3, 3'-diamino-4, 4'-oxazafurazan multi-stage geode and preparation method thereof

A technology of azofurazan oxide and diamino, which is applied in organic chemistry methods, offensive equipment, organic chemistry, etc., can solve the problems that DAAF self-assembled crystal multi-level structure has not been reported, and achieves mild experimental conditions and good safety , The effect of broadening the application field

Active Publication Date: 2019-08-27
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Judging from the existing public information, there are currently only some DAAF synthetic route improvements and DAAF submicron or nanoparticle preparation methods at home and abroad, but there are no reports on the crystallization process control of DAAF and the preparation of self-assembled crystalline multi-level structures.

Method used

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  • 3, 3'-diamino-4, 4'-oxazafurazan multi-stage geode and preparation method thereof
  • 3, 3'-diamino-4, 4'-oxazafurazan multi-stage geode and preparation method thereof
  • 3, 3'-diamino-4, 4'-oxazafurazan multi-stage geode and preparation method thereof

Examples

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Effect test

Embodiment 1

[0023] Weigh 0.3 g of 3,3’-diamino-4,4’-azofurazan and 20 mL of dimethyl sulfoxide at room temperature, stir and place the beaker in an ultrasonic oscillator until completely dissolved. Put the beaker in a constant temperature incubator, set the temperature at 30°C, and slowly evaporate the solvent. After the solvent is completely evaporated, filter it under reduced pressure, and rinse it with ultrapure water and absolute ethanol to wash away the residual solvent in the explosive. . Vacuum-dried for 3-4 hours to obtain 3,3'-diamino-4,4'-azofurazan multi-level crystal balls. figure 1 and figure 2 They are the scanning electron micrographs and the cross-sectional electron micrographs of the 3,3'-diamino-4,4'-azoxide multi-level structure explosive obtained according to this example, respectively. The size of the microspheres is 300 μm to 450 μm, the size of the small nanoparticles constituting the microspheres is 10 μm to 20 μm, and the product purity is 99.6%. When dimethyl...

Embodiment 2

[0025] Weigh 0.3g of 3,3'-diamino-4,4'-azofurazan at room temperature, measure 30mL of acetone, stir and place the beaker in an ultrasonic oscillator until completely dissolved. Put the beaker in a constant temperature incubator, set the temperature at 30°C, and slowly evaporate the solvent. After the solvent is completely evaporated, filter it under reduced pressure, and rinse it with ultrapure water and absolute ethanol to wash away the residual solvent in the explosive. . Vacuum-dried for 3-4 hours to obtain 3,3'-diamino-4,4'-azofuroxan. image 3 It is a scanning electron micrograph of the 3,3'-diamino-4,4'-azoxyl explosive obtained according to this example. The product is a strip crystal with a length of about 100 μm, and the product purity is 99.0%. Acetone has a low polarity (5.4), and will generate intermolecular forces with the secondary growth crystal planes, and the growth rate of this plane is inhibited, resulting in the rapid growth of the main growth crystal pl...

Embodiment 3

[0027] Weigh 0.3g of 3,3'-diamino-4,4'-azofurazan and 45mL of ethyl acetate at room temperature, stir and place the beaker in an ultrasonic oscillator until completely dissolved. Put the beaker in a constant temperature incubator, set the temperature at 30°C, and slowly evaporate the solvent. After the solvent is completely evaporated, filter it under reduced pressure, and rinse it with ultrapure water and absolute ethanol to wash away the residual solvent in the explosive. . Vacuum-dried for 3-4 hours to obtain 3,3'-diamino-4,4'-azofurazan multi-level crystal balls. figure 1 and figure 2 They are the scanning electron micrographs and the cross-sectional electron micrographs of the 3,3'-diamino-4,4'-azoxide multi-level structure explosive obtained according to this embodiment, respectively. The product is massive broken crystals with a wide range of particle size distribution, about 10 μm to 100 μm, and the product purity is 99.4%. Ethyl acetate is less polar (4.3), and wi...

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Abstract

The invention discloses a 3, 3'-diamino-4, 4'-oxazafurazan multi-stage geode and a preparation method thereof. The 3, 3'-diamino-4, 4'-oxazafurazan multi-stage geode comprises the following steps of dissolving 3, 3'-diamino-4, 4'-oxazafurazan explosive into an organic solvent till the 3, 3'-diamino-4, 4'-oxazafurazan explosive is completely dissolved; enabling an obtained mixture to stand in a constant temperature incubator; enabling the solvent to volatilize; and after the solvent completely volatilizes, carrying out suction filtration, flushing and vacuum drying on the mixture to finally obtain the 3, 3'-diamino-4, 4'-oxazafurazan multi-stage geode. The 3, 3'-diamino-4, 4'-oxazafurazan multi-stage geode disclosed by the invention has the advantages that the impurity content of an explosive product prepared by the preparation method is less, the purity of the explosive product is high, and the 3, 3'-diamino-4, 4'-oxazafurazan multi-stage geode is beneficial for studying crystal habitsof high energy insensitive high explosive 3, 3'-diamino-4, 4'-oxazafurazan multi-stage geode and expanding the application range of the high energy insensitive high explosive 3, 3'-diamino-4, 4'-oxazafurazan multi-stage geode.

Description

technical field [0001] The invention belongs to the field of energetic materials, and in particular relates to a preparation method of 3,3'-diamino-4,4'-azofurazan multilevel crystal spheres. Background technique [0002] With the emergence of elemental explosives such as triaminotrinitrobenzene (TATB) and hexanitrostilbene (HNS), the problems of safe charge and use of shock plate detonators have been gradually solved, but there are still problems such as high detonation threshold and detonation energy. Low, detonators are difficult to miniaturize and other issues. Therefore, designing and synthesizing the initiator for shock-disc detonators with good short-pulse detonation performance, high detonation energy and good stability is a hot and difficult point of research. 3,3'-diamino-4,4'-azofurazan (DAAF) is an insensitive compound with a standard enthalpy of formation of 442.6kJ / mol, a crystal density of 1.747g / cm3, and a thermal decomposition temperature of 259°C. High-en...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D271/08C06B49/00C06B21/00
CPCC06B21/00C06B49/00C07B2200/13C07D271/08
Inventor 高寒姚笑璐黄明蔡贾林索志荣黄荣黄薇罗观
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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