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Preparation method of high-energy explosive 3,4-bis(nitrofurazanyl)furazan oxide

A technology of nitrofurazan group and furoxan oxide is applied in directions such as organic chemistry, can solve problems such as incapability of engineering application, and achieves the effects of high yield and low cost

Active Publication Date: 2015-11-11
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention overcomes the deficiencies of the prior art, and provides an embodiment of a preparation method of high-energy explosive 3,4-dinitrofurazanylfuroxan, which can efficiently and safely prepare high-energy explosive 3,4 at a low cost - Dinitrofurazanyl furoxan, overcome the defects that the existing technology cannot be applied in engineering

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  • Preparation method of high-energy explosive 3,4-bis(nitrofurazanyl)furazan oxide
  • Preparation method of high-energy explosive 3,4-bis(nitrofurazanyl)furazan oxide
  • Preparation method of high-energy explosive 3,4-bis(nitrofurazanyl)furazan oxide

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Embodiment 1

[0025] (1) Preparation of intermediate 3,4-di(aminofurazanyl)furazan oxide

[0026] Add 7.96g (0.049mol) of 3-amino-4-chlorooximinofuran to 98mL of tetrahydrofuran, cool the mixture to 0°C-3°C, keep the temperature under mechanical stirring, and add 6.76g ( 0.0245mol) silver carbonate. The mixture was reacted below 10°C for 3.0h. Filtrate, collect the filtrate, remove tetrahydrofuran by vacuum distillation, collect the solid, and dry to obtain 4.94g of 3,4-bis(aminofurazanyl)furoxan, with a yield of 80%. After recrystallization from ethanol, it is a white powdery solid, melting point 167℃~168℃. Elemental Analysis: C 6 N 8 o 4 h 4 Calculated: C28.6; H1.6; N44.4; Found: C27.8; H1.3; N44.2. IR (KBr pellet, cm -1 ): 3455, 3321 (-NH 2 ); 1638, 1027 (furoxan ring); 1608, 1532, 1383, 1004 (furoxan ring). MS(EI): m / z252(M + ), 236 (M-NH 2 ), 222(M-NO), 58(NH 2 -C=N-O), 30(NO). 1 HNMR (DMSO, 300MHz): δ6.374 (2H, -NH 2 )δ6.472 (2H, -NH 2 )ppm. 13 CNMR (CDCl 3 , 300MHz)...

Embodiment 2

[0032] (1) Preparation of intermediate 3,4-di(aminofurazanyl)furazan oxide

[0033] Add 15.92g (0.098mol) of 3-amino-4-chlorooximinofurazan to 200mL of acetonitrile, cool the mixture to 0°C-3°C, keep the temperature under mechanical stirring, and add 14.87g in batches (0.054 mol) silver carbonate. The mixture was reacted below 10°C for 3.5h. Filtrate, collect the filtrate, remove acetonitrile by vacuum distillation, filter, collect the solid, and dry to obtain 9.26g of 3,4-bis(aminofurazanyl)furazan oxide with a yield of 75% and a melting point of 167.5°C to 168.2°C.

[0034] (2) Preparation of high-energy explosive BNFF

[0035] Under ice bath and stirring, add 50.0ml solute mass fraction in there-necked flask and be 50% hydrogen peroxide solution, add 15.0ml solute mass fraction and be 98% concentrated sulfuric acid, add crude product BAFF5.04g (0.02mol) then; Keep the temperature below 10°C for 1.5h; then raise the temperature to 70°C for 3h. After the reaction, the rea...

Embodiment 3

[0039] (1) Preparation of intermediate 3,4-di(aminofurazanyl)furazan oxide

[0040] Add 10.0g (0.062mol) of 3-amino-4-chloroximifurazan to 125mL of dimethylformamide (DMF), cool the mixture to 0°C-3°C, keep the temperature under mechanical stirring, and divide 10.26 g (0.037 mol) of silver carbonate were added in small portions. The mixture was reacted below 10°C for 4.0h. Filtrate, collect the filtrate, remove DMF by vacuum distillation, filter, collect the solid, and dry to obtain 6.4g of 3,4-bis(aminofurazanyl)furazan oxide, with a yield of 82% and a melting point of 167.6°C to 168.5°C.

[0041] (2) Preparation of high-energy explosive BNFF

[0042] Under ice bath and stirring, add 60.0ml solute mass fraction in there-necked flask and be 30% hydrogen peroxide solution, add 20.0ml solute mass fraction and be 98% concentrated sulfuric acid, add crude product BAFF5.04g (0.02mol) then; Keep the temperature below 10°C for 1.5h; then raise the temperature to 70°C for 4.0h. Af...

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Abstract

The invention discloses a preparation method of high-energy explosive 3,4-di(nitrofurazano)furoxan. Raw material 3-amino-4-acyl chloride oximidofurazan reacts with weak base solid silver carbonate in solvents such as tetrahydrofuran to generate an intermediate 3,4-di(amino furazano)furoxan with the yield of 80%. The preparation method disclosed by the invention overcomes the defects in the prior art, and no BAFF (B Cell Activating Factor) isomer 3,6-bi(3-amino furazan-4-base)-1,4-dioxa-2,5-diazacyclohexane-2,5-diene is generated; then, the BAFF is oxidized by using a mixture of hydrogen peroxide and concentrated sulfuric acid as an oxidant to generate the high-energy explosive BNFF, and the yield can reach 80%. The preparation method of the high-energy explosive BNFF is high in production efficiency, low in material cost, mature, stable, safe and reliable, and has engineering application prospect.

Description

technical field [0001] Embodiments of the present invention relate to the field of preparation of energetic materials, and more specifically, embodiments of the present invention relate to a preparation method of high-energy explosive 3,4-bis(nitrofurazanyl)furazan. Background technique [0002] After more than 30 years of research by the Zelinsky Institute of Organic Chemistry of the Russian Academy of Sciences (Propellants, Explosive, Pyrotechnics23, 142-149, 1998), it has been shown that a large class of furan-containing The high energy density material compounds (HEDMs) of the (furazan) ring, because the furazan ring and the furazan ring itself are explosive groups, endow this type of compound with excellent detonation performance, thus becoming an important class of high energy density materials. Energy Density Materials. Among them, 3,4-bis(nitrofurazanyl)furrazan oxide (BNFF or DNTF) is one of them. National defense patent 02101092.7 has introduced a kind of prepara...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D271/08
CPCC07D271/08
Inventor 王军李金山杨光成周小清马卿黄靖伦张丽媛
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS