An inner salt type high heat-resistant explosive and a preparation method thereof

Abstract

The application discloses an inner salt type high-heat-resistant explosive and a preparation method thereof, and 2,6-diamino-9-amino-3,5-dinitrodipyrazolotriazine, namely ZDPT, is prepared. In addition to the performance advantages of high energy and high heat resistance, the ZDPT also has the advantages of simple synthesis method and low process cost. Single crystal X-ray diffraction test shows that the ZDPT has a unique inner salt type and three-fused ring skeleton structure and is insoluble in water and conventional organic solvents. The thermal decomposition temperature of the ZDPT is as high as 380 DEG C, the actual measured impact sensitivity is greater than 40 J, the friction sensitivity is greater than 360 N, and the ZDPT has great application potential in the field of high-energy heat-resistant explosives.

Description

Technical Field

[0001] This invention relates to the field of energetic materials technology, and in particular to an internal salt type high heat-resistant explosive and its preparation method. Background Technology

[0002] Heat-resistant explosives have important applications in petroleum exploration and advanced weaponry. With the development of modern weaponry, increasingly higher requirements are being placed on the performance of heat-resistant explosives. However, the low energy of existing heat-resistant explosives seriously restricts the development of weaponry. Developing new high-energy heat-resistant explosives is an urgent need for the development of weaponry. In response to this situation, various military industrial units and related colleges and universities in China have carried out a great deal of work on the creation of high-energy heat-resistant explosives. At present, there are two main ideas for designing and synthesizing high-energy heat-resistant explosives: (1) constructing a single-ring explosive with a TATB-like skeleton structure; (2) constructing a multi-ring explosive with a large π-electron conjugated system. Based on the above design ideas, a large number of new explosives with novel structures and excellent performance have been synthesized in recent years. Some of these also have high energy and high heat resistance. However, the new explosives designed and synthesized using this strategy generally have the defect of complex synthesis process. Summary of the Invention

[0003] The purpose of this invention is to address the problems of existing heat-resistant explosives having low energy, failing to meet the needs of modern weaponry development, and having complex synthesis processes. This invention provides an internal salt-type high heat-resistant explosive and its preparation method. Using 3,5-diamino-4-nitropyrazole as a raw material, this invention develops a simple synthesis process with mild reaction conditions and high yield for an internal salt-type high heat-resistant explosive. Furthermore, it synthesizes a novel high heat-resistant explosive, ZDPT, with excellent comprehensive performance, which has enormous application potential in the field of heat-resistant explosives.

[0004] The present invention achieves the above objectives through the following technical solutions:

[0005] An internal salt type high heat-resistant explosive, the structural formula of which is as follows:

[0006]

[0007] In another aspect, this invention provides a method for preparing an internal salt type high heat-resistant explosive, which is carried out through the following synthetic route:

[0008] A further proposed method includes the following steps in the preparation process:

[0009] Add 3,5-diamino-4-nitropyrazole to a sufficient amount of organic solvent and stir continuously until completely dissolved. Then add an inorganic alkaline aqueous solution, followed by cyanogen bromide solution. React at room temperature for 40-90 minutes. After the reaction is complete, stop stirring and an orange powder precipitate will form. Under ice bath conditions, add the orange precipitate to concentrated hydrochloric acid and stir for 30-90 minutes. Filter and dry to obtain the target product ZDPT.

[0010] A further embodiment is that the organic solvent includes one or more of DMF and DMSO.

[0011] A further embodiment is that the inorganic base includes one or more of LiOH, NaOH, and KOH.

[0012] A further embodiment is that the molar ratio of the 3,5-diamino-4-nitropyrazole, the inorganic base, and the cyanogen bromide is 2:1.80-2.10:0.9-1.1.

[0013] The beneficial effects of this invention are as follows:

[0014] This invention discloses an internal salt-type high-heat-resistant explosive and its preparation method, producing 2,6-diamino-9-amino-3,5-dinitropyrazolotriazine, or ZDPT. Besides its high energy and high heat resistance, ZDPT also boasts advantages such as a simple synthesis method and low processing cost. Single-crystal X-ray diffraction analysis shows that ZDPT possesses a unique internal salt-type, triple-fused-ring framework structure and is insoluble in water and common organic solvents. ZDPT exhibits a thermal decomposition temperature as high as 380℃, a measured impact sensitivity greater than 40J, and a friction sensitivity greater than 360N, demonstrating significant application potential in the field of high-energy heat-resistant explosives. Attached Figure Description

[0015] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0016] Figure 1 The high heat-resistant explosive ZDPT of this invention 1 HNMR spectrum.

[0017] Figure 2 This is a molecular structure diagram of the high heat-resistant explosive ZDPT of the present invention.

