应用化学 ›› 2011, Vol. 28 ›› Issue (03): 284-289.DOI: 10.3724/SP.J.1095.2011.00345

• 研究论文 • 上一篇    下一篇

(C5H7N2)3(AsMo12O40)·3C5H6N2·2H2O的水热合成、晶体结构及催化性能

蔡铁军*,申晓明,吕数子,彭振山,刘金,邓谦   

  1. (湖南科技大学化学化工学院 湘潭 411201)
  • 收稿日期:2010-06-17 修回日期:2010-08-13 出版日期:2011-03-10 发布日期:2011-03-10
  • 通讯作者: 蔡铁军,教授; Tel:0731-58290491; E-mail:tjcai53@163.com; 研究方向:多酸化学及多相催化
  • 基金资助:
    理论化学与分子模拟省部共建教育部重点实验室资助项目(教技函[2008]153号)

Hydrothermal synthesis, crystal structure and Catalytic performance of (C5H7N2)3(AsMo12O40)·3C5H6N2·2H2O

CAI Tiejun*, SHEN Xiaoming, LV Shuzi, PENG Zhenshan, LIU Jin, DENG Qian   

  1. (School of Chemistry and Chemical Engineering,Hunan University of Science and Technology,Xiangtan 411201)
  • Received:2010-06-17 Revised:2010-08-13 Published:2011-03-10 Online:2011-03-10
  • Contact: tiejun cai

摘要:

采用水热法合成了一种新的3-氨基吡啶砷钼多金属氧酸盐配合物(C5H7N2)3(AsMo12O40)·3C5H6N2·2H2O。 通过单晶X射线衍射、红外光谱、紫外光谱和差热-热重对其进行了表征。 用催化消除丙酮的反应为模式反应,测试了配合物的催化性能。 研究结果表明,标题配合物是由Keggin结构[AsMo12O40]3-杂多阴离子、[C5H7N2]+阳离子、[C5H6N2]分子和结晶水分子组成。 配合物属于单斜晶系,P21/n空间群;晶胞参数a=1.33820(12) nm,b=2.2542(2) nm,c=1.9848(2) nm,β=100.27(3)°,V=5.8912(10) nm3,Z=4,Rgt(F)=0.0590,wRref(F2)=0.1882。 配合物对催化消除丙酮具有较好的的活性,催化实验结果表明,160 ℃下,0.20 g的催化剂可将初始浓度均为1.3 g/m3,流速为4.5 mL/min的丙酮完全消除。

关键词: 多金属氧酸盐, 丙酮, 水热合成, 晶体结构, 催化性能

Abstract:

A novel compound, (C5H7N2)3(AsMo12O40)·3C5H6N2·2H2O, has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction, IR, UV/Vis and TG-DTA. Using catalytic elimination reaction of acetone as a model reaction, the catalytic performance of the title compound has been tested. The results indicate that the structure of the title compound consists of [AsMo12O40]3- heteropolyoxoanion, [C5H7N2]+ cations, [C5H6N2] molecules and water molecules. The compound crystallizes in the monoclinic, space group P21/n, a=1.33820(12) nm,b=2.2542(2) nm,c=1.9848(2) nm,β=100.27(3) °,V=5.891 2(10) nm3,Z=4,Rgt(F)=0.0590,wRref(F2)=0.1882. The compound has a good catalytic activity for the elimination of acetone. When the initial concentration of acetone is 1.3 g/m3 in the air with a flow velocity of 4.5 mL/min, the acetone is completely eliminated at 160 ℃ over 0.20 g of the title compound.

Key words: polyoxometalate, acetone, hydrothermal synthesis, crystal structure, catalytic performance

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