CN112745178A - Method for coating hexogen by high-voltage electrostatic spraying - Google Patents
Method for coating hexogen by high-voltage electrostatic spraying Download PDFInfo
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- CN112745178A CN112745178A CN202110002358.8A CN202110002358A CN112745178A CN 112745178 A CN112745178 A CN 112745178A CN 202110002358 A CN202110002358 A CN 202110002358A CN 112745178 A CN112745178 A CN 112745178A
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- hexogen
- nitrocotton
- coating
- voltage electrostatic
- electrostatic spraying
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/18—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component
- C06B45/20—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an organic explosive or an organic thermic component
- C06B45/22—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an organic explosive or an organic thermic component the coating containing an organic compound
- C06B45/24—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an organic explosive or an organic thermic component the coating containing an organic compound the compound being an organic explosive or an organic thermic component
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0083—Treatment of solid structures, e.g. for coating or impregnating with a modifier
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Abstract
The invention discloses a method for coating hexogen by high-voltage electrostatic spraying, which comprises the steps of taking acetone as a solvent, dissolving hexogen in the acetone, adding nitrocotton after the hexogen is completely dissolved, carrying out ultrasonic treatment and stirring to uniformly disperse the hexogen to obtain a precursor solution, carrying out high-voltage electrostatic spraying on the precursor solution, and drying to obtain the hexogen coated by the nitrocotton. The method has the advantages of simple equipment, convenient operation, higher sphericity of the coated hexogen, uniform coating and good application prospect.
Description
Technical Field
The invention belongs to the field of modification of energetic materials, and particularly relates to a method for coating hexogen by high-voltage electrostatic spraying,
background
Hexogen is widely used in the field of propellants due to its high energy, high performance, insensitive, low signature, and other characteristics. The addition of hexogen to the propellant significantly increases the energy of the propellant, but as its content increases, the problem also follows, which is the phenomenon of "dewetting". The so-called dewetting phenomenon is that when the propellant is subjected to a certain load, the interface between the solid filler and the adhesive is destroyed, so that the debonding phenomenon occurs, and the sensitivity of the propellant is increased, and the performance is deteriorated. Researches show that the intermolecular force between the hexogen and surrounding components can be effectively improved and the occurrence of the dehumidification phenomenon can be reduced or avoided by coating a coating layer on the surface of the hexogen. At present, the method for coating hexogen is multiple, and can be classified into: physical methods and chemical methods. The physical method is that the physical reaction is carried out on the surface of the hexogen by a certain means, such as a method of adding a precipitator, and finally a layer of compact coating layer is formed on the surface of the hexogen; the chemical method is to form a coating layer on the surface of the solid propellant by chemical reaction, such as metathesis reaction, polymerization reaction, etc. The common surface coating methods mainly include: phase separation method, water suspension method, chemical deposition method, mechanical grinding method, etc. The methods play an important role in the field of coating hexogen, but also show a plurality of limitations, for example, although the mechanical grinding method has the advantages of simple operation, environmental protection, low cost, continuous production and the like, the mechanical grinding method can cause the damage of crystal structure, the increase of crystal surface defects, the non-uniform coating layer and the like (Pacining, Lifengsheng, the preparation of coated superfine composite particles, the bulletin of explosives and dynasties, 2002,1: 33-35.).
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a brand-new method for coating hexogen, namely a high-voltage electrostatic spraying method, and the prepared coated hexogen has smooth surface and uniform coating layer.
In order to realize the technical task, the invention adopts the following technical scheme to realize:
a method for coating hexogen by high-voltage electrostatic spraying comprises the following steps:
step 1: dissolving hexogen by using acetone as a solvent to obtain a hexogen solution, adding nitrocotton, and carrying out ultrasonic stirring to obtain a nitrocotton/hexogen precursor solution;
step 2: and (3) taking the metal aluminum foil as a receiver, and performing high-voltage electrostatic spraying on the nitrocotton/hexogen precursor solution to obtain the hexogen coated by the nitrocotton.
Further, in the step 1, the mass concentration of the hexogen solution is 50-70 mg/g, and the mass ratio of the nitrocotton to the hexogen is 3/70-1/10.
