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Composite method of high-energy insensitive explosive 2,6-diamino-3,5-dinitro pyridine-1-oxide

A technology of dinitropyridine and a synthesis method, applied in the field of explosive synthesis, can solve the problems of difficulty in industrialization, multiple impurities, high cost, etc., and achieve the effects of simple product post-processing, simple process, and strong market competitiveness

Inactive Publication Date: 2010-06-16
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although foreign researchers have vague and simple reports on this class of compounds (see: Hollins R, et al, J Heterocycl Chem, 1996, 33: 896-904), their synthetic routes and techniques have determined that they can only be It is low yield (<50%), many impurities and high cost, it is difficult to realize industrialization

Method used

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  • Composite method of high-energy insensitive explosive 2,6-diamino-3,5-dinitro pyridine-1-oxide
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  • Composite method of high-energy insensitive explosive 2,6-diamino-3,5-dinitro pyridine-1-oxide

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Experimental program
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Effect test

Embodiment 1

[0032] For the synthesis of 2,6-diamino-3,5-dinitropyridine, see accompanying drawing II for the synthetic route. In a 100mL three-neck flask equipped with a stirrer and a thermometer, add 75mL of 98% concentrated H 2 SO 4 , add 2.18g 2,6-diaminopyridine under stirring, after the solid is completely dissolved, continue to stir until the temperature of the mixture drops below 30°C; add 0.075mol KNO within 10min 3 (Ice-water bath controls the temperature of the mixture below 30°C), adding KNO 3 Keep stirring vigorously during the process; after the reaction is over for three hours, pour the mixture into crushed ice, stir, and a large amount of tan solid precipitates, filter and wash with water; transfer it to a 100mL flask after vacuum drying, add 50mL 2molL -1 NaOH, stirred for 2 hours, cooled, filtered, washed with water, dried, the obtained solid was boiled in distilled water for one hour, filtered, dried, weighed, and the yield was 75%.

Embodiment 2

[0034] For the synthesis of 2,6-diamino-3,5-dinitropyridine, see accompanying drawing II for the synthetic route. In a 100mL three-neck flask equipped with a stirrer and a thermometer, add 15ml of 65% fuming H 2 SO 4 , add 2.18g 2,6-diaminopyridine under stirring, after the solid is completely dissolved, continue to stir until the temperature of the mixture drops below 20°C; add 0.04mol NaNO within 10min 3 (Ice-water bath controls the temperature of the mixture below 20°C), maintain vigorous stirring during the addition of nitrate; after the reaction for three hours, pour the mixture into crushed ice, stir, and precipitate a large amount of yellow-brown solid, filter, wash with water; vacuum dry Then transfer to a 100ml flask, add 50ml2molL -1 NaOH, stirred for 2 hours, cooled, filtered, washed with water, and dried. The resulting solid was boiled in distilled water for one hour, filtered, and dried. The yield was 90%.

Embodiment 3

[0036] For the synthesis of 2,6-diamino-3,5-dinitropyridine, see accompanying drawing II for the synthetic route. In a 5L three-necked flask equipped with a stirrer and a thermometer, add 2400ml of 20% fuming sulfuric acid, add 300g of 2,6-diaminopyridine under stirring, and continue stirring until the temperature of the mixture drops below 30°C after the solid is completely dissolved; Add 240ml fuming HNO within 15min 3 (Ice-water bath controls the temperature of the mixture below 30°C), add fuming HNO 3 Keep stirring vigorously during the process; after the reaction for three hours, pour the mixture into crushed ice, stir, and a large amount of yellow-brown solid precipitates, filter and wash with water; after vacuum drying, transfer into 5000ml2molL -1 The NaOH solution was stirred for 2 hours, cooled, filtered, washed with water, and dried. The resulting solid was boiled in distilled water for one hour, filtered, and dried. The yield was 93%.

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Abstract

The invention relates to a composite method of high-energy insensitive explosive 2,6-diamino-3,5-dinitro pyridine-1-oxide. In the method, 2,6-diamino pyridine is nitrified in a mixed acid or super acid nitrifying system; mixture is poured into trash ice to separate out yellow sediment; solid obtained by filtering is boiled by distilled water, and yellowish-brown solid is obtained by filtering; in acetic acid, or trifluoroacetic acid or organic acid solution, the nitrogen oxidation reaction of the 2,6-diamino-3,5-dinitro pyridine is realized at the temperature of 75-250 DEG C in the presence of peroxy acid and catalyst; and luminous yellow solid is obtained by filtering after reaction ends. The invention has moderate reaction condition, does not need special devices, has abundant raw material resources, low cost, simple technology, safe and reliable production, simple product aftertreatment and small harm on environment and satisfies the basic requirements of industrial scale-up production; in addition, the invention has high total yield of target products, obviously lowers cost and has stronger market competitiveness.

Description

technical field [0001] The present invention relates to a kind of explosive synthesis technology, especially a kind of high-energy insensitive explosive 2,6-diamino-3,5-dinitropyridine-1-oxide (2,6-diamino-3,5-dinitropyridine- 1-oxide, abbreviated as: DADNPO) synthetic method. Background technique [0002] TATB (triaminotrinitrobenzene) is the most widely used high-energy heat-resistant explosive at home and abroad. Because of its extremely high tolerance to heat and mechanical action, it is favored in special fields such as missiles, rockets, aerospace and other military equipment, ultra-deep exploration seismic source bombs, and civilian blasting. However, TATB has high cost, high price (up to 2 million US dollars / ton), high pollution and high toxicity, which seriously limit its mass production and application. Along with the development trend of strengthening military industry and strengthening economy at home and abroad, people urgently need to develop some high-energy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/89C06B25/34
Inventor 刘祖亮成健姚其正
Owner NANJING UNIV OF SCI & TECH
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