Method for preparing micro-ammonium perchlorate

An ammonium perchlorate and fine technology, applied in the directions of ammonium perchlorate composition, perchloric acid, perchlorate, etc., can solve the problems of high cost and high equipment requirements, and achieve flexible output, flexible adjustment, and continuous reaction. The effect of stability

Active Publication Date: 2016-01-20
NANJING UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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Method used

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  • Method for preparing micro-ammonium perchlorate
  • Method for preparing micro-ammonium perchlorate
  • Method for preparing micro-ammonium perchlorate

Examples

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example 1

[0029] A flow-focused micro-mixer consisting of an imperial Φ1 / 64 stainless steel pipe as the inner channel, that is, the inner diameter of the inner channel is about 0.3mm, and a metric Φ0.5mm FEP tube as the outer channel, that is, the inner diameter of the outer channel is about 0.5mm. The residence time of the total material in the outer channel is 0.6s, ethyl acetate is used as anti-solvent, and the volume ratio of saturated solution to anti-solvent is 1:20. The ultrasonic power is 100W, the ultrasonic frequency is 40KHz, and the ultrasonic water temperature is 13°C.

[0030] Mix 0.5 g of ammonium perchlorate, 10 ml of methanol and 0.1% sodium lauryl sulfate based on the total mass of ammonium perchlorate and methanol to prepare a clear solution. Firstly, ethyl acetate enters the outer channel at a flow rate of 40ml / min, and the ultrasound is turned on. The methanol solution was delivered to the inner channel at a flow rate of 2 ml / min. The resulting sample (denoted as ...

example 2-4

[0032] Experiments were carried out in the same manner as in Example 1. By fixing the inner diameter of the outer channel and changing the inner diameter of the inner channel, the spacing between the inner and outer channels of the flow-focusing micromixer was changed to 0.24, 0.4, and 0.44, respectively. The ammonium perchlorate crystals obtained successively are A2, A3, and A4. From the scanning electron microscope pictures of the obtained crystals, it can be seen that the crystal shape of A2 is regular and cuboid, the average particle size is 0.58 μm, and the particle size distribution is 0.34-1.01 μm. The crystal morphology of A3 is cuboid, the average particle size is 0.59 μm, and the particle size distribution is 0.23-1.07 μm. The crystal morphology of A4 is cuboid, the average particle size is 0.66 μm, and the particle size distribution is 0.35-1.1 μm. It can be seen that the channel spacing of the flow focusing micro-mixer has a great influence on the particle size of...

example 5

[0034] Experiments were carried out using the same experimental method as in Example 1, and the inner diameter of the inner channel was changed from 0.3 mm to 0.1 mm when the distance between the inner and outer channels was fixed at 0.2 mm. From the scanning electron microscope image of the product, it can be seen that the crystal morphology of A5 is cuboid, the average particle size is 0.41 μm, and the particle size distribution is 0.2-0.68 μm. It can be seen that when the distance between the inner and outer channels of the flow-focusing type is fixed, the average particle size of ammonium perchlorate crystals decreases as the inner diameter of the inner channel decreases.

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Abstract

The invention relates to a method for preparing micro-ammonium perchlorate. The method comprises the specific steps that an ammonium perchlorate saturated solution containing a surface active agent is prepared; an anti-solvent is conveyed to enter an external channel of a flowing focused type micro-mixer, ultrasound is started, a saturated solution is conveyed to enter an internal channel of the flowing focused type micro-mixer to be mixed with the anti-solvent; the obtained product is filtered and dried to obtain the micro-ammonium perchlorate with the good dispersity. The inner diameter of the internal channel, the distance between the internal channel and the external channel, the standing time of total materials inside the external channel, the volume ratio of the solvent to the saturated solution to the anti-solvent, ultrasonic parameters and the like are adjusted to prepare the micro-ammonium perchlorate with the controllable average grain diameter being 0.3-2 micrometers and the regular morphology. The process of preparing the micro-ammonium perchlorate by means of the flowing focused type micro-mixer is continuous and controllable, and the method has the advantages of being simple in technology, rapid, high in yield and safety performance, free of amplification effects and the like.

Description

technical field [0001] The invention relates to a method for preparing fine ammonium perchlorate, in particular to a method for preparing fine ammonium perchlorate by using a flow-focused micro-mixer in combination with an anti-solvent crystallization method and ultrasonic assistance. Background technique [0002] Ammonium perchlorate (NH 4 ClO 4 ) is widely used as an oxidant for solid propellants because of its high oxygen content, no heavy metal ions, and low price. Its content is generally 60% to 80% of the total mass. Therefore, the burning rate and thermal stability of ammonium perchlorate have a direct impact on the performance of the solid propellant. Studies have shown that the particle size of ammonium perchlorate has a great influence on the burning rate of ammonium perchlorate. Wang Da'an and others have found that when the particle size of ammonium perchlorate is reduced from 30 μm to 1.5 μm, the burning rate of ammonium perchlorate can jump from 27.7 mm / s to...

Claims

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Application Information

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IPC IPC(8): C01B11/18C06B29/22
Inventor 张利雄亓云飞马振叶王重庆
Owner NANJING UNIV OF TECH
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