A DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation properties and its preparation method

Abstract

This invention discloses a DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation characteristics and its preparation method, comprising: dispersing DNTF in water and stirring to obtain a DNTF dispersion; adding a nickel acetate tetrahydrate solution to the DNTF dispersion and stirring to obtain a mixed solution system; adding an aqueous dispersion of HHTP organic ligands to the mixed solution system and stirring to obtain a mixed solution system; after the reaction, performing solid-liquid separation, washing, and drying to obtain the DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation characteristics. This invention utilizes Ni3(HHTP)2 material with high conductivity and, through process control, forms a conductor with rod-like structure on the surface of DNTF, forming an effective conductive path. The volume resistivity of the composite energetic material reaches the electrostatic dissipation range, effectively promoting the dissipation of accumulated static electricity and improving the electrostatic safety of the powder energetic material.

Description

Technical Field

[0001] This invention belongs to the technical field of composite energetic materials, and relates to a DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation characteristics and its preparation method. Background Technology

[0002] During the production, transportation, and use of energetic powder materials, static charge can easily accumulate after contact with and separation from the external environment. Excessive static charge accumulation, reaching the electrostatic breakdown field strength, can easily trigger electrostatic discharge, leading to safety accidents such as combustion and explosion. Therefore, eliminating static charge accumulation in energetic powder materials is of great significance for their efficient application.

[0003] To reduce the accumulation of static electricity in energetic powder materials and improve electrostatic safety, antistatic modification of energetic materials is an effective way to reduce static electricity accumulation. Common antistatic modification methods mainly involve adding conductive materials during the production or use of energetic powder materials. Researchers Wang Qian et al. (“Energetic Materials”, Vol. 26, No. 10) added rGO (reduced graphene oxide) to a B / KNO3 ignition source, resulting in a decrease in the resistivity of the energetic material to 1.11 × 10⁻⁶. 5 Ω·cm is a conductive material, but the rapid transfer of static charge from a high electrostatic potential can easily trigger electrostatic discharge, causing safety accidents. Researchers Hou Guanchen et al. (Journal of Explosives and Pyrotechnics, Vol. 39, No. 1) added carbon nanotubes as conductive fillers to nitrocellulose, reducing the resistivity of the nitrocellulose composite material to 1.02 × 10⁻⁶. 11 While the volume resistivity is high (Ω·cm), it falls under the category of insulating materials and cannot effectively dissipate static electricity. Research on antistatic modification of energetic powder materials has not yielded high-performance static dissipative materials. When the volume resistivity is too high, the accumulation of static electricity on the material surface is difficult to eliminate; when the resistivity is too low, the accumulated static electricity conduction speed is too fast, resulting in a rapid transfer from high to low electrostatic potential. This static discharge can easily lead to accidents such as combustion and explosion. Therefore, there is an urgent need for a method to effectively improve the conductivity of energetic powder materials, effectively combine them with other energetic powder materials, and reduce the volume resistivity of energetic powder materials to within the range of static dissipation, thereby promoting the safe application of energetic materials. Summary of the Invention

[0004] One object of the present invention is to solve at least the above-mentioned problems and / or defects, and to provide at least the advantages described below.

[0005] To achieve these objectives and other advantages according to the present invention, a method for preparing a DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation properties is provided, comprising the following steps:

[0006] Step 1: Disperse DNTF in water and stir to obtain a DNTF dispersion.

[0007] Step 2: Add nickel acetate tetrahydrate solution to DNTF dispersion, stir and react to obtain a mixed solution system;

[0008] Step 3: Add the aqueous dispersion of HHTP organic ligand to the mixed solution system obtained in Step 2, stir the reaction, and synthesize the DNTF@Ni3(HHTP)2 product;

[0009] Step 4: After the reaction is complete, perform solid-liquid separation, washing, and drying to obtain DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation characteristics.

[0010] Preferably, in step one, the mass ratio of DNTF to water is 1 to 2:10, and the water is deionized water; the stirring method is mechanical stirring, the stirring speed is 280 to 350 rpm, and the stirring time is 0.5 to 1 hour.

[0011] Preferably, in step two, the preparation method of the nickel acetate tetrahydrate solution is as follows: dissolve nickel acetate tetrahydrate in deionized water to obtain the nickel acetate tetrahydrate solution; the mass ratio of nickel acetate tetrahydrate to deionized water is 3:25-150.

