在无有机模板剂的条件下,以Na+离子为结构导向剂,通过水热合成法制备了一种与利用1,3-丙二胺合成的Uio-14具有相同层结构的二维磷酸铝化合物Na4[A14P4O18].H2O(1),通过单晶X射线衍射确定了其拓扑结构.利用粉末x射线衍射、扫描电子显微镜、电感耦合等离子体(ICP)元素分析和热重分析等对其物理化学性质进行了表征.结果表明,化合物1属于单斜晶系,空间群为Jp2,/c,晶胞参数a=1.00887(9)nm,b=0.86747(8)nm,c=0.97580(9)nm,V=0.77387(12)nm3,Z=2,其阴离子层由铝氧三角双锥(A10,)和磷氧四面体(PO。)构成,层间通过Na+离子平衡电荷;与Uio-14相比,化合物1具有更高的热稳定性,在400℃空气条件下煅烧后结构仍然保持完好.对化合物1的质子电导性能测试结果表明,相比于传统的分子筛类材料,化合物1展现出优异的质子电导性能,在55℃下质子电导率可达到1.19×10-3S/cm。
In the organotemplate-free system, a layered aluminophosphate Na4 [ Al4 P4 O18 ] · H2 O ( 1 ) was synthesized with Na+ ion as the structure-directing agent under hydrothermal condition. The structure was determined by single-crystal X-ray diffraction, and further characterized by powder X-ray diffraction( PXRD) , scanning electron microscopy( SEM) , inductively coupled plasma( ICP) and thermal gravimetric( TG) analy-ses. Compound 1 crystallizes in the monoclinic space group P21/c with a=1. 00887(9) nm, b=0. 86747(8) nm, c=0. 97580(9) nm, V=0. 77387(12) nm3, and Z=2, and its framework consists of AlO5 and PO4 units. Compound 1 possesses high thermal stability, and the crystal structure remains unchanged after calcination at 400 ℃ in air. The proton conductivity measurement gives that compound 1 possesses excellent conductivity withσthe value of 1. 19 ×10-3 S/cm when immersed in water at 55℃, which is higher than those of traditional zeolitic materials.