Nano explosive particle preparation device and method based on acoustic resonance high-frequency vibration

Abstract

The invention belongs to the technical field of energetic material preparation, and particularly relates to a method for preparing nano explosive particles based on an acoustic resonance assisted ball milling technology. Comprising the following steps: weighing and measuring acoustic resonance materials; refining explosive particles through acoustic resonance high-frequency vibration; filtering and drying the nano explosive particles; acoustic resonance high-frequency vibration is applied to the refining process of explosive particles, zirconium oxide beads in a ball milling tank collide at a fixed same frequency under the action of same-frequency resonance, so that an efficient and stable working space is formed in a limited space of the ball milling tank, the explosive particles flow among the zirconium oxide beads through ball milling liquid, and the explosive particles are refined. And under the impact and resonance effects of the zirconium oxide beads, the explosive particles are crushed and refined, and finally the nano explosive particles are prepared. According to the invention, the acoustic resonance frequency is highly matched with the characteristics of the zirconia beads, so that a better synergistic effect can be generated, and the nanocrystallization degree of explosive particles is improved; in addition, the application range of the acoustic resonance technology is expanded through the refinement principle.

Description

Technical Field

[0001] This invention belongs to the field of energetic materials preparation technology, specifically relating to a device and method for preparing nano-explosive particles based on high-frequency acoustic resonance vibration. Background Technology

[0002] As modern weapon systems rapidly evolve towards lightweighting, miniaturization, and high efficiency, higher demands are being placed on the performance of energetic materials. Against this backdrop, nanomaterials with energetic properties have become an important frontier research direction due to their higher reactivity, faster energy release rate, and superior controllability. The nanostructuring of energetic materials not only helps improve combustion and explosion performance and safety, but also enables precise control of the energy release process. There are two main preparation methods for nanomaterials with energetic properties: one based on crystallization technology and the other based on mechanical grinding technology. Among the many methods for preparing nanomaterials with energetic properties, mechanically driven ball milling technology has received increasing attention in recent years due to its advantages such as simple process, low cost, environmental friendliness, and suitability for large-scale preparation. Domestic and international scholars have already used mechanical ball milling to prepare nano-sized HMX, RDX, CL-20, HNS, and TATB explosive particles. This method relies on high-intensity mechanical external force and achieves effective control over the particle size and morphology of the material by precisely controlling parameters such as the ball-to-particle ratio, the type and size of the grinding media, the ball milling speed, and the grinding time. However, this method mainly relies on the mechanical forces such as impact, compression, and shearing of energetic material particles by grinding balls in a liquid medium to gradually break the particles. It generally takes several hours or even longer to obtain nanoscale energetic material particles with narrow particle size distribution, resulting in low preparation efficiency and affecting the further development and application of this preparation technology. Summary of the Invention

[0003] To address the problem of low efficiency in the current mechanical grinding technology for preparing energetic nanomaterials, this invention provides a device and method for preparing nano-explosive particles based on high-frequency acoustic resonance vibration.

[0004] To solve the above-mentioned technical problems, the technical solution adopted by the present invention is: a nano-explosive particle preparation device based on acoustic resonance high-frequency vibration, including an acoustic resonance fixture and a low-temperature circulating container; The acoustic resonance fixture includes a fixture base plate, on which two vertically arranged support columns are welded. A horizontal support rod is installed on the top of the two support columns. A vertically arranged screw rod passes through the middle of the horizontal support rod. A cover plate is fitted on the bottom of the screw rod. Both ends of the cover plate are slidably fitted on the support columns. A reinforcing buckle is threaded on the screw rod located above the cover plate. The cryogenic circulation container includes a base plate, on which an acoustic resonance container is mounted. The interior of the acoustic resonance container is a water circulation cavity. The lower part of the side wall of the acoustic resonance container has a water inlet, and the upper part has a water outlet. The top of the acoustic resonance container has a tank cover plate. The base plate has positioning holes that match the size of the support column. The cryogenic circulation container is installed between the clamp base plate and the cover plate through the positioning holes.

[0005] As a further limitation of the technical solution of the present invention, the outer side of the can opening of the acoustic resonance container is provided with a cover sealing rubber ring, and the inner side of the can opening of the acoustic resonance container is provided with a ball mill jar protective rubber ring.

