Acta Chimica Sinica ›› 2011, Vol. 69 ›› Issue (24): 3033-3036.DOI: 10.6023/A1106152 Previous Articles     Next Articles

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草酸/四丙基溴化铵体系中磷酸锆晶体的离子热合成与表征

刘雷*, 王巍, 危海波, 张通, 董晋湘   

  1. (太原理工大学精细化工研究所 太原 030024)
  • 收稿日期:2011-06-15 修回日期:2011-08-01 出版日期:2011-12-28 发布日期:2011-08-26
  • 通讯作者: 刘雷 E-mail:liulei@tyut.edu.cn
  • 基金资助:

    国家自然科学基金;山西省青年科技研究基金

Ionothermal Synthesis and Characterization of Crystalline Zirconium phosphate from Oxalic Acid/Tetrapropyl Ammonium Bromide System

LIU Lei, WANG Wei, WEI Hai-Bo, ZHANG Tong, DONG Jin-Xiang   

  1. (Institute of Special Chemicals, Taiyuan University of Technology, Taiyuan 030024)
  • Received:2011-06-15 Revised:2011-08-01 Online:2011-12-28 Published:2011-08-26
  • Contact: Lei Liu E-mail:liulei@tyut.edu.cn

By ionothermal synthesis method, a series of syntheses have been performed in an attempt to synthesize novel zirconium phosphate materials in an oxalic acid/tetrapropyl ammonium bromide ionic eutectic mixture. The two different zirconium phosphate materials, α-Zr(HPO4)2•H2O and (NH4)Zr2(PO4)3 have been achieved by changing the synthetic conditions, tetrapropyl ammonium cation could not play its template role to form a new zirconium phosphate and the latter was synthesized at a high temperature (220 ℃) by templating the cation in situ generated from the ionothermal decomposition of the tetrapropyl ammonium (TPA) component. However, after adding a small amount of N-containing heterocyclic compound (piperazine), a known open-framework zirconium phosphate with 8-ring pore channels was obtained. The protonated piperazine not only plays a template role to form the zirconium phosphate framework but also acts as counter-ions to balance the anion framework. The used deep-eutectic solvent, therefore, can be used as an excellent ionic reaction medium to synthesize zirconium phosphate materials, the organic amine could be added to the initial reaction mixture to induce zirconium phosphate framework.

Key words: ionothermal synthesis, eutectic mixture, zirconium phosphate, crystal structure