Keggin型硅取代钨钴酸盐[Co~ⅢW_(11)O_(40)(SiOH)_2]^(5-)的合成和表征  

Synthesis and Characterization of Silanol Derivative of Keggin Tungstocobaltate [Co~ⅢW_(11)O_(40)( SiOH)_2]^(5-)

作　　者：张建平[1] 杨春[1] 

机构地区：[1]南京师范大学化学与材料科学学院,江苏南京210097

出　　处：《南京师大学报（自然科学版）》2013年第3期48-52,共5页Journal of Nanjing Normal University(Natural Science Edition)

基　　金：江苏省高校优势学科建设工程资助项目

摘　　要：以CoⅢW11和TEOS为原料,在乙醇-水混合溶剂中首次合成了Keggin型硅取代的钨钴酸盐[CoⅢW11O40(SiOH)2]5-.用IR、UV-vis、TG-DTA和元素分析技术对样品进行了结构和组成表征.表征结果显示,两个SiOH基团进入了CoⅢW11的空位,并形成了Si-O-Si桥,产物的对称性介于饱和与缺位结构之间.同时,考察了反应条件对合成产物的影响.结果表明,pH和乙醇-水的配比对合成产物的影响很大.酸度与醇用量须有一个合适的匹配,只有在pH=1,V EtOH∶V H20=2∶1的条件下,才能得到高产率和高纯度的产物.The Keggin-type silanol substituted tungstocobahate [ CoⅢ W1104o （SiOH） 2 ] 5- was synthesized for the first time by using Cox WH and TEOS as start materials in an ethanol-water mixing solvent. The structure and composition of the products were characterized by IR, UV-vis, TG-DTA and elemental analysis techniques. The results showed that two Si atoms were inserted into the vacancy of CoⅢ W11 and a Si-O-Si bridge was formed between two Si atoms. The symmetry of the product is between saturated and vacant Keggin structure. Moreover,the effect of synthesis conditions on the product was also investigated. It is demonstrated that the pH and the volume ratio of ethanol to water greatly influence the yield and the purity of the product. A proper matching of acidity and ethanol dosage is necessary. The product with good yield and high purity was obtained under pH = 1 and VEtOH ： VH20 = 2 ： 1.

关 键 词：钨钴酸盐 硅取代 KEGGIN结构 合成与表征 

分 类 号：O611.4[理学—无机化学]