CN115819168B - Composite explosive structure and preparation method thereof - Google Patents
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- CN115819168B CN115819168B CN202211700609.0A CN202211700609A CN115819168B CN 115819168 B CN115819168 B CN 115819168B CN 202211700609 A CN202211700609 A CN 202211700609A CN 115819168 B CN115819168 B CN 115819168B
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Abstract
The invention discloses a composite explosive structure and a preparation method thereof, wherein the composite explosive structure comprises coated particles, and the forming process of the coated particles is as follows: wrapping DAP-4 on RDX to form a mosaic structure compound RDX@DAP-4; EVA is coated on the compound RDX@DAP-4; filling gaps between EVA and outermost DAP-4 particles by DOA to form coated particles; the preparation method of the composite explosive structure comprises the following steps: 1) Adding RDX into a modified solvent, heating to 90-100 ℃ to prepare a saturated solution of RDX, adding DAP-4, stirring and cooling, separating out RDX in the saturated solution of RDX and wrapping the RDX on the surface of DAP-4, filtering, washing with water and drying to obtain an RDX@DAP-4 compound; 2) Dissolving EVA in petroleum ether, adding RDX@DAP-4 compound and DOA, stirring and volatilizing a solvent to obtain coated particles; 3) The composite explosive is prepared by using the coated particles, and the safety and the process formability of the DAP-4 based explosive can be improved by using the explosive structure and the preparation method thereof.
Description
Technical Field
The invention belongs to the technical field of energetic materials, and relates to a composite explosive structure and a preparation method thereof.
Background
(H 2 dabco)[NH 4 (ClO 4 ) 3 ](abbreviated as DAP-4 in which H 2 dabco 2+ =1, 4-diazabicyclo [2.2.2]Octane-1, 4-dionium ion) is a component formed by ionic oxidation of ClO 4 - With an organic fuel component H 2 dabco 2+ The novel metal-free multi-component energetic material formed by alternately and closely stacking perovskite structures is taken as a novel energetic material with the advantages of low cost, high explosion performance, high stability and the like, and DAP-4 is expected to be taken as an excellent simple substance component, so that the novel metal-free multi-component energetic material has good application prospect in civil and military mixed explosive. For DAP-4 type molecular perovskite energetic materials, the nh4+ ions are in the B site, and the orientation of the hydrogen is double disordered. The NH4+ ion is adjacent to 6 ClO 4-anions at the X-site, each ClO 4-anionThe ions are adjacent to two adjacent NH4+ ions, so that a three-dimensional anion skeleton consisting of cube cage-shaped units is formed; organic cation 1, 4-dihydro-1, 4-diazabicyclo [2.2.2 ] in the A-position]Octane ammonium ions (C6H 14 n22+) are filled in the cavities of each cubic cage unit. This structure results in a material surface that is non-adhesive, affecting its use in polymer-based composites.
DAP-4 is sensitive to mechanical stimulus, BAM test result is 5N, national army standard test result is 100%, and potential danger is brought to sample processing and transportation. Since the polymer cannot form a stable protective film on the surface, the coating feel cannot be used. Since DAP-4 is a new material invented in recent years, there is little research on its surface modification, and the modification mode is not reported in the literature. By reference to the research results of the nitro-amine energetic materials, a feasible theoretical guidance in the industry is to form eutectic materials, such as CL-20/TATB eutectic, by adopting two types of energetic materials. However, DAP-4, CL-20, RDX and HMX cannot form a eutectic structure under limited experimental selection, so that DAP-4-based explosive is difficult to apply and has poor process formability and safety.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a composite explosive structure and a preparation method thereof, wherein the composite explosive structure and the preparation method thereof can improve the safety and the process formability of the DAP-4 based explosive.
In order to achieve the above object, the composite explosive structure of the present invention includes coated particles, wherein the process of forming the coated particles is as follows: wrapping DAP-4 on RDX to form a mosaic structure compound RDX@DAP-4; EVA is coated on the compound RDX@DAP-4; the interstices between the EVA and the outermost DAP-4 particles are filled by DOA to form coated particles.
