Hsu Cheng-Ye, Chiang Anthony S T, Selvin Rosilda, Thompson Robert W
Department of Chemical & Materials Engineering, National Central University, 300 JungDa Rd., Chung Li, Taiwan ROC 32054.
J Phys Chem B. 2005 Oct 13;109(40):18804-14. doi: 10.1021/jp0526391.
A rapid synthesis procedure for nonagglomerated silicalite nanocrystals has been developed. This was achieved by concentrating the precursor sol before 10-12 h of aging at 80 degrees C, followed by hydrothermal synthesis at 175 degrees C for 90 min. The high silica concentration in the concentrated sol accelerated the aggregation of primary units that were present early in the system. Thus, little silica nutrients were left for growth when the secondary particles were converted to zeolite during hydrothermal reaction. As a result, fully dispersible nanocrystals were obtained within a day instead of weeks as reported previously. The aggregation of primary units during the 80 degrees C aging process as well as the conversion of these aggregates into zeolite has been followed by DLS, XRD, and FTIR. In light of the new results, the nucleation and growth mechanisms of MFI zeolite that have been under debate in the literature were reexamined.
已开发出一种用于合成非团聚硅沸石纳米晶体的快速合成方法。这是通过在80℃老化10 - 12小时之前浓缩前驱体溶胶,然后在175℃水热合成90分钟来实现的。浓缩溶胶中的高二氧化硅浓度加速了系统早期存在的初级单元的聚集。因此,在水热反应期间二次颗粒转化为沸石时,几乎没有二氧化硅养分剩余用于生长。结果,在一天内就获得了完全可分散的纳米晶体,而不是像之前报道的那样需要数周时间。通过动态光散射(DLS)、X射线衍射(XRD)和傅里叶变换红外光谱(FTIR)跟踪了80℃老化过程中初级单元的聚集以及这些聚集体向沸石的转化。鉴于这些新结果,对文献中一直存在争议的MFI沸石的成核和生长机制进行了重新审视。