双模板剂气相转移法合成杂原子磷铝分子筛

采用气相转移法、用双模板剂(即在制备干胶的过程中加入不易挥发的三乙醇胺、在液相中加入易挥发的三乙胺)合成了杂原子磷铝分子筛MeAPO-5(Me=Cr,Fe,Ni,Mn,Cu)。考察了有机胺模板剂的加入方式、干胶中金属含量对合成MeAPO-5分子筛的影响。采用X射线衍射、扫描电子显微镜、傅里叶变换红外光谱、等离子发射光谱、BET比表面积和热重分析等方法对合成产物进行了表征。表征结果显示,合成产物均具有AFI结构,为MeAPO-5分子筛;用双模板剂合成的MeAPO-5分子筛的结晶度高于用单模板剂合成的MeAPO-5分子筛。干胶中的n(MeO):n(Al2O3)=0.10～0.20时,有利于合成结晶度高的MeAPO-5分子筛及过渡金属杂原子进入磷铝分子筛的骨架。

Synthesis of MeAPO-5 by Vapor Phase Transport Using Dual Templates

Heteroatomic aluminophosphate molecular sieves MeAPO-5(Me=Cr,Fe,Ni,Mn,Cu) with AFI topology were synthesized by vapor phase transport method,using dry gel containing triethanolamine and liquid phase containing triethylamine as dual templates.Studies were carried out by varying contents of metal in dry gel and the way of adding templates.The MeAPO-5 samples were characterized by means of XRD,SEM,FTIR,ICP,BET and TG.The synthesized molecular sieves have crystalline structure of AFI.Comparing with single template either in dry gel or in liquid phase,MeAPO-5 synthesized by adding dual templates in dry gel and in liquid phase is high in crystallinity.When n(MeO):n(Al_2O_3) in dry gel is from 0.10 to 0.20,MeAPO-5 with high crystallinity can be synthesized and metallic ions are proved to be incorporated into framework of AlPO_4-5.