化工进展
化工進展
화공진전
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
2015年
3期
820-824
,共5页
郑厦蓉%李永祥%王建龙%曹端林%王艳红%程晓燕
鄭廈蓉%李永祥%王建龍%曹耑林%王豔紅%程曉燕
정하용%리영상%왕건룡%조단림%왕염홍%정효연
九硝基三联苯%合成%表征%热分解
九硝基三聯苯%閤成%錶徵%熱分解
구초기삼련분%합성%표정%열분해
2,2′,2″,4,4′,4″,6,6′,6″-nonanitroterphenyl%synthesis%characterization%thermal decomposition
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。
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）為原料，在活化銅粉的催化下，通過混閤烏爾曼反應閤成2,2′,2″,4,4′,4″,6,6′,6″-九硝基三聯苯（NONA），利用柱色譜將目標產物與其他副產物進行瞭分離。採用紅外光譜、質譜和覈磁共振氫譜對目標產物及主要副產物的結構進行瞭錶徵，結果錶明目標產物為NONA，主要副產物為六硝基二聯苯（HNB）和十二硝基四聯苯（DODECA）。利用DSC對NONA進行瞭熱分解研究，結果錶明NONA的熱分解溫度為380℃，證明閤成的NONA具有良好的熱穩定性。本工藝採用更加經濟的DCTNB代替二溴三硝基苯作為原料更加經濟，反應條件更加溫和，具有良好的應用前景。
이2,4-이록-1,3,5-삼초기분（DCTNB）화2,4,6-삼초기록분（고기록）위원료，재활화동분적최화하，통과혼합오이만반응합성2,2′,2″,4,4′,4″,6,6′,6″-구초기삼련분（NONA），이용주색보장목표산물여기타부산물진행료분리。채용홍외광보、질보화핵자공진경보대목표산물급주요부산물적결구진행료표정，결과표명목표산물위NONA，주요부산물위륙초기이련분（HNB）화십이초기사련분（DODECA）。이용DSC대NONA진행료열분해연구，결과표명NONA적열분해온도위380℃，증명합성적NONA구유량호적열은정성。본공예채용경가경제적DCTNB대체이추삼초기분작위원료경가경제，반응조건경가온화，구유량호적응용전경。
s: 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 (PiCl) 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 DiBrTNB,and reaction conditions were more moderate. It had a good application prospect.
