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Citation: LU Hui-Ying, LIU Shu, XU Jun, YAN Wen-Fu, LIU Zhi-Qiang, DENG Feng, XU Ru-Ren. Crystallization Process of Open-Framework Aluminophosphate AlPO4-12[J]. Chinese Journal of Inorganic Chemistry, ;2015, 31(9): 1885-1893. doi: 10.11862/CJIC.2015.251 shu

Crystallization Process of Open-Framework Aluminophosphate AlPO4-12

  • 1.

    1. State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012, China;

  • 2.

    2. National Center for Mass spectrometry, Changchun Institute of Applied Chemistry, Changchun 130022, China;

  • 3.

    3. State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, National Center for Magnetic Resonance in Wuhan, Wuhan Institute of Physics and Mathematics, Chinese Academy of Sciences, Wuhan 430071, China

  • Corresponding author: YAN Wen-Fu,  XU Ru-Ren, 
  • Received Date: 8 June 2015
    Available Online: 24 July 2015

    Fund Project: 国家自然科学基金(No.21171063) (No.21171063)国家优秀青年科学基金(No.21222103) (No.21222103)国家重点基础研究发展规划项目(No.2011CB808703) (No.2011CB808703)长江学者和创新团队发展计划(No.IRT101713018)资助项目。 (No.IRT101713018)

  • Upon heating the initial mixture with the composition of nAl2O3:nP2O5:nen:nH2O=1:1:2:226 at 200℃ for 12 h, where en is ethylenediamine, a three-dimensional open-framework aluminophosphate AlPO4-12 was obtained. The crystallization process of AlPO4-12 was investigated using X-ray diffraction, elemental analysis, pH measurement, liquid NMR, and electrospray ionization mass spectra (ESI-MS). On the basis of the ESI-MS data, a method was developed to systematically enumerate the formula of the fragments formed during the crystallization of AlPO4-12. It was found that intermediate phases of layered aluminophosphates UiO-15 and UiO-13 were formed prior the crystallization of AlPO4-12. The concentration of Al species in the liquid throughout the crystallization was extremely low. A gradual increase of P-OH group in the P species in the liquid and a gradual protonation of ethylenediamine during the crystallization were observed. The formation of 4- and 6-membered rings was confirmed by the ESI-MS data. The utilization of ESI-MS in the investigation of the crystallization process of microporous crystalline materials may allow us to determine the structural information and the formula of the fragments formed during the crystallization.
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