Synthetic method for 3-(4-aminofurazan-3-radical)-4-(4-nitrofurazan-3-radical) furazan

A technology of aminofurazan and nitrofurazan, applied in the direction of organic chemistry, can solve the problems of large thermal expansion and contraction, difficult melting and casting process, hidden safety hazards, etc., and achieve the goal of reducing usage, improving safety and yield Effect

Inactive Publication Date: 2016-05-11
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

However, TNT-based melt-cast explosives generally have the following disadvantages: due to the low-melting impurities such as dinitrobenzene, mononitrobenzene, and asymmetric trinitrobenzene that are difficult to separate, the castings leak oil and reduce the filling density of explosives; After condensation, TNT forms a flaky coarse crystal structure and is brittle, and is prone to fracture surfaces; it is prone to cracks after thermal cycles, and the degree of thermal expansion and contraction is large
[0003] Due to its low melting point, furoxan-like energetic compounds are expected to

Method used

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  • Synthetic method for 3-(4-aminofurazan-3-radical)-4-(4-nitrofurazan-3-radical) furazan
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  • Synthetic method for 3-(4-aminofurazan-3-radical)-4-(4-nitrofurazan-3-radical) furazan

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Synthesis of intermediate 3,4-bis(3′-aminofurazan-4′-yl)furazan

[0028] At room temperature, dissolve 3,4-bis(3'-aminofurazan-4'-yl)furoxan (10g) in anhydrous methanol, stir to dissolve, then add concentrated hydrochloric acid (22ml), add in batches Stannous chloride dihydrate (27g) was reacted under reflux for 3h, cooled, a yellow solid precipitated, filtered off with suction, washed with ice water, and dried under vacuum to obtain 4.0g of a pale yellow solid BATF, with a yield of 42.7%.

[0029] (2) Synthesis of 3-(4-aminofurazan-3-yl)-4-(4-nitrofurazan-3-yl)furazan

[0030] At 0℃, dissolve sodium tungstate (2.94g) in 98% concentrated sulfuric acid (4.4ml), stir to dissolve, slowly add 30% H dropwise 2 O 2 (10.2ml), the temperature of the dripping process should not exceed 10℃, and stir. After the configuration is completed, heat up to 20°C, add 3,4-bis(3′-aminofurazan-4′-yl)furazan (2.36g), keep it for 3h, let stand for a period of time to filter, add the filtrate to ...

Embodiment 2

[0032] (1) Synthesis of intermediate 3,4-bis(3′-aminofurazan-4′-yl)furazan

[0033] At room temperature, dissolve 3,4-bis(3'-aminofurazan-4'-yl)furoxan (10g) in anhydrous methanol, stir to dissolve, then add concentrated hydrochloric acid (22ml), add in batches Stannous chloride dihydrate (27g) was reacted under reflux for 3.5h, cooled, and a yellow solid precipitated, filtered off with suction, washed with ice water, and dried in vacuo to obtain 5.8 g of BATF as a pale yellow solid, with a yield of 62.0%.

[0034] (2) Synthesis of 3-(4-aminofurazan-3-yl)-4-(4-nitrofurazan-3-yl)furazan

[0035] At 0℃, dissolve sodium tungstate (2.94g) in 98% concentrated sulfuric acid (8.1ml), stir to dissolve, slowly add 25% H dropwise 2 O 2 (18.7ml), the temperature of the dripping process does not exceed 10 ℃, and stir. After the configuration is completed, heat up to 25°C, add 3,4-bis(3'-aminofurazan-4'-yl)furazan (2.36g), keep it for 4h, let it stand for a period of time to filter, and add the ...

Embodiment 3

[0037] (1) Synthesis of intermediate 3,4-bis(3′-aminofurazan-4′-yl)furazan

[0038] At room temperature, dissolve 3,4-bis(3'-aminofurazan-4'-yl)furoxan (10g) in anhydrous methanol, stir to dissolve, then add concentrated hydrochloric acid (22ml), add in batches Stannous chloride dihydrate (30g) was reacted under reflux for 4.5h, cooled, a yellow solid precipitated, filtered off with suction, washed with ice water, and dried in vacuo to obtain 5.0g of a pale yellow solid BATF, with a yield of 53.4%.

[0039] (2) Synthesis of 3-(4-aminofurazan-3-yl)-4-(4-nitrofurazan-3-yl)furazan

[0040] At 0℃, dissolve sodium tungstate (2.94g) in 98% concentrated sulfuric acid (8.1ml), stir to dissolve, slowly add 25% H dropwise 2 O 2 (18.7ml), the temperature of the dripping process does not exceed 10 ℃, and stir. After the configuration is completed, heat up to 25°C, add 3,4-bis(3'-aminofurazan-4'-yl)furazan (2.36g), keep it for 4h, let it stand for a period of time to filter, and add the filtrate...

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Abstract

The invention provides a synthetic method for 3-(4-aminofurazan-3-radical)-4-(4-nitrofurazan-3-radical) furazan. 3-(4-aminofurazan-3-radical)-4-(4-nitrofurazan-3-radical) furazan (ANTF) is a low-melting-point (100 DEG C) explosive, is expected to replace TNT to be used in casting explosives, and is also an intermediate for synthesizing other novel explosives. An existing synthetic method of ANTF has the defects of being large in acid use amount, low in synthesis yield, strict in reaction condition and the like. 3,4-bis(3'-aminofurazan-4'-radical) furoxan (BAFF) is adopted as a raw material, 3,4-bis(3'-aminofurazan-4'-radical) furoxan (BAFF) and SnCl2.2H2O are firstly subjected to a reduction reaction to obtain 3,4-bis(aminofurazan-4-raidcal) furazan, and then 3,4-bis(aminofurazan-4-raidcal) furazan and H2O2 are subjected to an oxidizing reaction to obtain the target product 3-(4-aminofurazan-3-radical)-4-(4-nitrofurazan-3-radical) furazan. 3,4-bis(aminofurazan-4-raidcal) furazan is adopted as the raw material, H2O2 (20%-30%) is adopted as an oxidizing agent, Na2WO4 is adopted as a catalyst, and 3-(4-aminofurazan-3-radical)-4-(4-nitrofurazan-3-radical) furazan is synthesized under the acidic condition through the oxidizing reaction. The synthetic method has the advantages of being easy and convenient to operate, high in safety, controllable in process and the like.

Description

Technical field [0001] The invention relates to a method for synthesizing molten cast explosives, in particular to the synthesis of 3-(4-aminofurazan-3-yl)-4-(4-nitrofurazan-3-yl)furazan (ANTF) method. Background technique [0002] Since the advent of TNT explosives, TNT-based melt-cast explosives have been widely used in various mixed explosives. However, TNT-based melt-cast explosives generally have the following shortcomings: because they contain low melting point impurities such as dinitrobenzene, mononitrobenzene, and asymmetric trinitrobenzene, which are difficult to separate, the castings leak oil and reduce the explosive filling density; TNT forms a flaky coarse crystalline structure after condensation and is brittle, prone to fracture surfaces; cracks are prone to occur after thermal cycles, and the degree of thermal expansion and contraction is large. These deficiencies have led to greater safety hazards in the use of TNT-based melt-cast explosives. For this reason, ...

Claims

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Application Information

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IPC IPC(8): C07D271/08
CPCC07D271/08
Inventor 易潜洪黄明梁德辉刘如沁刘玉存索志荣
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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