[0012] Preferably, in step two, the mass of nickel acetate tetrahydrate in the nickel acetate tetrahydrate solution is 0.59% to 2.36% of the mass of DNTF in the DNTF dispersion, and the stirring reaction is carried out by mechanical stirring or ultrasound; the mechanical stirring speed is 280 to 350 rpm, and the stirring reaction time is 1.5 to 3 hours.

[0013] Preferably, in step three, the method for preparing the HHTP organic ligand aqueous dispersion is as follows: add HHTP organic ligand to deionized water and ultrasonically disperse for 15-30 minutes to obtain the HHTP organic ligand dispersion; the mass ratio of HHTP organic ligand to deionized water is 1:10-75.

[0014] Preferably, in step three, the mass ratio of HHTP organic ligand in the HHTP organic ligand aqueous dispersion to nickel acetate tetrahydrate in the nickel acetate tetrahydrate solution is 10:6-9.

[0015] Preferably, in step three, the stirring reaction is carried out by mechanical stirring or ultrasound.

[0016] Preferably, in step three, the stirring reaction time is 8-16 hours.

[0017] Preferably, in step four, the solid-liquid separation method is either vacuum filtration or centrifugal filtration, the washing reagent is deionized water, the washing is performed multiple times, the temperature is maintained at 45℃~55℃ during the drying process, and the drying time is 8~12h.

[0018] This invention also provides a DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation characteristics prepared by the preparation method described above, wherein the volume resistivity of the DNTF@Ni3(HHTP)2 composite energetic material is 1×10⁻⁶. 8 ~8×10 10 Ω·cm; the electrostatic accumulation of the DNTF@Ni3(HHTP)2 composite energetic material is -12 to -6 nC·g. -1 .

[0019] This invention addresses the electrostatic safety issues associated with the application of energetic powder materials. It presents an antistatic modified composite energetic material that reduces the resistivity of the energetic material, enhances the dissipation of accumulated static electricity, and improves the safety of energetic powder materials during application.

[0020] This invention utilizes Ni3(HHTP)2 material with high conductivity and, through process control, forms a conductor with rod-like structure on the surface of DNTF, thus creating an effective conductive path. The volume resistivity of the composite energetic material reaches the electrostatic dissipation range, effectively promoting the dissipation of accumulated static electricity and improving the electrostatic safety of the powder energetic material.

[0021] The present invention has at least the following beneficial effects:

[0022] (1) This invention prepares a powder composite energetic material with excellent electrostatic dissipation capability and high electrostatic safety. This invention prepares Ni3(HHTP)2 material with excellent conductivity on the surface of the powder energetic material through in-situ synthesis. By controlling the process and regulating the conductive network formed on the DNTF surface, the volume resistivity of the composite energetic material reaches 10⁻⁶. 8 -10 10 Ω·cm, belonging to the category of electrostatic dissipative materials, allows the accumulation of static electricity to be transferred through the conductive network on its surface. The static dissipation rate is slower than that of conductive materials, avoiding electrostatic discharge caused by rapid static dissipation and improving electrostatic safety.

[0023] (2) The present invention has a simple operation method and good environmental friendliness. The invention is carried out in an aqueous solution, eliminating the need for environmentally harmful chemical reagents, thus being environmentally friendly. The preparation process does not involve high-temperature and high-pressure reactions, making it simple and feasible to operate. It is suitable for a wide range of applications.

[0024] Other advantages, objectives and features of the present invention will become apparent in part from the following description, and in part from those skilled in the art through study and practice of the invention. Attached image description:

[0025] Figure 1 This is a schematic diagram of the preparation method of the present invention;

[0026] Figure 2 SEM image of the DNTF@Ni3(HHTP)2 composite energetic material when the Ni3(HHTP)2 content is 1% and the HHTP reaction time is 12h;

[0027] Figure 3 SEM image of the DNTF@Ni3(HHTP)2 composite energetic material when the Ni3(HHTP)2 content is 2% and the HHTP reaction time is 12h;

[0028] Figure 4 SEM image of the DNTF@Ni3(HHTP)2 composite energetic material when the Ni3(HHTP)2 content is 4% and the HHTP reaction time is 12h;

[0029] Figure 5 SEM image of the DNTF@Ni3(HHTP)2 composite energetic material when the Ni3(HHTP)2 content is 2% and the HHTP reaction time is 8h;

[0030] Figure 6 SEM image of the DNTF@Ni3(HHTP)2 composite energetic material when the Ni3(HHTP)2 content is 2% and the HHTP reaction time is 16h in Example 5.

