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柠檬酸钒(Ⅳ)酰钡热分解制备焦钒酸钡Ba2[VO(cit)]2·4H2O纯相
Barium Pyrovanadate Prepared from Thermal Decomposition of Barium Dimeric(citrato)oxovanadium(Ⅳ)
【摘要】 由柠檬酸钒酰钠与氯化钡的水溶液反应得到柠檬酸钒 ( )酰钡配合物 .通过凝胶扩散法得到该配合物的晶体 ,并用 X射线衍射测定其结构 .该晶体的空间群为 P2 1 n,晶胞参数 a=0 .9896 0 ( 9) nm,b=0 .87746 ( 5) nm,c=1 .2 1 0 75( 8) nm,β=93.1 1 9( 7)°,Z=2 ,R=0 .0 45.该配合物在空气中分解得到白色粉末 ,经 XRD粉末衍射分析确定为焦钒酸钡纯相 .
【Abstract】 Barium dimeric(citrato)oxovanadium(Ⅳ) tetrahydrates Ba\-2\{\\}\-2·4H\-2O has been prepared by the reaction of sodium dimeric(citrato)oxovanadium(Ⅳ) and barium chloride. Its single crystal was obtained by diffusion method in silica\|gel. The complex crystallizes in monoclinic space group P2\-1/n with unit cell parameters: a =0\^989 60(9) nm, b =0\^877 46(5) nm, c =1\^210 75(8) nm, β =93\^119(7)°, Z =2, R =0\^045 for 1 260 reflections with I≥3σ(I) . Thermal decomposition shows the barium salt undergoes with three major processes, including dehydration, ligand elimination and formation of mixed oxide as its final step, in which the latter is confirmed as pure phase of barium pyrovanadate by XRD analysis.
【Key words】 Citrate method; Oxovanadium complexes; Barium vanadate; Crystal Structure; Composite oxide;
- 【文献出处】 高等学校化学学报 ,CHEMICAL RESEARCH IN CHINESE UNIVERSITIES , 编辑部邮箱 ,1999年08期
- 【分类号】O614.2
- 【被引频次】4
- 【下载频次】129