知识与财富的链接
以二氯乙二肟为起始原料,通过一锅法合成了四水合1,1'-二羟基-5,5'-联四唑钠盐(SBTD·4H2O),并用红外、元素分析、扫描电子显微镜对其进行了表征,测试了目标化合物的单晶结构,结果表明其属于三斜晶系,P-1空间群,晶胞参数为a=5.6440(11),b=6.4476(17),c=8.303(11),α=100.131(5)°,β=96.789(3)°,γ=112.157(3)°,V=1,Dc=1.761 g·cm-3,F(000)=146,μ(Mo Kα)=0.227 mm-1。采用热重-差示扫描量热联用(TG-DSC)对其进行了热行为分析,在加热速率为10 K·min-1的条件下,该化合物从83.9℃开始失去结晶水,368.1℃开始分解,分解峰值温度为398.6℃,热稳定性良好。依据GJB772A-1997对SBT D·4H2O的感度进行了测试,撞击感度H50100 cm,摩擦感度为0%,这表明其对机械撞击和摩擦不敏感。
Sodium 5, 5′-bistetrazole-1, 1′-diolate tetrahydrate (SBTD·4H2O), a key intermediate for the synthesis of energetic salts based on 1, 1′-dihydryoxl-5, 5′-bistetrazole (BTD), was synthesized by one-pot using dichloroglyoxime as starting material, and was characterized by infrared spectrum (IR), elemental analysis (EA) and scanning electron microscopy (SEM). The crystal structure of SBTD·4H2O was determined by X-ray diffraction and its thermal behavior was determined by differential scanning calorimetry (DSC)-thermogravimetric (TG) analysis. Additionally, the impact and friction sensitivity of SBTD·4H2O were determined according to GJB772A-1997. Results show that SBTD·4H2O belongs to triclinic space groups P-1 with the density of 1.761 g·cm-3, and the cell parameters are as following: a=5.6440(11) Å, b=6.4476(17) Å, c=8.303(11) Å, α=100.131(5)°, β=96.789(3)°, γ=112.157(3)°, V=1, Dc=1.761 g·cm-3, F(000)=146, μ(Mo Kα)=0.227 mm-1. SBTD·4H2O starts to loss the crystal water at 84.4 ℃ with the heating rate of 10 K·min-1, and it begins to decompose at 368.8 ℃ with the peak decomposition temperature of 398.6 ℃, which demonstrates that SBTD·4H2O has good thermal stability. H50 of SBTD·4H2O is greater than 100 cm and friction sensitivity is 0%, showing the title compound insensitive to impact and friction.
