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ryq1212 发布于2017-07-16 23:19
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二过氧化四亚甲基二脲的合成

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二过氧化四亚甲基二脲(TMDD)的合成

二过氧化四亚甲基二脲(1,2,8,9-四氧-4,6,11,13-四氮杂-5,12-二酮;TMDD)由Girsewald于1914年首次合成。他用尿素和甲醛在硝酸催化下与过氧化氢反应制得了TMDD。TMDD被报道可以作为起爆药组分使用。目前关于TMDD的文献报道很少,国内则没有相关报道。

1 理化性质
TMDD是白色晶体,熔点为180℃。TMDD不溶于水、乙醇、甲醇、氯仿、吡啶和其它的有机溶剂,但可以溶于浓硫酸和浓硝酸中,向溶液中加水,TMDD又会沉淀析出。TMDD不吸湿。TMDD在煮沸的稀酸或稀碱中会分解,但产物不同。TMDD不能用重结晶的方法来纯化,因为它在大部分溶剂中的溶解度都很低,所以只能用溶剂来去除其中的可溶性杂质。

2 实验部分
2.1 试剂
尿素,30%过氧化氢,68%硝酸,36%甲醛均为分析纯。
2.2 TMDD的制备
取尿素25.0g(0.4mol微过量)置于反应器中,加入30%过氧化氢47.0mL(0.4mol更过量),溶液温度略微降低。加适量水使尿素溶解完全后加入68%硝酸10.0ml,此时温度略升高,上冷水浴并慢速搅拌。硝酸加完后尽快加入36%甲醛61.0mL(0.8mol适量),温度继续升高。加快搅拌转速,控制加料时反应液温度不超过45℃。加入45ml左右溶液中即开始有白色沉淀生成。加完后,继续搅拌并冷水浴,反应72h。
反应完后,向容器内加入蒸馏水,搅拌至沉淀稍分散,过滤,洗涤,干燥。
收集产物,得白色固体42.6g,产率90.25%。

3 结果与讨论
3.1 TMDD的感度
根据试验,TMDD的摩擦感度与撞击感度均不高。在完全开放条件下非明火加热时TMDD剧烈分解产生气体但不爆轰,不点火。

4 结论
制得了目标产物TMDD,产率可喜。TMDD原料易得,条件温和,制备简单,稳定安全,成本低廉,是一种优秀的含能材料。然而相关性能数据还有待测算,望引起国内各同行的关注。
[ryq1212于2017-07-19 13:52编辑了帖子]
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红盟大使 发布于2017-07-19 08:38
沙发F
觉得挺不错的,改天制备一些分析一下,楼主有这个能材性能的详细参数嘛?
水可载舟亦可赛艇!
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ryq1212 发布于2017-07-19 13:45
板凳F
参考文献

图片:P70705-110546.jpg

图片:P70705-110504.jpg

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ryq1212 发布于2017-07-19 13:47
地板F
红盟大使:觉得挺不错的,改天制备一些分析一下,楼主有这个能材性能的详细参数嘛?回到原帖
基本没有,有的都在图片里了。本来关于这个的研究就不多
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ryq1212 发布于2017-07-19 14:16
4楼F
红盟大使:觉得挺不错的,改天制备一些分析一下,楼主有这个能材性能的详细参数嘛?回到原帖
另外,这个的摩擦感度试验是我拿研钵试的,撞击感度试验是拿锤子试的,当然,都是小米粒大小的试样,可能不准。如果可以我也想知道一些更准确的感度数据
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硝化棉小王子 发布于2017-07-20 22:44
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话说书是起爆药学吗?TMDD起爆能力不是很好的
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ryq1212 发布于2017-07-21 19:21
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硝化棉小王子:话说书是起爆药学吗?TMDD起爆能力不是很好的回到原帖
是的,我在资源区发过这本书的目录
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momo 发布于2020-11-25 14:12
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Mvnfs93d01 发布于2020-11-26 11:05
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