Further, the propelling speed of the injection pump for high-voltage electrostatic spraying in the step 2 is 0.1-0.5 mL/h, the distance between the receiver and the spray head is 8-12 cm, the voltage is 16-20 kV, and the inner diameter of the spray head opening is 0.3-0.6 mm.
Further, in the step 1, the ultrasonic time is 10-30 min, and the stirring time is 2-10 h.
Preferred parameters for step 1 of the present invention are: the concentration of the hexogen solution is 70mg/g, and the mass ratio of the nitrocotton to the hexogen is 3/70.
Preferred parameters for step 2 of the present invention are: the ultrasonic time is 20min, the stirring time is 6h, the propelling speed of a syringe pump is 0.3mL/h, the distance between a receiver and a spray head is 10cm, and the voltage is 18 kV.
Compared with the prior art, the invention has the following technical beneficial effects:
compared with the prior art, such as an evaporation solvent method, a solvent-nonsolvent method, a high-energy ball milling method and the like, the high-voltage electrostatic spraying method has the advantages of simple process and strong operability, the coating effect of the hexogen can be controlled by adjusting parameters such as solution concentration, solvent type, the type of a coating material, propulsion speed, the distance between a receiver and a spray head, voltage and the like, the adjustable range of the process is large, the properties such as the appearance, granularity, coating degree and the like of the coated hexogen can be adjusted more flexibly, the edges and corners on the surface of the hexogen disappear after coating, the surface is smooth, the particle size is uniform, the coating layer is uniform, and the existing coating technology is difficult to remove the edges and corners on the surface of the hexogen and also difficult to control the state. In addition, in the process of coating the hexogen by the high-voltage electrostatic spraying method, the hexogen is dissolved in the solvent, so that safety accidents of the hexogen under the stimulation of high-voltage static electricity, machinery and the like can not occur under the protection of the inert solvent, and the hexogen in the prior art exists in the state of crystal particles and is easy to generate combustion and explosion under the conditions of stirring, collision and thermal stimulation.
Drawings
FIG. 1 is a morphology chart of coated hexogen when the nitrocotton content is high.
FIG. 2 is a topographical view of hexogen coated by mechanical grinding.
Fig. 3 is an SEM image of hexogen as received.
FIG. 4 is an SEM image of nitrocotton coated hexogen (mass ratio of nitrocotton to hexogen is 3: 70).
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Detailed Description
The technical idea of the invention is as follows: high-voltage electrostatic spraying is widely applied to modification and performance regulation of energetic materials as a special form of high-voltage electrostatic spinning at present, but sensitive energetic materials such as nitramine explosives (hexogen, octogen and the like) and nitrocotton are easy to burn and explode under the stimulation of high-voltage static electricity, so that the application of the technology in the modified sensitive energetic materials is limited. Nitrocotton is a polymer with a very large molecular weight, has good bonding and compatibility with the surface of hexogen, and is also a common coating material for hexogen, but the common coating method for preparing the nitrocotton coated hexogen can not uniformly coat the surface of hexogen, the edges and corners of hexogen crystals can not be removed, the surface of the hexogen crystals is rough, if the coating is realized in the process of hexogen crystallization, the crystal structure of hexogen can be changed, the surface of hexogen is smoother, and the nitrocotton can also uniformly coat the surface of hexogen. According to the conception, the insensitive solvent acetone is adopted, the requirements of high-voltage electrostatic spraying on good conductivity and easy volatilization of the solvent are met, the hexogen and the nitrocotton have better dissolving capacity, and the precursor solution prepared by the high-voltage electrostatic spraying dissolves the hexogen and the nitrocotton in the acetone, so that the combustion explosion of the hexogen caused by high-voltage static electricity is avoided. In the high-voltage electrostatic spraying process, the hexogen is crystallized and separated out along with the volatilization of the solvent, and meanwhile, the nitrocotton is separated out and coated on the surface of the hexogen, so that the hexogen with smooth surface and regular appearance is finally prepared.
