气相转移法合成AEL型磷铝分子筛

Synthesis of AEL Topology Aluminophosphate Molecular Sieves by Vapor Phase Transport Method

采用气相转移(VPT)法合成具有AEL结构的锰掺杂的磷铝分子筛(MnAPO-11)。考察了晶化温度、晶化时间、模板剂的添加方式和干胶组成等对MnAPO-11分子筛合成的影响,并采用X射线衍射(XRD)、扫描电镜(SEM)、N2低温吸附(BET)和傅立叶红外光谱(FT-IR)等手段对样品进行了表征。结果表明,采用VPT法合成MnAPO-11分子筛的晶化时间长于水热(HTS)法,且晶化温度略高,合成MnAPO-11分子筛的比表面积较HTS法的大。干胶中MnO与Al2O3物质的量之比为0.00～0.15,二异丙胺与Al2O3物质的量之比为1～2,晶化时间12～24 h,晶化温度160～200℃,所合成的MnAPO-11分子筛结晶度高。采用VPT法,以二异丙胺为模板剂合成的MnAPO-11单个晶体为条柱状,以二正丙胺为模板剂,合成的MnAPO-11团聚呈花瓣形。

Manganese incorporated aluminophosphate molecular sieves（MnAPO-11） with AEL topology were synthesized by vapor phase transport（VPT） method.The effects of the synthesis parameters,such as crystallization temperature and crystallization time,the way of adding template,and the composition of the dry gel were investigated.The samples were characterized by X-ray diffraction（XRD）,scanning electron microscopy（SEM）,low-temperature nitrogen adsorption-desorption technique（BET） and Fourier infrared spectroscopy（FT-IR）.The results showed that crystallization time by VPT method was longer than that by hydro-thermal（HTS） method,and the crystallization temperature was higher than that by HTS method.MnAPO-11 prepared by VPT method had higher surface area than that by HTS method.High crystallinity MnAPO-11 were obtained under the conditions of molar ratio of MnO to Al2O3 0.00-0.15,the molar ratio of diisopropylamine to Al2O3 1-2,crystallization time 12-24 h and crystallization temperature 160-200 ℃.The crystal of the MnAPO-11 synthesized using diisopropylamine as template by VPT method was columnar,while using dipropylamine as template,the crystal of the MnAPO-11 was petal-shaped crystal.