[0006] As a further limitation of the technical solution of the present invention, the following steps are included: S1. Weighing and measuring materials for acoustic resonance Weigh out the explosive particles, grinding media, and grinding balls, and put them into a grinding jar. After all the materials have been added, seal the container with the lid. The grinding media is an inorganic and organic solvent that is insoluble or slightly soluble in the explosive. S2. Acoustic Resonance Container Assembly and Fixing The grinding tank containing the material is placed in the acoustic resonance container of the low-temperature circulating container. The inlet and outlet are connected to the inlet and outlet water pipes, respectively. After assembly, the circulation temperature and flow rate are set, and then the whole assembly is installed between the clamp base plate and the cover plate of the acoustic resonance fixture. The acoustic resonance fixture is assembled on the acoustic resonance platform. S3. Preparation of nano-explosive particles by acoustic resonance-assisted mechanical grinding Set the acoustic resonance mixing process parameters, such as amplitude, acceleration, and resonance time, on the acoustic resonance control computer; turn on the acoustic resonance equipment and the low-temperature circulating container, and obtain a suspension containing nano-explosive particles after resonance according to the set process conditions; S4. Filtration and drying of ultrafine explosives After the acoustic resonance stops, the acoustic resonance container is removed from the acoustic resonance fixture, the container lid is opened, and the resulting suspension is filtered and dried to obtain ultrafine explosive particles.

[0007] As a further limitation of the technical solution of the present invention, the grinding medium in step S1 is at least one of water, ethanol, methanol, isopropanol and ethyl acetate.

[0008] As a further limitation of the technical solution of the present invention, the grinding ball in step S1 is an ultrahard zirconia grinding ball, a steel grinding ball, or a corundum grinding ball, and the diameter of the grinding ball is from 0.05mm to 5mm.

[0009] As a further limitation of the technical solution of the present invention, the mass ratio of explosive to liquid grinding medium in step S1 is 1:5-1:50; the mass ratio of explosive to grinding ball is 1:10-1:40.

[0010] As a further limitation of the technical solution of the present invention, in step S2, the gap between the inner wall of the acoustic resonance container 8 and the outer wall of the grinding tank is 1-3mm, and the acoustic resonance container is cooled by the inflow of liquid medium, the temperature of the liquid medium being 10-20℃.

[0011] As a further limitation of the technical solution of the present invention, the acoustic resonance amplitude and frequency are determined by the equipment according to the material characteristics, the acceleration range is 20g-100g, and the resonance time is 1-20min.

[0012] As a further limitation of the technical solution of the present invention, step S4 filtration adopts vacuum filtration, pressure filtration or centrifugal filtration; washing is to rinse the explosive particles with non-solvent and wash the solvent; drying is water bath drying, vacuum drying or freeze drying.

[0013] Compared with the prior art, the present invention has the following beneficial effects: This invention utilizes low-frequency acoustic vibration to drive the movement of explosive particles within a sealed container. By setting the acoustic frequency to be the same as or close to the material's natural frequency, a good synergistic effect can be achieved. When the vibration reaches a steady state, the explosive particles resonate, creating alternating shear and compressive composite loads at the microscale. This lowers the equivalent yield stress threshold of the particles and causes stress concentration at lattice defects, pores, or interfaces. These conditions promote the spontaneous initiation and propagation of cracks along weak planes, exhibiting spontaneous fragmentation, which is beneficial for material refinement. Figure 8 As shown.

[0014] Under the influence of acoustic resonance, materials are driven not only by microscopic forces from a single point to a localized area, but also by macroscopic, interwoven forces. The complex and multidirectional movement trajectory of the materials can significantly increase the contact frequency between powder particles, grinding balls, and the mill wall, achieving a multiplied energy gain locally. The mechanism is as follows: Figure 9 As shown. Compared with ordinary ball milling technology, the grinding time of this invention can be shortened from several hours to a few minutes, and the efficiency of preparing nano-explosive particles is greatly improved. Attached Figure Description

[0015] Figure 1 This is a front view of the acoustic resonance fixture of the present invention.

[0016] Figure 2 This is a three-dimensional schematic diagram of the acoustic resonance fixture of the present invention.

[0017] Figure 3 This is a front view of the cryogenic circulating container of the present invention.

[0018] Figure 4 This is a three-dimensional schematic diagram of the temperature circulation container of the present invention.

[0019] Figure 5 This is a front view of the device for preparing nano-explosive particles based on high-frequency vibration of acoustic resonance according to the present invention.

[0020] Figure 6 This is a side view of the nano-explosive particle preparation device based on high-frequency acoustic resonance vibration of the present invention.

[0021] Figure 7 This is a three-dimensional schematic diagram of the nano-explosive particle preparation device based on high-frequency vibration of acoustic resonance according to the present invention.