In the embodiment of the invention, the injection pump adopts an RSP01-B push-pull mode injection pump, Carcharie electronic technology, Inc., a positive high-voltage power supply of 0-30 kV, TE4020 and Dalian Teiman technology, Inc.
Example 1
(1) Preparing a precursor solution: weighing 1g of acetone, adding the acetone into a 10mL glass bottle, adding 50mg of hexogen, dissolving, adding 3mg of nitrocotton, carrying out ultrasonic treatment for 10min, and carrying out magnetic stirring for 2h to obtain a nitrocotton/hexogen precursor solution.
(2) Electrostatic spraying: the precursor solution is filled into a 10mL injector, a flat-mouth needle (the inner diameter is 0.3mm) is used as a nozzle, the precursor solution flows out of a metal nozzle by using an injection pump, the metal nozzle is connected with a positive high-voltage power supply, and a metal aluminum foil is used as a receiver. Electrostatic spraying process parameters: the propelling speed is 0.1mL/h, the distance between the receiver and the spray head is 8cm, the voltage is 16kV, the ambient temperature is 25 ℃, and the hexogen coated by the nitrocotton is collected.
Example 2
(1) Preparing a precursor solution: weighing 1g of acetone, adding the acetone into a 10mL glass bottle, adding 70mg of hexogen, dissolving, adding 10mg of nitrocotton, performing ultrasonic treatment for 20min, and performing magnetic stirring for 10h to obtain a nitrocotton/hexogen precursor solution.
(2) Electrostatic spraying: the precursor solution is filled into a 10mL injector, a flat-mouth needle (the inner diameter is 0.5mm) is used as a nozzle, the precursor solution flows out of a metal nozzle by using an injection pump, the metal nozzle is connected with a positive high-voltage power supply, and a metal aluminum foil is used as a receiver. Electrostatic spraying process parameters: the propelling speed is 0.5mL/h, the distance between the receiver and the spray head is 12cm, the voltage is 18kV, the ambient temperature is 35 ℃, and the hexogen coated by the nitrocotton is collected.
Example 3
(1) Preparing a precursor solution: weighing 1g of acetone, adding the acetone into a 10mL glass bottle, adding 70mg of hexogen, dissolving, adding 3mg of nitrocotton, carrying out ultrasonic treatment for 10min, and carrying out magnetic stirring for 4h to obtain a nitrocotton/hexogen precursor solution.
(2) Electrostatic spraying: the precursor solution is filled into a 10mL injector, a flat-mouth needle (the inner diameter is 0.6mm) is used as a nozzle, the precursor solution flows out of a metal nozzle by using an injection pump, the metal nozzle is connected with a positive high-voltage power supply, and a metal aluminum foil is used as a receiver. Electrostatic spraying process parameters: the propelling speed is 0.1mL/h, the distance between the receiver and the spray head is 10cm, the voltage is 16kV, the ambient temperature is 35 ℃, and the hexogen coated by the nitrocotton is collected.
Example 4
(1) Preparing a precursor solution: weighing 1g of acetone, adding the acetone into a 10mL glass bottle, adding 60mg of hexogen, dissolving, adding 5mg of nitrocotton, carrying out ultrasonic treatment for 30min, and carrying out magnetic stirring for 6h to obtain a nitrocotton/hexogen precursor solution.
(2) Electrostatic spraying: the precursor solution is filled into a 10mL injector, a flat-mouth needle (the inner diameter is 0.5mm) is used as a nozzle, the precursor solution flows out of a metal nozzle by using an injection pump, the metal nozzle is connected with a positive high-voltage power supply, and a metal aluminum foil is used as a receiver. Electrostatic spraying process parameters: the propelling speed is 0.3mL/h, the distance between the receiver and the spray head is 10cm, the voltage is 20kV, the ambient temperature is 20 ℃, and the hexogen coated by the nitrocotton is collected.
Example 5
(1) Preparing a precursor solution: weighing 1g of acetone, adding the acetone into a 10mL glass bottle, adding 60mg of hexogen, dissolving, adding 7mg of nitrocotton, carrying out ultrasonic treatment for 15min, and carrying out magnetic stirring for 5h to obtain a nitrocotton/hexogen precursor solution.
