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Preparation method for torispherical ammonium dinitramide crystal

An ammonium dinitramide, quasi-spherical technology, applied in the generation of compressed gas, chemical instruments and methods, selection of crystallization auxiliary conditions, etc.

Active Publication Date: 2019-11-08
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can obtain ADN with better morphology, it introduces the inert substance NaF at the same time.

Method used

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  • Preparation method for torispherical ammonium dinitramide crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The first step is to configure the ADN solution, mix 1 gram of ADN with 10ml of methanol and 2ml of butyl acetate in a 100ml round bottom flask.

[0022] In the second step, put magnets into the flask and heat in a water bath at 40° C., stir and dissolve for 30 minutes with magnets at a stirring speed of 300 r / min to obtain an ADN solution.

[0023] The third step is to transfer the ADN solution to a 100ml beaker, pour ten times the non-solvent dichloromethane of the mixed solvent into the ADN solution, and let it stand for 2 hours in an undisturbed state, separate layers after standing, and filter with suction. The sample obtained after suction filtration was dried in a vacuum oven at 50° C. for 2 hours to obtain ADN crystals.

Embodiment 2

[0025] The first step is to configure the ADN solution, mix 1 gram of ADN with 10ml of ethanol and 2ml of methyl formate in a 100ml round bottom flask.

[0026] In the second step, put magnets into the flask and heat in a water bath at 40° C., stir and dissolve for 30 minutes with magnets at a stirring speed of 300 r / min to obtain an ADN solution.

[0027] The third step is to transfer the ADN solution to a 100ml beaker, pour ten times the non-solvent dichloromethane of the mixed solvent into the ADN solution, and let it stand for 2 hours in an undisturbed state, separate layers after standing, and filter with suction. The sample obtained after suction filtration was dried in a vacuum oven at 50° C. for 2 hours to obtain ADN crystals.

Embodiment 3

[0029] The first step is to configure the ADN solution, mix 1 gram of ADN with 10ml of isopropanol and 2ml of ethyl acetate in a 100ml round bottom flask.

[0030] In the second step, put magnets into the flask and heat in a water bath at 40° C., stir and dissolve for 30 minutes with magnets at a stirring speed of 300 r / min to obtain an ADN solution.

[0031] The third step is to transfer the ADN solution to a 100ml beaker, pour ten times the non-solvent dichloromethane of the mixed solvent into the ADN solution, and let it stand for 2 hours in an undisturbed state, separate layers after standing, and filter with suction. The sample obtained after suction filtration was dried in a vacuum oven at 50° C. for 2 hours to obtain ADN crystals.

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Abstract

The invention relates to a preparation method for a torispherical ammonium dinitramide (ADN) crystal. The method for preparing the torispherical ADN crystal is realized by testing different proportions and different temperatures of ADN and a solvent. The method is characterized by comprising the following steps: preparing an ADN solution at a certain temperature in a certain proportion, and addingnon-solvent dichloromethane so as to obtain the torispherical ADN crystal. The torispherical ADN crystal prepared by using the preparation method provided by the invention is free of addition of anyinert substances. The ADN crystal has a regular morphology and a torispherical crystal structure. Compared with a crystal obtained by using a method in the prior art, the torispherical ADN crystal prepared by using the preparation method provided by the invention is greatly reduced in impact sensitivity and has low hygroscopicity.

Description

technical field [0001] The invention relates to a preparation method of ammonium dinitramide crystal, which belongs to the field of material processing and preparation. Background technique [0002] Ammonium dinitramide (ADN) has received widespread attention since it was first synthesized by the former Soviet Union in the 1970s. Compared with the traditional oxidant ammonium perchlorate (AP), ADN has the advantages of high energy, large amount of gas, clean gas, low toxicity, and environmental friendliness. It can greatly increase the energy of solid propellants, reduce the characteristic signal, and significantly improve the Comprehensive performance. Conventional ADN crystals are needle-like, have high hygroscopicity and high sensitivity, and are difficult to be used in solid propellants and mixed explosives. Mechanical sensitivity is an important indicator of energetic materials, which is greatly affected by the morphology of crystals. In the case of the same crystal ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01C1/00B01D9/02C06B31/00C06D5/00
CPCC01C1/00B01D9/005C06B31/00C06D5/00C01P2004/32
Inventor 杨荣杰巩丽李建民
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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