[0031] Figure 7 SEM images of the DNTF@Ni3(HHTP)2 composite energetic material when the Ni3(HHTP)2 content is 0.5% and the HHTP reaction time is 12h (for Comparative Example 1).

[0032] Figure 8 SEM image of the DNTF@Ni3(HHTP)2 composite energetic material when the content of 2Ni3(HHTP)2 is 6% and the HHTP reaction time is 12h;

[0033] Figure 9 SEM images of the DNTF@Ni3(HHTP)2 composite energetic material when the content of 3Ni3(HHTP)2 is 2% and the HHTP reaction time is 4h, for the comparative example.

[0034] Figure 10SEM images of the DNTF@Ni3(HHTP)2 composite energetic material were obtained when the Ni3(HHTP)2 content was 2% and the HHTP reaction time was 20 h, as a comparative example. Detailed implementation method:

[0035] The present invention will now be described in further detail with reference to the accompanying drawings, so that those skilled in the art can implement it based on the description.

[0036] It should be understood that terms such as “having,” “comprising,” and “including” as used herein do not imply the presence or addition of one or more other elements or combinations thereof.

[0037] Resistance testing of this invention:

[0038] The volume resistivity of the powder energetic material samples before and after modification was tested using a GEST-121 ultra-micro current powder volume resistivity tester from Beijing Guance Precision Instrument Equipment Co., Ltd.; the test voltage was 500V.

[0039] Electrostatic accumulation test of the present invention:

[0040] The electrostatic accumulation of the powder energetic material before and after modification was tested using the HTGT electrostatic accumulation test device of Beijing Huace Testing Instrument Co., Ltd.: the slide used for the test was a stainless steel slide, and the slide angle was adjusted to 45°.

[0041] Example 1:

[0042] A method for preparing a DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation properties includes the following steps:

[0043] (1) Dispersion of DNTF explosive: Weigh 10g of DNTF raw material and place it in a 250ml three-necked flask. Add 100ml of deionized water and stir thoroughly for 1h at room temperature with a mechanical stirring speed of 280rpm to disperse DNTF evenly and obtain DNTF dispersion.

[0044] (2) Coordination of nickel ions with DNTF: Weigh 59 mg of nickel acetate tetrahydrate and dissolve it in 20 mL of deionized water. Add the resulting nickel acetate tetrahydrate solution to the DNTF dispersion in step one. Keep the stirring speed at 280 rpm and continue the reaction for 2 h to obtain a mixed solution system.

[0045] (3) Synthesis of Ni3(HHTP)2 on DNTF surface: 41 mg of HHTP organic ligand was weighed and dispersed in 15 mL of deionized water and ultrasonically dispersed for 20 min to obtain an aqueous dispersion of HHTP organic ligand; the aqueous dispersion of HHTP organic ligand was added to the mixed solution system in step two, and the stirring speed was controlled at 280 rpm. The reaction was carried out at room temperature for 12 h. After the reaction, the precipitate was collected by centrifugation and washed multiple times with deionized water. The washed sample was dried in a vacuum oven at 50 °C for 12 h to obtain DNTF@Ni3(HHTP)2 composite energetic material.

[0046] (4) The volume resistivity of the prepared DNTF@Ni3(HHTP)2 composite energetic material was tested using an ultra-micro current powder volume resistivity tester, and the obtained volume resistivity was 7.75 × 10⁻⁶. 10 The electrostatic accumulation (Ω·cm) falls under the category of electrostatic dissipative materials. The electrostatic accumulation of the DNTF@Ni3(HHTP)2 composite material was measured using an electrostatic accumulation tester, yielding a value of -11.16 nC·g. -1 Compared to the raw material DNTF, the electrostatic accumulation was reduced by 46.29%. Figure 2 When the Ni3(HHTP)2 content is 1% and the HHTP reaction time is 12h, the SEM of the DNTF@Ni3(HHTP)2 composite energetic material shows that the DNTF surface has obvious Ni3(HHTP)2 rod-shaped structure, which is widely dispersed and has a low content.

