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Preparation method of energetic compound 2,4,6-triamino-5-nitropyrimidine-1,3-dioxide

A technology of triaminopyrimidine and nitropyrimidine, which is applied in the field of energetic material synthesis, can solve the problems affecting the miniaturization process of combat damage parts and low energy, and achieve low cost of raw materials and solvents, short synthesis steps, and simple post-processing Effect

Inactive Publication Date: 2018-04-20
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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Problems solved by technology

But so far, the only approved and widely used high-energy insensitive explosive is triaminotrinitrobenzene (TATB), but the energy of TATB is low, only equivalent to 1,3,5,7-tetranitro-1, 65% of 3,5,7-tetraazacycloctane (HMX), which significantly affects its miniaturization progress as a battle-damaged site

Method used

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  • Preparation method of energetic compound 2,4,6-triamino-5-nitropyrimidine-1,3-dioxide
  • Preparation method of energetic compound 2,4,6-triamino-5-nitropyrimidine-1,3-dioxide
  • Preparation method of energetic compound 2,4,6-triamino-5-nitropyrimidine-1,3-dioxide

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preparation example Construction

[0019] The structural formula of 2,4,6-triamino-5-nitropyrimidine-1,3-dioxide synthesized by the preparation method of the present invention is:

[0020]

[0021] The preparation method of the present invention adopts following three synthetic routes:

[0022] Route 1: Using 2,4,6-triaminopyrimidine as the reaction raw material, the energetic compound 2,4,6-triamino-5-nitropyrimidine-1,3- dioxide.

[0023] Under the condition of temperature -10~50℃, slowly add 2,4,6-triaminopyrimidine in batches to a certain amount of nitration reagent, the nitration reagent used includes 90%~100% nitric acid, Nitric acid / sulfuric acid mixture, nitric acid / acetic acid mixture, nitric acid / trifluoroacetic acid mixture, nitric acid / trifluoromethanesulfonic acid mixture, nitric acid / acetic anhydride mixture, nitric acid / trifluoroacetic anhydride mixture, or tetrafluoroboric acid One of the nitroxyl reagents; continue to react for 1 to 24 hours after the addition, then cool the reaction syste...

Embodiment 1

[0031] Preparation of 2,4,6-triamino-5-nitropyrimidine-1,3-dioxide (Route 1)

[0032] (1) At -10°C, slowly add 8ml of fuming nitric acid dropwise into 8ml of concentrated sulfuric acid, and add 2g (16mmol) of 2,4,6-triaminopyrimidine to the above mixed acid several times in batches. After the addition, The reaction system was reacted at this temperature for 5 hours, the reaction liquid was poured into ice water, the solid was suction filtered and dried to obtain 2,4,6-triamino-5-nitropyrimidine with a yield of 90%.

[0033] (2) Dissolve 1 g (5.9 mmol) of 2,4,6-triamino-5-nitropyrimidine in 5 ml of trifluoroacetic acid at -10°C and stir slowly, and slowly add 2.5 ml of aqueous hydrogen peroxide (over Hydrogen oxide mass fraction: 20%), after the dropwise addition, react at this temperature for 24 hours, and filter with suction to obtain a solid. The solid was dissolved in water, neutralized with saturated aqueous sodium carbonate solution to neutrality, and the solid was filte...

Embodiment 2

[0035] Preparation of 2,4,6-triamino-5-nitropyrimidine-1,3-dioxide (Route 1)

[0036] (1) At 0°C, in 20 ml of nitric acid with a mass fraction of 100%, 2 g (16 mmol) of 2,4,6-triaminopyrimidine was added to the above acid several times in batches. After the addition, the reaction system was React at this temperature for 4 hours, pour the reaction solution into ice water, filter the solid with suction, and dry to obtain 2,4,6-triamino-5-nitropyrimidine with a yield of 92%.

[0037] (2) Dissolve 1g (5.9 mmol) of 2,4,6-triamino-5-nitropyrimidine in 10 ml of concentrated sulfuric acid at 20°C and stir, slowly add 5 ml of hydrogen peroxide aqueous solution (hydrogen peroxide Mass fraction: 27%), after the dropwise addition, react at this temperature for 12 hours, and filter with suction to obtain a solid. The solid was dissolved in water, neutralized with saturated potassium carbonate aqueous solution to neutrality, and the solid was filtered with suction to obtain 2,4,6-triamino-...

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Abstract

The invention discloses a preparation method of an energetic compound 2,4,6-triamino-5-nitropyrimidine-1,3-dioxide. The preparation method comprises the following steps: with 2,4,6-triaminopyrimidineand a substituent thereof as reaction raw materials, performing a nitration reaction; performing an oxidation reaction; performing an acid-alkali neutralization reaction to obtain the needed product,namely the 2,4,6-triamino-5-nitropyrimidine-1,3-dioxide. The preparation method has the advantages of short synthesis steps, low cost of used raw materials and used solvents, simple post treatment, small damage to people, equipment and the environment and the like; the compound synthesized by the preparation method provided by the invention has the characteristics of high density, high energy, insensitiveness to mechanical stimulation and the like, and has a relatively good market prospect in the field of application of energetic materials.

Description

technical field [0001] The invention relates to the technical field of energetic material synthesis, in particular to a preparation method of an energetic compound 2,4,6-triamino-5-nitropyrimidine-1,3-dioxide. Background technique [0002] Energetic materials are the power source and source of damage to achieve weapons strike targets, and their energy levels directly affect the performance of weapon systems. However, while increasing the energy of energetic materials, their safety performance often decreases. High-energy insensitive explosives have always been an unremitting goal in the field of energetic materials. But so far, the only approved and widely used high-energy insensitive explosive is triaminotrinitrobenzene (TATB), but the energy of TATB is low, only equivalent to 1,3,5,7-tetranitro-1, 65% of 3,5,7-tetraazacyclooctane (HMX), which significantly affects its miniaturization progress as a battle-damaged site. Therefore, it is of great significance to develop new...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/50
CPCC07D239/50
Inventor 张庆华王毅刘雨季宋思维
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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