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将磷酸氢二钠、偏钒酸钠、钼酸钠溶液按化学计量系数混合,通过反应制备具有Keggin结构的磷钼钒杂多酸H3+xPMo12-xVxO40(x=1~3)。将制备的H3+xPMo12-xVxO40(x=0~3)与一定量的1-丁基-3-甲基咪唑溴离子液体([Bmim]Br)反应,合成[Bmim]3+xPMo12-xVxO40(x=0~3)有机-无机的杂多酸杂化材料。采用傅里叶红外光谱(FTIR)、X射线衍射(XRD)对[Bmim]3+xPMo12-xVxO40(x=0~3)杂化材料进行表征,结果表明,所合成的磷钼钒杂多酸杂化材料具有Keggin结构。以Si O2为载体制备负载型的杂多酸杂化材料[Bmim]3+xPMo12-xVxO40/Si O2(x=0~3),采用间歇釜式反应器,以双氧水作为氧化剂,将该催化剂应用于降解有机偶氮染料甲基橙的研究,确定最优反应条件为:[Bmim]5PMo10V2O40/Si O2的负载量为50%(质量分数),反应温度为50℃、双氧水用量为5 m L,此时,氧化体系对甲基橙降解率最高,可达94%。催化剂具有很好的重复使用性能,可以重复使用至少7次,而对甲基橙氧化降解活性没有明显下降。
The phosphomolybdovanadophosphoric acid H3 + xPMo12-xVxO40 (x = 1-3) with Keggin structure is prepared by mixing stannous sodium phosphate, sodium metavanadate and sodium molybdate solution in stoichiometric ratio. The prepared H3 + xPMo12-xVxO40 (x = 0~3) was reacted with a certain amount of 1-butyl-3-methylimidazolium bromide ionic liquid ([Bmim] Br) to synthesize [Bmim] 3 + xPMo12-xVxO40 x = 0 ~ 3) organic-inorganic heteropoly acid hybrid material. The [Bmim] 3 + xPMo12-xVxO40 (x = 0 ~ 3) hybrid materials were characterized by Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The results showed that the synthesized phosphomolybdic vanadyl heteropolyacids Hybrid materials have a Keggin structure. The supported heteropoly acid hybrid material [Bmim] 3 + xPMo12-xVxO40 / Si O2 (x = 0 ~ 3) was prepared with Si O2 as the carrier. The batch reactor type reactor was used with hydrogen peroxide as oxidant. For the degradation of organic azo dye methyl orange, the optimal reaction conditions were as follows: [Bmim] 5 PMo10V2O40 / SiO2 loading was 50%, the reaction temperature was 50 ℃, the amount of hydrogen peroxide was 5 mL, At this point, the highest degradation rate of methyl orange oxidation system, up to 94%. The catalyst has good reusability and can be reused for at least 7 times without any significant decrease in oxidative degradation of methyl orange.