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Refining method of 2,6-diamino-3,5-dinitropyridine-1-oxide

The technology of a dinitropyridine and a refining method is applied in the refining field of 2,6-diamino-3,5-dinitropyridine-1-oxide, and can solve the problem of large consumption of organic solvent and solvent trifluoroacetic acid. Problems such as high toxicity, to achieve the effect of low solvent toxicity

Inactive Publication Date: 2015-05-20
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing ANPyO refining method still has the disadvantages of high toxicity of the solvent trifluoroacetic acid, large consumption of commonly used polar organic solvents (10g / 100ml), and the need for three steps in the acetylation refining process.

Method used

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  • Refining method of 2,6-diamino-3,5-dinitropyridine-1-oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1)Cu(ANPyO) 2 Preparation of complexes

[0029] In a 100ml three-necked flask equipped with a magnet and a thermometer, add 43.0mLDMSO and 4.30g of 2,6-diamino-3,5-dinitropyridine-1 oxide (20mmol) with a purity of 90% under stirring , after adding, heat to 80°C, keep warm for 0.5h, then add 2.42g Cu(NO 3 ) 2 ·3H 2 O (10mmol), keep warm for 2h, filter while hot, recover the DMSO filtrate, wash the filter cake with water, wash with acetone, and dry to obtain 4.40g of 2,6-diamino-3,5-dinitropyridine-1-oxide Copper complex, yield 99.0%.

[0030] Structure Identification:

[0031] DSC decomposition peak temperature: 384.1°C;

[0032] Infrared spectrum (KBr, cm -1 )γ: 3405, 3356, 3287, 3080, 1635, 604, 546;

[0033] The above structural identification data confirm that the substance obtained in this step is 2,6-diamino-3,5-dinitropyridine-1-oxide copper complex.

[0034] (2) Acidification to remove copper ions to obtain ANPyO

[0035] In a 100ml three-necked flask eq...

Embodiment 2

[0042] (1)Cu(ANPyO) 2 Preparation of complexes

[0043] In a 100ml three-necked flask equipped with a magnet and a thermometer, 86.0mL DMF and 4.30g of 2,6-diamino-3,5-dinitropyridine-1 oxide (20mmol ), heated to 80°C after the addition, kept the temperature for 0.5h, then added 2.40g Cu(OOCCH 3 ) 2 ·H 2 O (12mmol), keep warm for 4h, filter while hot, recover the DMF filtrate, wash the filter cake with water, wash with acetone, and dry to obtain 4.50g of 2,6-diamino-3,5-dinitropyridine-1-oxide Copper complex, yield 97.9%.

[0044] (2) Acidification to remove copper ions to obtain ANPyO

[0045] In a 250ml three-neck flask equipped with a stirrer and a thermometer, add 17.3ml of sulfuric acid, and add 2.47g (5mmol) of the above-mentioned 2,6-diamino-3,5-dinitropyridine-1 oxide copper complex under stirring After the addition, the temperature was raised to 80°C. After the solid matter was completely dissolved, it was kept warm for 0.5h, and the insoluble copper sulfate sol...

Embodiment 3

[0047] (1)Cu(ANPyO) 2 Preparation of complexes

[0048] In a 100ml three-necked flask equipped with a magnet and a thermometer, add 50mL DMSO and 4.30g of 2,6-diamino-3,5-dinitropyridine-1 oxide (20mmol) with a purity of 93% under stirring , after adding, heat to 80°C, keep warm for 0.5h, then add 3.00g Cu(SO 4 ) 2 ·5H 2 O (12mmol), keep warm for 1h, filter while hot, recover the DMSO filtrate, wash the filter cake with water, wash with acetone, and dry to obtain 4.40g of 2,6-diamino-3,5-dinitropyridine-1-oxide Copper complex, yield 95.8%.

[0049] (2) Acidification to remove copper ions to obtain ANPyO

[0050] In a 100ml three-necked flask equipped with a stirrer and a thermometer, add 12ml of sulfuric acid, and add 2.47g (5mmol) of the above-mentioned 2,6-diamino-3,5-dinitropyridine-1 oxide copper complex under stirring, After the addition, the temperature was raised to 80°C. After the solid matter was completely dissolved, the heat was kept for 0.5h. The insoluble co...

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Abstract

The invention relates to a refining method of 2,6-diamino-3,5-dinitropyridine-1-oxide. The refining method comprises the following steps of: adding crude 2,6-diamino-3,5-dinitropyridine-1-oxide and copper salt into a polarity organic solvent, carrying out coordination reaction to obtain a 2,6-diamino-3,5-dinitropyridine-1-oxide copper complex, separating impurities by utilizing the characteristics that the complex is difficult to dissolve and the impurities are easy to dissolve, and removing copper ion in the complex under acidic conditions so as to obtain the refined 2,6-diamino-3,5-dinitropyridine-1-oxide. The refining method provided by the invention has the characteristics of being low in solvent toxicity, use amount and refining step and has the industrialized application prospect; the refining method is used for refining the 2,6-diamino-3,5-dinitropyridine-1-oxide; and therefore, the 2,6-diamino-3,5-dinitropyridine-1-oxide with the purity of being more than 99% can be obtained.

Description

technical field [0001] The invention relates to a method for refining 2,6-diamino-3,5-dinitropyridine-1-oxide, which belongs to the field of organic synthesis. Background technique [0002] 2,6-diamino-3,5-dinitropyridine-1-oxide (ANPyO) is a new type of high-energy, low-sensitivity, heat-resistant elemental explosive with excellent performance, and its crystal density is 1.886g / cm 3 , the detonation velocity and detonation pressure are respectively 7900m / s (1.84g / cm 3 ), 28GPa (1.84g / cm 3 ), the DSC decomposition peak temperature is greater than 350°C (10°C / min), and the impact sensitivity is H 50 =250cm, friction sensitivity 0%, can be used in special weapons, ultra-high temperature petroleum perforating bullets, explosives and other fields. [0003] The synthesis of ANPyO is mainly through the preparation method of 2,6-diamino-3,5-dinitropyridine as an intermediate, using hydrogen peroxide oxidation in acetic acid or trifluoroacetic acid, which is a commonly used proce...

Claims

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Application Information

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IPC IPC(8): C07D213/89
CPCC07D213/89
Inventor 张蒙蒙黄凤臣王友兵周杰文张创军李媛胡琳琳席伟汪强
Owner XIAN MODERN CHEM RES INST
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