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A method for the separation and preparation of high-energy oxidant ammonium dinitramide

A technology of ammonium dinitramide and oxidant, applied in chemical instruments and methods, ammonia compounds, inorganic chemistry, etc., can solve the problems of difficult removal, difficult separation and purification of ADN, high production cost, etc., and achieve complex purification process, safe and reliable Contaminants, the effect of simple methods

Active Publication Date: 2022-04-01
BEIJING INSTITUTE OF TECHNOLOGYGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The intermediate product HN(NO2)2 of this method is unstable under acidic conditions and will gradually decompose. It is necessary to continuously sample and measure the concentration of HN(NO2)2 in the solution to reach the maximum before the next step of neutralization operation, so the operation process is more cumbersome. In addition, a large amount of nitrate and sulfate by-products can be produced in the synthesis process of this method, which is difficult to remove, resulting in the difficulty of ADN separation and purification, and various separation and purification methods can not obtain high-purity ADN products. The purification method currently used, The production cost is high, a large amount of solid or liquid waste is generated, and the environment is seriously polluted

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1, this example provides a method for the separation and preparation of high-energy oxidant ammonium dinitramide

[0025] First, put 200G reverse-phase chromatography filler PS / DVB (SKN10P) filler into a 500ml chromatography column, use 2000ml purified water to press the column to prepare for sample loading, and the flow rate of purified water into the column is 2000ml / H. Dispersed polymer chromatographic packing (PS / DVB) packing is based on styrene / divinylbenzene (PS / DVB) or acrylate polymer, produced by patented technology, covering normal phase, reversed phase, ion exchange, affinity, Chromatography such as product exclusion. The specific surface area and particle size and pore size distribution of this series of products have been precisely controlled, which makes this series of products more selective and can meet various separation and purification requirements from laboratory analysis and testing to pilot scale and industrial scale production. It has a s...

Embodiment 2

[0030] Example 2, this example provides a method for the separation and preparation of ammonium dinitramide, a high-energy oxidant

[0031] First, put 200G, 40um capped C18 reverse phase chromatography filler into a 400ml chromatography column, use 1500ml water to press the column to prepare for sample loading, the flow rate of purified water into the column is 1000ml / H, and the particle size of the filler is 10~150um, preferably 40um reverse phase packing with uniform particle size. In this embodiment, the choice of 40um packing is mainly due to low price, low cost, low requirements for column packing, low requirements for column packing equipment, and simple operation.

[0032] Then, the crude product containing 7.21 grams of ADN synthesized by the mixed acid method was added with water to make up to 100ml, and was pumped into the column chromatography system at a feed flow rate of 500ml / H per hour for loading;

[0033] Rinse the chromatographic column after loading with 80...

Embodiment 3

[0036] Example 3, this example provides a method for the separation and preparation of ammonium dinitramide, a high-energy oxidant

[0037] First, put 200G, 40um capped C18 reverse phase chromatography filler into a 400ml chromatography column, use 1500ml water to press the column to prepare for sample loading, and the flow rate of purified water into the column is 1000ml / H;

[0038] Then, the ADN crude product containing 7.67 grams synthesized by the mixed acid method was added with water to make the volume to 100ml, and was pumped into the column chromatography system at a feed flow rate of 500ml / H per hour for loading;

[0039] Then wash the chromatographic column after loading with 800ml of purified water (containing 0.5‰ acetic acid), and the washing speed is selected as 150ml / H. The main purpose of adding acetic acid is to improve the resolution of ADN from impurities.

[0040] Use 10% methanol (containing 0.5‰ acetic acid) aqueous solution to elute the loaded chromatog...

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Abstract

The invention belongs to the technical field of ammonium dinitramide purification and application, and in particular relates to a method for the separation and preparation of ammonium dinitramide, a novel high-energy oxidant. The method comprises the following effective steps: firstly, adding the reverse phase chromatography filler into the chromatographic column for use; using ammonium sulfamate as a raw material, the ADN crude product synthesized by the mixed acid method is prepared for use; the ADN-containing crude product synthesized by the mixed acid method Add water to constant volume, and pump it into the chromatographic column system according to the flow rate to load the sample; wash the ADN crude product chromatographic column with purified water after the sample is loaded; / water to elute the loaded ADN crude product chromatography column; the elution process is detected and analyzed by high-performance liquid chromatography (HPLC), and high-purity ADN fractions are collected; the collected high-purity ADN fractions are concentrated and then crystallized at low temperature , to obtain high-purity ADN products. The method of the invention is simple and has an operation scheme. It is safe, reliable and produces no pollutants, and is suitable for large-scale promotion and use.

Description

technical field [0001] The invention belongs to the technical field of ammonium dinitramide purification and application, and in particular relates to a method for the separation and preparation of ammonium dinitramide, a high-energy oxidant. 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 ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01C1/00C06D5/00C06B31/00
CPCC01C1/00C06D5/00C06B31/00C01P2006/80
Inventor 李玉川朱海洋孙海云刘颖慧苗香艳张培训崔峰秦庆洪
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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