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A kind of method adopting emulsion template to control dinitramide ammonium particle size

A technology of ammonium dinitramide and emulsion template, which is applied in the production of compressed gas, explosives, attack equipment, etc., can solve problems such as potential safety hazards, recrystallization of ammonium dinitramide, affecting product appearance, etc. Effect

Active Publication Date: 2021-04-13
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But, adopt above method to prepare dinitramide ammonium still there are following deficiencies: (1) preparation process needs to add emulsion stabilizer, unfavorable to the preparation high-quality ammonium dinitramide; (2) preparation and aftertreatment process all need to use a large amount of solvents, The residual solvent in the product may lead to the recrystallization of ammonium dinitramide, thereby affecting the appearance of the product; (3) ammonium dinitramide is in a high-temperature molten state, which brings great safety hazards to the operation

Method used

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  • A kind of method adopting emulsion template to control dinitramide ammonium particle size
  • A kind of method adopting emulsion template to control dinitramide ammonium particle size
  • A kind of method adopting emulsion template to control dinitramide ammonium particle size

Examples

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Embodiment 1

[0028] This embodiment provides a kind of method that adopts emulsion template to control the particle size of dinitramide ammonium, and this method specifically comprises the following steps:

[0029] Step 1, surface modification of template graphene oxide

[0030] Add 0.1g of graphene oxide into 100mL of deionized water; dissolve 1.0g of dodecylamine in 100mL of absolute ethanol by mass; mix the above two parts, stir at 90°C for 24h, and condense the reaction system to reflux, Filtrate, ultrasonically disperse the filtered product in 100 mL of absolute ethanol for 30 minutes, and filter to obtain the precipitated reaction product; repeat the above process 4 times, and vacuum-dry the filtered product at 60°C to obtain alkylamine-modified graphene oxide;

[0031] Step 2, preparation of water-in-oil emulsion

[0032] Ultrasonically disperse 0.005g of alkylamine-modified graphene oxide in 10mL of toluene for 30min, ultrasonic power 1000W, frequency 200Hz, temperature 30°C; add ...

Embodiment 2

[0038] This example provides a method for controlling the particle size of ammonium dinitramide by using an emulsion template. Steps 1, 2, and 3 of this method are the same as those in Example 1, except for Step 4.

[0039] Step 4, the preparation of ammonium dinitramide powder

[0040] Let the emulsion stand at 20°C for 24h, remove the unemulsified toluene solvent in the upper layer of the emulsion, then place the product in a vacuum freeze dryer, and dry it at -50°C, 10Pa vacuum environment for 5h to obtain alkylamine-modified graphene-coated Ammonium dinitramide solid phase composite powder.

Embodiment 3

[0042] This embodiment provides a kind of method that adopts emulsion template to control the particle size of dinitramide ammonium, and this method specifically comprises the following steps:

[0043] Step 1, template agent silica surface modification

[0044] Add 1.0 g of silicon dioxide to chloroform / oleic acid (molar ratio 1:2), stir for 3 h, and then add methanol to the above mixture to obtain a precipitate of silicon dioxide nanoparticles. The obtained product was dispersed in chloroform, and then methanol was added to precipitate, and the above operation was repeated 4 times to remove excess oleic acid. Then the last precipitated product was dried at 120° C. to obtain oleic acid hydrophobically modified silica.

[0045] Step 2, preparation of water-in-oil emulsion

[0046] Ultrasonically disperse 0.005g of oleic acid-modified silica in 10mL of toluene for 30min, ultrasonic power is 1000W, frequency is 200Hz, temperature is 30°C; The above two dispersions were mixed a...

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Abstract

The invention discloses a method for controlling the particle size of ammonium dinitramide by using an emulsion template, which can simultaneously solve the problems of controlling the particle size of ammonium dinitramide in moisture absorption and spheroidization. In the method, deionized water is used as ammonium dinitramide solvent, functional filler is used as a template agent, and a solvent insoluble in ammonium dinitramide is used as a dispersion medium for template agent, and a water-in-oil emulsion system is prepared through the action of a high-speed homogenizer at normal temperature. The solvent is removed by vacuum drying, so as to obtain the ammonium dinitramide composite powder coated with the template agent. By adjusting the oil / water volume ratio, the concentration of ammonium dinitramide aqueous solution, the concentration of template agent dispersion, the mass ratio of template agent / ammonium dinitramide and other parameters to control the droplet size of ammonium dinitramide aqueous phase, and finally realize the spherical dinitramide Control of particle size of ammonium amide powder. The emulsion template method strategy provided by the invention can simultaneously adjust the particle size and hygroscopicity of ammonium dinitramide. The object of the emulsion template method is ammonium dinitramide aqueous solution, and the experimental operation is simple and safe.

Description

technical field [0001] The invention relates to a method for controlling the particle size of ammonium dinitramide by using an emulsion template, and belongs to the technical field of material shape control. Background technique [0002] As an ionic high-energy oxidant, ammonium dinitramide does not contain carbon and halogen in the molecule. Adding it to the propellant can meet the requirements of high energy, low characteristic signal and clean combustion of the engine charge. Ammonium dinitramide, as a green and environment-friendly oxidant, is considered to be an ideal substitute for traditional propellant oxidizers such as ammonium perchlorate and ammonium nitrate. However, the ammonium dinitramide synthesis products are mostly needle-shaped, flaky and other high-defect crystals, with high sensitivity, strong hygroscopicity, easy to agglomerate and agglomerate, difficult to disperse, low filling rate in the propellant, and high viscosity of the slurry. It affects the p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C06B31/00C06B45/32C06B21/00C06D5/00
CPCC06B21/00C06B31/00C06B45/32C06D5/00
Inventor 闫宁边城李宏岩栾涛时艺娟
Owner XIAN MODERN CHEM RES INST
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