开展了微波辅助法合成MCM-22分子筛的研究,经过29h微波晶化得到了与传统水热法合成5d相同的100%晶化的样品,有效地缩短了合成时间.通过XRD,SEM,FT-IR,ICP和27AlMASNMR技术表征,微波辅助合成样品具有高纯度、均一形貌,Al原子有效进入骨架等特征.对合成中的关键性条件,如结构导向剂的含量进行了深入研究,并给出了可能的合成机理.此外,通过在合成液中添加少量高介电损失物质,进一步缩短了合成时间.
MCM-22 zeolite has been synthesized successfully from hydrogels with microwave (MW) heating method,the process of which was compared with that of conventional hydrothermal synthesis (HTS).The MW-assisted heating showed a significant advantage that it reduced greatly the crystallization time.For instance,it led to a fully crystallized MCM-22 within 29 h in contrast to 5 d required by HTS synthesis.Microwave-assisted MCM-22 had good quality in phase purity,crystallinity,textual properties and incorporated tetrahedral Al ions as evidence by the characterizations with XRD,SEM,FT-IR,ICP and 27Al MAS NMR techniques.The paramount role of structure-directing agent in the MW-assisted process has been investigated to give a possible mechanism of crystallization.Moreover,by adding a small amount of alcohols in the initial gels,the crystallization time was further shortened to 24 h.