四水合1,1'-二羟基-5,5'-联四唑钠盐的合成、晶体结构及性能  

Synthesis,Crystal Structure and Properties of Sodium 5,5'-Bistetrazole-1,1'-diolate Tetrahydrate

作　　者：黄海丰[1] 杨军[1] 杨普[1] 李晓强[1] 李慧[1] 俞艳[1] 

机构地区：[1]中国科学院上海有机化学研究所,上海200032

出　　处：《含能材料》2014年第4期462-466,共5页Chinese Journal of Energetic Materials

摘　　要：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H50>100 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-l,l＇-diolate tetrahydrate （SBTD · 4H20）, 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 · 4H20 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 · 4H20 were deter- mined according to GJB772A-1997. Results show that SBTD · 4H20 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 ）＋A, b=6.4476（17）＋A, c=8.303（11 ） A, α=I00.131 （5）°, β= 96.789（3）°, y=112.157（3）°, V=I, Dc=1.761 g. cm-3, F（000）= 146, μ（Mo K ）=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 thatSBTD -4H20 has good thermal stability. Hse ofSBTD .4H20 is greater than 100 cm and friction sensitivity is 0% ,showing the title compound insensitive to impact and friction.

关 键 词：应用化学 四水合1 1'-二羟基-5 5'-联四唑钠盐(SBTD·4H2O) 热分解 晶体结构 感度 sodium 5 5'-bistetrazole-1 1'-diolate tetrahedrate (SBTD·4H2O) 

分 类 号：TQ261.1[化学工程—有机化工] TQ560.1