本文采用离子热合成法,以磷酸为磷源、异丙醇铝为铝源,在溴化1-丁基-3-甲基咪唑鎓([BMIM]Br)离子液体中于280℃快速合成了AlPO4-42分子筛,并用该方法快速合成了其他类型的磷酸铝分子筛。通过X射线衍射、扫描电镜、比表面积孔隙率分析、固体核磁等表征手段研究了不同物料配比、模板剂、晶化时间对合成AlPO4-42分子筛的影响以及AlPO4-42分子筛的比表面积、孔容大小和孔道中的填充物。结果发现,在4min时已经形成了AlPO4-42分子筛的结构。合成出的AlPO4-42分子筛具有十四面体的形貌,这与采用常规方法得到的AlPO4-42分子筛晶体的立方体形貌明显不同,而且AlPO4-42分子筛的比表面积和孔容都有所改变。在合成AlPO4-42分子筛的过程中离子液体和模板剂协同导向产物的形成。
In this work, A1PO4-42 molecular sieves was rapidly synthesized by ionothermal synthesis with phosphoric acid as phosphorus sources and isopropanol aluminum as aluminum sources in ionic liquid [ BMIM ] Br at 280℃ , and some other type aluminophosphate molecular sieves were synthesized by this way. XRD, SEM, BET and solid-state mas NMR were used to investigate the influence of the ratio of materials, template agent and different crystallization time on synthesis. The specific surface area, size of the entrance and filler in the pore for as-prepared A1PO4-42 molecular sieves were characterized as well. The results indicated that the structure of AIPO4-42 molecular sieves has been already formed after 4 rain. The synthesized ALP04-42 molecular sieves had a tetrakaidecahedron morphology, which is obviously difierem with the AIPO4-42 molecular sieves of cube morphology obtained hy conventional approach, and the specific sm'face area and pore volume of A1PQ-42 molecular sieves were changed too. In the process of synthesis AIPO4-42 molecular sieves, the coordinated action of ionic liquid and template led to tbrm the products.