[0047] Example 2:

[0048] A method for preparing a DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation properties includes the following steps:

[0049] (1) Dispersion of DNTF explosive: Weigh 10g of DNTF raw material and place it in a 250ml three-necked flask. Add 100ml of deionized water and stir thoroughly for 1h at room temperature with a mechanical stirring speed of 280rpm to disperse DNTF evenly and obtain DNTF dispersion.

[0050] (2) Coordination of nickel ions with DNTF: Weigh 118 mg of nickel acetate tetrahydrate and dissolve it in 20 mL of deionized water. Add the resulting nickel acetate tetrahydrate solution to the DNTF dispersion in step one. Keep the stirring speed at 280 rpm and continue the reaction for 2 h to obtain a mixed solution system.

[0051] (3) Synthesis of Ni3(HHTP)2 on DNTF surface: 82 mg of HHTP organic ligand was weighed and dispersed in 15 mL of deionized water and ultrasonically dispersed for 20 min to obtain an aqueous dispersion of HHTP organic ligand; the aqueous dispersion of HHTP organic ligand was added to the mixed solution system in step two, and the stirring speed was controlled at 280 rpm. The reaction was carried out at room temperature for 12 h. After the reaction was completed, the precipitate was collected by centrifugation and washed multiple times with deionized water. The washed sample was dried in a vacuum oven at 50 °C for 12 h to obtain DNTF@Ni3(HHTP)2 composite energetic material.

[0052] (4) The volume resistivity of the prepared DNTF@Ni3(HHTP)2 composite energetic material was tested using an ultra-micro current powder volume resistivity tester. The obtained volume resistivity was 5.15 × 10⁻⁶. 9 The electrostatic accumulation (Ω·cm) falls under the category of electrostatic dissipative materials. The electrostatic accumulation of the DNTF@Ni3(HHTP)2 composite material was measured using an electrostatic accumulation tester, yielding a value of -8.20 nC·g. -1 Compared to the raw material DNTF, the electrostatic accumulation was reduced by 60.54%. Figure 3 When the Ni3(HHTP)2 content is 2% and the HHTP reaction time is 12h, the SEM of the DNTF@Ni3(HHTP)2 composite energetic material shows a significant increase in rod-like structures on the DNTF surface.

[0053] Example 3:

[0054] A method for preparing a DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation properties includes the following steps:

[0055] (1) Dispersion of DNTF explosive: Weigh 10g of DNTF raw material and place it in a 250ml three-necked flask. Add 100ml of deionized water and stir thoroughly for 1h at room temperature with a mechanical stirring speed of 280rpm to disperse DNTF evenly and obtain DNTF dispersion.

[0056] (2) Coordination of nickel ions with DNTF: Weigh 236 mg of nickel acetate tetrahydrate and dissolve it in 20 ml of deionized water. Add the resulting nickel acetate tetrahydrate solution to the DNTF dispersion in step one. Keep the stirring speed at 280 rpm and continue the reaction for 2 h to obtain a mixed solution system.

[0057] (3) Synthesis of Ni3(HHTP)2 on DNTF surface: 164 mg of HHTP organic ligand was weighed and dispersed in 15 ml of deionized water and ultrasonically dispersed for 20 min to obtain an aqueous dispersion of HHTP organic ligand; the aqueous dispersion of HHTP organic ligand was added to the mixed solution system in step two, and the stirring speed was controlled at 280 rpm. The reaction was carried out at room temperature for 12 h. After the reaction, the precipitate was collected by centrifugation and washed multiple times with deionized water. The washed sample was dried in a vacuum oven at 50 ℃ for 12 h to obtain DNTF@Ni3(HHTP)2 composite energetic material.

[0058] (4) The volume resistivity of the prepared DNTF@Ni3(HHTP)2 composite energetic material was tested using an ultra-micro current powder volume resistivity tester, and the obtained volume resistivity was 3.46 × 10⁻⁶. 8 The electrostatic accumulation (Ω·cm) falls under the category of electrostatic dissipative materials. The electrostatic accumulation of the DNTF@Ni3(HHTP)2 composite material was measured using an electrostatic accumulation tester, yielding a value of -6.89 nC·g. -1 Compared to the raw material DNTF, the electrostatic accumulation was reduced by 66.84%. Figure 4 When the Ni3(HHTP)2 content is 4% and the HHTP reaction time is 12h, the SEM of the DNTF@Ni3(HHTP)2 composite energetic material shows that the Ni3(HHTP)2 rod-shaped structure on the NTF surface continues to increase and is relatively uniformly distributed.

[0059] Example 4:

[0060] A method for preparing a DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation properties includes the following steps:

[0061] (1) Dispersion of DNTF explosive: Weigh 10g of DNTF raw material and place it in a 250ml three-necked flask. Add 100ml of deionized water and stir thoroughly for 1h at room temperature with a mechanical stirring speed of 280rpm to disperse DNTF evenly and obtain DNTF dispersion.

[0062] (2) Coordination of nickel ions with DNTF: Weigh 118 mg of nickel acetate tetrahydrate and dissolve it in 20 mL of deionized water. Add the resulting nickel acetate tetrahydrate solution to the DNTF dispersion in step one. Keep the stirring speed at 280 rpm and continue the reaction for 2 h to obtain a mixed solution system.

[0063] (3) Synthesis of Ni3(HHTP)2 on DNTF surface: 82 mg of HHTP organic ligand was weighed and dispersed in 15 mL of deionized water and ultrasonically dispersed for 20 min to obtain an aqueous dispersion of HHTP organic ligand; the aqueous dispersion of HHTP organic ligand was added to the mixed solution system in step two, and the stirring speed was controlled at 280 rpm. The reaction was carried out at room temperature for 8 h. After the reaction was completed, the precipitate was collected by centrifugation and washed multiple times with deionized water. The washed sample was dried in a vacuum oven at 50 °C for 12 h to obtain DNTF@Ni3(HHTP)2 composite energetic material.

[0064] (4) The volume resistivity of the prepared DNTF@Ni3(HHTP)2 composite energetic material was tested using an ultra-micro current powder volume resistivity tester. The obtained volume resistivity was 6.93 × 10⁻⁶. 10 The electrostatic accumulation (Ω·cm) falls under the category of electrostatic dissipative materials. The electrostatic accumulation of the DNTF@Ni3(HHTP)2 composite material was measured using an electrostatic accumulation tester, yielding a value of -9.79 nC·g. -1 Compared to the raw material DNTF, the electrostatic accumulation was reduced by 52.88%. Figure 5 When the Ni3(HHTP)2 content is 2% and the HHTP reaction time is 8h, the SEM of the DNTF@Ni3(HHTP)2 composite energetic material shows that there are fewer Ni3(HHTP)2 rod-like structures on the DNTF surface.

[0065] Example 5:

[0066] A method for preparing a DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation properties includes the following steps:

[0067] (1) Dispersion of DNTF explosive: Weigh 10g of DNTF raw material and place it in a 250ml three-necked flask. Add 100ml of deionized water and stir thoroughly for 1h at room temperature with a mechanical stirring speed of 280rpm to disperse DNTF evenly and obtain DNTF dispersion.

[0068] (2) Coordination of nickel ions with DNTF: Weigh 118 mg of nickel acetate tetrahydrate and dissolve it in 20 mL of deionized water. Add the resulting nickel acetate tetrahydrate solution to the DNTF dispersion in step one. Keep the stirring speed at 280 rpm and continue the reaction for 2 h to obtain a mixed solution system.

[0069] (3) Synthesis of Ni3(HHTP)2 on DNTF surface: 82 mg of HHTP organic ligand was weighed and dispersed in 15 mL of deionized water and ultrasonically dispersed for 20 min to obtain an aqueous dispersion of HHTP organic ligand; the aqueous dispersion of HHTP organic ligand was added to the mixed solution system in step two, and the stirring speed was controlled at 280 rpm. The reaction was carried out at room temperature for 16 h. After the reaction, the precipitate was collected by centrifugation and washed multiple times with deionized water. The washed sample was dried in a vacuum oven at 50 °C for 12 h to obtain DNTF@Ni3(HHTP)2 composite energetic material.

[0070] (4) The volume resistivity of the prepared DNTF@Ni3(HHTP)2 composite energetic material was tested using an ultra-micro current powder volume resistivity tester. The obtained volume resistivity was 2.04 × 10⁻⁶. 9 The electrostatic accumulation (Ω·cm) falls under the category of electrostatic dissipative materials. The electrostatic accumulation of the DNTF@Ni3(HHTP)2 composite material was tested using a self-made electrostatic accumulation testing device, yielding an electrostatic accumulation of -7.92 nC·g. -1 Compared to the raw material DNTF, the electrostatic accumulation was reduced by 61.89%. Figure 6 When the Ni3(HHTP)2 content is 2% and the HHTP reaction time is 16h, the SEM of the DNTF@Ni3(HHTP)2 composite energetic material shows that the Ni3(HHTP)2 rod-shaped structure on the DNTF surface gradually becomes complete and is uniformly distributed on the surface.

