A kind of method for preparing fine ammonium perchlorate

A kind of ammonium perchlorate, fine technology, applied in the direction of ammonium perchlorate composition, perchloric acid, perchlorate, etc., can solve the problems of high equipment requirements, high cost, etc., achieve flexible output, flexible adjustment, avoid The effect of the amplification effect

Active Publication Date: 2017-10-24
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the pressure is as high as 9MPa, which requires high equipment and high cost

Method used

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  • A kind of method for preparing fine ammonium perchlorate
  • A kind of method for preparing fine ammonium perchlorate
  • A kind of method for preparing fine ammonium perchlorate

Examples

Experimental program
Comparison scheme
Effect test

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 fine ammonium perchlorate. The specific steps are as follows: preparing a saturated solution of ammonium perchlorate containing a surfactant; transporting an anti-solvent into an outer channel of a flow-focusing micro-mixer, turning on ultrasonic waves, and transporting saturated The solution enters the inner channel of the flow focusing micro-mixer and is mixed with the anti-solvent; the obtained product is filtered and dried to obtain fine ammonium perchlorate with good dispersibility. By adjusting the inner diameter of the inner channel, the distance between the inner and outer channels, the residence time of the total material in the outer channel, the volume ratio of the solvent, the saturated solution and the anti-solvent, and the ultrasonic parameters, the average particle size of 0.3-2 μm can be prepared. Morphologically regular ammonium perchlorate. The process of preparing fine ammonium perchlorate by using a flow-focusing micro-mixer is continuous and controllable, and the method has the advantages of simple process, rapidity, high yield and safety performance, and no amplification effect.

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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Patent Type & Authority Patents(China)
IPC IPC(8): C01B11/18C06B29/22
Inventor 张利雄亓云飞马振叶王重庆
Owner NANJING TECH UNIV
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