微波合成纳米NaX分子筛的研究与表征.pdfVIP

石油化工 • 956. PETROCHEMICAL TECHNOLOGY 2013 年第42 卷第9 期 微波合成纳米NaX分子筛的研究与表征 程志林，刘赞，韩贵 (扬州大学化学化工学院，江苏扬州 225(02) [摘要]在常压回流微疲加热条件下合成了NaX分子筛，并对其进行了XRD， FTIR , TEM , NMR表征，考察了合成配比对 NaX分子筛的晶粒尺寸、形貌、硅铝比及相对结晶度的影响。表征结果显示，合成配比对NaX分子筛的晶粒尺寸、形貌、硅 铝比及相对结晶度具有较为显著的影响。 XRD和TEM表征结果显示，合成的NaX分子筛的品粒尺寸为30 - 100 nmo FTIR表 征结果显示，当熔烧温度高于600 c时，纳米NaX分子筛的骨架开始崩塌，表明纳米NaX分子筛的热稳定性低于常规NaX分 子筛。 NMR表征结果显示，合成的纳米NaX分子筛具有较低的硅铝比，且硅物种配位峰的化学位移向高场偏移。微波合成的 NaX分子筛的晶粒度明显小于常规合成的NaX分子筛，且品化时间明显缩短，充分证明了微波加热快速均匀且能得到较小晶 粒度的分子筛。 [关键词]微波诱导;纳米; NaX分子筛;表征 [文章编号 1 1000 - 8144 (2013) 09 - 0956 - 06 [中图分类号1 TQ 426 [文献标志码1 A Studyand Characterization of Nanosized N aX Zeolite Synth臼ized by Microwave Heating Cheng Zhilin , Liu Zan , Han Gui (Col1ege of Chemistry and Chemical Engineeri鸣， Yangzhou University , Yangzhou Jiangsu 225002 , China) [ Abstract ] Nanosízed NaX zeolites were synthesized by microwave heating under reflux and characterized by means of XRD , FTIR , TEM and NMR. The effects of n(Na 0) : 2 n(Si0 ) : n(A1 0 ) : n(H 0) on the size , morphology , silica-alumina ratio and relative crystallinity 2 2 3 2 of the naosized NaX zeolites were investigated. The XRD and TEM results indicated that the crystal size of the synthesized NaX zeolites was in the range of 30-100 nm. The FTIR result showed that the skeleton of the nanoszied FAU-type zeolites collapsed at calcination temperature of 600 C, which meant that the thermal stability ofthe nanosized NaX zeolites was lower than that of conventional NaX zeo