Hollow ultrafine ammonium perchlorate and preparation method thereof

A technology of ammonium perchlorate and ammonium chlorate, which is applied in the direction of perchloric acid and perchlorate, can solve the problems of being unable to prepare hollow ultrafine ammonium perchlorate materials, and achieve good dispersion and regularity, Easy operation and uniform particle size

Inactive Publication Date: 2012-10-10
NANJING NORMAL UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The above methods all couple or integrate the anti-solvent-recrystallization method with other methods to...

Method used

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  • Hollow ultrafine ammonium perchlorate and preparation method thereof
  • Hollow ultrafine ammonium perchlorate and preparation method thereof

Examples

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Embodiment 1

[0027] Hollow superfine ammonium perchlorate and preparation method thereof, the steps are as follows:

[0028] First, at room temperature, take a certain amount of spherical ammonium perchlorate with a size of about 250 μm and dissolve it in an equal volume of N,N-dimethylformamide (DMF) / acetone mixed solvent to make perchloric acid ammonium saturated solution; then add 10 ml of ammonium perchlorate saturated solution to 200 ml of ethyl acetate, keep stirring at 1000 rpm during the addition process, ammonium perchlorate crystals will crystallize out due to supersaturation; finally pump the mixture Filter, wash with ethyl acetate, and dry the product in an oven at 80°C to obtain hollow ultrafine ammonium perchlorate.

[0029] The electron micrograph of the hollow ultrafine ammonium perchlorate that makes is as follows figure 1 and figure 2 , with a cubic hollow shape, a multi-layer cavity structure in the middle of the particle, and a particle size of about 10 μm to 15 μm. ...

Embodiment 2

[0032] Hollow superfine ammonium perchlorate and preparation method thereof, the steps are as follows:

[0033] First, at 40 °C, a certain amount of spherical ammonium perchlorate with a size of about 250 μm was dissolved in a mixed solvent of DMF / acetone with a volume ratio of 3:1 to prepare a saturated solution of ammonium perchlorate; then 10 Add the saturated ammonium perchlorate solution in 250 ml to 250 ml of ethyl acetate, keep the stirring speed of 1500 rpm during the addition process, the ammonium perchlorate crystals will crystallize out due to supersaturation; finally the mixed solution is suction filtered, washed with ethyl acetate, The product is dried in an oven at 50-150 °C to obtain hollow ultrafine ammonium perchlorate.

[0034] The prepared hollow ultrafine ammonium perchlorate has a cubic hollow shape, and the middle part of the particle has a multi-layer cavity structure, and the particle size is about 5 μm to 10 μm.

[0035]

Embodiment 3

[0037] Hollow superfine ammonium perchlorate and preparation method thereof, the steps are as follows:

[0038] First, at 30 °C, a certain amount of spherical ammonium perchlorate with a size of about 250 μm was dissolved in a mixed solvent of DMF / acetone with a volume ratio of 1:4 to prepare a saturated solution of ammonium perchlorate; then 10 Add 1 ml ammonium perchlorate saturated solution to 100 ml ethyl acetate, keep the stirring speed of 2000 rpm during the addition process, ammonium perchlorate crystals will crystallize out due to supersaturation; finally the mixed solution is suction filtered, washed with ethyl acetate, The product is dried in an oven at 50-150 °C to obtain hollow ultrafine ammonium perchlorate.

[0039] The prepared hollow ultrafine ammonium perchlorate has a cuboid hollow shape, the middle part of the particle has a multi-layer cavity structure, and the particle size is about 10 μm to 20 μm.

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Abstract

The invention relates to a hollow ultrafine ammonium perchlorate and a preparation method thereof. The ammonium perchlorate is a material with a multilayer cavity structure in the middle part and has the particle size of 1-100mu m. The preparation method adopts a desolvation-recrystallization method, and comprises the following steps of: (1) dissolving the ammonium perchlorate into an N,N-dimethyl formamide/ acetone mixed solvent to prepare a saturated solution; (2) under the conditions of certain stirring speed and solvent-anti solvent volume ratio, adding the ammonium perchlorate saturated solution into anti solvent ethyl acetate, and separating out the ammonium perchlorate by crystallization when supersaturation; and (3) after crystallization, filtering, washing and drying the product, thus obtaining the hollow ultrafine ammonium perchlorate. The ammonium perchlorate is an ultrafine powder material and has hollow morphology, thus being good in dispersity and ordered in structure and effectively improving the performance of a solid propellant. The desolvation-recrystallization method is simple, safe and convenient in operation.

Description

technical field [0001] The invention belongs to the technical field of energetic materials, and relates to an ultrafine particle and a preparation method thereof, in particular to a hollow ultrafine ammonium perchlorate and an antisolvent-recrystallization method thereof. Background technique [0002] In the field of solid propellants, ammonium perchlorate (AP) is one of the most commonly used oxidizers in solid propellants, and its weight ratio in solid propellants is as high as 60 to 80%. Therefore, the performance of solid propellant will change with the change of ammonium perchlorate characteristics, especially the particle size and morphology of AP. Ammonium perchlorate with ultra-fine or / and hollow morphology with a high specific surface area can effectively improve the performance of the propellant, and the smaller the particle size and the more hollow structures, the better the performance of the propellant. [0003] At present, various traditional methods for prepa...

Claims

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Application Information

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IPC IPC(8): C01B11/18
Inventor 马振叶赵凤起张利雄仪建华纪明卫
Owner NANJING NORMAL UNIVERSITY
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