CN111908989A - Preparation method of high-energy explosive filled three-dimensional graphene framework composite structure - Google Patents
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- 239000002360 explosive Substances 0.000 title claims abstract description 113
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 100
- 239000002131 composite material Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 239000002086 nanomaterial Substances 0.000 claims abstract description 6
- 238000011049 filling Methods 0.000 claims description 12
- 238000001953 recrystallisation Methods 0.000 claims description 11
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- 238000011068 loading method Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 5
- 230000002829 reductive effect Effects 0.000 claims description 5
- 238000001338 self-assembly Methods 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 238000003763 carbonization Methods 0.000 claims description 2
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- 230000035945 sensitivity Effects 0.000 abstract description 23
- 238000012546 transfer Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 description 23
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 20
- 239000000243 solution Substances 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 7
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- 239000007864 aqueous solution Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
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- 238000013461 design Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
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- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000004317 sodium nitrate Substances 0.000 description 2
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- 238000005303 weighing Methods 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
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- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
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- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002210 supercritical carbon dioxide drying Methods 0.000 description 1
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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
- C06B45/04—Compositions or products which are defined by structure or arrangement of component of product comprising solid particles dispersed in solid solution or matrix not used for explosives where the matrix consists essentially of nitrated carbohydrates or a low molecular organic explosive
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- 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 preparation method of a high-energy explosive filled three-dimensional graphene frame composite structure, which is characterized in that a two-dimensional graphene oxide nano material is used for reducing and self-assembling to prepare a three-dimensional graphene frame structure as a template, a high-energy explosive solution is introduced into the three-dimensional graphene frame structure, the explosive solution is recrystallized in the frame structure of the template by using external acting force to form explosive crystals which directionally grow in a limited space of the frame structure, the explosive filled frame composite structure is constructed, and the high-energy explosive filled three-dimensional graphene frame composite structure is obtained by introducing and crystallizing the explosive solution for multiple times. The method can improve the dispersibility of the graphene in the composite explosive system, improve the mass transfer and heat transfer characteristics of the composite system, effectively reduce the impact sensitivity, the friction sensitivity and the electrostatic spark sensitivity of the explosive, and improve the safety performance.
Description
Technical Field
The invention belongs to a design and regulation method of an energetic material composite structure, and particularly relates to a preparation method of an explosive filled three-dimensional graphene framework composite structure.
Background
Generation of material, generation of equipment. The updating speed of energetic materials is directly related to the development process of weapon equipment modernization. The development targets of weapons with accurate striking, efficient damage, high survivability and environmental friendliness put forward more and higher requirements on energetic materials, such as higher energy density, better safety performance, better energy release efficiency, better environmental stability and the like.
The graphene-based composite energetic material has excellent mechanical strength (tensile strength of 130GPa and Young modulus of 1 TPa) and heat conductivity (5000 W.m) of graphene-1·K-1) Ultra-fast electron transport characteristics (2 x 10)5cm2·V-1·S-1) And good conductivity (-10)8S/m), and the like, and the continuous attention in the field of energetic materials is gained. Relevant researches show that by introducing the graphene material into the energetic material, the detonation performance and the mechanical property of the composite explosive system can be effectively enhanced, the external stimulus response is reduced to improve the safety of the composite system, and the energy release efficiency of the composite system can be promoted.
However, due to the electrostatic cluster effect of the nano graphene material, graphene in the composite system cannot be completely and uniformly dispersed in the composite explosive system, so that a great difference exists between the actual performance improvement degree of the composite explosive and the theory.
How to realize the uniform dispersion of a large amount of graphene nano materials in energetic materials is a key technical problem to be solved and is also a common problem faced by the development of the current graphene-based composite energetic materials. Therefore, accurate regulation and control of graphene in a composite energetic material system are realized by different methods, the method is a key for solving the problem that nano graphene is easy to agglomerate and clamp necks, and an important basis for ensuring that the graphene can exert potential in the composite system as much as possible is also provided.
On the other hand, research on the application of high explosive is a major concern in the development of weapons. And because of the inherent contradiction between energy and safety of energetic materials, the higher the energy of the explosive, the poorer the safety of the explosive. Although researchers have great expectations for high explosives (HMX, CL-20), due to safety, the high explosives are relatively rarely used at present and cannot be applied to large-scale equipment.
Disclosure of Invention
The invention aims to provide a preparation method of a high-energy explosive filled three-dimensional graphene frame composite structure, which constructs an explosive filled frame composite structure material by combining preparation of a three-dimensional graphene frame structure template and recrystallization of an explosive solution, so as to improve the dispersibility of graphene in a composite explosive system, improve the mass transfer and heat transfer characteristics of the composite system, effectively reduce the sensitivity of the explosive, improve the safety performance, realize the improvement of explosive performance and improve the comprehensive performance of the composite explosive system.
The preparation method of the high-energy explosive filled three-dimensional graphene framework composite structure comprises the following steps:
1) preparing a three-dimensional graphene frame macroscopic body by using a two-dimensional graphene oxide nano material as a raw material in a reduction self-assembly mode, and freeze-drying to obtain a three-dimensional graphene frame structure constructed by two-dimensional graphene nanosheet minimum construction units;
2) introducing a high-energy explosive solution into the three-dimensional graphene frame structure by taking the three-dimensional graphene frame structure as a template, and recrystallizing the explosive solution in the frame structure of the template by using external acting force to form explosive crystals which directionally grow in a confined space of the frame structure, so as to construct an explosive filling frame composite structure;
3) and repeating the introduction and crystallization process of the high-energy explosive solution for many times until the high-energy explosive loading capacity in the framework structure template meets the requirement, thereby obtaining the high-energy explosive filled three-dimensional graphene framework composite structure.
By adopting the preparation method, the filling composite structure explosive with high explosive loading capacity can be prepared by uniformly dispersing the high-energy explosive in the three-dimensional graphene frame structure.
In the preparation method, the three-dimensional graphene framework structure is a large-scale three-dimensional graphene framework macroscopic body which is formed by reducing and self-assembling two-dimensional graphene oxide nano material units and has an internal cross-linked network structure confinement space.
Specifically, the reductive self-assembly method may be any one of a hydrothermal method, a sol-gel method, and a template high-temperature carbonization method.
According to the preparation method, after a high-energy explosive solution is introduced into a three-dimensional graphene framework structure, under the action of a recrystallization condition, explosive molecules are promoted to crystallize and nucleate, the formed explosive crystals grow directionally in a confined space under the limitation of an inner layered network confined space of the three-dimensional graphene framework structure, and finally the explosive filling framework composite structure is constructed.
Specifically, the method adopts a mode of adsorbing an explosive solution by a template, and introduces the high-energy explosive solution into the template with the three-dimensional graphene frame structure.
Further, in the preparation method of the invention, the high explosive is one or more of HMX, CL-20, ADN, DAAF and TKX-50 explosives.
In the preparation method of the invention, the external force recrystallization mode can be any one of natural volatilization recrystallization, evaporation recrystallization and cooling recrystallization.
According to the invention, through structural design and performance regulation and control of a graphene-based energetic material composite structure, a mesoscale confined frame filling method is utilized, and a mode of combining three-dimensional graphene frame structure template preparation and explosive solution recrystallization is adopted, so that explosive molecules are crystallized, nucleated, oriented, grown and recrystallized in a graphene network confined space, and further, the explosive filled three-dimensional graphene frame composite structure material is obtained.
By adopting the method, the explosive loading capacity of the composite structure can be quantitatively regulated and controlled according to later-stage application requirements, and the high-energy explosive filled three-dimensional graphene framework composite structure with different filling densities can be obtained. Furthermore, the graphene frame structure with different dimensionalities can be designed according to actual needs, so that the sensitivity of the explosive is effectively reduced, the safety performance is improved, and the improvement of the explosive performance is realized.
The appearance structure characterization result shows that in the high-energy explosive filled three-dimensional graphene framework composite structure prepared by the method, explosive crystals grow directionally in the network structure confinement space of the three-dimensional graphene framework, the graphene materials are regularly distributed, and the common problem that the graphene materials cannot be uniformly distributed in a composite explosive system is effectively solved. Furthermore, the frame structure also constructs a continuous heat and mass transfer cross-linked network for the composite explosive system, which is beneficial to enhancing the heat conduction characteristic of the composite explosive system. Therefore, compared with the high-energy explosive raw material, the impact sensitivity, the friction sensitivity and the electrostatic spark sensitivity of the three-dimensional graphene framework composite structure filled with the high-energy explosive are obviously improved.
Drawings
FIG. 1 is a topographic map of the CL-20 explosive filled three-dimensional graphene framework composite structure of example 1.
In the figure, a represents a three-dimensional graphene framework structure; b represents an explosive crystallization adhering precipitation process of a CL-20 explosive filling frame structure; and c represents a densified CL-20 explosive filled three-dimensional graphene framework composite structure.
Detailed Description
The following examples further describe embodiments of the present invention. The following examples are only for illustrating the technical solutions of the present invention more clearly, and do not limit the scope of the present invention. Various changes, modifications, substitutions and alterations to these embodiments will be apparent to those skilled in the art without departing from the principles and spirit of this invention.
Weighing 1g of graphite powder and 1g of sodium nitrate respectively, putting the graphite powder and the sodium nitrate into a 250ml flat-bottomed flask containing 40-60 ml of nitric-sulfuric mixed acid, and stirring the mixture in an ice-water bath for 1 hour. 6g of potassium permanganate were then added continuously, heated to 35 ℃ and the reaction was stirred continuously at 300rpm/min for 2 h.
After the reaction is finished, diluting the reaction solution with deionized water, and adding hydrogen peroxide for repeated washing. Impurities were removed by centrifugation, and freeze-dried to obtain graphene oxide as a raw material used in the following examples.
In addition to the above preparation method of graphene oxide, the graphene oxide used as a raw material in each embodiment of the present invention may be prepared by other various conventional methods, and the present invention is not limited thereto.
Example 1.
Weighing 15ml of graphene oxide aqueous solution with the concentration of 2mg/ml, placing the graphene oxide aqueous solution in a stainless steel reaction kettle with a polytetrafluoroethylene lining, sealing the reaction kettle, and heating the reaction kettle in an oven to 180 ℃ for hydrothermal reaction for 24 hours. And taking out the product to obtain graphene gel, rinsing for multiple times, and freeze-drying to obtain the three-dimensional graphene framework structure.
Fig. 1(a) is an SEM image of a three-dimensional graphene framework structure, and a distinct network structure can be seen, illustrating that the three-dimensional graphene framework structure was successfully prepared.
And taking the obtained three-dimensional graphene frame structure as a template, adding a CL-20 acetone saturated solution into the three-dimensional graphene frame structure by adopting a mode of introducing a template adsorption explosive solution, heating the three-dimensional graphene frame structure in a vacuum drying oven at a constant temperature of 60 ℃ for 20-25 min, and evaporating the acetone serving as a solvent to obtain the CL-20 explosive filling frame composite structure.
Fig. 1(b) shows the SEM morphology of the CL-20 explosive filled frame composite structure, and it can be seen that the CL-20 explosive is attached to the mesh holes of the three-dimensional graphene frame structure, showing the explosive crystallization attachment precipitation process of the CL-20 explosive filled frame structure.
And (3) continuously adding the CL-20 acetone saturated solution into the obtained CL-20 explosive filling frame composite structure by adopting the introduction mode of the template adsorption explosive solution again, and carrying out evaporative crystallization under the same conditions.
Repeating for 5 times to obtain a densified CL-20 explosive filled three-dimensional graphene framework composite structure with high explosive loading.
Fig. 1(c) shows the SEM morphology of the densified CL-20 explosive filled three-dimensional graphene framework composite structure, and it can be seen that after multiple times of filling, the mesh pores of the three-dimensional graphene framework structure are completely filled with CL-20 explosive, forming a densified CL-20 explosive filled three-dimensional graphene framework composite structure material.
As can be seen by combining the shapes of the cross-sectional microstructures in fig. 1, the confined space of the three-dimensional graphene frame structure is occupied by CL-20 explosive crystals to form a CL-20 explosive filled three-dimensional graphene frame composite structure; the three-dimensional graphene framework structure forms a cross-linked network framework, and the cross-linked network framework is inserted into the composite structure and effectively dispersed in an explosive system.
The impact sensitivity was measured by the WL-1 type impact sensitivity meter according to 601.2 (characteristic falling height method) of GJB-770B-2005, with a falling weight of 2.0Kg, a sample mass of 30mg, and a sample number of 25. The friction sensitivity was measured according to 602 (explosion probability method) in GJB-770B-2005, with a pendulum weight of 2.0Kg, a pendulum angle of 90 °, a pressure of 3.92MPa, a sample mass of 30mg, and a sample number of 25. The electrostatic spark sensitivity test is carried out by adopting a GJB/z 736.11-90 'Electrostatic sensitivity test for initiating explosive device test method for electric initiating explosive device', and the sample amount is 2 mg.
The results of the sensitivity test evaluation are shown in table 1. The result shows that the impact sensitivity, the friction sensitivity and the electrostatic spark sensitivity of the obtained CL-20 explosive filled three-dimensional graphene frame composite structure material are insensitive to the raw material CL-20.
Example 2.
20ml of graphene oxide aqueous solution with the concentration of 1mg/ml is measured and placed in a sample bottle with a sealing cover, and 0.12g of reducing agent ethylenediamine is added. Covering a sealing cover, uniformly shaking, and placing in an oven at 85 ℃ for heating reaction for 24 hours. And taking out the product, slowly transferring the product to deionized water for soaking, cleaning for many times, removing unreacted reducing agents and impurities, and freeze-drying to obtain the three-dimensional graphene frame structure.
And taking the obtained three-dimensional graphene frame structure as a template, adding an HMX acetone saturated solution into the three-dimensional graphene frame structure by adopting a mode of introducing a template adsorption explosive solution, evaporating at a constant temperature of 60 ℃ for 20min in a vacuum drying oven, and evaporating solvent acetone to obtain the HMX explosive filled frame composite structure.
And (3) continuously adding the HMX acetone saturated solution into the obtained HMX explosive filled frame composite structure by adopting the introduction mode of the template adsorbed explosive solution again, and carrying out evaporative crystallization under the same conditions.
And repeating the steps for 5 times to obtain a densified HMX explosive filled three-dimensional graphene framework composite structure with high explosive loading.
The composite structure was evaluated for safety according to the procedure of example 1, and the results are shown in Table 2.
The result shows that the impact sensitivity, the friction sensitivity and the electrostatic spark sensitivity of the obtained material with the HMX explosive filled in the three-dimensional graphene framework composite structure are obviously improved compared with those of the material HMX, and the safety performance of the HMX explosive filled in the three-dimensional graphene framework composite structure is effectively improved.
Example 3.
200ml of a graphene oxide aqueous solution with a concentration of 20mg/ml is measured and placed in a 250ml beaker, and 2g of resorcinol, 1g of formaldehyde and 10mg of catalyst sodium carbonate are added. The mixture was transferred to a glass mold, sealed and placed in an oven at 80 ℃ for a reaction time of 96 h. Taking out the graphene gel product from the mold, soaking and cleaning the graphene gel product by acetone, and performing supercritical CO2Drying the wet gel in N2Heating for 3h at 1050 ℃ in the atmosphere to obtain the three-dimensional graphene frame structure.
And taking the obtained three-dimensional graphene frame structure as a template, adding a DAAF acetone saturated solution into the three-dimensional graphene frame structure by adopting a mode of introducing a template adsorption explosive solution, evaporating at a constant temperature of 60 ℃ for 20min in a vacuum drying oven, and evaporating solvent acetone to obtain the DAAF explosive filling frame composite structure.
And (3) continuously adding the DAAF acetone saturated solution into the obtained DAAF explosive filling frame composite structure by adopting the introduction mode of the template adsorption explosive solution again, and carrying out evaporation crystallization under the same conditions.
And repeating the steps for 5 times to obtain a densified DAAF explosive filled three-dimensional graphene framework composite structure with high explosive loading.
The composite structure was evaluated for safety according to the method of example 1 and the results are shown in Table 3.
The result shows that the impact sensitivity, the friction sensitivity and the electrostatic spark sensitivity of the obtained DAAF explosive filled three-dimensional graphene frame composite structure material are obviously improved compared with those of the DAAF raw material, and the safety performance of the DAAF explosive filled three-dimensional graphene frame composite structure is effectively improved.
Claims (7)
1. A preparation method of a high-energy explosive filled three-dimensional graphene framework composite structure is characterized by comprising the following steps of:
1) preparing a three-dimensional graphene frame macroscopic body by using a two-dimensional graphene oxide nano material as a raw material in a reduction self-assembly mode, and freeze-drying to obtain a three-dimensional graphene frame structure constructed by two-dimensional graphene nanosheet minimum construction units;
2) introducing a high-energy explosive solution into the three-dimensional graphene frame structure by taking the three-dimensional graphene frame structure as a template, and recrystallizing the explosive solution in the frame structure of the template by using external acting force to form explosive crystals which directionally grow in a confined space of the frame structure, so as to construct an explosive filling frame composite structure;
3) and repeating the introduction and crystallization process of the high-energy explosive solution for many times until the high-energy explosive loading capacity in the framework structure template meets the requirement, thereby obtaining the high-energy explosive filled three-dimensional graphene framework composite structure.
2. The preparation method of claim 1, wherein the three-dimensional graphene framework structure is a large-scale three-dimensional graphene framework macroscopic body which is formed by reduction self-assembly of two-dimensional graphene oxide nano material units and has an internal cross-linked network structure confinement space.
3. The method according to claim 1, wherein the reductive self-assembly method is any one of a hydrothermal method, a sol-gel method, and a template high-temperature carbonization method.
4. The preparation method of claim 1, wherein the high-energy explosive solution is introduced into the three-dimensional graphene framework structure template in a mode of adsorbing the explosive solution by the template.
5. The method of claim 1, wherein the high explosive is one or more of HMX, CL-20, ADN, DAAF, TKX-50 explosives.
6. The method according to claim 1, wherein the recrystallization by external force is any one of natural volatilization recrystallization, evaporative recrystallization, and temperature-reduced recrystallization.
7. The filled composite structure explosive prepared by the preparation method of claim 1 and uniformly dispersing the high-energy explosive in the three-dimensional graphene framework structure.
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| US20160031769A1 (en) * | 2013-10-10 | 2016-02-04 | Battelle Energy Alliance, Llc. | Methods of reducing ignition sensitivity of energetic materials, methods of forming energetic materials having reduced ignition sensitivity, and related energetic materials |
| CN106220460A (en) * | 2016-08-15 | 2016-12-14 | 中北大学 | A kind of preparation method of graphene-based Composite Energetic Materials |
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| US20160031769A1 (en) * | 2013-10-10 | 2016-02-04 | Battelle Energy Alliance, Llc. | Methods of reducing ignition sensitivity of energetic materials, methods of forming energetic materials having reduced ignition sensitivity, and related energetic materials |
| CN106220460A (en) * | 2016-08-15 | 2016-12-14 | 中北大学 | A kind of preparation method of graphene-based Composite Energetic Materials |
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| 王华煜等: "TKX-50／GO复合含能材料的制备及热分解特性", 《火炸药学报》 * |
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| CN114988972A (en) * | 2022-07-13 | 2022-09-02 | 西南科技大学 | Method for reducing mechanical and electrostatic sensitivity of explosive by coating with nano carbon material |
| CN114988972B (en) * | 2022-07-13 | 2023-09-29 | 西南科技大学 | Method for reducing mechanical and electrostatic sensitivity of explosive by coating nano carbon material |
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