[0071] Comparative Example 1:

[0072] A method for preparing a DNTF@Ni3(HHTP)2 composite energetic material includes the following steps:

[0073] (1) Dispersion of DNTF explosive: Weigh 10g of DNTF raw material and place it in a 250ml three-necked flask. Add 100ml of deionized water and stir thoroughly for 1h at room temperature with a mechanical stirring speed of 280rpm to disperse DNTF evenly and obtain DNTF dispersion.

[0074] (2) Coordination of nickel ions with DNTF: Weigh 30 mg of nickel acetate tetrahydrate and dissolve it in 20 ml of deionized water. Add the resulting nickel acetate tetrahydrate solution to the DNTF dispersion in step one. Keep the stirring speed at 280 rpm and continue the reaction for 2 h to obtain a mixed solution system.

[0075] (3) Synthesis of Ni3(HHTP)2 on DNTF surface: 20 mg of HHTP organic ligand was weighed and dispersed in 15 ml of deionized water and ultrasonically dispersed for 20 min to obtain an aqueous dispersion of HHTP organic ligand; the aqueous dispersion of HHTP organic ligand was added to the mixed solution system in step two, and the stirring speed was controlled at 280 rpm. The reaction was carried out at room temperature for 12 h. After the reaction, the precipitate was collected by centrifugation and washed multiple times with deionized water. The washed sample was dried in a vacuum oven at 50 ℃ for 12 h to obtain DNTF@Ni3(HHTP)2 composite energetic material.

[0076] (4) The volume resistivity of the prepared DNTF@Ni3(HHTP)2 composite energetic material was tested using an ultra-micro current powder volume resistivity tester. The obtained volume resistivity was 1.53 × 10⁻⁶. 12 The electrostatic accumulation (Ω·cm) is not considered a dissipative material. The electrostatic accumulation of the DNTF@Ni3(HHTP)2 composite material was measured using an electrostatic accumulation tester, yielding a value of -16.91 nC·g. -1 . Figure 7 When the Ni3(HHTP)2 content is 0.5% and the HHTP reaction time is 12h, the SEM of the DNTF@Ni3(HHTP)2 composite energetic material shows that no Ni3(HHTP)2 rod-like structure can be observed on the DNTF surface.

[0077] Comparative Example 2:

[0078] A method for preparing a DNTF@Ni3(HHTP)2 composite energetic material includes the following steps:

[0079] (1) Dispersion of DNTF explosive: Weigh 10g of DNTF raw material and place it in a 250ml three-necked flask. Add 100ml of deionized water and stir thoroughly for 1h at room temperature with a mechanical stirring speed of 280rpm to disperse DNTF evenly and obtain DNTF dispersion.

[0080] (2) Coordination of nickel ions with DNTF: Weigh 354 mg of nickel acetate tetrahydrate and dissolve it in 20 ml of deionized water. Add the resulting nickel acetate tetrahydrate solution to the DNTF dispersion in step one. Keep the stirring speed at 280 rpm and continue the reaction for 2 h to obtain a mixed solution system.

[0081] (3) Synthesis of Ni3(HHTP)2 on DNTF surface: 246 mg of HHTP organic ligand was weighed and dispersed in 15 ml of deionized water and ultrasonically dispersed for 20 min to obtain an aqueous dispersion of HHTP organic ligand; the aqueous dispersion of HHTP organic ligand was added to the mixed solution system in step two, and the stirring speed was controlled at 280 rpm. The reaction was carried out at room temperature for 12 h. After the reaction, the precipitate was collected by centrifugation and washed multiple times with deionized water. The washed sample was dried in a vacuum oven at 50 ℃ for 12 h to obtain DNTF@Ni3(HHTP)2 composite energetic material.

