper was tofind out an improved synthetic method in whichhigher yield of Mo(CO)? could be achieved atlow temperature and ordinary pressure.Usingsuitable ratio of benzene to ether as the solventand adding iron during hydrolysis were favorableto higher yield of Mo(CO)6.The best yield ofMo(CO)6 was 43.8%.

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