高等学校化学学报

高等学校化学学报 ›› 2000, Vol. 21 ›› Issue (7): 1005.

• 论文 • 上一篇    下一篇

[Ni(CHZ)3](TNR)·5H2O的制备、晶体结构和热分解机理

吕春华1, 张同来1, 张建国1, 蔡瑞娇1, 郁开北2   

  1. 1. 北京理工大学机电工程系, 北京 100081;
    2. 中国科学院成都分院分析测试中心, 成都 610041
  • 收稿日期:1999-09-16 出版日期:2000-07-24 发布日期:2000-07-24
  • 通讯作者: 张同来(1960年出生),男,博士,教授,从事含能配合物研究.

Preparation, Crystal Structure and Thermal Decomposition Mechanisms of [Ni(CHZ)3] (TNR)·5H2O

LU Chun-Hua1, ZHANG Tong-Lai1, ZHANG Jian-Guo1, CAI Rui-Jiao1   

  1. 1. Department of Mechano electric Engineering, Beijing Institute of Technology, Beijing 100081, China;
    2. Centerof Analysis Testof Chengdu Branch, Chinese Academyof Sciences, Chengdu 610041, China
  • Received:1999-09-16 Online:2000-07-24 Published:2000-07-24

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摘要： 用2,4,6三硝基间苯二酚(斯蒂芬酸,TNR)镍的水溶液和碳酰肼(CHZ,NH2NHCONHNH2)水溶液反应,制备出配合物[Ni(CHZ)3](TNR)·5H2O,测定了其晶体结构,并用TGDTG,DSC和IR技术研究了其热分解机理.该晶体属三斜晶系,P1空间群,晶胞参数a=1.04540(10)nm,b=1.1671(2)nm,c=1.2278(2)nm,α=109.190(10)°,β=121.168(12)°,γ=99.700(10)°,V=1.2613(3)nm3,Z=2,Dc=1.744g/cm3,μ(Mo,Kα)=0.873mm-1,F(000)=688,R=0.0419,Rw=0.1053.在该配合物分子中,碳酰肼为双齿配体,由羰基O原子和1位N原子与Ni2+离子配位,分子中共形成3个五元平面螯合环,中心离子为六配位八面体结构.该配合物在程序升温条件下,分两步脱去所含结晶水,第一步失去4个结晶水,第二步失去1个结晶水,在500℃时的最终分解产物为Ni2O3.

关键词: 碳酰肼, 斯蒂芬酸镍, 晶体结构, 热分解机理

Abstract: The compound [Ni(CHZ)3] (TNR)·5H2Owas prepared by using nickel carbonate, the aqueous solution of styphnic acid and carbohydrazide as reagents. The crystal structure of [Ni(CHZ)3] (TNR)·5H2Owas determined by using single crystal diffraction analysis. Thermal decomposition mechanisms of the compound were studied by using TG DTG, DSCand IRtechniques. The crystalline was in triclinic system with space group P1 The unit cell parameters are as follows: a =1.04540(10) nm, b =1.1671(2) nm , c =1.2278(2) nm, α =109.190(10)°, β =121.168(12)°, γ =99.700(10)°, {V =}1.2613(3) nm3, Z =2, Dc=1.744 g/cm3, μ(Mo, Kα)=0.873 mm-1 , F (000)=688, R =0.0419, Rw=0.1053. Carbohydrazide served as a bidentate, coordinating to nickel cation with its carbonyl oxygen atom and the first nitrogen atom so that a five membered chelating ring is formed. There are three such rings in the molecule. The coordination number is six and its configuration is deformed octahedral. The decomposition mechanisms confirm that the first dehydration process lost four water molecules, and the second step dehydrate one molecule. The residue is Ni2O3 at 500 ℃, finally.

Key words: Carbohydrazide, Nickel styphnate, Crystal structure, Thermal decomposition mechanism

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