[0022] Figure 8 This is one of the schematic diagrams illustrating the principle of acoustic resonance in the preparation of explosive particles.

[0023] Figure 9 The second diagram illustrates the principle of acoustic resonance in the preparation of explosive particles.

[0024] Figure 10 Scanning electron microscope image and particle size distribution diagram of the explosive particles prepared in Example 2.

[0025] Figure 11 The image shows the XRD results of the explosive particles prepared in Example 2.

[0026] Figure 12 The image shows the infrared spectrum of the explosive particles prepared in Example 2.

[0027] Figure 13 The isothermal adsorption-desorption curves prepared in Example 2 are shown.

[0028] The markings in the image are as follows: 1-Screw, 2-Horizontal support rod, 3-Reinforcing buckle, 4-Cover plate, 5-Support column, 6-Clamp base plate, 7-Base plate, 8-Acoustic resonance container, 9-Inlet, 10-Outlet, 11-Tank cover plate, 12-Positioning hole, 13-Cover plate sealing rubber ring, 14-Grinding jar protective rubber ring. Detailed Implementation

[0029] The present invention will be further described below with reference to specific embodiments. Example 1

[0030] like Figure 5-7 As shown, a device for preparing nano-explosive particles based on high-frequency vibration of acoustic resonance includes an acoustic resonance fixture and a low-temperature circulating container. like Figure 1 and 2 As shown, the acoustic resonance fixture includes a fixture base plate 6, on which two vertically arranged support columns 5 are welded. A horizontal support rod 2 is installed on the top of the two support columns 5. A vertically arranged screw rod 1 passes through the middle of the horizontal support rod 2. A cover plate 4 is fitted on the bottom of the screw rod 1. Both ends of the cover plate 4 are slidably fitted on the support column 5. A reinforcing buckle 3 is threaded on the screw rod 1 located above the cover plate 4. like Figure 3 and 4 As shown, the cryogenic circulation container includes a base plate 7, on which an acoustic resonance container 8 is mounted. The interior of the acoustic resonance container 8 is a water circulation cavity. The lower part of the side wall of the acoustic resonance container 8 is provided with a water inlet 9, and the upper part is provided with a water outlet 10. The top of the acoustic resonance container 8 is provided with a tank cover plate 11. The base plate 7 has a positioning hole 12, which matches the size of the support column 5. The cryogenic circulation container is installed between the clamp base plate 6 and the cover plate 4 through the positioning hole 12.

[0031] Furthermore, the outer side of the opening of the acoustic resonance container 8 is provided with a cover sealing rubber ring 13, and the inner side of the opening of the acoustic resonance container 8 is provided with a ball mill jar protective rubber ring 14. Example 2

[0032] The preparation of a nano-explosive particle, using the apparatus described in Example 1 above, includes the following steps: 5g of HNS raw material, 175g of 0.05mm zirconia beads, and 50g of a ethanol-water mixture were added to a ball mill jar. The jar was then placed in a low-temperature circulating container and fixed using an acoustic resonance fixture mounted on the acoustic resonance platform. The temperature of the water bath circulating container was set to 10℃, the acceleration to 70g, and the acoustic resonance time to 8min. The acoustic resonance machine was started, and the system automatically matched the amplitude and frequency according to the acceleration. At 70g, the stable amplitude was 21.3%, and the frequency fluctuated slightly between 63.78Hz and 63.86Hz. After the machine finished running, the explosive suspension was removed, washed, filtered, and freeze-dried under vacuum to obtain the finished product. The microstructure of the HNS was obtained using SEM (Scanning Electron Microscopy), and the particle size distribution was calculated using Nano Measurer software. Figure 10 As shown; further data such as the crystal form of nano-HNS were obtained using XRD diffraction, infrared spectroscopy, and specific surface area and pore size analysis, as shown in the figures. Figure 11 , Figure 12 , Figure 13 As shown, under these optimal conditions, micron-sized HNS particles can be broken down into nano-sized particles within 8 minutes, with a concentrated particle size distribution, high sphericity, and smooth edges. The crystal form and functional groups remain unchanged during ball milling, and the specific surface area reaches approximately 25.7 m². 2 / g.