[0082] (4) The volume resistivity of the prepared DNTF@Ni3(HHTP)2 composite energetic material was tested using an ultra-micro current powder volume resistivity tester, and the obtained volume resistivity was 3.67 × 10⁻⁶. 5 The electrostatic charge is Ω·cm, classifying it as an electrostatic conductor. The electrostatic charge accumulation of the DNTF@Ni3(HHTP)2 composite material was measured using an electrostatic charge accumulation tester, yielding a value of -1.36 nC·g. -1 . Figure 8 When the Ni3(HHTP)2 content is 6% and the HHTP reaction time is 12h, the SEM of the DNTF@Ni3(HHTP)2 composite energetic material shows that the DNTF surface is basically covered with Ni3(HHTP)2 rod-shaped structure.

[0083] Comparative Example 3:

[0084] A method for preparing a DNTF@Ni3(HHTP)2 composite energetic material includes the following steps:

[0085] (1) Dispersion of DNTF explosive: Weigh 10g of DNTF raw material and place it in a 250ml three-necked flask. Add 100ml of deionized water and stir thoroughly for 1h at room temperature with a mechanical stirring speed of 280rpm to disperse DNTF evenly and obtain DNTF dispersion.

[0086] (2) Coordination of nickel ions with DNTF: Weigh 118 mg of nickel acetate tetrahydrate and dissolve it in 20 ml of deionized water. Add the resulting nickel acetate tetrahydrate solution to the DNTF dispersion in step one. Keep the stirring speed at 280 rpm and continue the reaction for 2 h to obtain a mixed solution system.

[0087] (3) Synthesis of Ni3(HHTP)2 on DNTF surface: 82 mg of HHTP organic ligand was weighed and dispersed in 15 ml of deionized water and ultrasonically dispersed for 20 min to obtain an aqueous dispersion of HHTP organic ligand; the aqueous dispersion of HHTP organic ligand was added to the mixed solution system in step two, and the stirring speed was controlled at 280 rpm. The reaction was carried out at room temperature for 4 h. After the reaction was completed, the precipitate was collected by centrifugation and washed multiple times with deionized water. The washed sample was dried in a vacuum oven at 50 ℃ for 12 h to obtain DNTF@Ni3(HHTP)2 composite energetic material.

[0088] (4) The volume resistivity of the prepared DNTF@Ni3(HHTP)2 composite energetic material was tested using an ultra-micro current powder volume resistivity tester, and the obtained volume resistivity was 2.79 × 10⁻⁶. 12 The electrostatic accumulation (Ω·cm) is not considered a dissipative material. The electrostatic accumulation of the DNTF@Ni3(HHTP)2 composite material was measured using an electrostatic accumulation tester, and the obtained electrostatic accumulation was -14.03 nC·g. -1 . Figure 9 When the Ni3(HHTP)2 content is 2% and the HHTP reaction time is 4h, the SEM of the DNTF@Ni3(HHTP)2 composite energetic material shows that there is no obvious rod-like structure on the DNTF surface.

[0089] Comparative Example 4:

[0090] A method for preparing a DNTF@Ni3(HHTP)2 composite energetic material includes the following steps:

[0091] (1) Dispersion of DNTF explosive: Weigh 10g of DNTF raw material and place it in a 250ml three-necked flask. Add 100ml of deionized water and stir thoroughly for 1h at room temperature with a mechanical stirring speed of 280rpm to disperse DNTF evenly and obtain DNTF dispersion.

[0092] (2) Coordination of nickel ions with DNTF: Weigh 118 mg of nickel acetate tetrahydrate and dissolve it in 20 ml of deionized water. Add the resulting nickel acetate tetrahydrate solution to the DNTF dispersion in step one. Keep the stirring speed at 280 rpm and continue the reaction for 2 h to obtain a mixed solution system.

[0093] (3) Synthesis of Ni3(HHTP)2 on DNTF surface: 82 mg of HHTP organic ligand was weighed and dispersed in 15 ml of deionized water and ultrasonically dispersed for 20 min to obtain an aqueous dispersion of HHTP organic ligand; the aqueous dispersion of HHTP organic ligand was added to the mixed solution system in step two, and the stirring speed was controlled at 280 rpm. The reaction was carried out at room temperature for 20 h. After the reaction was completed, the precipitate was collected by centrifugation and washed multiple times with deionized water. The washed sample was dried in a vacuum oven at 50 ℃ for 12 h to obtain DNTF@Ni3(HHTP)2 composite energetic material.

