Preparation method of high energy density material
A technology with high energy density and concentration, applied in organic chemistry, nitrated acyclic/alicyclic/heterocyclic amine explosive compositions, etc., can solve the problems of complex process, high production cost, dangerous operation process, etc., and achieve experimental process safety. , widely used, and the effect of simple synthesis methods
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Embodiment 1
[0018] Take 12mL 30%H 2 O 2 Put it into a 50mL three-necked bottle, set the low temperature bath to -20°C, and slowly add 24 mL of 98% H dropwise. 2 SO 4 , the temperature is controlled below 0°C during the dropwise addition, and after the dropwise addition is completed, 4,4'-2(4-amino-1,2,5-oxadiazol-3-yl)-2,2'- Combined 1,2,4-oxadiazole (feed about 1h). Continue the reaction for 12h at 35℃, and check whether the reaction is complete. After the reaction, the reaction solution was poured into 50 mL of ice water, stirred for 1 h, extracted with ether, washed with water, dried, and evaporated to dryness to obtain white 4,4'-2(4-nitro-1,2,5-oxadiazole) -3-yl)-2,2'-bi-1,2,4-oxadiazole (3) in about 89% yield. The measured density of the high energy density material is 1.948g / cm 3 , the single crystal density is 1.965g / cm 3 , Soluble in most common solvents such as acetone, ethyl acetate and methanol. The melting point is 165.15°C, the thermal decomposition temperature is 26...
Embodiment 2
[0021] Below 0°C, 4,4'-2(4-amino-1,2,5-oxadiazol-3-yl)-2,2'-bi-1,2,4-oxadiazole was slowly added to oxidize System H 2 O 2 / (NH 4 ) 2 S 2 O 8 / H 2 SO 4 After the addition, the reaction system was heated to 30 °C and kept for 24 h. After the reaction, it was poured into ice, extracted with ether, washed, dried and evaporated to dryness to obtain 4,4'-2(4-nitro-1,2,5-oxadiazol-3-yl)-2, 2'-bi-1,2,4-oxadiazole in 86% yield.
[0022] 4,4'-2(4-Amino-1,2,5-oxadiazol-3-yl)-2,2'-bi-1,2,4-oxadiazole and oxidation system H 2 O 2 / (NH 4 ) 2 S 2 O 8 / H 2 SO 4 The mass-to-volume ratio of 1g:25mL, the oxidation system H 2 O 2 / (NH 4 ) 2 S 2 O 8 / H 2 SO 4 Medium H 2 O 2 The concentration is 30%, H 2 SO 4 The concentration of 98%, (NH 4 ) 2 S 2 O 8 For pure solid matter.
Embodiment 3
[0024] Below 0°C, 4,4'-2(4-amino-1,2,5-oxadiazol-3-yl)-2,2'-bi-1,2,4-oxadiazole was slowly added to oxidize System H 2 O 2 / Na 2 WO 4 / H 2 SO 4 After the addition, the reaction system was heated to 30 °C and kept for 24 h. After the reaction, it was poured into ice, extracted with ether, washed, dried and evaporated to dryness to obtain 4,4'-2(4-nitro-1,2,5-oxadiazol-3-yl)-2, 2'-bi-1,2,4-oxadiazole in 84% yield.
[0025] 4,4'-2(4-Amino-1,2,5-oxadiazol-3-yl)-2,2'-bi-1,2,4-oxadiazole and oxidation system H 2 O 2 / Na 2 WO 4 / H 2 SO 4 The mass-to-volume ratio of 1g:50mL, H 2 O 2 The concentration is 30%, H 2 SO 4 The concentration is 98%, Na 2 WO 4 For pure solid matter.
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