A kind of full deuterated ammonium dinitramide and preparation method thereof

Abstract

The invention discloses a fully deuterated ammonium dinitramide and a preparation method thereof, belonging to the technical field of synthesis of deuterated energetic materials. The invention is simple in purification, and high-purity products can be obtained without adsorption and solvent elution; the product does not contain metal ions such as potassium ions, does not cause catalyst poisoning during use, and can increase the application range of the product. The invention judges the progress of the reaction by measuring the pH of the solution, and the judgment method of the reaction end point is simple; the deuterated ammonia gas can be recycled after being collected, the waste of deuterated raw materials is reduced, and the production cost is reduced. Compared with ordinary ammonium dinitramide, the initial decomposition temperature of perdeuterated ammonium dinitramide is increased to about 150°C, and the thermal stability is significantly increased; the crystal density is increased, and the energy characteristics are also significantly improved. The invention can realize the preparation of perdeuterated ammonium dinitramide, and provides a reference for the industrial production of perdeuterated ammonium dinitramide.

Description

technical field [0001] The invention relates to a fully deuterated ammonium dinitramide and a preparation method thereof, belonging to the synthesis technology of deuterated energetic materials. Background technique [0002] Ammonium dinitramide is code-named ADN, which has the characteristics of high oxygen content and high heat of formation, so it can be used as an explosive and is often used as an oxidant for solid propellants. Compared with ammonium perchlorate, the molecular structure of ammonium dinitramide does not contain chlorine, and the combustion product is smokeless, which can increase the concealment of missile launch and reduce environmental pollution. The specific impulse and characteristic velocity of ammonium dinitramide are 2003N s / kg and 1282.6m / s respectively, which are much higher than ammonium perchlorate. By replacing ammonium perchlorate with ammonium dinitramide, the thrust of the aerospace booster can be increased by 14%, and the load can be incre...

AI Technical Summary

Problems solved by technology

The intermediate product HN(NO 2 ) 2 It is unstable under acidic conditions and will gradually decompose. It is necessary to continuously take samples to measure the HN(NO 2 ) 2 When the concentration reaches the maximum, the next step of neutralization operation can be carried out, so the operation process is comparatively loaded down with trivial details; in addition, by-products such as ammonium nitrate and ammonium sulfate need to be removed by adsorption separation and solvent elution, which increases the difficulty of preparation (WO97 / 06099[ P].1997-02-20.)

In 2005, VOERDE disclosed an improved production method, which neutralized the intermediate product HN(NO 2 ) 2 N-amidinourea dinitramide salt is generated, which is subsequently reacted with potassium hydroxide to generate KN(NO 2 ) 2 , KN(NO 2 ) 2 Carry out ion exchange with ammonium sulfate again to obtain product dinitramide ammonium; This technological method has significantly reduced the consumption of raw material, has shortened reaction time, but contains a large amount of potassium ions in the dinitramide ammonium produced by this method, will be lost during use Cause catalyst poisoning and deactivation (WO2005 / 070823[P].2005-08-04.)

The above methods are all methods for preparing non-deuterated ammonium dinitramide, and the preparation of non-deuterated ammonium dinitramide cannot be completed by simply replacing the raw materials of the above method