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Preparation method of high-energy explosive 3,4-di(nitrofurazano)furoxan

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: 2014-08-06
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-di(nitrofurazano)furoxan
  • Preparation method of high-energy explosive 3,4-di(nitrofurazano)furoxan
  • Preparation method of high-energy explosive 3,4-di(nitrofurazano)furoxan

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Embodiment 1

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

[0026] 7.96g (0.049mol) of 3-amino-4-chlorooximidofurazan was added to 98mL of tetrahydrofuran, the mixture was cooled to 0°C to 3°C, and under mechanical stirring, maintaining this temperature, 6.76g ( 0.0245 mol) silver carbonate. The mixture was reacted below 10°C for 3.0h. Filtration, collecting the filtrate, vacuum distillation to remove tetrahydrofuran, collecting the solid, drying to obtain 4.94g of 3,4-bis(aminofurazanyl)furazan oxide, yield 80%, white powdery solid after recrystallization from ethanol, 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 tablet, cm -1 ): 3455, 3321(-NH 2 ); 1638, 1027 (furazan ring); 1608, 1532, 1383, 1004 (oxyfurazan ring). MS(EI): m / z252 (M + ), 236(M-NH 2 ), 222(M-NO), 58(NH 2 -C=N-O), 30 (NO). 1 H NMR (DMSO, 300MHz): δ 6.374 (2H, -NH 2 )δ6.472(2H,-NH 2 )ppm. 13 C ...

Embodiment 2

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

[0033] Add 15.92g (0.098mol) of 3-amino-4-chlorooximidofurazan to 200mL of acetonitrile, cool the mixture to 0℃~3℃, keep this temperature under mechanical stirring, add 14.87g in small amounts in batches (0.054 mol) silver carbonate. The mixture was reacted below 10°C for 3.5h. Filtration, collecting the filtrate, vacuum distillation to remove acetonitrile, filtering, collecting the solid, drying to obtain 9.26g of 3,4-bis(aminofurazanyl)furazan oxide, yield 75%, melting point 167.5℃~168.2℃.

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

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

Embodiment 3

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

[0040] Add 10.0 g (0.062 mol) of 3-amino-4-chlorooximofurazan to 125 mL of dimethylformamide (DMF), cool the mixture to 0°C to 3°C, maintain this 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. Filtration, collection of filtrate, vacuum distillation to remove DMF, filtration, collection of solids, drying to obtain 6.4 g of 3,4-bis(aminofurazanyl)furazan oxide, yield 82%, melting point 167.6°C~168.5°C.

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

[0042] Under ice bath and stirring, add 60.0ml of hydrogen peroxide solution with a solute mass fraction of 30% in a three-necked flask, add 20.0ml of concentrated sulfuric acid with a solute mass fraction of 98%, and then add crude BAFF5.04g (0.02mol); The reaction was kept at a temperature below 10°C for 1.5h; then the temperat...

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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 particularly, embodiments of the present invention relate to a method for preparing high-energy explosive 3,4-bis(nitrofurazanyl)furazan oxide. Background technique [0002] The Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences (Propellants, Explosive, Pyrotechnics 23, 142-149, 1998), after more than 30 years of research, has shown that a large class of fur-containing compounds prepared from 3,4-diaminofurazan (DAF) as the starting material The high-energy-density material compounds (HEDMs) of the zan (furazan oxide) ring are explosive groups, which endow these compounds with excellent detonation properties, thus becoming an important class of high-energy-density materials. energy density material. Among them, 3,4-bis(nitrofurazanyl)oxyfurazan (BNFF or DNTF) is one of the best ones. National defense patent 02101092.7 introduces ...

Claims

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Application Information

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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
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