球磨-再晶化法合成磷酸铝分子筛  

Synthesis of Aluminophosphate Molecular Sieves by Ball Milling and Recrystallization

作　　者：王双 于越 白璞 刘健聪 李霖 宋晓伟[1,2] WANG Shuang;YU Yue;BAI Pu;LIU Jiancong;LI Lin;SONG Xiaowei(State Key Laboratory of Inorganic Synthesis and Preparative Chemistry,College of Chemistry, Jilin University,Changchun 130012,Chin;Department of Physical and Macromolecular Chemistry,Faculty of Science,Charles University in Prague, 12843 Prague 2,Czech Republic)

机构地区：[1]吉林大学化学学院,无机合成与制备化学国家重点实验室,长春130012 [2]布拉格查尔斯大学理学院物理和高分子化学系,布拉格12843

出　　处：《高等学校化学学报》2018年第9期1859-1866,共8页Chemical Journal of Chinese Universities

摘　　要：以热稳定性较差的二维层状磷酸铝AlPO-IM([C_3H_5N_2]_2[Al_3P_4O_(16)H])为前驱体,经过球磨-再晶化快速合成出具有AWO拓扑结构的磷酸铝分子筛AlPO-CJ73a及具有LAU拓扑结构的磷酸铝分子筛MgAPOCJ73b和ZnAPO-CJ73c.通过对合成条件的详细研究,发现金属杂原子在合成过程中对LAU结构的生成起到导向作用,结合共振拉曼光谱和CSh M值计算研究了相转变机制.利用球磨-再晶化法不仅极大缩短了晶化时间,而且可在无溶剂条件下将二维层状磷酸铝前驱体转变为三维分子筛,实现了分子筛合成中对环境的零排放.与传统的水热/溶剂热法相比,该方法具有高效、节能的特点,拓展了磷酸铝分子筛的合成路线.A rapid synthetic strategy through ball milling and recrystallization was successfully developed.Aluminophosphate molecular sieve with AWO topology was prepared by the precursor of two-dimensional(2D)layered aluminophosphate AlPO-IM.Simultaneously,metal-containing aluminophosphate molecular sieves with LAU topology were synthesized by introducing the metal heteroatoms in the ball-milling process.The phase transformation mechanism was comprehensively analyzed by Raman spectroscopy and CShM calculation.The results show that metal heteroatoms have an inorganic structure-directing effect in the synthesis of LAU molecular sieves.The ball milling-recrystallization method not only greatly shortens the crystallization time,but also converts the 2D layered aluminophosphates into a 3D molecular sieve under solvent-free conditions.Compared with the traditional hydrothermal/solvothermal synthesis,the ball milling-recrystallization method has the characteristics of high efficiency and energy saving,which expands the synthetic route of aluminophosphate molecular sieves.

关 键 词：球磨法 磷酸铝 结构转变 绿色合成 

分 类 号：O611[理学—无机化学]