摘要
以2,4-二氯-1,3,5-三硝基苯（DCTNB）和2,4,6-三硝基氯苯（苦基氯）为原料,在活化铜粉的催化下,通过混合乌尔曼反应合成2,2′,2″,4,4′,4″,6,6′,6″-九硝基三联苯（NONA）,利用柱色谱将目标产物与其他副产物进行了分离。采用红外光谱、质谱和核磁共振氢谱对目标产物及主要副产物的结构进行了表征,结果表明目标产物为NONA,主要副产物为六硝基二联苯（HNB）和十二硝基四联苯（DODECA）。利用DSC对NONA进行了热分解研究,结果表明NONA的热分解温度为380℃,证明合成的NONA具有良好的热稳定性。本工艺采用更加经济的DCTNB代替二溴三硝基苯作为原料更加经济,反应条件更加温和,具有良好的应用前景。
In this study, 2,2′,2″,4,4′,4″,6,6′,6″-nonanitroterphenyl（NONA） was synthesized starting from 2,4-chloro-1,3,5-trinitrobenzene（DCTNB） and 2,4,6-trinitrochlorobenzene（Pi Cl） through the Ullmann reaction with active copper powder as catalyst. The target product and other by-products were separated through column chromatography.The structures of target product and other by-products were characterized by IR,MS and 1HNMR. The target product was NONA,and the main by-products were HNB and DODECA. Thermal decomposition of NONA was measured by DSC. The pyrolysis temperature of NONA was 380 ℃ and NONA had good heat stability. This technology cost less by selecting DCTNB as raw material instead of Di Br TNB,and reaction conditions were more moderate. It had a good application prospect.
出处
《化工进展》
EI
CAS
CSCD
北大核心
2015年第3期820-824,共5页
Chemical Industry and Engineering Progress
关键词
九硝基三联苯
合成
表征
热分解
2
2′
2″
4
4′
4″
6
6′
6″-nonanitroterphenyl
synthesis
characterization
thermal decomposition