The preparation method of the composite explosive structure comprises the following steps:
1) Adding RDX into a modified solvent, heating to 90-100 ℃ to prepare a saturated solution of RDX, adding DAP-4, stirring and cooling, separating out RDX in the saturated solution of RDX and wrapping the RDX on the surface of DAP-4, filtering, washing with water and drying to obtain an RDX@DAP-4 compound;
2) Dissolving EVA in petroleum ether, adding RDX@DAP-4 compound and DOA, stirring and volatilizing a solvent to obtain coated particles;
3) And preparing the composite explosive by using the coated particles.
The washing temperature in the step 1) is less than or equal to 30 ℃.
The specific operation of the step 3) is as follows: and directly pressing and forming the coated particles to obtain the composite explosive.
The specific operation of the step 3) is as follows: the composite explosive is prepared by taking the coated particles as an energy-containing component, and using a binder, metal powder and an oxidant through a press-fitting process or a casting process.
The mass parts of DAP-4 and RDX in the RDX@DAP-4 compound are 100 parts and (50-200 parts) respectively.
The modifying solvent consists of 100 parts of cyclohexanone and 0.1-0.2 part of liquid paraffin.
The mass parts of RDX@DAP-4 compound, EVA and DOA in the coated particles are respectively 100 parts, (1-5) parts and (0.1-0.2) parts.
The invention has the following beneficial effects:
the invention relates to a composite explosive structure and a preparation method thereof, wherein a physical structure similar to eutectic is designed under the condition that eutectic cannot be formed when the composite explosive structure is specifically operated, DAP-4 is partially or completely wrapped by adopting high-energy ammonium nitrate explosive, the problem that DAP-4 cannot be bonded with a polymer is solved, and the structure design of the DAP-4 is specifically designed by partially or completely wrapping the ammonium nitrate explosive, and the DAP-4 is recrystallized on the surface of DAP-4 particles by utilizing a recrystallization process of the ammonium nitrate explosive, so that DAP-4 is partially or completely wrapped to form mosaic structure composite particles; and then the composite particles are coated by adopting an adhesive, and the polymer adhesive cannot be adhered to the DAP-4, so that a coating layer is formed by adhering the polymer and the ammonium nitrate explosive, and a thermoplastic elastomer or a plasticizer is used as a filler to fill the gap between the coating layer and the DAP-4 particles so as to improve the safety and the process formability of the DAP-4-based explosive.
Drawings
FIG. 1 is a schematic structural view of a composite explosive particle;
FIG. 2 is a scanning electron microscope image of a RDX@DAP-4 sample;
FIG. 3 is a photograph of a sample pellet obtained in example one;
FIG. 4 is a CT scan of a second charge of an embodiment;
FIG. 5 is a graph of the results of a test of example two charges at a 32.88mm baffle;
FIG. 6 is a graph showing the results of a shock wave baffle test of example three charges at different sizes.
Detailed Description
In order to make the present invention better understood by those skilled in the art, the following description will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments, but not intended to limit the scope of the present disclosure. In addition, in the following description, descriptions of well-known structures and techniques are omitted so as not to unnecessarily obscure the concepts of the present disclosure. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
In the accompanying drawings, there is shown a schematic structural diagram in accordance with a disclosed embodiment of the invention. The figures are not drawn to scale, wherein certain details are exaggerated for clarity of presentation and may have been omitted. The shapes of the various regions, layers and their relative sizes, positional relationships shown in the drawings are merely exemplary, may in practice deviate due to manufacturing tolerances or technical limitations, and one skilled in the art may additionally design regions/layers having different shapes, sizes, relative positions as actually required.
Referring to fig. 1, the composite explosive structure of the present invention comprises coated particles, wherein the process of forming the coated particles is as follows: wrapping DAP-4 on RDX to form a mosaic structure compound RDX@DAP-4; EVA is coated on the compound RDX@DAP-4; the interstices between the EVA and the outermost DAP-4 particles are filled by DOA to form coated particles.
