SCI和EI收录∣中国化工学会会刊

›› 2009, Vol. 17 ›› Issue (1): 58-63.

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Preparation, Characterization and Catalytic Behavior of 12-Molybdophosphoric Acid Encapsulated in the Supercage of Cs+-exchanged Y Zeolite

魏瑞平1,2, 郭麦平1, 王军1   

  1. 1. State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing 210009, China;
    2. School of Chemistry and Chemical Engineering, Southeast University, Nanjing 211189, China
  • 收稿日期:2008-01-16 修回日期:2008-10-28 出版日期:2009-01-28 发布日期:2009-01-28
  • 通讯作者: WANG Jun, E-mail: junwang@njut.edu.cn
  • 基金资助:
    Supported by the National Natural Science Foundation of China (20476046);the “Qinglan” Project of Jiangsu Province for Young Researchers

Preparation, Characterization and Catalytic Behavior of 12-Molybdophosphoric Acid Encapsulated in the Supercage of Cs+-exchanged Y Zeolite

WEI Ruiping1,2, GUO Maiping1, WANG Jun1   

  1. 1. State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemistry and Chemical Engineering, Nanjing University of Technology, Nanjing 210009, China;
    2. School of Chemistry and Chemical Engineering, Southeast University, Nanjing 211189, China
  • Received:2008-01-16 Revised:2008-10-28 Online:2009-01-28 Published:2009-01-28
  • Supported by:
    Supported by the National Natural Science Foundation of China (20476046);the “Qinglan” Project of Jiangsu Province for Young Researchers

摘要: In order to solve the serious leaching problem of supported heteropoly acid catalysts in polar reaction media,12-molybdophosphoric acid encapsulated in the supercage of Cs+-exchanged Y zeolite was prepared by the "ship in the bottle" synthesis.The influence of ion-exchange conditions and the synthesis parameters on the encapsulation of PMo12 were investigated.The obtained solid sample was characterized by X-ray diffraction(XRD),31P magic angle spin nuclear magnetic resonance(MAS NMR) and Fourier Transform Infrared Spectroscopy(FT-IR),and its catalytic activity in the esterification of acetic acid and n-butanol was tested.The ion-exchange time,concentration of aqueous Cs+ solution,pH value,and amount of Mo added in the synthesis mixture were revealed to influence the encapsulation very remarkably.Under the optimal conditions,12-molybdophosphoric acid could be successfully encapsulated in the supercage of CsY zeolite,and the samples showed considerable catalytic activity and excellent reusability in the esterification reaction.

关键词: Y zeolite, 12-molybdophosphoric acid, ship in the bottle, esterification

Abstract: In order to solve the serious leaching problem of supported heteropoly acid catalysts in polar reaction media, 12-molybdophosphoric acid encapsulated in the supercage of Cs+-exchanged Y zeolite was prepared by the "ship in the bottle" synthesis.The influence of ion-exchange conditions and the synthesis parameters on the encapsulation of PMo12 were investigated.The obtained solid sample was characterized by X-ray diffraction(XRD), 31P magic angle spin nuclear magnetic resonance(MAS NMR) and Fourier Transform Infrared Spectroscopy(FT-IR), and its catalytic activity in the esterification of acetic acid and n-butanol was tested.The ion-exchange time, concentration of aqueous Cs+ solution, pH value, and amount of Mo added in the synthesis mixture were revealed to influence the encapsulation very remarkably.Under the optimal conditions, 12-molybdophosphoric acid could be successfully encapsulated in the supercage of CsY zeolite, and the samples showed considerable catalytic activity and excellent reusability in the esterification reaction.

Key words: Y zeolite, 12-molybdophosphoric acid, ship in the bottle, esterification