磷酸铝分子筛[Al3P3O12F][C5H5NH]·0．2H2O的蒸气相合成与结构表征

Vapor Phase Transport Synthesis and Structure Characterization of an Aluminophosphate Molecular Sieve [Al_3P_3O_(12)F][C_5H_5NH]·0.2H_2O

采用蒸气相合成法以吡啶作为蒸气源,在吡啶气氛下磷酸铝固态凝胶被转化为一种三维骨架结构的磷酸铝微孔化合物,用X射线单晶衍射法测定了其晶体结构,[Al3P3O12F][C5H5NH]·0.2H2O微孔化合物属三斜晶系,空间群P-1(2),晶胞参数a=9.127(2),b=9.185(3),c=9.346(2),α=85.563(14)°,β=77.346(6)°,γ=89.628(17)°,V=762.2(4)3,Z=2,Dc=2.074Mg/m3,Mr=468.09,F(000)=474,μ=0.64mm-1.其和以前报道的磷酸铝分子筛UT-6具有相同的骨架结构,起始凝胶组分中的氟离子参与了骨架生成(Al-F-Al),骨架中有三种相互独立的8元环孔道互相交叉最终形成类似于AlPO4-CHA型沸石的笼型结构.XRD,TG-DTA研究结果表明,合成的样品具有较高的热稳定性,400℃煅烧后,其骨架结构保持不变.

By a vapor phase transport synthesis method, the aluminophosphate solid gel has been trans- formed into a 3-dimensional aluminophosphate framework under pyridine atmosphere. It＇s structure was solved by X-ray single crystal diffraction, which shows that the compound [Al3P3O12F][C5H5NH]·0.2H2O crystallizes in a triclinic system, space group P- 1 （2） with cell parameters a = 9.127（2） A, b =9.185（3） A, c = 9.346（2） A, α=85.563（14）°,β=77.346（6）°, γ=89.628（17）°, V=762.2（4） A^3, Z=2, Dc=2.074 Mg/m^3, Mr=468.09, F（000）=474 and μ=0.64 mm^-1. Its structure is identical to that of the previously reported compound UT-6, the fluorine ions as a component of starting gel are introduced into the framework and bridge the Al atoms, and the independent 8-ring channels in the framework are interconnected to constitute cage structures analogous to AlPO4-CHA zeolite-like. The results from XRD and TG-DTA analyses indicate that the sample has higher thermal stability, and its framework structure is intact after calcination at 400 ℃.