高等学校化学学报

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二十元环超大孔磷酸亚磷酸锌锰的合成与结构

杨扬, 赵永男, 余建国   

  1. 天津工业大学纳米结构材料研究所, 天津市改性与功能纤维重点实验室, 天津 300160
  • 收稿日期:2007-07-24 修回日期:1900-01-01 出版日期:2007-12-10 发布日期:2007-12-10
  • 通讯作者: 赵永男

Synthesis and Structure of Manganese Zinc Phosphate-phosphite with Extra Large Twenty-membered Ring Channels

YANG Yang, ZHAO Yong-Nan*, YU Jian-Guo   

  1. Institute of Nanostructured Materials, Tianjin Key Laboratory of Fiber Modification and Functional Fiber, Tianjin Polytechnic University, Tianjin 300160, China
  • Received:2007-07-24 Revised:1900-01-01 Online:2007-12-10 Published:2007-12-10
  • Contact: ZHAO Yong-Nan

摘要: 本文以1,3-环己二甲胺[1,3-Cyclohexanebis(methylamine), CHBMA]为模板剂, 采用水热法合成了微孔磷酸亚磷酸锌锰 [H2CHBMA][Zn1.5Mn(HPO3)2(PO4)]·H2O(命名为TJPU-3Mn), 单晶结构解析显示该化合物为首个与超大孔磷酸铝JDF-20具有相同拓扑结构的微孔晶体, 沿c方向具有二十元环超大孔道, 孔道中的CHBMA分子均为顺式构象, 有望用于分离和识别CHBMA异构体.

关键词: 水热合成, 磷酸亚磷酸锌锰, 单晶结构

Abstract: A novel three-dimensional manganese zinc phosphatophosphite [H2CHBMA][Zn1.5Mn(HPO3)2(PO4)]·H2O(TJPU-3Mn) with extra-large twenty-membered ring channels was isolated by 1,3-cyclohexanebis(methylamine) as the template under hydrothermal conditions. Single crystal structure refinement reveals that TJPU-3Mn crystallizes in the monoclinic space group C2/c, with cell parameters, a=3.3929(7) nm, b=1.3045(3) nm, c=0.89713(18) nm, β=104.37(3)°, V=3.8465(13) nm3, Z=2. The connectivities of the ZnO4, MnO4, PO4 and HPO3 groups create a three-dimensional porous architecture with extra-large twenty-membered ring channels intersected by eight-membered rings. It is the first structure analogue to the famous aluminophsphate JDF-20. More interestingly, the diprotonated CHBMA cations in the channel are all in cis configuration, indicating the potential for separation and recognition of CHBMA isomers. Powder X-ray patterns reveal the structure of TJPU-3Mn sustains after the emission of water molecules obtained by calcining at 150 ℃ for 2 h.

Key words: Hydrothermal synthesis, Zinc manganese phosphate-phosphite, Single crystal structure

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