The preparation method of the composite explosive structure comprises the following steps:
1) Preparing an RDX@DAP-4 complex;
the specific process is as follows: adding RDX into a modified solvent, heating to 90-100 ℃ to prepare a saturated solution of RDX, adding DAP-4, slowly stirring and cooling, separating out RDX in the saturated solution of RDX and wrapping the RDX on the surface of DAP-4, filtering, washing with water and drying to obtain an RDX@DAP-4 compound, wherein the washing temperature is less than or equal to 30 ℃;
2) Preparation of coated particles
Adopting a direct method for coating, dissolving EVA in petroleum ether, adding RDX@DAP-4 compound and DOA, stirring and volatilizing a solvent to obtain coated particles;
3) Preparation of composite explosive
The coated particles are directly pressed and molded, or the coated particles are used as energy-containing components and are prepared into the composite explosive through a pressing process or a pouring process together with a binder, metal powder and an oxidant.
The mass parts of DAP-4 and RDX in the RDX@DAP-4 compound are 100 parts and (50-200 parts) respectively; the modified solvent consists of 100 parts of cyclohexanone and 0.1-0.2 part of liquid paraffin, wherein the liquid paraffin is a nonpolar solvent, and is used as a polarity regulator to regulate and reduce the polarity of the cyclohexanone and reduce the influence of DAP-4 on RDX recrystallization.
The mass parts of RDX@DAP-4 compound, EVA and DOA in the coated particles are respectively 100 parts, (1-5) parts and (0.1-0.2) parts.
Example 1
The preparation method of the composite explosive structure comprises the following steps:
1) Preparation of the Complex
100g of DAP-4 is weighed, and not less than 300g of RDX is prepared; the modified solvent consists of cyclohexanone and liquid paraffin, wherein the cyclohexanone is 1000g, the liquid paraffin is 2g, the modified solvent is heated to 90-100 ℃, and RDX is added to prepare saturated solution; adding DAP-4, slowly stirring and cooling, and separating out RDX in saturated solution to wrap the surface of DAP-4; filtering, washing with water and drying to obtain RDX@DAP-4 compound, wherein the washing temperature is not higher than 30 ℃; after drying, a total of 300g of RDX@DAP-4 complex was obtained, indicating that 100g of DAP-4 and 200g of RDX were present in the RDX@DAP-4 complex.
2) Preparation of coated particles
Coating by adopting a direct method, dissolving 5g of EVA in petroleum ether, heating to 60 ℃, adding 100g of RDX@DAP-4 compound and 0.2g of DOA, stirring, volatilizing a solvent, and drying to obtain coated particles.
3) Preparation of composite explosive
The coated particles were directly compression molded at a pressure of 100MPa.
The coated particles were tested for impact sensitivity according to GJB772A-97 method 601.1 and the results are shown in the following table: SEM photographs of RDX@DAP-4 complex morphology
Example two
The preparation method of the composite explosive structure comprises the following steps:
1) Preparation of the Complex
Weighing 100g of DAP-4, and preparing not less than 300g of RDX; the modified solvent consists of cyclohexanone and liquid paraffin, wherein the cyclohexanone is 1000g, the liquid paraffin is 1g, the modified solvent is heated to 90-100 ℃, and RDX is added to prepare saturated solution; adding DAP-4, slowly stirring and cooling, and separating out RDX in saturated solution to wrap the surface of DAP-4; controlling the precipitation amount of RDX through time and temperature; filtering, washing with water and drying to obtain RDX@DAP-4 compound, wherein the washing temperature is not higher than 30 ℃; a total of 150g of RDX@DAP-4 complex was obtained after drying, indicating 100g of DAP-4 and 50g of RDX in the RDX@DAP-4 complex.
2) Preparation of coated particles
Coating by adopting a direct method, dissolving 1g of EVA in petroleum ether, heating to 60 ℃, adding 100g of RDX@DAP-4 compound and 0.1g of DOA, stirring, volatilizing a solvent, and drying to obtain coated particles.
3) Preparation of composite explosive: adopting a casting process, and preparing a casting explosive according to the proportion described in a reference of typical casting PBX explosive quasi-static compression mechanical behavior (Xi Peng, blasting equipment, 2021.02), wherein the RDX is replaced by coated particles; the explosive was poured into a metal mold and cured for 7d.
CT scanning is carried out on the solidified composite explosive; referring to the card type baffle method experimental method in GJB772A-97, the shock wave baffle is tested, the thickness of the shock wave baffle of the explosive is tested, the main explosive column is passivated black cable gold, the diameter is 40mm, the height is 30mm, the diameter of the explosive column to be tested is 40mm, the height is 90mm, and the baffle is an aluminum baffle.
Example III
Example three the shock wave sensitivity of the grain was tested according to the comparative example made in reference "quasi-static compression mechanical behaviour of a typically cast PBX explosive" (Xi Peng, blasting equipment, 2021.02).
The results are shown in Table 1, in terms of impact sensitivity and shock wave sensitivity:
TABLE 1
Example 1 | Example 2 | Example 3 | |
Impact sensitivity | 12% | — | 86% |
Shock wave sensitivity | — | 31.28 | 35.24 |
FIG. 2 is a scanning electron microscope image of a RDX@DAP-4 sample, and as can be seen from FIG. 2, the RDX@DAP-4 structure designed by the invention implements the technical idea of the invention as shown in FIG. 1. As can be seen from fig. 3 and 4, the bonding effect of the composite particles with the binder is improved, and the composite particles can be compression molded or cast molded.
Fig. 5 shows the test result of the second charge of the example at a baffle of 31.88mm, fig. 6 shows the test result of the third charge of the example at a baffle of different sizes, and comparing fig. 5 and 6, it can be seen that the impact wave sensitivity of the explosive column is obviously reduced relative to the simple substance RDX by adopting the structure of the invention, and the impact sensitivity of the first charge of the example is reduced to 24% and lower than 50% as can be seen from table 1.
In conclusion, the invention improves the combination effect of the composite particles and the binder, the composite particles can be pressed or cast, the safety is improved, the impact sensitivity of the composite particles is reduced to below 50 percent, and the thickness of the shock wave separator is superior to that of the ammonium nitrate explosive.
Example IV
The preparation method of the composite explosive structure comprises the following steps:
1) Preparation of RDX@DAP-4 Complex
The specific process is as follows: adding RDX into a modified solvent, heating to 90 ℃ to prepare a saturated solution of RDX, adding DAP-4, slowly stirring and cooling, separating out RDX in the saturated solution of RDX and wrapping the RDX on the surface of DAP-4, filtering, washing with water and drying to obtain a RDX@DAP-4 compound, wherein the washing temperature is equal to 30 ℃;
2) Preparation of coated particles
Adopting a direct method for coating, dissolving EVA in petroleum ether, adding RDX@DAP-4 compound and DOA, stirring and volatilizing a solvent to obtain coated particles;
3) Preparation of composite explosive
And directly pressing and forming the coated particles to obtain the composite explosive.
The mass parts of DAP-4 and RDX in the RDX@DAP-4 compound are respectively 100 parts and 50 parts; the modifying solvent consists of 100 parts of cyclohexanone and 0.1 part of liquid paraffin, wherein the liquid paraffin is a nonpolar solvent, and is used as a polarity regulator to regulate and reduce the polarity of the cyclohexanone and reduce the influence of DAP-4 on RDX recrystallization.
The mass parts of RDX@DAP-4 compound, EVA and DOA in the coated particles are respectively 100 parts, 1 part and 0.1 part.
Example five
The preparation method of the composite explosive structure comprises the following steps:
1) Preparation of RDX@DAP-4 Complex
The specific process is as follows: adding RDX into a modified solvent, heating to 100 ℃ to prepare a saturated solution of RDX, adding DAP-4, slowly stirring and cooling, separating out RDX in the saturated solution of RDX and wrapping the RDX on the surface of DAP-4, filtering, washing with water and drying to obtain a RDX@DAP-4 compound, wherein the washing temperature is 20 ℃;
2) Preparation of coated particles
Adopting a direct method for coating, dissolving EVA in petroleum ether, adding RDX@DAP-4 compound and DOA, stirring and volatilizing a solvent to obtain coated particles;
3) Preparation of composite explosive
The composite explosive is prepared by taking the coated particles as an energy-containing component, and using a binder, metal powder and an oxidant through a press-fitting process or a casting process.
The mass parts of DAP-4 and RDX in the RDX@DAP-4 compound are respectively 100 parts and 200 parts; the modifying solvent consists of 100 parts of cyclohexanone and 0.2 part of liquid paraffin.
