溶胶—凝胶法合成12—硅钼酸盐及其结构研究

本文报导了用溶胶—凝胶法自生压力下水热合成12—硅钼酸盐,并成功培养出结晶完美的大单晶体。四圆x射线衍射研究结果证明,这种12—硅钼酸盐具有Keggin结构。晶体由SiMo_(12)O_(40)~(4-)杂多阴离子及NH_4~+(C_4H_9)_2N~+H_2和H_2O分子组成,杂多阴离子SiMo_(12)O_(40)~(4-)按晶体所属空间群对称性要求,在三维空间中排列成网状结构,正离子NH_4~+,(C_4H_9)_2N~+H_2及中性水分子则处于网状结构所具有的结构孔道中,以其正电荷及氢键形成能力连接杂多阴离子网状结构,首次将二正丁胺引入杂多酸骨架,且二正丁胺以质子化的形式存在于结构中。

Study on the Synthesis by Sol-Gel Method and Structure of 12-Silicomolybdenate

In this paper, we had used sol-gel method to synthesize 12-silicomolybdenate under autogeneror pressure and successfully obtained perfect large single crystals. The research results of four-circle X-ray diffraction showed that this 12-silicomolybdenate had Keggin type structure. The crystals were composed of heteropolyanion (SiMo_(12)O_(40))~(4-). NH_4~+ cations, protonated dibutylamine molecules and H_2 O molecules. The heteropolyanion (SiMo_(12)O_(40))~(4-) had arranged to network structure in three-dimensional space based on symmetry of space group. The cations NH_4~+, (C_4 H_9)_2 NH_2~+ and neutral water molecules located in the structural channels of the network structure, and joined heteropolyanionic network structure together by their positive charges and capacity forming hydrogen bond. We had first introduced dibutylamine molecules into the framework of heteropolyacid, and the dibutylamine molecules is protonated the structure.