[0094] (4) The volume resistivity of the prepared DNTF@Ni3(HHTP)2 composite energetic material was tested using an ultra-micro current powder volume resistivity tester. The obtained volume resistivity was 4.55 × 10⁻⁶. 11 The electrostatic accumulation (Ω·cm) is not considered a dissipative material. The electrostatic accumulation of the DNTF@Ni3(HHTP)2 composite material was measured using an electrostatic accumulation tester, and the obtained electrostatic accumulation was -13.77 nC·g. -1 . Figure 10 When the Ni3(HHTP)2 content is 2% and the HHTP reaction time is 20h, the SEM of the DNTF@Ni3(HHTP)2 composite energetic material shows that there is no obvious rod-like structure on the DNTF surface.

[0095] Table 1 shows the electrostatic properties of the DNTF@Ni3(HHTP)2 composite energetic materials prepared in Examples 1-5;

[0096] Table 1

[0097]

[0098] Although embodiments of the present invention have been disclosed above, they are not limited to the applications listed in the specification and embodiments. They can be applied to various fields suitable for the present invention. For those skilled in the art, other modifications can be easily made. Therefore, without departing from the general concept defined by the claims and their equivalents, the present invention is not limited to the specific details and illustrations shown and described herein.

Claims

1. A method for preparing a DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation characteristics, characterized in that, Includes the following steps: Step 1: Disperse DNTF in water and stir to obtain a DNTF dispersion. Step 2: Add nickel acetate tetrahydrate solution to DNTF dispersion, stir and react to obtain a mixed solution system; Step 3: Add the aqueous dispersion of HHTP organic ligand to the mixed solution system obtained in Step 2, stir the reaction, and synthesize the DNTF@Ni3(HHTP)2 product; Step 4: After the reaction is complete, perform solid-liquid separation, washing, and drying to obtain DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation characteristics; In step two, the mass of nickel acetate tetrahydrate in the nickel acetate tetrahydrate solution is 0.59% to 2.36% of the mass of DNTF in the DNTF dispersion, and the stirring reaction is carried out by mechanical stirring or ultrasound; the mechanical stirring speed is 280 to 350 rpm, and the stirring reaction time is 1.5 to 3 h. In step three, the mass ratio of HHTP organic ligand in the HHTP organic ligand aqueous dispersion to nickel acetate tetrahydrate in the nickel acetate tetrahydrate solution is 10:6~9.

2. The preparation method of the DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation characteristics as described in claim 1, characterized in that, In step one, the mass ratio of DNTF to water is 1~2:10, and the water is deionized water; the stirring method is mechanical stirring, the stirring speed is 280~350 rpm, and the stirring time is 0.5~1 hour.

3. The preparation method of the DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation characteristics as described in claim 1, characterized in that, In step two, the preparation method of nickel acetate tetrahydrate solution is as follows: nickel acetate tetrahydrate is dissolved in deionized water to obtain nickel acetate tetrahydrate solution; the mass ratio of nickel acetate tetrahydrate to deionized water is 3:25~150.

4. The method for preparing the DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation characteristics as described in claim 1, characterized in that, In step three, the preparation method of the HHTP organic ligand aqueous dispersion is as follows: add HHTP organic ligand to deionized water and ultrasonically disperse for 15-30 min to obtain HHTP organic ligand dispersion; the mass ratio of HHTP organic ligand to deionized water is 1:10-75.

5. The preparation method of the DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation characteristics as described in claim 1, characterized in that, In step three, the stirring reaction is carried out by mechanical stirring or ultrasound.

6. The method for preparing the DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation characteristics as described in claim 1, characterized in that, In step three, the stirring reaction time is 8-16 hours.

7. The preparation method of DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation characteristics as described in claim 1, wherein in step four, the solid-liquid separation method is either vacuum filtration or centrifugal filtration, the washing reagent is deionized water, the washing is performed multiple times, the temperature maintained during the drying process is 45℃~55℃, and the drying time is 8~12 h.

8. A DNTF@Ni3(HHTP)2 composite energetic material with electrostatic dissipation characteristics prepared by the preparation method according to any one of claims 1 to 7, characterized in that, The volume resistivity of the DNTF@Ni3(HHTP)2 composite energetic material is 1×10⁻⁶. 8 ~8×10 10 Ω·cm; the electrostatic accumulation of the DNTF@Ni3(HHTP)2 composite energetic material is -12 to -6 nC·g. -1 .

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