(2) Electrostatic spraying: the precursor solution is filled into a 10mL injector, a flat-mouth needle (the inner diameter is 0.6mm) is used as a nozzle, the precursor solution flows out of a metal nozzle by using an injection pump, the metal nozzle is connected with a positive high-voltage power supply, and a metal aluminum foil is used as a receiver. Electrostatic spraying process parameters: the propelling speed is 0.4mL/h, the distance between the receiver and the spray head is 8cm, the voltage is 19kV, the ambient temperature is 28 ℃, and the hexogen coated by the nitrocotton is collected.
In the process of repeated experimental demonstration, the applicant finds that if the added hexogen is excessive, the concentration of the hexogen is too high, and a spray head is easy to block in the electrostatic spraying process; the added hexogen is too little, the concentration is too low, acetone in liquid drops formed in the spraying process cannot be volatilized in time, and a receiver cannot obtain crystallized hexogen. If the content of the added nitrocotton is too low, the phenomenon that acetone in liquid drops formed in the spraying process cannot be volatilized in time and a receiver cannot obtain crystallized hexogen can also be caused. If the content of the added nitrocotton is too high, the prepared particles have irregular shapes because the winding effect of the nitrocotton molecular chain is strong, the solution concentration is high, the solvent is volatilized quickly, and the hexogen cannot be crystallized and shaped, which is shown in figure 1.
A large number of experiments show that 70mg of hexogen and 3-10 mg of nitrocotton are added into 1g of acetone, so that a metal spray head is not blocked in the electrostatic spraying process, and meanwhile, crystallized hexogen can be obtained in a receiver.
The process is simple, the RDX coating can be completed only by controlling parameters such as the propelling speed, the distance between a receiver and a spray nozzle, the voltage and the like, the coating of the nitramine explosive can be realized only by adjusting parameters such as stirring granularity, stirring time, reaction temperature, the physicochemical characteristics of the coating material and the like by the existing hexogen coating technology (such as a mechanical grinding method, the preparation of Pating Ming. coated superfine composite particles, the bulletin for explosives and powders 2002,1:33-35), and the physicochemical characteristics of the coating material are difficult to control, so that the surface of the nitramine explosive is difficult to uniformly coat. In the process, the RDX is dissolved in the solvent and protected by the inert solvent, combustion and explosion cannot be caused under the action of high-voltage static electricity, the safety of the process can be ensured, the coated RDX particles are uniform and have regular shapes, the RDX surface is completely coated, the shape of the coated RDX is shown in figure 4, and compared with common methods such as a mechanical grinding method, an emulsion polymerization method and a phase separation method, the method has higher safety and more uniform RDX coating.
In contrast, the morphology of the RDX coated by the mechanical grinding method is shown in fig. 2, and it can be seen from the figure that the RDX surface is not completely coated by the coating material, the particle size is not uniform, and the surface is rough.
As can be seen from the above, under certain environmental conditions, the invention can coat hexogen with nitrocotton only by adjusting the propelling speed, the distance between the receiver and the spray head and the voltage, the coating layer is uniformly distributed on the surface of the hexogen, and the surface of the hexogen is smooth, while the coating of nitramine can be realized by the existing technology for coating hexogen (such as a mechanical grinding method, Pertingmin, preparation of coated superfine composite particles, explosive science and report 2002,1:33-35) only by adjusting parameters such as stirring granularity, stirring time, reaction temperature, the physical and chemical properties of the coating material, and the like, and the physical and chemical properties of the coating material are difficult to control and the surface of the nitramine explosive is difficult to be uniformly coated. In addition, the high-voltage electrostatic spraying coating of the hexogen can realize recrystallization purification and spheroidization of the hexogen. FIG. 3 is a scanning electron micrograph of the original hexogen used, from which it can be seen that the morphology of the original hexogen is irregular. The scanning electron microscope image of the nitrocotton-coated hexogen is shown in fig. 4, and it can be seen from the image that the coated hexogen has a regular shape and a high sphericity, and the surface of the coated hexogen is uniformly coated by the nitrocotton.
