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A kind of spherical adn particle, preparation method and application thereof

A particle and spherical technology, applied in chemical instruments and methods, offensive equipment, chemical/physical/physical-chemical reactors, etc., can solve the problems of difficult to prepare spherical ADN, high process risk, difficult implementation, etc., to reduce the temperature , high quality and good reproducibility

Active Publication Date: 2022-04-12
HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the above method, high-quality spherical ADN can be prepared by melting granulation technology, but in the process of process implementation, ADN needs to be melted at high temperature before granulation, which has high process risk, high equipment requirements, and great difficulty in implementation; while the crystal form Inhibition technology has mild reaction conditions, but it is necessary to introduce inert crystal inhibitors, making it difficult to prepare high-quality spherical ADN

Method used

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  • A kind of spherical adn particle, preparation method and application thereof
  • A kind of spherical adn particle, preparation method and application thereof
  • A kind of spherical adn particle, preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0052] Weigh 5 g of ADN and dissolve in 15 g of acetone, and stir at 25° C. to completely dissolve the ADN to form an ADN solution. Take 100mL of simethicone in a beaker as anti-solvent A, and take 200mL of simethicone in a three-necked flask as anti-solvent B. Take a coaxial microchannel reactor with an inner channel inner diameter of 0.1 mm and an outer channel inner diameter of 0.5 mm, respectively use a peristaltic pump to inject the ADN solution into the inner channel of the microreactor at a drop rate of 0.05 mL / min, and simultaneously inject anti-solvent A with Dropping speed 0.5mL / min into the outer channel of the microreactor to form micro-droplets, drop the micro-droplets into the anti-solvent B, keep the reaction solution ultrasonically stirred, wherein the ultrasonic power is 800W, the stirring speed is 500rpm, after the dropwise addition, Turn off the ultrasound, continue to react for 2 hours, filter with suction, wash with dichloromethane three times, and dry the...

Embodiment 2

[0054] Weigh 4g of ADN and dissolve in 15g of acetonitrile, and stir to completely dissolve ADN to form an ADN solution. Take 100mL liquid paraffin in a beaker as anti-solvent A. Take 200mL liquid paraffin in a three-necked flask as anti-solvent B. Take a coaxial microchannel with an inner channel inner diameter of 0.8 mm and an outer channel inner diameter of 2 mm, respectively use a peristaltic pump to inject the ADN solution into the inner channel of the microreactor at a drop rate of 0.3 mL / min, and simultaneously inject anti-solvent A at a rate of 1.5 mL / min. Inject the micro-droplets into the outer channel of the microreactor at a drop speed of min to form micro-droplets, drop the micro-droplets into the anti-solvent B, and keep the reaction solution ultrasonically stirred, wherein the ultrasonic power is 1000W, and the stirring speed is 500rpm. After the dropwise addition, the ultrasound was turned off, and the reaction was continued for 2 hours, filtered with suction,...

Embodiment 3

[0056] Weigh 5g of ADN and dissolve in 20g of methyl ethyl ketone, and stir to completely dissolve ADN to form an ADN solution. Take 100mL white oil in a beaker as anti-solvent A. Take 200mL white oil in a three-necked flask as anti-solvent B. Take a coaxial microchannel reactor in which the inner diameter of the inner channel is 0.2 mm and the inner diameter of the outer channel is 1 mm. Use a peristaltic pump to inject the ADN solution into the inner channel of the microreactor at a drip rate of 0.2mL / min, inject the anti-solvent A0.8mL / min into the outer channel of the microreactor to form micro-droplets, and drop the micro-droplets into In the anti-solvent B, keep the reaction solution under ultrasonic stirring, wherein the ultrasonic power is 800W, and the stirring speed is 500rpm. After the dropwise addition, the ultrasound was turned off, and the reaction was continued for 2 hours, filtered with suction, washed with dichloromethane three times, and the solid was vacuu...

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Abstract

The invention relates to a method for preparing spherical ammonium dinitramide (ADN) particles based on confinement microdroplets of microchannels, the ammonium dinitramide (ADN) particles prepared by the method and applications thereof. Above-mentioned method configures ADN solution at first, and selects suitable anti-solvent, then ADN solution and anti-solvent are formed ADN solution-anti-solvent micro-droplet by coaxial microchannel reactor with certain flow rate, micro-droplet is dispersed in specific In the solvent, supplemented by ultrasound or stirring, the ADN spherical particle suspension is obtained, and finally the spherical ADN particle is obtained by suction filtration, washing and vacuum drying. The invention adopts a microchannel reactor, and the particle size of spherical ADN particles can be adjusted through the diameter ratio of the microchannel and the flow rate ratio of the solution and the antisolvent, and the particle size distribution is narrow, the reaction efficiency is high, the conditions are mild, and no heating is required. The microsphere is simple and safe, and is conducive to scale-up production. The microsphere has a significantly lower moisture absorption rate, a high sphericity, and is easy to be made into a drug, and can be extended to the preparation of spherical particles of other energetic materials.

Description

technical field [0001] The invention relates to a method for preparing spherical ammonium dinitramide (ADN) particles based on confined micro-droplets of microchannels, spherical ammonium dinitramide (ADN) particles and applications thereof, belonging to the field of energetic materials. Background technique [0002] The new generation of high-performance weapons and equipment all put forward the requirements of high energy, low characteristic signal, low risk and low pollution. The molecular structure of ADN has both oxidant and fuel components, and the oxygen content is high, and the heat of formation is -148.4~-149.6kJ / mol. It can be used as both an explosive and an oxidizer for a solid propellant. Different from the widely used oxidant AP (heat of formation is -295.5kJ / mol) currently used in propellants, the molecular structure of ADN does not contain halogen, and the combustion product has no "smoke", which makes the launch of the missile have a lower characteristic sig...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01C1/00B01J19/00C06B31/00C06D5/00
CPCC01C1/00B01J19/0093C06B31/00C06D5/00C01P2004/32C01P2004/03C01P2004/51
Inventor 陈红李磊赵辉王艳薇黄丹椿汪慧思陶博文杜芳顾健
Owner HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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