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A crystalline AlPO4-5 intermediate: designed synthesis, structure, and phase transformation
Dalton Transactions ( IF 4 ) Pub Date : 2017-08-21 00:00:00 , DOI: 10.1039/c7dt02772a
Cong Lin 1, 2, 3, 4, 5 , Jian Li 4, 5, 6, 7 , Fengjuan Pan 4, 5, 6, 7 , Yifang Zhao 4, 5, 6, 7 , Le Xu 4, 5, 6, 7 , Yanquan Yang 4, 5, 6, 7 , Xin Du 4, 5, 6, 7 , Xiaohuan Lin 4, 5, 6, 7 , Fuhui Liao 4, 5, 6, 7 , Jianhua Lin 4, 5, 6, 7 , Tao Yang 1, 2, 3, 4 , Junliang Sun 4, 5, 6, 7
Affiliation  

AlPO4-5 is the most extensively studied material in exploring the crystallization mechanism of aluminophosphate molecular sieves, and it can be synthesized using 4-dimethylaminopyridine (DMAP) as an organic structure-directing agent (OSDA). Achieving the AlPO4-5 intermediate in the crystalline form would be of great importance and significance for this purpose. In this study, we proposed a concept that by carefully regulating the synthesis conditions, crystalline alumimophosphate intermediates could be rationally prepared. A crystalline AlPO4-5 intermediate, (C7H11N2)2(H3O)(Al3P4O16)·(H2O)2.5 (1), was, therefore, synthesized by significantly increasing the amounts of orthophosphoric acid and DMAP. The intermediate 1 consists of alternating organic DMAP and inorganic [Al3P4O16]3− layers with abundant hydrogen bonds and can transform to the AlPO4-5 framework upon heating in air or through a steam-assisted conversion (SAC) method. To unravel the role of DMAP in the transformation, pure AlPO4-5 (2) was also synthesized by altering the synthesis conditions. The supramolecular assembly templating (SAT) effects of DMAP in 1 and 2 were verified via fluorescence spectra. Thus, the π–π stacking interactions between the DMAP molecules and the abundant hydrogen bonds between the adjacent layers are considered to be important for the phase transformation of 1. This crystalline intermediate would promote the understanding of the crystallization mechanism in the system of aluminophosphate molecular sieves.

中文翻译:

结晶的AlPO 4 -5中间体:设计合成,结构和相变

AlPO 4 -5是探索铝磷酸盐分子筛结晶机理的最广泛研究的材料,可以使用4-二甲基氨基吡啶(DMAP)作为有机结构导向剂(OSDA)来合成。为此目的,以结晶形式获得AlPO 4 -5中间体将具有重要意义。在这项研究中,我们提出了一个概念,即通过仔细调节合成条件,可以合理地制备结晶磷酸铝铝中间体。结晶AlPO 4 -5中间体(C 7 H 11 N 22(H 3 O)(Al 3 P 4 O因此,通过显着增加正磷酸和DMAP的量来合成16)·(H 2 O) 2.5 1)。中间体1由交替的有机DMAP和具有丰富氢键的无机[Al 3 P 4 O 16 ] 3−层组成,可以在空气中加热或通过蒸汽辅助转化(SAC)方法转化为AlPO 4 -5骨架。为了揭示DMAP在转化中的作用,还通过改变合成条件合成了纯AlPO 4 -5( 2)。DMAP在分子中的超分子组装模板(SAT)效应。通过荧光光谱验证图1和图2。因此,DMAP分子与相邻层之间丰富的氢键之间的π-π堆积相互作用被认为对1的相变很重要。该结晶中间体将促进对磷酸铝分子筛系统中结晶机理的理解。
更新日期:2017-09-20
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