Synthesis, Crystal Structure and Thermal Behavior of GZTO·H2O  

作　　者：钟益堂 黄洁 宋纪蓉 徐抗震 赵丹 王立勤 张新瑜 

机构地区：[1]Department of Chemical Engineering/Shaanxi Key Laboratory of Physico-lnorganic Chemistry, Northwest University, Xi'an, Shaanxi 710069, China [2]Conservation Technology Department, the Palace Museum, BeOing 100009, China

出　　处：《Chinese Journal of Chemistry》2011年第8期1672-1676,共5页中国化学（英文版）

基　　金：Project Supported by the National Natural Science Foundation of China （No. 20803058） and the Natural Science Foundation of Shaanxi Province （No. 2007B08）.

摘　　要：Guanidimium-4,4-azo-l-hydro-1,2,4-triazol-5-one （GZTO·H2O） was synthesized from 4-amino-1,2,4-triazol- 5-one as a starting material by two-step including oxidation coupling using acid KMnO4 and reaction with （NH2）2C=NHoHNO3 （GN） in KOH solution. The single crystal of the title compound was obtained by slow evapo- ration method at room temperature, and its structure was firstly determined with X-ray single-crystal diffractometer. It is a orthorhombic crystal, space group Pbca with cell dimensions of a = 1.0459（2） nm, b =- 1.3584（3） nm, c= 1.6103（3） nm, a= 90.00（10）°, β=90.00（11）°,γ=90.00（11）°, V=2.2878（8） nm3, Z=8, De= 1.587 gocm-3, F（000） = 1136,/l = 0.132 mm- 1, R1 = 0.0455, wR2 = 0. 1397. The thermal behavior of GZTO·H2O was studied under a non-isothermal condition by DSC-TGA method, and its thermal decomposition process can be divided into three stages, and the first stage is an intense exothermic decomposition process. The second stage and the third stage are slow exothermic decomposition processes. The critical temperature of thermal explosion is 237.74℃.Guanidimium-4,4-azo-l-hydro-1,2,4-triazol-5-one （GZTO·H2O） was synthesized from 4-amino-1,2,4-triazol- 5-one as a starting material by two-step including oxidation coupling using acid KMnO4 and reaction with （NH2）2C=NHoHNO3 （GN） in KOH solution. The single crystal of the title compound was obtained by slow evapo- ration method at room temperature, and its structure was firstly determined with X-ray single-crystal diffractometer. It is a orthorhombic crystal, space group Pbca with cell dimensions of a = 1.0459（2） nm, b =- 1.3584（3） nm, c= 1.6103（3） nm, a= 90.00（10）°, β=90.00（11）°,γ=90.00（11）°, V=2.2878（8） nm3, Z=8, De= 1.587 gocm-3, F（000） = 1136,/l = 0.132 mm- 1, R1 = 0.0455, wR2 = 0. 1397. The thermal behavior of GZTO·H2O was studied under a non-isothermal condition by DSC-TGA method, and its thermal decomposition process can be divided into three stages, and the first stage is an intense exothermic decomposition process. The second stage and the third stage are slow exothermic decomposition processes. The critical temperature of thermal explosion is 237.74℃.

关 键 词：X-ray diffraction high-nitrogen energetic materials 4-amino-1 2 4-triazol-5-one （ATO） crystal struc-ture azo-compound THERMOCHEMISTRY 

分 类 号：O614.121[理学—无机化学] TM612[理学—化学]