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层状H1-xNb1-xW1+xO6固体酸的制备与表征
Preparation and Characterization of Layered Solid Acids H1-xNb1-xW1+xO6
【摘要】 采用高温固相法合成Li1-x Nb1-x W1+x O6(x=0.1,0,-0.1),通过H+交换制备出相应的固体酸H1-x-Nb1-x W1+x O6。采用XRD和FT-IR技术表征固体酸的物相和层板骨架结构,NH3-TPD方法表征其酸性特征。结果表明,3种酸样品的物相相同,但它们的主晶面(002)面间距略有变化。与HNbWO6中的NbO6和WO6八面体结构单元相比,H0.9Nb0.9W1.1O6和H1.1Nb1.1W0.9O6中的NbO6和WO6八面体发生变形。3种酸样品均有两种不同强度的酸位,它们的弱酸位强度基本相等,强酸位强度大小顺序为H1.1Nb1.1W0.9O6>H0.9Nb0.9W1.1O6>HNbWO6,两种酸位的酸量大小顺序均为H1.1Nb1.1W0.9O6>HNbWO6>H0.9Nb0.9W1.1O6。
【Abstract】 Layered solid acids H1-xNb1-xW1+xO6 were prepared by proton exchange of Li1-xNb1-xW1+xO6(x=0.1,0,-0.1),which were obtained by the high-temperature solid-state method.The phase structure and laminate structure of the as-prepared solid acids were studied by means of powder X-ray diffraction(XRD)and Fourier transform infrared spectroscopy(FT-IR).The acid characteristics of the as-prepared sample were characterized with method of ammonia temperature-programmed desorption(NH3-TPD).The results of XRD indicated that there is the same phase structure and slight difference in the(002)crystal plane spacing for the three acid samples.And FT-IR analysis state clearly that the NbO6 and WO6 octahedral unit in H0.9Nb0.9W1.1O6 and H1.1Nb1.1W0.9O6 are deformed comparing to HNbWO6.The results of NH3-TPD show that there are two acid sites for each as-prepared sample.For the weak acid sites,their strength is almost equal.However,the acid site strength with higher strong is in order of H1.1Nb1.1W0.9O6> H0.9Nb0.9W1.1O6> HNbWO6.The acid amounts of the two acid sites for the three samples are all in order of H1.1Nb1.1W0.9O6> HNbWO6> H0.9Nb0.9W1.1O6.
【Key words】 layered compound; H1-xNb1-xW1+xO6; structure; acidic property;
- 【文献出处】 材料导报 ,Materials Review , 编辑部邮箱 ,2013年16期
- 【分类号】O643.36
- 【下载频次】50