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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 被引量:3

Study on the Process of Synthesizing 1,5-Diacetyl-3,7-dinitro-1,3,5,7-tetraazacyclooctane by Small-Molecule Method
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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%。 1,5-diacetyl-3,7-dinitro-1,3,5,7-tetraazacyclooctane (DADN) was obtained via condensation, acylation and nitrolysis using formaldehyde and ammonia as the starting materials without isolation of intermediates. The effects of the ratio of formaldehyde and ammonia, condensation time, aeylation time, amount of HNO3 ,molar ratio of HNO3 and H2SO4, feeding temperature and nitrolysis time On the yield of DADN were studied. The yield of DADN was improved to 84.4 % under optimized conditions : n(HCHO) : n (NH3) = 1 : 1.5, condensation time 60 min, acylation time 25 rain, n(HNO3) : n(H2SO4)=1 : 3, nitrolysis time 25 min and feeding temperature 18℃.
出处 《火炸药学报》 EI CAS CSCD 北大核心 2013年第2期13-15,19,共4页 Chinese Journal of Explosives & Propellants
关键词 有机化学 1 5-二乙酰基-3 7-二硝基-1 3 5 7 -四氮杂辛烷 小分子法 硝解 organic chemistry 1,5-diacetyl-3,7-dinitro-1,3,5,7-tetraazacyclooctane small-molecule method nitrolysis
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