[0018] Figure 3 This is the TG-DSC diagram of the high heat-resistant explosive ZDPT of this invention. Detailed Implementation

[0019] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be described in detail below. Obviously, the described embodiments are merely some embodiments of this invention, and not all embodiments. Based on the embodiments of this invention, all other implementation methods obtained by those skilled in the art without creative effort are within the scope of protection of this invention.

[0020] Example 1. Synthesis of ZDPT, a high-heat-resistant explosive

[0021] 2.88 g of 3,5-diamino-4-nitropyrazole was weighed and dissolved in 30 mL of N,N-dimethylformamide. After complete dissolution, 20 mL of 1 M KOH aqueous solution was added, followed by 20 mL of 0.5 M cyanoacetonitrile bromide solution. The mixture was stirred at room temperature for 40 minutes. After the reaction was complete, stirring was stopped, and a large amount of orange powder precipitate formed. Under ice bath conditions, the orange precipitate was added to 20 mL of concentrated hydrochloric acid and stirred for 30 minutes. After filtration and drying, the target product ZDPT was obtained, with a yield of approximately 62%. The test results are shown in […]. Figures 1-3 .

[0022] Example 2. Synthesis of ZDPT, a high-heat-resistant explosive

[0023] 2.88 g of 3,5-diamino-4-nitropyrazole was weighed and dissolved in 30 mL of N,N-dimethylformamide. After complete dissolution, 20 mL of 1 M NaOH aqueous solution was added, followed by 20 mL of 0.5 M cyanoacetonitrile bromide solution. The mixture was stirred at room temperature for 40 minutes. After the reaction was complete, stirring was stopped, and a large amount of orange powder precipitate formed. Under ice bath conditions, the orange precipitate was added to 20 mL of concentrated hydrochloric acid and stirred for 30 minutes. After filtration and drying, the target product ZDPT was obtained, with a yield of approximately 56%.

[0024] Example 3. Synthesis of ZDPT, a high-heat-resistant explosive

[0025] 2.88 g of 3,5-diamino-4-nitropyrazole was weighed and dissolved in 30 mL of N,N-dimethylformamide. After complete dissolution, 20 mL of 1 M KOH aqueous solution was added, followed by 20 mL of 0.5 M N,N-dimethylformamide bromide solution. The mixture was stirred at room temperature for 40 minutes. After the reaction was complete, stirring was stopped, and a large amount of orange powder precipitate formed. Under ice bath conditions, the orange precipitate was added to 20 mL of concentrated hydrochloric acid and stirred for 30 minutes. After filtration and drying, the target product ZDPT was obtained, with a yield of approximately 60%.

[0026] This invention prepares 2,6-diamino-9-amino-3,5-dinitropyrazolotriazine, or ZDPT, which solves the problem of low energy in existing heat-resistant explosives. The ZDPT synthesis process is simple, overcoming the complexity of existing heat-resistant explosive synthesis processes. ZDPT's excellent overall performance and simple synthesis process make it of significant practical application value.

[0027] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims. It should also be noted that the various specific technical features described in the above embodiments can be combined in any suitable manner without contradiction. To avoid unnecessary repetition, the present invention will not describe the various possible combinations separately. Furthermore, various different embodiments of the present invention can also be arbitrarily combined, as long as they do not violate the spirit of the present invention, they should also be considered as the content disclosed in the present invention.

Claims

1. An inner salt type high heat-resistant explosive, having the following structural formula: 。 2. The method for preparing an internal salt type high heat-resistant explosive as described in claim 1, characterized in that, Prepared by the following synthetic route: .

3. The method for preparing an internal salt type high heat-resistant explosive as described in claim 1, characterized in that, comprising the following steps: 3,5-diamino-4-nitro pyrazole is added to a sufficient amount of organic solvent, continuously stirred, after complete dissolution, an aqueous solution of inorganic base is added, the inorganic base is selected from one or more of KOH, NaOH, then cyanogen bromide solution is added, and the reaction is carried out at room temperature for 40-90 minutes; after the reaction is completed, the stirring is stopped, and orange powder precipitate is separated out; under ice bath conditions, the orange precipitate is added to concentrated hydrochloric acid, stirred for 30-90 minutes, filtered, and dried to obtain the target product.

4. The method of claim 3, wherein the inner salt type high heat-resistant explosive is prepared by adding 0.1 to 0.3 parts by weight of the compound of formula (I) to 100 parts by weight of the inner salt type high heat-resistant explosive. The organic solvent is one or more of DMF, DMSO.

5. The method of claim 3, wherein the inner salt type high heat-resistant explosive is prepared by adding 0.1 to 0.3 parts by weight of the compound of formula (I) to 100 parts by weight of the inner salt type high heat-resistant explosive. The mass ratio of 3,5-diamino-4-nitro pyrazole, inorganic base and cyanogen bromide is 2:1.80~2.10:0.9~1.1.

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