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Three lacunary Keggin type polyoxometalate based on {XW9} (X=P, As) synthesis and properties of ester tin derivatives

Author: YangHe
Tutor: ZhangLanZuo
School: Liaoning Normal University
Course: Inorganic Chemistry
Keywords: Trivacant Keggin structure Tungstophosphates Tungstoarsenate Estertinderivatives Catalytic oxidation
CLC: O627
Type: Master's thesis
Year: 2013
Downloads: 6
Quote: 0
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Abstract


Two sandwich-type and one boat-like polyoxometalate （abbreviated as POM） estertinderivatives have been synthesized in acetate buffer solutions through routine synthetic methodby using a tungstophosphate Na9PW9O347H2O, a tungstoarsenate Na9[AsW9O33]·27H2O, anddilacunary tungstoarsenate K14[As2W19O67（H2O）]·31.5H2O (abbreviated as {PW9}、{AsW9}and {As2W19}, respectively) as inorganic precursors and the estertin （Cl3Sn（CH2）2COOCH3）as a organic precursor. They have been characterized by single-crystal X-ray diffraction,elemental analysis, IR spectroscopy, TG analysis, electrochemical analysis and NMR. Theelectrocatalytic activity towards the reduction of hydrogen peroxide and catalytic activity forthe oxidation of cyclohexanol to cyclohexanone were also investigated.1. One sandwich-type POM （compound1） functionalized with estertin groups has beensynthesized through the assembly in aqueous solution by using {PW9} as a building block,and Cl3Sn（CH2）2COOCH3as an organic precursor. In other synthetic method, we have alsoobtained compound1by the reaction of {AsW9} with Cl3Sn（CH2）2COOCH3by introducingphosphate. Furthermore, in the synthetic process, the estertin has hydrolyzed into thecarboxyethyltin, the molecular formula is as follows:Na3K8[K3{Sn（CH2）2COO}2(A-α-PW9O34)2]·18H2O （1）2. One sandwich-type POM （compound2） has been isolated at first through the assemblyin aqueous solution by using {As2W19} as a building block, Cl3Sn（CH2）2COOCH3as anorganic precursor, and then one boat-like POM （compound3） was got after the balance of themother liquid for a long time. The estertin also hydrolyzed into the carboxyethyltin, theirmolecular formulas are as follows:Na6K8[{Sn（CH2）2COO}2·(B-α-AsW9O33)2]·25H2O （2）Na10K7[H{Sn（CH2）2COO}4·(W4O16)·(B-α-AsW9O33)2]·27H2O （3）

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CLC: > Mathematical sciences and chemical > Chemistry > Organic Chemistry > Elements in organic compounds
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