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
View PDF1 Cites 3 Cited by
  • 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

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Refining method of 2,6-diamino-3,5-dinitropyridine-1-oxide

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0027] Example 1:

[0028] (1) Cu(ANPyO) 2 Preparation of the complex

[0029] In a 100ml three-necked flask equipped with a magnet and a thermometer, 43.0mL of DMSO and 4.30g of 2,6-diamino-3,5-dinitropyridine-1 oxide (20mmol) with a purity of 90% were sequentially added under stirring. After adding, heat to 80℃, keep for 0.5h, then add 2.42g Cu(NO 3 ) 2 ·3H 2 O (10mmol), heat preservation reaction for 2h, filter while hot, and recover the DMSO filtrate. The filter cake is washed with water, acetone, and dried to obtain 4.40g of 2,6-diamino-3,5-dinitropyridine-1-oxide The yield of copper complex is 99.0%.

[0030] Structure Identification:

[0031] DSC decomposition peak temperature: 384.1℃;

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

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

[0034] (2) Acidification to remove copper ions to obt...

Example Embodiment

[0041] Example 2:

[0042] (1) Cu(ANPyO) 2 Preparation of the complex

[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) with a purity of 93% were sequentially added under stirring. ), heat to 80℃ after adding, keep for 0.5h, then add 2.40g Cu(OOCCH 3 ) 2 ·H 2 O (12mmol), heat preservation reaction for 4h, filter while hot, and recover the DMF filtrate. The filter cake is washed with water, acetone, and dried to obtain 4.50g of 2,6-diamino-3,5-dinitropyridine-1-oxide The yield of copper complex is 97.9%.

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

[0045] In a 250ml three-necked flask equipped with a stirrer and a thermometer, add 17.3ml of sulfuric acid, and add the above 2,6-diamino-3,5-dinitropyridine-1 oxide copper complex 2.47g (5mmol) under stirring. After the addition, the temperature is raised to 80°C, after the solid matter is completely dissolved, th...

Example Embodiment

[0046] Example 3:

[0047] (1) Cu(ANPyO) 2 Preparation of the complex

[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℃, keep for 0.5h, then add 3.00g Cu(SO 4 ) 2 ·5H 2 O (12mmol), heat preservation reaction for 1h, filter while hot, and recover the DMSO filtrate. The filter cake is washed with water, acetone, and dried to obtain 4.40g of 2,6-diamino-3,5-dinitropyridine-1-oxide Copper complex, the yield is 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 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 temperature was kep...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap