CN113415809A - Spherical ADN particle, preparation method and application thereof - Google Patents
Spherical ADN particle, preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a method for preparing spherical Ammonium Dinitramide (ADN) particles based on domain-limited micro-droplets of micro-channels, Ammonium Dinitramide (ADN) particles prepared by the method and application thereof. Firstly preparing an ADN solution, selecting a proper anti-solvent, then enabling the ADN solution and the anti-solvent to pass through a coaxial microchannel reactor at a certain flow rate to form ADN solution-anti-solvent micro-droplets, dispersing the micro-droplets in a specific solvent, assisting with ultrasound or stirring to obtain an ADN spherical particle suspension, and finally obtaining spherical ADN particles through suction filtration, washing and vacuum drying. The invention adopts the microchannel reactor, can adjust the particle size of the spherical ADN particles through the microchannel tube diameter ratio and the flow rate ratio of the solution and the anti-solvent, has narrow particle size distribution, high reaction efficiency, mild conditions, no need of heating, simple and safe operation, contribution to amplification production, obvious reduction of the moisture absorption rate of the microsphere, high sphericity, easy drug formation and popularization to the preparation of spherical particles of other energetic materials.
Description
Technical Field
The invention relates to a method for preparing spherical Ammonium Dinitramide (ADN) particles by domain-limited micro-droplets based on micro-channels, the spherical Ammonium Dinitramide (ADN) particles and application thereof, and belongs to the field of energetic materials.
Background
The new generation of high-performance weaponry all puts forward the requirements of high energy, low characteristic signal, low danger, low pollution and the like. The molecular structure of ADN contains both oxidant and fuel components, and has high oxygen content and heat of formation of-148.4-149.6 kJ/mol, and can be used as explosive and oxidant of solid propellant. Different from an oxidant AP (generated heat is-295.5 kJ/mol) widely used by the current propellant, the ADN does not contain halogen in a molecular structure, combustion products do not have smoke, the missile has lower characteristic signals when being launched, the environmental pollution is small, the specific impulse of the propellant with low characteristic signals is generally lower than that of the propellant with less smoke and smoke for 6-14 s according to statistics, and if the ADN is used for replacing the AP, the specific impulse of the propellant with low characteristic signals can be expected to be greatly improved. Therefore, ADN is one of the most promising new generation solid propellant high-energy components urgently needed by future strategic and tactical missiles as a novel oxidant.
However, ADN has problems of high moisture absorption, poor stability, poor mechanical properties, chemical incompatibility with isocyanates, and the like, and the most troublesome is the strong moisture absorption of ADN (ADN can be dissolved in 100 g of water at 20 ℃) and is difficult to apply in solid propellants. ADN synthesized by conventional methods is generally needle-shaped or plate-shaped crystal, and has extremely strong hygroscopicity. The results of the study show that the hygroscopicity of ADN is reduced after spherical granulation. Currently, the main methods for ADN spherical granulation include a melt granulation technique and a crystal form inhibition technique. However, in the above method, the melting granulation technology can prepare high-quality spherical ADN, but the ADN needs to be melted at high temperature and then granulated in the process, so that the process has high risk, high equipment requirement and high implementation difficulty; the reaction conditions of the crystal form inhibition technology are mild, but an inert crystal form inhibitor needs to be introduced, so that high-quality spherical ADN is difficult to prepare.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a method for preparing spherical Ammonium Dinitramide (ADN) particles by using domain-limited micro-droplets based on microchannels, the spherical Ammonium Dinitramide (ADN) particles and application thereof.
In order to achieve the above purpose, the invention provides the following technical scheme:
a method for preparing spherical ADN particles is characterized by comprising the following steps:
(1) adding ADN into a solvent, and stirring to obtain an ADN solution;
(2) simultaneously dripping the ADN solution obtained in the step (1) and the antisolvent A into the antisolvent B by using a limited-area micro-droplet method under the dispersion action;
continuously reacting after the dropwise adding is finished to obtain a solid-liquid mixed system containing ADN microspheres and a solvent;
the domain-limited micro-droplet method is carried out by adopting a coaxial micro-channel reactor;
(3) and (3) carrying out post-treatment on the solid-liquid mixed system obtained in the step (2) to obtain the ADN microspheres.
Further, in the step (2), the coaxial microchannel reactor comprises an inner channel and an outer channel which are coaxial, wherein the inner diameter of the inner channel is 0.1-1 mm, and the inner diameter of the outer channel is 0.5-3 mm; the material of the coaxial microchannel reactor is glass or stainless steel.
Further, in the step (2), the flow rate of the ADN solution obtained in the step (1) is 0.05 mL/min-0.5 mL/min, and the flow rate of the antisolvent A is 0.20 mL/min-5 mL/min.
Further, in the step (2), the ratio of the flow rate of the ADN solution obtained in the step (1) to the flow rate of the antisolvent A is 1:4 to 1: 10.
Further, in the step (2), the dispersing action is stirring and ultrasonic waves which are applied simultaneously, wherein the ultrasonic power is 600-2000W, and the stirring speed is 300-800 rpm.
Further, in the step (1), the solvent is one or more of acetonitrile, acetone, butanone, ethanol and isopropanol.
Further, in the step (2), the anti-solvent A is one or more of white oil, liquid paraffin, fatty oil and simethicone; in the step (2), the anti-solvent B is one or more of white oil, liquid paraffin, fatty oil and simethicone.
Further, in the step (3), the post-treatment process sequentially comprises suction filtration, washing and vacuum drying; the washing process adopts one or more of cyclohexane, hexane or dichloromethane as a washing solvent; and the vacuum drying condition is drying for 2-24 hours at the temperature of 40-60 ℃.
Further, in the step (2), the reaction is continued for 1 to 4 hours after the dropwise addition is completed.
The spherical ADN particle prepared by the preparation method of the spherical ADN particle has the particle size difference between the maximum particle size and the minimum particle size of less than or equal to 100 mu m.
Further, the spherical ADN is applied to the field of solid propellants, explosives or fireworks agents.
Compared with the prior art, the invention has the following beneficial effects:
(1) the spherical ADN energetic particle with narrow particle size distribution is prepared by the preparation method of the spherical ADN energetic particle, and has the characteristics of high reaction efficiency, accurate control of the spherical shape and particle size distribution, adjustable particle size, mild reaction condition, high preparation speed, good reproducibility, compact structure, good sphericity, high quality and the like.
(2) The preparation method of the spherical ADN particles is different from the conventional preparation method of the spherical ADN, adopts high-temperature melting spheroidization or high-temperature spray granulation, or adopts a refined recrystallization method of a crystal form control agent, adopts a limited domain micro-droplet method, not only reduces the spheroidization temperature, but also can accurately control the particle size distribution, simultaneously does not need to adopt the crystal form control agent, and improves the quality of the spheroidized ADN.
(3) The invention relates to a preparation method of spherical ADN particles, which designs the sizes of an inner channel and an outer channel in a coaxial microchannel reactor, simultaneously selects the flow rates of an ADN solution and an anti-solvent in the coaxial microchannel reactor and the flow rate proportional relation of the ADN solution and the anti-solvent in the coaxial microchannel reactor through a large number of experiments, enables the reaction condition to reach the optimum, controls the particle size and the sphericity of ADN microspheres by adjusting the inner diameter of a microchannel and the relative flow rate of a solution phase and an anti-solvent phase, and further improves the sphericity and the quality of spherical ADN;
(4) the invention relates to a preparation method of spherical ADN particles, which comprises the steps of selecting a proper anti-solvent, enabling an ADN solution and the anti-solvent to pass through a coaxial microchannel reactor at a certain flow rate to form stable ADN solution-anti-solvent micro-droplets, and dispersing to obtain a stable ADN spherical particle suspension;
(5) according to the preparation method of the spherical ADN particles, inert substances are not required to be introduced, the quality of the ADN microspheres can be obviously improved, and the preparation method is simple, safe and efficient and is easy for industrial production;
(6) the preparation method of the spherical ADN particles has the advantages of mild, simple, safe and rapid process conditions, controllable sphericity and particle size, suitability for industrial production, and good application prospect in the fields of solid propellants, explosives, firework agents and the like.
Drawings
FIG. 1 is a scanning electron micrograph of ADN particles obtained in example 6 of the present invention;
FIG. 2 is a graph showing the particle size distribution of ADN particles obtained in example 1 of the present invention;
FIG. 3 is a graph showing the particle size distribution of ADN particles obtained in example 6 of the present invention;
FIG. 4 is a graph showing the particle size distribution of ADN particles obtained in example 7 of the present invention.
Detailed Description
The features and advantages of the present invention will become more apparent and appreciated from the following detailed description of the invention.
The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments. While the various aspects of the embodiments are presented in drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
A method for preparing spherical Ammonium Dinitramide (ADN) particles based on domain-limited micro-droplets of micro-channels, which comprises the following steps:
(1) adding ADN into a solvent according to a certain proportion, and uniformly stirring to obtain an ADN solution for later use;
(2) simultaneously dripping the ADN solution obtained in the step (1) and the antisolvent A into an antisolvent B by using a limited-area micro-droplet method under the dispersion action to obtain a solid-liquid mixed system containing ADN microspheres and a solvent, namely an ADN spherical particle suspension;
the domain-limited micro-droplet method is carried out by adopting a coaxial micro-channel reactor;
(3) and (3) carrying out post-treatment on the solid-liquid mixed system obtained in the step (2) to obtain the ADN microspheres.
Further, in the step (2), the coaxial microchannel reactor comprises an inner channel and an outer channel which are coaxial, wherein the inner diameter of the inner channel is 0.1 mm-1 mm, and the inner diameter of the outer channel is 0.5 mm-3 mm; the material of the coaxial microchannel reactor is glass or stainless steel.
Further, in the step (2), the flow rate of the ADN solution obtained in the step (1) is 0.05 mL/min-0.5 mL/min, and the flow rate of the antisolvent A is 0.20 mL/min-5 mL/min.
Further, in the step (2), the ratio of the flow rate of the ADN solution obtained in the step (1) to the flow rate of the antisolvent A is 1:4 to 1: 10.
Further, in the step (2), the dispersion effect is stirring and ultrasonic waves which are simultaneously applied, namely the ultrasonic waves and the stirring are kept in the dropping process, the ultrasonic power is 600-2000W, and the stirring speed is 300-800 rpm.
Further, in the step (1), the solvent is one or more of acetonitrile, acetone, butanone, ethanol and isopropanol.
Further, in the step (2), the antisolvent A is one or more of white oil, liquid paraffin, fatty oil and simethicone; in the step (2), the anti-solvent B is one or more of white oil, liquid paraffin, fatty oil and simethicone; antisolvent a and antisolvent B may be the same or different.
Further, in the step (3), the post-treatment process sequentially comprises suction filtration, washing and vacuum drying; the washing process adopts one or more of cyclohexane, hexane or dichloromethane as a washing solvent; and the vacuum drying condition is drying for 2-24 hours at the temperature of 40-60 ℃.
Further, in the step (1), the ADN solution is a saturated solution.
The spherical ADN particles are prepared by adopting the method for preparing the spherical ADN particles by the domain-limited micro-droplets based on the micro-channels, and the difference between the particle size of the largest particle and the particle size of the smallest particle in the spherical ADN particles is less than or equal to 100 mu m.
The application of spherical ADN particles is applied to the field of solid propellants, explosives or fireworks agents.
The method comprises the steps of firstly preparing an ADN solution, selecting a proper anti-solvent, then enabling the ADN solution and the anti-solvent to pass through a coaxial microchannel reactor at a certain flow rate to form ADN solution-anti-solvent micro-droplets, dispersing the micro-droplets in a specific solvent, assisting with ultrasound or stirring to obtain an ADN spherical particle suspension, and finally obtaining spherical ADN particles through suction filtration, washing and vacuum drying. The invention adopts the microchannel reactor, can adjust the particle size of the spherical ADN particles through the microchannel tube diameter ratio and the flow rate ratio of the solution and the anti-solvent, has narrow particle size distribution, high reaction efficiency, mild conditions, no need of heating, simple and safe operation, contribution to amplification production, obvious reduction of the moisture absorption rate of the microsphere, high sphericity, easy drug formation and popularization to the preparation of spherical particles of other energetic materials.
Example 1
5g of ADN was dissolved in 15g of acetone and stirred at 25 ℃ to dissolve ADN completely to form an ADN solution. 100mL of dimethicone was taken as antisolvent A in a beaker, and 200mL of dimethicone was taken as antisolvent B in a three-necked flask. Taking a coaxial microchannel reactor with an inner channel inner diameter of 0.1mm and an outer channel inner diameter of 0.5mm, respectively injecting an ADN solution into an inner channel of the microreactor at a dropping speed of 0.05mL/min by using a peristaltic pump, simultaneously injecting an antisolvent A into an outer channel of the microreactor at a dropping speed of 0.5mL/min to form micro droplets, dropping the micro droplets into an antisolvent B, keeping the reaction liquid ultrasonically stirred, wherein the ultrasonic power is 800W, the stirring speed is 500rpm, turning off the ultrasonic after the dropping is finished, continuing to react for 2 hours, performing suction filtration, washing with dichloromethane three times, and performing vacuum drying on the solid at 40 ℃ for 24 hours. 5g of untreated ADN material and 5g of the spherical ADN granules obtained were each subjected to a hygroscopicity test at a temperature of 25 ℃ and a relative humidity of 50%. The results showed that the moisture absorption before and after ADN treatment was 1.37% and 0.42%, respectively.
Example 2
4g of ADN were weighed out and dissolved in 15g of acetonitrile and stirred to dissolve the ADN completely to form an ADN solution. 100mL of liquid paraffin was taken as the antisolvent A in the beaker. 200mL of liquid paraffin was taken as the antisolvent B in a three-necked flask. Taking a coaxial microchannel with the inner channel inner diameter of 0.8mm and the outer channel inner diameter of 2mm, respectively injecting an ADN solution into the inner channel of the microreactor at a dropping speed of 0.3mL/min by using a peristaltic pump, simultaneously injecting an antisolvent A into the outer channel of the microreactor at a dropping speed of 1.5mL/min to form a micro-droplet, dropping the micro-droplet into an antisolvent B, and keeping the reaction liquid ultrasonically stirred, wherein the ultrasonic power is 1000W, and the stirring speed is 500 rpm. After the dropwise addition, the ultrasonic treatment is turned off, the reaction is continued for 2 hours, the filtration is carried out, the washing is carried out for three times by using dichloromethane, and the solid is dried in vacuum for 24 hours at the temperature of 60 ℃. 2g of untreated ADN raw material and 2g of prepared ADN microspheres are respectively taken and subjected to a hygroscopicity test under the conditions of 25 ℃ and 50% relative humidity. The results showed that the moisture absorption before and after ADN treatment was 1.37% and 0.43%, respectively.
Example 3
5g of ADN were weighed out and dissolved in 20g of butanone and stirred to dissolve ADN completely to form an ADN solution. 100mL of white oil was taken in a beaker as antisolvent A. 200mL of white oil was taken in a three-necked flask as antisolvent B. A coaxial micro-channel reactor with the inner diameter of an inner channel being 0.2mm and the inner diameter of an outer channel being 1mm is taken. Respectively injecting ADN solution into an inner channel of the microreactor at a dropping speed of 0.2mL/min by using a peristaltic pump, injecting an antisolvent A0.8mL/min into an outer channel of the microreactor to form micro-droplets, dropping the micro-droplets into an antisolvent B, and keeping the reaction liquid ultrasonically stirred, wherein the ultrasonic power is 800W, and the stirring speed is 500 rpm. After the dropwise addition, the ultrasound was turned off, the reaction was continued for 2 hours, suction filtration was carried out, washing was carried out three times with dichloromethane, and the solid was dried under vacuum at 40 ℃ for 24 hours. 2g of untreated ADN raw material and 2g of prepared ADN microspheres are respectively taken and subjected to a hygroscopicity test under the conditions of 25 ℃ and 50% relative humidity. The results show that the moisture absorption before and after ADN treatment was 1.37% and 0.48%, respectively.
Example 4
5g of ADN was weighed into 15g of isopropanol and stirred to dissolve the ADN completely to form an ADN solution. 100mL of fatty oil was taken in a beaker as antisolvent A. 200mL of fatty oil was taken in a three-necked flask as antisolvent B. Taking a coaxial microchannel reactor with the inner diameter of an inner channel being 0.4mm and the inner diameter of an outer channel being 2.0mm, respectively injecting an ADN solution into the inner channel of the microreactor at a dropping speed of 0.2mL/min by adopting a peristaltic pump, simultaneously injecting an antisolvent A into the outer channel of the microreactor at a dropping speed of 0.8mL/min to form micro-droplets, dropping the micro-droplets into an antisolvent B, and keeping the reaction liquid ultrasonically stirred, wherein the ultrasonic power is 2000W, and the stirring speed is 800 rpm. After the dropwise addition, the ultrasonic treatment is turned off, the reaction is continued for 2 hours, the filtration is carried out, the washing is carried out for three times by using dichloromethane, and the solid is dried in vacuum for 12 hours at the temperature of 60 ℃. 2g of untreated ADN raw material and 2g of prepared ADN microspheres are respectively taken and subjected to a hygroscopicity test under the conditions of 25 ℃ and 50% relative humidity. The results showed that the moisture absorption before and after ADN treatment was 1.37% and 0.54%, respectively.
Example 5
4g of ADN were weighed out and dissolved in 12g of ethanol, and the ADN was dissolved completely with stirring to form an ADN solution. 100mL of liquid paraffin was taken as the antisolvent A in the beaker. 200mL of dimethicone was taken as the antisolvent B in a three-necked flask. Taking a coaxial microchannel with the inner channel inner diameter of 0.5mm and the outer channel inner diameter of 1.2mm, respectively injecting an ADN solution into the inner channel of the microreactor at a dropping speed of 0.1mL/min by using a peristaltic pump, simultaneously injecting an antisolvent A into the outer channel of the microreactor at a dropping speed of 0.5mL/min to form a micro-droplet, dropping the micro-droplet into an antisolvent B, and keeping the reaction solution ultrasonically stirred, wherein the ultrasonic power is 800W, and the stirring speed is 500 rpm. After the dropwise addition, the ultrasonic treatment is turned off, the reaction is continued for 2 hours, the filtration is carried out, the washing is carried out for three times by using dichloromethane, and the solid is dried in vacuum for 24 hours at the temperature of 60 ℃. 2g of untreated ADN raw material and 2g of prepared ADN microspheres are respectively taken and subjected to a hygroscopicity test under the conditions of 25 ℃ and 50% relative humidity. The results showed that the moisture absorption before and after ADN treatment was 1.37% and 0.62%, respectively.
Example 6
5g of ADN were weighed out and dissolved in 15g of acetone, and the solution was stirred to dissolve ADN completely. 100mL of liquid paraffin was taken as the antisolvent A in the beaker. 200mL of liquid paraffin was taken as the antisolvent B in a three-necked flask. Taking a coaxial microchannel reactor with the inner diameter of an inner channel being 0.5mm and the inner diameter of an outer channel being 1.2mm, respectively injecting an ADN solution into the inner channel of the microreactor at a dropping speed of 0.2mL/min by adopting a peristaltic pump, simultaneously injecting an antisolvent A into the outer channel of the microreactor at a dropping speed of 0.8mL/min to form micro-droplets, dropping the micro-droplets into an antisolvent B, and keeping the reaction liquid ultrasonically stirred, wherein the ultrasonic power is 800W, and the stirring speed is 500 rpm. After the dropwise addition, the ultrasonic treatment is turned off, the reaction is continued for 2 hours, the filtration is carried out, the washing is carried out for three times by using dichloromethane, and the solid is dried in vacuum for 24 hours at the temperature of 60 ℃. 2g of untreated ADN raw material and 2g of prepared ADN microspheres are respectively taken and subjected to a hygroscopicity test under the conditions of 25 ℃ and 50% relative humidity. The results showed that the moisture absorption before and after ADN treatment was 1.37% and 0.62%, respectively.
Example 7
10g of ADN was dissolved in 50g of acetonitrile and stirred at 25 ℃ to dissolve the ADN completely to form an ADN solution. 600mL of liquid paraffin was taken as the antisolvent A in the beaker. 300mL of liquid paraffin was taken as the antisolvent B in a three-necked flask. Taking a coaxial microchannel reactor with the inner diameter of an inner channel being 1mm and the inner diameter of an outer channel being 3mm, respectively injecting an ADN solution into the inner channel of the microreactor at a dropping speed of 0.5mL/min by using a peristaltic pump, simultaneously injecting an antisolvent A into the outer channel of the microreactor at a dropping speed of 5mL/min to form a micro-droplet, dropping the micro-droplet into an antisolvent B, and keeping the reaction liquid ultrasonically stirred, wherein the ultrasonic power is 600W, and the stirring speed is 300 rpm. After the dropwise addition, the ultrasound was turned off, the reaction was continued for 2 hours, then the filtration was carried out, the solid was washed three times with cyclohexane, and the solid was dried in vacuum at 40 ℃ for 24 hours. 2g of untreated ADN raw material and 2g of prepared ADN microspheres are respectively taken and subjected to a hygroscopicity test under the conditions of 25 ℃ and 50% relative humidity. The results showed that the moisture absorption before and after ADN treatment was 1.37% and 0.62%, respectively.
As shown in fig. 1, fig. 2, fig. 3 and fig. 4, which are respectively a scanning electron micrograph of the ADN particles obtained in example 6, a particle size distribution map of the ADN particles obtained in example 1, a particle size distribution map of the ADN particles obtained in example 6 and a particle size distribution map of the ADN particles obtained in example 7, it can be seen that the ADN microspheres prepared by the method of the present invention have a narrow particle size distribution, adjustable particle size and good sphericity; meanwhile, the moisture absorption rate of the ADN microspheres obtained by the method is compared with that of the ADN raw material which is not subjected to the micro-spheroidization by the method through the moisture absorption test in the embodiments 1-7, and the moisture absorption rate of the ADN microspheres obtained by the method is greatly reduced, so that the ADN microspheres obtained by the method are proved to have good sphericity and high quality, the application difficulty caused by the strong moisture absorption of the ADN is greatly reduced, and the method has a wide application prospect in the fields of solid propellants, explosives or fireworks agents, and can be popularized to the preparation of spherical particles of other energetic materials.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Those skilled in the art will appreciate that those matters not described in detail in the present specification are well known in the art.
Claims (11)
1. A method for preparing spherical ADN particles is characterized by comprising the following steps:
(1) adding ADN into a solvent, and stirring to obtain an ADN solution;
(2) simultaneously dripping the ADN solution obtained in the step (1) and the antisolvent A into the antisolvent B by using a limited-area micro-droplet method under the dispersion action;
continuously reacting after the dropwise adding is finished to obtain a solid-liquid mixed system containing ADN microspheres and a solvent;
the domain-limited micro-droplet method is carried out by adopting a coaxial micro-channel reactor;
(3) and (3) carrying out post-treatment on the solid-liquid mixed system obtained in the step (2) to obtain the ADN microspheres.
2. The method for preparing spherical ADN particles according to claim 1, wherein in step (2), the coaxial microchannel reactor comprises an inner channel and an outer channel which are coaxial, the inner diameter of the inner channel is 0.1 mm-1 mm, and the inner diameter of the outer channel is 0.5 mm-3 mm; the material of the coaxial microchannel reactor is glass or stainless steel.
3. The method for preparing spherical ADN particles according to claim 1, wherein in the step (2), the flow rate of the ADN solution obtained in the step (1) is 0.05mL/min to 0.5mL/min, and the flow rate of the anti-solvent A is 0.20mL/min to 5 mL/min.
4. The method of claim 1 or 3, wherein in step (2), the ratio of the ADN solution flow rate obtained in step (1) to the anti-solvent A flow rate is 1:4 to 1: 10.
5. The method for preparing spherical ADN particles according to claim 1, wherein in the step (2), the dispersion is simultaneously applied with stirring and ultrasound, the ultrasound power is 600-2000W, and the stirring speed is 300-800 rpm.
6. The method for preparing spherical ADN particles as claimed in claim 1, wherein in step (1), the solvent is one or more selected from acetonitrile, acetone, butanone, ethanol and isopropanol.
7. The method for preparing spherical ADN particles according to claim 1, wherein in the step (2), the antisolvent A is one or more of white oil, liquid paraffin, fatty oil and simethicone; in the step (2), the anti-solvent B is one or more of white oil, liquid paraffin, fatty oil and simethicone.
8. The method for preparing spherical ADN particles according to claim 1, wherein in the step (3), the post-treatment process comprises suction filtration, washing and vacuum drying in sequence; the washing process adopts one or more of cyclohexane, hexane or dichloromethane as a washing solvent; and the vacuum drying condition is drying for 2-24 hours at the temperature of 40-60 ℃.
9. The method for preparing spherical ADN particles according to claim 1, wherein in the step (2), the reaction is continued for 1-4 hours after the dropwise addition.
10. A spherical ADN particle produced by the method of any one of claims 1-9, wherein the difference between the largest and smallest particle diameters of the spherical ADN particles is 100 μm or less.
11. Use of spherical ADN particles according to claim 10 in the field of solid propellants, explosives or fireworks agents.
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| CN117024227A (en) * | 2023-08-16 | 2023-11-10 | 福建省巨颖高能新材料有限公司 | Device and method for producing spherical-like dinitramide ammonium |
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