Synthesis process of 3-methyl-4-nitroimino perhydro-1,3,5-oxadiazine
A nitroimide-based, synthetic process technology, applied in organic chemistry and other directions, can solve the problems of low utilization rate of equipment, large amount of three wastes, complicated post-processing, etc., and achieves optimized production process, easy generation of three wastes, and comprehensive utilization. Effect
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Embodiment 1
[0012] Embodiment 1: synthetic chemical formula such as figure 1 , in a 5000L reactor equipped with a thermometer and stirring, add 1652Kg methylnitroguanidine (14Kmol), 1444Kg paraformaldehyde (96%, 46.2Kmol), 1000Kg water, 200Kg98% concentrated sulfuric acid, and heat to 68-71 ℃, heat preservation reaction for 16 hours, after the reaction, lower the temperature to below 10 ℃, cool and crystallize, filter and recover the crude oxadiazine and the reaction mother liquor. The crude oxadiazine is first washed with the previous batch of recrystallization mother liquor, then mixed with a total of 3000L of water supplemented with a small amount of fresh water, heated to 80-85°C to completely dissolve, filtered while hot, and the filtrate is cooled to crystallize, filtered and dried Obtained product oxadiazine: 1915Kg, analyzed by liquid chromatography, product oxadiazine content: 99.75%, methyl nitroguanidine content is less than 0.04%, other single impurity content <0.1%, molar yie...
Embodiment 2
[0013] Embodiment 2: in the 5000L reactor that thermometer, agitation are housed, add the last batch reaction mother liquor 1200Kg of metering, its sulfuric acid content: 9.20%, paraformaldehyde content: 24.5%, then add 1652Kg methyl nitroguanidine ( 14mol), add 1150Kg paraformaldehyde (96%, 36.8Kmol), 92Kg concentrated sulfuric acid, heat to 68-72°C, keep warm for 16 hours, after the reaction, cool down to below 10°C, cool and crystallize, filter and recover the crude product Diazine and reaction mother liquor. The crude oxadiazine is first washed with the recrystallization mother liquor of the previous batch, then mixed with a total of 3000L of water supplemented with a small amount of fresh water, heated to 80-85°C to completely dissolve, filtered while hot, and the filtrate is cooled to crystallize, filtered and dried Obtained product oxadiazine: 1992Kg, analyzed by liquid chromatography, product oxadiazine content: 99.62%, methyl nitroguanidine content is less than 0.03%,...
Embodiment 3
[0014] Embodiment 3: in the 3000L vacuum still that thermometer, heating coil, stirring are housed, add whole reaction mother liquor that embodiment 1 reclaims earlier, its sulfuric acid content: 9.20%, paraformaldehyde content: 24.5%, then in about Vacuum distillation between -750mmHg and 40-70°C until about 1200-1300Kg of mother liquor remains in the kettle, the vacuum distillation is over, and the contents of paraformaldehyde and sulfuric acid in the mother liquor are detected to be 26.8% and 10.1%, respectively. Transfer 1200Kg of the remaining mother liquor to a 5000L enamel reaction kettle, add 1652Kg methylnitroguanidine (14mol), add 1100Kg paraformaldehyde (96%, 35.2Kmol), 80Kg concentrated sulfuric acid, and heat to 68-72°C , heat preservation reaction for 16 hours, after the reaction, lower the temperature to below 10°C, cool and crystallize, filter and recover the crude oxadiazine and the reaction mother liquor. The crude oxadiazine is first washed with the recrysta...
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