机构地区:[1]State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012, P. R. China [2]State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Institute of Physics and Mathematics, Chinese Academy of Sciences, Wuhan 430071, P R. China [3]Jilin Province Product Quality Supervision Testing Institute, Changchun 130012, P. R. China
出 处:《Chemical Research in Chinese Universities》2017年第6期853-859,共7页高等学校化学研究(英文版)
基 金:Supported by the National Natural Science Foundation of China(Nos.21571075, 21320102001, 21621001), the National Key Research and Development Program of China(No.2016YFB0701100) and the Programme of Introducing Talents of Discipline to Universities(the 111 Project), China(No.B 17020).
摘 要:The crystallization behavior of the initial mixture with the composition of Al2O3:4.0P2O5:3.0 diethylenetriamine(DETA):xHF:153H2O was investigated at 180 ℃, where 0≤x≤3. If x≤1.8, three-dimensional openframework aluminophosphate AIPO-CJ31 was obtained. If 2 ≤x≤3, a chain-like aluminophosphate(1) was obtained. The crystallization process of both compounds was investigated by means of powder X-ray diffraction(XRD) and the concentrations of A1 and P in the liquid product during the crystallization process were analysed by means of induc- tively coupled plasma atomic emission spectroscopy(ICP-AES). The evolution of the coordination state of A1, P and F during the crystallization was monitored with 27A1, 31p and 19F MAS NMR technique. The influence of the fluoride ions and the source of fluoride ions on the structure-directing effect of DETA was discussed. It was found that the fluoride ions changed the crystallization direction of the initial mixture, i.e., the structure-directing effect of DETA, via altering the distribution or micro-structure of the inorganic fragments.The crystallization behavior of the initial mixture with the composition of Al2O3:4.0P2O5:3.0 diethylenetriamine(DETA):xHF:153H2O was investigated at 180 ℃, where 0≤x≤3. If x≤1.8, three-dimensional openframework aluminophosphate AIPO-CJ31 was obtained. If 2 ≤x≤3, a chain-like aluminophosphate(1) was obtained. The crystallization process of both compounds was investigated by means of powder X-ray diffraction(XRD) and the concentrations of A1 and P in the liquid product during the crystallization process were analysed by means of induc- tively coupled plasma atomic emission spectroscopy(ICP-AES). The evolution of the coordination state of A1, P and F during the crystallization was monitored with 27A1, 31p and 19F MAS NMR technique. The influence of the fluoride ions and the source of fluoride ions on the structure-directing effect of DETA was discussed. It was found that the fluoride ions changed the crystallization direction of the initial mixture, i.e., the structure-directing effect of DETA, via altering the distribution or micro-structure of the inorganic fragments.
关 键 词:Zeolite ALUMINOPHOSPHATE OPEN-FRAMEWORK Structure-directing effect FLUORIDE
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