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以CoIIIW11和有机硅烷为原料,在pH=1,乙醇-水(体积比=2∶1)的混合溶剂中,首次合成了Keggin型有机硅取代的钨钴酸盐[CoIIIW11O40(SiR)2]5-(CoIIIW11(SiR)2,R=CH=CH2,OH).这里,乙醇作为共溶剂增加硅烷在溶液中的溶解度,使CoIIIW11在转化为饱和结构之前能够快速与硅烷相遇并反应.产物的组成和结构用IR,UV-Vis,NMR,TG-DTA,元素分析等技术进行了全面表征.结果显示,两个SiR基团进入了CoIIIW11的空位,并形成Si—O—Si桥,得到与先前报道的硅取代钨硅酸盐和钨磷酸盐相似的结构.还运用此条件成功合成了以往需要在固-液相转移条件下合成的[PW11O40(SiR)2]3-[PW11(SiR)2,R=CH=CH2,OH],进一步证明了此方法在合成有机硅取代的多金属氧酸盐方面的可行性和通用性.
Using CoIIIW11 and organosilane as raw materials, Keggin type organosilicon-substituted tungsten cobaltite [CoIIIW11O40 (SiR) 2] 5 was synthesized for the first time in a mixed solvent of pH = 1 and ethanol-water - (CoIIIW11 (SiR) 2, R═CH═CH2, OH). Here, ethanol acts as a cosolvent to increase the solubility of the silane in solution so that CoIIIW11 can quickly react with silane and react before it is converted to a saturated structure. And their structures were characterized by IR, UV-Vis, NMR, TG-DTA and elemental analysis. The results show that two SiR groups enter the vacancy of CoIIIW11 and form Si-O-Si bridges. Reported the silicon-substituted tungstosilicate and tungstophosphate similar structure.Utilization of this condition was also successfully synthesized in the past under the solid-liquid phase synthesis conditions [PW11O40 (SiR) 2] 3- [PW11 (SiR) 2 , R = CH = CH2, OH], further evidence of the feasibility and versatility of this method in the synthesis of organosilicon-substituted polyoxometallates.