Claims (6)
1. A method for coating hexogen by high-voltage electrostatic spraying is characterized by comprising the following steps: the method comprises the following steps:
step 1: dissolving hexogen by using acetone as a solvent to obtain a hexogen solution, adding nitrocotton, and carrying out ultrasonic stirring to obtain a nitrocotton/hexogen precursor solution;
step 2: and (3) taking the metal aluminum foil as a receiver, and performing high-voltage electrostatic spraying on the nitrocotton/hexogen precursor solution to obtain the hexogen coated by the nitrocotton.
2. The method of claim 1, wherein the coating of hexogen by high voltage electrostatic spray comprises: in the step 1, the mass concentration of the hexogen solution is 50-70 mg/g, and the mass ratio of the nitrocotton to the hexogen is 3/70-1/10.
3. The method of claim 1, wherein the coating of hexogen by high voltage electrostatic spray comprises: the propelling speed of the injection pump for high-voltage electrostatic spraying in the step 2 is 0.1-0.5 mL/h, the distance between the receiver and the spray head is 8-12 cm, the voltage is 16-20 kV, and the inner diameter of the spray head opening is 0.3-0.6 mm.
4. The method for coating hexogen by high-voltage electrostatic spraying according to claim 1, wherein in the step 1, the ultrasonic time is 10-30 min, and the stirring time is 2-10 h.
5. The method for coating hexogen by high voltage electrostatic spray according to claim 1 or 2, wherein the preferred parameters of step 1 are: the mass concentration of the hexogen solution is 70mg/g, and the mass ratio of the nitrocotton to the hexogen is 3/70.
6. The method for coating hexogen with high voltage electrostatic spray according to claims 1-3, wherein the preferred parameters of step 2 are: the ultrasonic time is 20min, the stirring time is 6h, the propelling speed of a syringe pump is 0.3mL/h, the distance between a receiver and a spray head is 10cm, and the voltage is 18 kV.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116283451A (en) * | 2023-02-16 | 2023-06-23 | 西安近代化学研究所 | Preparation method of fluffy nitrocotton-based energetic compound |
| CN116354777A (en) * | 2021-12-28 | 2023-06-30 | 南京理工大学 | Electric field controlled explosive granulating method |
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| CN103342619A (en) * | 2013-07-24 | 2013-10-09 | 中国工程物理研究院化工材料研究所 | Surface coating method for explosive particles |
| CN107304150A (en) * | 2016-04-19 | 2017-10-31 | 南京理工大学 | A kind of method that high-voltage electrostatic spraying prepares boron/potassium nitrate/nitrocellulose complex microsphere |
| CN107400033A (en) * | 2016-05-19 | 2017-11-28 | 北京理工大学 | A kind of energetic material complex microsphere and its preparation method and application |
| CN109206282A (en) * | 2018-11-02 | 2019-01-15 | 西南科技大学 | The preparation method of super hydrophobic porous spherical shape nitrocotton base explosive compound |
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2021
- 2021-01-04 CN CN202110002358.8A patent/CN112745178A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5026443A (en) * | 1989-10-14 | 1991-06-25 | Fraunhofer-Gesellschaft Zur Forderung Der Angewandten | Stabilized explosive and its production process |
| CN103342619A (en) * | 2013-07-24 | 2013-10-09 | 中国工程物理研究院化工材料研究所 | Surface coating method for explosive particles |
| CN107304150A (en) * | 2016-04-19 | 2017-10-31 | 南京理工大学 | A kind of method that high-voltage electrostatic spraying prepares boron/potassium nitrate/nitrocellulose complex microsphere |
| CN107400033A (en) * | 2016-05-19 | 2017-11-28 | 北京理工大学 | A kind of energetic material complex microsphere and its preparation method and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116354777A (en) * | 2021-12-28 | 2023-06-30 | 南京理工大学 | Electric field controlled explosive granulating method |
| CN116283451A (en) * | 2023-02-16 | 2023-06-23 | 西安近代化学研究所 | Preparation method of fluffy nitrocotton-based energetic compound |
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Application publication date: 20210504 |