Claims

1. A device for preparing nano-explosive particles based on high-frequency acoustic resonance vibration, characterized in that, Including acoustic resonance fixtures and cryogenic circulating containers; The acoustic resonance fixture includes a fixture base plate (6), on which two vertically arranged support columns (5) are welded. A horizontal support rod (2) is installed on the top of the two support columns (5). A vertically arranged screw rod (1) is inserted through the middle of the horizontal support rod (2). A cover plate (4) is fitted on the bottom of the screw rod (1). Both ends of the cover plate (4) are slidably fitted on the support column (5). A reinforcing buckle (3) is threaded on the screw rod (1) above the cover plate (4). The cryogenic circulation container includes a base plate (7), on which an acoustic resonance container (8) is provided. The interior of the acoustic resonance container (8) is a water circulation cavity. The lower part of the side wall of the acoustic resonance container (8) is provided with a water inlet (9), and the upper part is provided with a water outlet (10). The top of the acoustic resonance container (8) is provided with a tank cover plate (11). The base plate (7) is provided with a positioning hole (12), which matches the size of the support column (5). The cryogenic circulation container is installed between the clamp base plate (6) and the cover plate (4) through the positioning hole (12).

2. The device for preparing nano-explosive particles based on acoustic resonance high-frequency vibration according to claim 1, characterized in that, The acoustic resonance container (8) has a cover sealing rubber ring (13) on the outside of the can opening, and a ball mill jar protective rubber ring (14) on the inside of the can opening.

3. A method for preparing nano-explosive particles based on acoustic resonance high-frequency vibration, comprising using the apparatus described in any one of claims 1-2, characterized in that, Includes the following steps: S1. Weighing and measuring materials for acoustic resonance Weigh out the explosive particles, grinding media, and grinding balls, and put them into a grinding jar. After all the materials have been added, seal the container with the lid. The grinding media is an inorganic and organic solvent that is insoluble or slightly soluble in the explosive. S2. Acoustic Resonance Container Assembly and Fixing The grinding tank containing the material is placed in the acoustic resonance container (8) of the low-temperature circulating container. The inlet (9) and outlet (10) are connected to the inlet and outlet water pipes respectively. After assembly, the circulating temperature and flow rate are set, and then the whole is installed between the clamp base plate (6) and the cover plate (4) of the acoustic resonance fixture. The acoustic resonance fixture is assembled on the acoustic resonance platform. S3. Preparation of nano-explosive particles by acoustic resonance-assisted mechanical grinding Set the acoustic resonance mixing process parameters, such as amplitude, acceleration, and resonance time, on the acoustic resonance control computer; turn on the acoustic resonance equipment and the low-temperature circulating container, and obtain a suspension containing nano-explosive particles after resonance according to the set process conditions; S4. Filtration and drying of ultrafine explosives After the acoustic resonance stops, the acoustic resonance container (8) is removed from the acoustic resonance fixture, the container cover is opened, and the resulting suspension is filtered and dried to obtain ultrafine explosive particles.

4. The method for preparing nano-explosive particles based on high-frequency acoustic resonance vibration according to claim 3, characterized in that, The grinding medium in step S1 is at least one of water, ethanol, methanol, isopropanol and ethyl acetate.

5. The method for preparing nano-explosive particles based on high-frequency acoustic resonance vibration according to claim 3, characterized in that, In step S1, the grinding balls are superhard zirconia grinding balls, steel grinding balls, or corundum grinding balls, with diameters ranging from 0.05 mm to 5 mm.

6. The method for preparing nano-explosive particles based on high-frequency acoustic resonance vibration according to claim 3, characterized in that, In step S1, the mass ratio of explosive to liquid grinding medium is 1:5-1:50; the mass ratio of explosive to grinding balls is 1:10-1:

40.

7. The method for preparing nano-explosive particles based on high-frequency acoustic resonance vibration according to claim 3, characterized in that, In step S2, the gap between the inner wall of the acoustic resonance container (8) and the outer wall of the grinding tank is 1-3 mm. The acoustic resonance container 8 is cooled by the inflow of liquid medium, and the temperature of the liquid medium is 10-20℃.

8. The method for preparing nano-explosive particles based on high-frequency acoustic resonance vibration according to claim 3, characterized in that, The acoustic resonance amplitude and frequency are determined automatically by the equipment based on the material characteristics, with an acceleration range of 20g-100g and a resonance time of 1-20min.

9. The method for preparing nano-explosive particles based on high-frequency acoustic resonance vibration according to claim 3, characterized in that, Step S4 filtration employs vacuum filtration, pressure filtration, or centrifugal filtration; washing involves rinsing the explosive particles with a non-solvent solution to remove the solvent; drying is achieved through water bath drying, vacuum drying, or freeze drying.

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