Chinese Journal of Applied Chemistry ›› 2015, Vol. 32 ›› Issue (2): 214-220.DOI: 10.11944/j.issn.1000-0518.2015.02.140133

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Synthesis and Catalytic Activity of a Strandberg-type Molybdophosphate Modified by Organic Cations

LIU Zhaoyub, ZHU Haotiana, LU Mingdaa, LI Xiaohuia, AN Yuea, *, ZHANG Lancuia, *   

  1. a School of Chemistry and Chemical Engineering,Liaoning Normal University,Dalian,Liaoning 116029
    b School of Chemistry,Jilin University,Changchun 130032,China
  • Received:2014-04-16 Revised:2014-09-24 Published:2015-02-10 Online:2015-02-10
  • Contact: Corresponding author:AN Yue, professor; Tel:0411-82156550; Fax:0411-82158559; E-mail:anyue_11@163.com; Research interests:organic synthesis
  • Supported by:

    ; Supported by National Undergraduate Innovation and Entrepreneurship Training Program(No.201310165014), the Natural Science Foundation of Liaoning Province(No.2013020128)

Abstract:

A Strandberg-type molybdophosphate {H4(H2biim)5(C(NH2)3)4}[H2P2Mo5O23]2·8H2O(1, H2biim=2,2'-biimidazole) modified by 2,2'-biimidazole and guanidinium cations was self-assembled in aqueous solution of pH=34 containing sodium molybdate, 2,2'-biimidazole, guanidine hydrochloride, and an excess of phosphoric acid, and was characterized by single crystal X-ray diffraction analysis, infrared spectroscopy(FT-IR), themogravimetry-differential thermal analysis(TG-DTA) and X-ray powder diffraction(XRD). Compound 1 has a stable 3D organic-inorganic hybrid framework. It was used as a catalyst for carbonyl-protection. The synthesis of cyclohexanone ethylene ketal was performed as an example to investigate some influence factors on the yield, such as catalyst loading, molar ratio of reactants and reaction time. The optimal conditions are: the molar ratio of catalyst(based on Mo) to ketone is 1:300, the molar ratio of ketone to alcohol is 1:1.4, and reaction time is 2.5 h. The catalytic activity of compound 1 for the synthesis of four other ketals was evaluated. The results show that compound 1 is a better catalyst for the synthesis of cyclohexanone ethylene ketal.

 

Key words: organic cation, Strandberg structure, molybdophosphate, carbonyl-protection, catalysis

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