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Preparation method of hydroxylamine dinitramide

A technology of dinitramide hydroxylamine and dinitramide ammonium, which is applied in the field of energetic material-dinitramide hydroxylamine 2, can solve the problems of catalyst poisoning, low yield, methanol harmful to human body, etc., and achieve full reaction and high yield Effect

Active Publication Date: 2019-04-30
HUBEI INST OF AEROSPACE CHEMOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The defective of this method is as follows: the first, gained product purity is not high
Since potassium dinitramide and potassium chloride have a certain solubility in methanol, the prepared HADN contains a small amount of potassium ions and chloride ions, which are difficult to completely remove during post-treatment. When applied to liquid propellants, they will not only corrode Stainless steel pipes, valves, and can cause catalyst poisoning
The second, hydroxylamine hydrochloride is difficult to dissolve completely in the methanol of heat, so this method reaction is insufficient, and productive rate is low, and needs to carry out repeated distillation, extraction, purification, step is loaded down with trivial details, separation difficulty
Third, the methanol used in this method is harmful to the human body and does not meet the requirements of green environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1) Rinse the macroporous polystyrene sulfonic acid type cation exchange resin whose brand is 732 with distilled water, soak it for 5 hours, and then soak it 3 times with dilute hydrochloric acid with a mass fraction of 3%, soaking it for 5 hours each time, dilute hydrochloric acid each time The dosage is about 2 times the volume of the cationic resin, and finally soaked in distilled water 3 times to make the pH of the resin neutral. Then soak the resin in an aqueous solution of 0.2% dioctadecyldimethylammonium chloride at 70° C. for 4 hours. Take it out and put it into a glass mixed bed with an inner diameter of 2.5cm and a column height of 50cm to obtain a resin bed;

[0048] (2) preparation mass fraction is 40% dinitramide ammonium transparent aqueous solution 310g, passes through the resin bed that step (1) obtains with 30cm / h flow rate, until the dinitramide ammonium transparent aqueous solution flows, then use about 100ml distilled water to Rinse the resin bed to...

Embodiment 2

[0051] (1) Rinse the macroporous polystyrene sulfonic acid type cation exchange resin with the grade of 732 in distilled water, soak it for 10 hours, and then soak it with dilute hydrochloric acid with a mass fraction of 5%, soaking it for 10 hours each time, the amount of dilute hydrochloric acid It is 3 times that of the cationic resin, and finally soaked in distilled water 4 times to make the pH of the resin neutral. Then soak the resin in an aqueous solution of 0.5% dioctadecyldimethylammonium chloride at 80° C. for 8 hours. Take it out and put it into a glass mixed bed with an inner diameter of 1.5cm and a column height of 40cm to obtain a resin bed;

[0052] (2) preparation mass fraction is 360g of dinitramide ammonium transparent aqueous solution 360g, passes through the resin bed that step (1) obtains with flow rate 50cm / h, until dinitramide ammonium transparent aqueous solution flows out, then uses the distilled water of about 90ml Rinse the resin bed to neutral at t...

Embodiment 3

[0055] (1) Rinse the macroporous polystyrene sulfonic acid type cation exchange resin whose brand is 732 with distilled water, soak it for 15 hours, and then soak it with dilute hydrochloric acid with a mass fraction of 8% for 5 times, each soaking for 12 hours, the amount of dilute hydrochloric acid It is twice as much as the cationic resin, and finally soaked in distilled water for 5 times to make the pH of the resin neutral. The resin was then soaked in an aqueous solution of 0.8% by mass percentage of dioctadecyldimethylammonium chloride at 90° C. for 12 hours. Take it out and put it into a glass mixed bed with an inner diameter of 2.5cm and a column height of 50cm to obtain a resin bed;

[0056] (2) preparation mass fraction is 420g of dinitramide ammonium transparent aqueous solution 420g, passes through the resin bed that step (1) obtains with flow rate 80cm / h, until the dinitramide ammonium transparent aqueous solution flows out, then use the distilled water of about 1...

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PUM

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Abstract

The invention provides a preparation method of hydroxylamine dinitramide. The method comprises the following steps: an aqueous solution of ammonium dinitramide goes through a cation resin exchange column at a certain flow rate, and the obtained effluent is collected; and the collected effluent is dropwise added to a hydroxylamine solution at a normal temperature while stirring, and vacuum freeze-drying is carried out after the addition is completed in order to obtain the hydroxylamine dinitramide. The method has the advantages of environmental protection, harmlessness and high yield, and allows the purity of HADN to be higher than 99.5%, the content of nitrate radicals to be less than 0.1%, the content of metal ions to be less than 5 ppm and the content of sulfate radicals to be less than8 ppm.

Description

technical field [0001] The present invention relates to a kind of energetic material-dinitroamide hydroxylamine (chemical formula NH 2 OH·HN(NO 2 ) 2 , abbreviated as HADN), the preparation method belongs to the field of material preparation. Background technique [0002] The space on-orbit propulsion system used by spacecraft has high cleanliness requirements for propellant combustion products, and pollution and corrosion of spacecraft instruments and equipment are not allowed. At present, the commonly used monopropellant for attitude control of satellite thrusters is hydrazine, and its biggest disadvantages are high toxicity, strong corrosiveness, and environmental pollution. [0003] The specific impulse of the unit hydrazine propellant is 200s, the specific impulse of the ammonium dinitramide (ADN)-based liquid monopropellant exceeds 230s, and the density specific impulse is 1.4 times that of the hydrazine propellant. The ADN non-toxic propulsion system represents th...

Claims

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Application Information

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IPC IPC(8): C01B21/087C06D5/04
CPCC01B21/087C06D5/04
Inventor 雷晴卢艳华何金选任晓婷叶丹阳丁宁
Owner HUBEI INST OF AEROSPACE CHEMOTECH
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