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Oxalyl dihydrazine nitrate metal complex suitable for solid propellant and preparation method of oxalyl dihydrazine nitrate metal complex

A technology of nitrate oxalyl dihydrazide and metal complex, which is applied in the preparation of hydrazide, nitrated acyclic/alicyclic/heterocyclic amine explosive compositions, attack equipment, etc., can solve the problem of poor safety performance and low self-energy level , the effect of improving the burning rate is not ideal, etc., to achieve the effect of good compatibility, high burning rate and smooth surface

Pending Publication Date: 2022-03-04
HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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  • Application Information

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Problems solved by technology

These fast combustibles have defects such as poor safety performance, or too low energy level, or unsatisfactory improvement in burning rate.

Method used

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  • Oxalyl dihydrazine nitrate metal complex suitable for solid propellant and preparation method of oxalyl dihydrazine nitrate metal complex
  • Oxalyl dihydrazine nitrate metal complex suitable for solid propellant and preparation method of oxalyl dihydrazine nitrate metal complex
  • Oxalyl dihydrazine nitrate metal complex suitable for solid propellant and preparation method of oxalyl dihydrazine nitrate metal complex

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preparation example Construction

[0050] The application also provides a preparation method of a class of oxalyl dihydrazide metal complexes, comprising the following steps:

[0051] Step (1), dissolving oxalodihydrazide in distilled water, heating at 85-95°C until dissolved and transparent to obtain an oxalodihydrazide solution with a molar concentration of 0.20-1.50 mol / L, adding nitric acid to adjust the pH value to 5-6 , adding dropwise a metal nitrate aqueous solution with a molar concentration of 0.30 to 1.00 mol / L, the metal nitrate being at least one of nickel nitrate, zinc nitrate, cobalt nitrate or chromium nitrate crystal hydrate to obtain a reaction solution, in the reaction solution, The molar ratio of oxalyl dihydrazine to metal nitrate is 3:1~3:1.2, after the dropwise addition, keep it at 85~95°C for 30min~300min, cool down to obtain solid oxalyldihydrazine nitrate metal complex;

[0052] Step (2), dissolving the oxalyl dihydrazide metal complex obtained in (1) in a polar solvent, the polar solven...

Embodiment 1

[0056] Dissolve 1.66g of oxalodihydrazide in 50ml of distilled water, heat to 85°C to dissolve and make it transparent, add dilute nitric acid dropwise to adjust the pH value to 5, add 15ml of 0.3mol / L nickel nitrate aqueous solution dropwise, and keep it at 85°C after the dropwise addition The reaction was continued for 30 minutes, and cooled naturally to obtain 4.62 g of nickel oxalyl dihydrazine nitrate complex with a purity of 96.4% and a yield of 61.2% as a light green solid.

[0057] Dissolve 4.62 g of nickel oxalyl dihydrazine nitrate obtained above in 25 g of methanol / water (volume ratio 3: 7) mixed solution, add 0.23 g of oxalyl dihydrazide mononitrate, and stir the mixed solution at 40°C for 15 min , step cooling, filter, get D 50 Nickel oxalodihydrazide nitrate with a thickness of about 121 μm has a purity of 99.2% and a final yield of 58.9%.

[0058] Characterization of nickel oxalyl dihydrazine nitrate:

[0059] Elemental analysis (Ni(C 2 N 4 h 6 o 2 ) 3 (N...

Embodiment 2

[0061] Dissolve 1.66g of oxalodihydrazine in 10ml of distilled water, heat to 90°C to dissolve and make it transparent, add dilute nitric acid dropwise to adjust the pH value to 6, add 9ml of 0.5mol / L cobalt nitrate aqueous solution dropwise, and keep at 90°C after the dropwise addition is completed After reacting for 60 minutes and cooling naturally, 4.45 g of cobalt oxalodihydrazine nitrate solid was obtained, with a purity of 97.3% and a yield of 58.9%.

[0062] Dissolve 4.45 g of cobalt oxalyl dihydrazine nitrate obtained above in 28 g of methanol / water (volume ratio 4: 6) mixed solution, add 0.36 g of oxalyl dihydrazide dinitrate, and stir the mixed solution at 50° C. for 30 min , step cooling, filter, get D 50 The cobalt oxalyl dihydrazide nitrate is about 135 μm in size, the purity of the cobalt oxalyl dihydrazide nitrate is 98.9%, and the final yield is 56.6%.

[0063] Characterization of cobalt oxalyl dihydrazine nitrate:

[0064] Elemental analysis (Co(C 2 N 4 h ...

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Abstract

According to the oxalyl dihydrazine nitrate metal complex and the preparation method thereof, reaction raw materials are selected, a reaction route is designed, reaction conditions and a proper crystallization additive are screened, and the oxalyl dihydrazine nitrate metal complex is obtained through a complexation reaction of oxalyl dihydrazine and metal nitrate. And a crystallization control agent is added, so that a series of oxalyl dihydrazine nitrate metal complexes suitable for the particle size of a solid propellant can be obtained. The complex is a novel energetic fast-burning substance, has the advantages of high burning rate, low sensitivity, good thermal stability, good compatibility with propellant components and the like, is mild in reaction and high in product yield in the preparation process, and has wide application prospects in the fields of energetic materials such as high-burning-rate propellants, weapon ammunition and civil blasting.

Description

technical field [0001] The application relates to a new type of energetic material suitable for solid propellants and propellants and explosives—oxalyl dihydrazine nitrate metal complex and a preparation method, which belong to the technical field of energetic materials. Background technique [0002] High-burning rate propellants can make solid rocket motors generate greater thrust in a short period of time, and can meet the requirements for propellant combustion performance of anti-tank missiles, air defense missiles, airborne missiles, interceptor missiles and high-speed kinetic energy bombs. Therefore, a substantial increase in burning rate is an urgent requirement for solid propellants in the development of rockets and missiles. [0003] At present, the technical approaches to increase the burning rate of solid propellants are mainly divided into physical methods and chemical methods. Among them, the chemical method is based on the high-speed decomposition reaction of p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C243/24C07C241/04C06B25/34C06D5/00
CPCC07C243/24C07C241/04C06B25/34C06D5/00
Inventor 雷晴丁宁何金选卢艳华张晓飞李涛颜炎陈豫红
Owner HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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