The mass parts of RDX@DAP-4 compound, EVA and DOA in the coated particles are respectively 100 parts, 5 parts and 0.2 part.
Example six
The preparation method of the composite explosive structure comprises the following steps:
1) Preparation of RDX@DAP-4 Complex
The specific process is as follows: adding RDX into a modified solvent, heating to 95 ℃ to prepare a saturated solution of RDX, adding DAP-4, slowly stirring and cooling, separating out RDX in the saturated solution of RDX and wrapping the RDX on the surface of DAP-4, filtering, washing with water and drying to obtain a RDX@DAP-4 compound, wherein the washing temperature is 20 ℃;
2) Preparation of coated particles
Adopting a direct method for coating, dissolving EVA in petroleum ether, adding RDX@DAP-4 compound and DOA, stirring and volatilizing a solvent to obtain coated particles;
3) Preparation of composite explosive
And directly pressing and forming the coated particles to obtain the composite explosive.
The mass parts of DAP-4 and RDX in the RDX@DAP-4 compound are 100 parts and 100 parts respectively; the modifying solvent consists of 100 parts of cyclohexanone and 0.15 part of liquid paraffin.
The mass parts of RDX@DAP-4 compound, EVA and DOA in the coated particles are respectively 100 parts, 3 parts and 0.15 part.
Finally, it should be noted that: the above embodiments are only for illustrating the technical aspects of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the above embodiments, it should be understood by those of ordinary skill in the art that: modifications and equivalents may be made to the specific embodiments of the invention without departing from the spirit and scope of the invention, which is intended to be covered by the claims.
Claims (8)
1. The composite explosive structure is characterized by comprising coated particles, wherein the forming process of the coated particles is as follows: wrapping RDX with DAP-4 to form a mosaic structure compound RDX@DAP-4; EVA is coated on the compound RDX@DAP-4; the interstices between the EVA and the outermost DAP-4 particles are filled by DOA to form coated particles.
2. The preparation method of the composite explosive structure is characterized by comprising the following steps of:
1) Adding RDX into a modified solvent, heating to 90-100 ℃ to prepare a saturated solution of RDX, adding DAP-4, stirring and cooling, separating out RDX in the saturated solution of RDX and wrapping the RDX on the surface of DAP-4, filtering, washing with water and drying to obtain an RDX@DAP-4 compound;
2) Dissolving EVA in petroleum ether, adding RDX@DAP-4 compound and DOA, stirring and volatilizing a solvent to obtain coated particles;
3) And preparing the composite explosive by using the coated particles.
3. The method of producing a composite explosive structure according to claim 2, wherein the washing temperature in step 1) is 30 ℃ or less.
4. The method of preparing a composite explosive structure according to claim 2, wherein the specific operations of step 3) are: and directly pressing and forming the coated particles to obtain the composite explosive.
5. The method of preparing a composite explosive structure according to claim 2, wherein the specific operations of step 3) are: the composite explosive is prepared by taking the coated particles as an energy-containing component, and using a binder, metal powder and an oxidant through a press-fitting process or a casting process.
6. The method for preparing a composite explosive structure according to claim 2, wherein the mass parts of DAP-4 and RDX in the RDX@DAP-4 composite are respectively 100 parts and 50-200 parts.
7. The method for preparing a composite explosive structure according to claim 2, wherein the modifying solvent is composed of 100 parts of cyclohexanone and 0.1 to 0.2 parts of liquid paraffin.
8. The method for preparing a composite explosive structure according to claim 2, wherein the mass parts of the RDX@DAP-4 compound, EVA and DOA in the coated particles are 100 parts, 1-5 parts and 0.1-0.2 part respectively.
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CN114262249A (en) * | 2021-11-15 | 2022-04-01 | 西安近代化学研究所 | Composite explosive particles and preparation method thereof |
CN114149295A (en) * | 2021-12-06 | 2022-03-08 | 中北大学 | Coated molecular perovskite energetic material and preparation method thereof |
CN115073249A (en) * | 2022-06-15 | 2022-09-20 | 湖北航天化学技术研究所 | High polymer bonded explosive, preparation method thereof and perforating bullet |
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