Post by Anders Hoveland on Mar 17, 2012 23:35:45 GMT -8
DPT
Dinitro-pentamethylenetetramine
3,7-dinitro-1,3,5,7 tetraazabicyclo [3,3,1] nonane
Since DPT is itself an explosive and can be prepared from a mixed H2SO4/HNO3 nitration on hexamine, it is surprising that this compound is not more popular.
The best method of obtaining DPT consists in introducing hexamine dinitrate to 90% sulfuric acid at 8-15 °C. After 45 minutes all is poured on ice and the solution is filtrated. The filtrate is neutralized with 28% conc. ammonia to pH = 5.5-6.5 and DPT precipitated.
DPT can also be prepared from sulfamic acid, H2N-SO3H.
To 100 ml of HNO3 (density 353g/ml or 53% conc.), cooled to +10 °C, was sprinkled 50g of sulfamic acid, a temperature rise is not observed. After mixing with stirring at 10° C for 30 minutes, 53g of DNU was made, the temperature is kept below 20 °. After holding at this temperature for 20 minutes, the reaction mixture was warmed to 30 °, then external heating was discontinued, but the reaction continued to increase in temperature by itself. After reaching 35-36 ° it was carried off to be gently cooled to 30 °C under running tap water. The temperature again continued to increase after reaching 35-37 °, and the mixture was again cooled to 30-33 °, and so on for as long as the temperature kept increasing. The reaction mixture was cooled to 15 °, and it becomes more viscous during this time. After dilution with 300ml of cold water, neutralization of sodium bicarbonate was carried out to pH = 6, by the end of the neutralization of the solution became dull, and formed a number of fine-grained sediment. After an exposure of 1 hour the solution was filtered, the precipitate was washed first with water and finally with isopropyl alcohol to facilitate drying. The mass of dry product was 3.5g or about 8% of the theoretical value (assuming the formation of DPT 1 mol to 1 mol DNU). The nature of combustion of the sample did not differ from the standard DPT. The measured melting point temperature of the sample amounted to about 195-198 °C. DPT obtained by the other more traditional method has a melting point of 200-201 °C.
Dinitro-pentamethylenetetramine
3,7-dinitro-1,3,5,7 tetraazabicyclo [3,3,1] nonane
Since DPT is itself an explosive and can be prepared from a mixed H2SO4/HNO3 nitration on hexamine, it is surprising that this compound is not more popular.
The best method of obtaining DPT consists in introducing hexamine dinitrate to 90% sulfuric acid at 8-15 °C. After 45 minutes all is poured on ice and the solution is filtrated. The filtrate is neutralized with 28% conc. ammonia to pH = 5.5-6.5 and DPT precipitated.
DPT can also be prepared from sulfamic acid, H2N-SO3H.
To 100 ml of HNO3 (density 353g/ml or 53% conc.), cooled to +10 °C, was sprinkled 50g of sulfamic acid, a temperature rise is not observed. After mixing with stirring at 10° C for 30 minutes, 53g of DNU was made, the temperature is kept below 20 °. After holding at this temperature for 20 minutes, the reaction mixture was warmed to 30 °, then external heating was discontinued, but the reaction continued to increase in temperature by itself. After reaching 35-36 ° it was carried off to be gently cooled to 30 °C under running tap water. The temperature again continued to increase after reaching 35-37 °, and the mixture was again cooled to 30-33 °, and so on for as long as the temperature kept increasing. The reaction mixture was cooled to 15 °, and it becomes more viscous during this time. After dilution with 300ml of cold water, neutralization of sodium bicarbonate was carried out to pH = 6, by the end of the neutralization of the solution became dull, and formed a number of fine-grained sediment. After an exposure of 1 hour the solution was filtered, the precipitate was washed first with water and finally with isopropyl alcohol to facilitate drying. The mass of dry product was 3.5g or about 8% of the theoretical value (assuming the formation of DPT 1 mol to 1 mol DNU). The nature of combustion of the sample did not differ from the standard DPT. The measured melting point temperature of the sample amounted to about 195-198 °C. DPT obtained by the other more traditional method has a melting point of 200-201 °C.