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[1]周诚,周彦水,霍欢,等.1,3,5-三硝基-六氢化-1,3,5-三嗪-2-酮的合成与表征[J].火炸药学报,2011,34(4):17-20.
 ZHOU Cheng,ZHOU Yan-shui,HUO Huan,et al.Synthesis and Characterization of 1,3,5-Trinitro-hexahydro-1,3,5-triazin-2(1H)-one[J].,2011,34(4):17-20.
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1,3,5-三硝基-六氢化-1,3,5-三嗪-2-酮的合成与表征()
     
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《火炸药学报》[ISSN:1007-7812/CN:61-1310/TJ]

卷:
34
期数:
2011年第4期
页码:
17-20
栏目:
出版日期:
2011-08-30

文章信息/Info

Title:
Synthesis and Characterization of 1,3,5-Trinitro-hexahydro-1,3,5-triazin-2(1H)-one
作者:
周诚周彦水霍欢王伯周张叶高
西安近代化学研究所
Author(s):

ZHOU ChengZHOU Yan-shuiHUO HuanWANG Bo-zhouZHANG Ye-gao

─3c/p>

Xi′an Modern Chemistry Research Institute
关键词:
有机化学135-三硝基-六氢化-135 三嗪-2-酮Keto-RDX
Keywords:
organic chemistry135-trinitro-hexahydro-135-triazin-2(1H)-oneKeto-RDX
分类号:
-
DOI:
-
文献标志码:
A
摘要:
以尿素、甲醛和叔丁胺为原料,通过Mannich缩合反应制备出5-叔丁基-1,3,5-三嗪-2-酮(TBT),再经硝酸 乙酸酐硝化合成出1,3,5-三硝基-六氢化-1,3,5-三嗪-2-酮(Keto-RDX),用核磁、红外光谱、质谱、元素分析等对TBT和Keto-RDX的结构进行了表征。探讨了TBT环化反应历程,确定了制备TBT的最佳工艺条件为:n(尿素):n(甲醛): n(叔丁胺)=1∶2∶1,尿素和甲醛的反应时间5min,叔丁胺的加料时间5min,反应温度50℃,反应时间8h,最高产率为62.0%。在n(硝酸):n(乙酸酐)=1∶1的硝化体系中,n(硝酸):n(TBT)=20∶1、硝化温度为20℃、反应时间为2h时,Keto RDX的产率为48.0%,纯度高达98.8%,不含RDX。
Abstract:

─3cspan lang="EN-US">5-t-Butyl-1,3,5-triazacyclohexan-2-one(TBT)was prepared via urea, formaldehyde and t-butyl amine as raw materials.1,3,5-Trinitro-hexahydro-1,3,5-triazin-2(1H)-one(Keto-RDX)was synthesized via nitration of TBT. The structures of TBT and Keto-RDX were characterizedby NMR, FT-IR,MS and elemental analysis. The mechanism of cyclization reactionwas discussed. The results showed that the optimal reaction conditions forpreparing TBT were: the molar ratio of n(urea):n(formaldehyde):n(t-butyl amine)=1∶21,reaction time of urea and formaldehyde 5min,feeding time of t-butylamine 5min,reaction temperature 50 and reaction time8h,the yield of TBT was up to 62.0%.When the molar ratio of n(nitric acid):n(aceticanhydride)=11 in the mixture of nitric acid and aceticanhydride, n(nitric acid):n(TBT)=201,nitrationreaction temperature 20 and reaction time 2h,the yieldof Keto-RDX was up to 48.0%,with high purity of 98.8%andRDX was not detected.

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