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[1]史楠,胡炳成,吕春绪.小分子法合成1, 5-二乙酰基-3,7-二硝基-1, 3, 5, 7-四氮杂辛烷工艺研究[J].火炸药学报,2013,36(2):13-15.
 SHI Nan,HU Bing-cheng,Lü Chun-xu.Study on the Process of Synthesizing 1,5-Diacetyl-3,7-dinitro-1,3,5,7-tetraazacyclooctane by Small Molecule Method[J].,2013,36(2):13-15.
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小分子法合成1, 5-二乙酰基-3,7-二硝基-1, 3, 5, 7-四氮杂辛烷工艺研究()
     
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《火炸药学报》[ISSN:1007-7812/CN:61-1310/TJ]

卷:
36
期数:
2013年第2期
页码:
13-15
栏目:
出版日期:
2013-04-30

文章信息/Info

Title:
Study on the Process of Synthesizing 1,5-Diacetyl-3,7-dinitro-1,3,5,7-tetraazacyclooctane by Small Molecule Method
作者:
史楠胡炳成吕春绪
南京理工大学化工学院
Author(s):
SHI NanHU Bing-chengLü Chun-xu
School of Chemical Engineering, Nanjing University of Science and Technology
关键词:
有机化学15-二乙酰基-37-二硝基-1357-四氮杂辛烷小分子法硝解
Keywords:
分类号:
-
DOI:
-
文献标志码:
A
摘要:
以甲醛、氨为起始原料,中间体不分离,经过缩合、乙酰化、硝解等反应得到1,5-二乙酰基-3,7-二硝基-1,3,5,7-四氮杂辛烷(DADN),考察了甲醛与氨的配比、缩合时间、乙酰化时间、硝酸用量及硝硫混酸的配比、加料温度和硝解时间等因素对DADN收率的影响,确立了最佳工艺。结果表明,当甲醛与氨的摩尔比为1∶1.5,缩合反应时间60min,乙酰化时间25min,硝硫混酸摩尔比 1∶3,加料温度18℃,硝解时间为25min,DADN产率为84.4%。
Abstract:

1,5-diacetyl-3,7-dinitro-1,3,5,7-tetraazacyclooctane(DADN) was obtained via condensation, acylation and nitrolysis usingformaldehyde and ammonia as the starting materials without isolation ofintermediates. The effects of the ratio of formaldehyde and ammonia,condensation time, acylation time, amount of HNO3 ,molar ratio of HNO3and H2SO4, feeding temperature and nitrolysis time on theyield of DADN were studied. The yield of DADN was improved to 84.4% underoptimized conditions: n(HCHO)n(NH3)=11.5,condensation time 60 min, acylation time 25 min, n(HNO3)n(H2SO4)=13,nitrolysis time 25 min and feeding temperature 18.

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