化学学报 ›› 1993, Vol. 51 ›› Issue (4): 368-372. 上一篇    下一篇

研究论文

固相配位化学反应研究 53: 一步法室温(准室温)固相化学反应合成8-羟基喹啉的Co(II)、Ni(II)、Cu(II)、Zn(II)配合物

贾殿赠;李昌雄;傅岩;忻新泉   

  1. 南京大学配位化学研究所
  • 发布日期:1993-04-15

Studies on solid state reactions of coordination compounds. 53. Synthesis of 8-hydroxyquinoline complexes with Co(II), Ni(II), Cu(II) and Zn(II) by one step solid state reaction

JIA DIANZENG;LI CHANGXIONG;FU YAN;XIN XINQUAN   

  • Published:1993-04-15

本文研究了Cu(OAc)2.4H2O、Ni(OAc)2.4H2O、Cu(OAc)2.H2O、Zn(OAc)2.2H2O与8-羟基喹啉在室温(准室温≤40℃)条件下的固-固相化学反应。讨论了反应物结构对固相反应的影响。通过固相反应一步合成了相应的配合物Co(oxin)2.2H2O、Ni(oxin)2.2H2O、Cu(oxin)2、Zn(oxin)2.H2O。经失重测定, 元素分析, IR, XRD,DTA测定, 确定了固相产物的组成。与液相合成方法比较, 固相反应合成配合物不用溶液, 产率较高等优点。

关键词: 红外分光光度法, 元素分析, 锌络合物, X射线衍射分析, 铜络合物, 钴络合物, 镍络合物, 差热分析, 羟基喹啉类, 固相反应

A-a- and A-b-K6H[GeW9V3O40].xH2O were synthesized from their lacunary precursors a- and b-GeW9O3410-, and characterized by elemental anal., IR, cyclic voltammetry and 51V and 183W NMR. The 183W NMR spectra of the anions consist of 2 lines (intensity ratio 2:1) as expected for the C3v structures of the trisubstituted A-a- and A-b-Keggin anions. The 2Jw-o-w couplings of the anions exhibits sharper lines (19.35 and 16.73 Hz, resp.), confirming the A-type [GeW9V3O40]7- structure, that is the new complexes contain the substituted V in adjacent corner-shared octahedra of a- and b-Keggin structures, resp.

Key words: INFRARED SPECTROPHOTOMETRY, ELEMENTAL ANALYSIS, ZINC COMPLEX, X-RAY DIFFRACTION ANALYSIS, COPPER COMPLEX, COBALT COMPLEX, NICKEL COMPLEX, DIFFERENTIAL THERMAL ANALYSIS, HYDROXY QUINOLINES, SOLID PHASE REACTION

中图分类号: