Influence of Fluoride Ions on the Structure-directing Effect of Organic Amine in the Synthesis of Aluminophosphate Open-frameworks

doi:10.1007/s40242-017-7131-9

高等学校化学研究 ›› 2017, Vol. 33 ›› Issue (6): 853-859.doi: 10.1007/s40242-017-7131-9

Influence of Fluoride Ions on the Structure-directing Effect of Organic Amine in the Synthesis of Aluminophosphate Open-frameworks

TIAN Ye^1,3, XU Jun², WANG Zi¹, DENG Feng², XU Ruren¹, YAN Wenfu¹

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

收稿日期:2017-04-11 修回日期:2017-06-26 出版日期:2017-12-01 发布日期:2017-07-21
通讯作者: YAN Wenfu,E-mail:yanw@jlu.edu.cn E-mail:yanw@jlu.edu.cn
基金资助:
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.B17020).

Influence of Fluoride Ions on the Structure-directing Effect of Organic Amine in the Synthesis of Aluminophosphate Open-frameworks

TIAN Ye^1,3, XU Jun², WANG Zi¹, DENG Feng², XU Ruren¹, YAN Wenfu¹

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

Received:2017-04-11 Revised:2017-06-26 Online:2017-12-01 Published:2017-07-21
Contact: YAN Wenfu,E-mail:yanw@jlu.edu.cn E-mail:yanw@jlu.edu.cn
Supported by:
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.B17020).

摘要/Abstract

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 open-framework aluminophosphate AlPO-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 Al and P in the liquid product during the crystallization process were analysed by means of inductively coupled plasma atomic emission spectroscopy(ICP-AES). The evolution of the coordination state of Al, P and F during the crystallization was monitored with ²⁷Al, 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

Abstract: 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 open-framework aluminophosphate AlPO-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 Al and P in the liquid product during the crystallization process were analysed by means of inductively coupled plasma atomic emission spectroscopy(ICP-AES). The evolution of the coordination state of Al, P and F during the crystallization was monitored with ²⁷Al, 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.

Key words: Zeolite, Aluminophosphate, Open-framework, Structure-directing effect, Fluoride

TIAN Ye, XU Jun, WANG Zi, DENG Feng, XU Ruren, YAN Wenfu. Influence of Fluoride Ions on the Structure-directing Effect of Organic Amine in the Synthesis of Aluminophosphate Open-frameworks[J]. 高等学校化学研究, 2017, 33(6): 853-859.

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Influence of Fluoride Ions on the Structure-directing Effect of Organic Amine in the Synthesis of Aluminophosphate Open-frameworks

Influence of Fluoride Ions on the Structure-directing Effect of Organic Amine in the Synthesis of Aluminophosphate Open-frameworks

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