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Idiosyncratic refined HMX (cyclotetramethylene tetranitramine) crystal and preparation method thereof

A crystal and special technology, which is applied in the field of special refined HMX crystal and preparation, can solve the problems that HMX cannot be directly applied, and achieve the effect of less anti-solvent consumption, mild reaction conditions and simple operation

Active Publication Date: 2014-07-23
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the HMX directly synthesized in the prior art cannot be directly applied due to reasons such as particle size and morphology, and needs to be recrystallized or processed by other methods.

Method used

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  • Idiosyncratic refined HMX (cyclotetramethylene tetranitramine) crystal and preparation method thereof
  • Idiosyncratic refined HMX (cyclotetramethylene tetranitramine) crystal and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0036] 5 g of HMX was dissolved in 9 mL of dimethyl sulfoxide, and the solution was filtered into a 100 mL reactor, which was placed in a constant temperature water bath at 35°C. Turn on the stirrer, the stirring rate is 100rpm, and start the dripping device to add ethanol dropwise to the reaction kettle at the rate of 0.1mL / min. The total amount of ethanol used was 45mL, and after all the addition was completed, the crystals were subjected to ultrasonic treatment in the mother liquor, the ultrasonic frequency was 45KHz, and the ultrasonic time was 2h. Wash, filter, dry, and weigh. The crystal weight is about 4.6 g, and the yield is 92%. According to the experimental determination, the HMX content is ≥99.9%; the density is 1.901g / cm 3 ; The appearance has no sharp edges and corners, the surface is smooth, and the crystal surface has no cracks; the ratio of the short and long axis of the crystal is 0.83; the median particle size of the precipitated crystal is 16 μm, and the p...

Embodiment 2

[0038] Dissolve 10 grams of HMX in 18 mL of dimethyl sulfoxide, filter the solution into a 150 mL reactor, and the reactor is placed in a constant temperature water bath at 30°C. Turn on the stirrer, the stirring rate is 80rpm, and start the dripping device to drip chloroform into the reaction kettle at the same time, the dropping rate is 0.16mL / min. The total amount of chloroform used was 90 mL. After all the drops were completed, the crystals were ultrasonically treated in the mother liquor. The ultrasonic frequency was 36 KHz and the ultrasonic time was 3 h. Wash, filter, dry, and weigh. The crystal weight is about 9.1 g, and the yield is 91%. According to the experimental determination, the HMX content is ≥99.9%; the density is 1.90g / cm 3 ; The appearance has no sharp edges and corners, the surface is smooth, and the crystal surface has no cracks; the ratio of the short and long axis of the crystal is 0.8; the median particle size of the precipitated crystal is 20 μm, an...

Embodiment 3

[0040] 5 g of HMX was dissolved in 9 mL of dimethyl sulfoxide, and the solution was filtered into a 100 mL reactor, which was placed in a constant temperature water bath at 35°C. Turn on the stirrer, the stirring rate is 100rpm, and start the dripping device to drip chloroform into the reaction kettle at the same time, the dripping rate is 0.4mL / min. The total amount of chloroform used was 45mL. After all the drops were completed, the crystals were subjected to ultrasonic treatment in the mother liquor, the ultrasonic frequency was 42KHz, and the ultrasonic time was 2h. Wash, filter, dry, and weigh. The crystal weight is about 4.5 g, and the yield is 90%. According to the experimental determination, the HMX content is ≥99.9%; the density is 1.901g / cm 3 ; The appearance has no sharp edges and corners, the surface is smooth, and the crystal surface has no cracks; the ratio of the short and long axis of the crystal is 0.81; the median particle size of the precipitated crystal i...

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Abstract

The invention discloses an idiosyncratic refined HMX (cyclotetramethylene tetranitramine) crystal and a preparation method thereof. The HMX content in the crystal is more than or equal to 99.9%, the crystal density is more than or equal to 1.90g / cm<3>, and the crystal short-long axis ratio is more than or equal to 0.8; the median particle diameter of the crystal is between 10 microns and 30 microns, and the particle size distribution is narrow. The preparation method comprises the steps of 1) dissolving HMX into an organic solvent in a crystallization kettle with a jacket to prepare a saturated solution; 2) controlling the water temperature in the jacket of the crystallization kettle to be 0-40 DEG C, stirring the saturated solution while dropping an anti-solvent into the saturated solution, forming a super-saturated solution, and performing crystal nucleus generation and crystal growth; 3) after the crystal is completely separated out, performing ultrasonic treatment on the crystal in mother liquor, wherein the ultrasonic treatment time is 2-4 hours, and the ultrasonic frequency is 30-50KHz. The idiosyncratic refined HMX crystal disclosed by the invention is simple in operation, less in anti-solvent dose, mild in reaction conditions, safe and reliable, and green and efficient.

Description

technical field [0001] The present invention relates to the field of energetic crystal materials, and more specifically, relates to a special refined HMX crystal and a preparation method thereof. Background technique [0002] Octojin (1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane, HMX) is currently the elemental manganese with the highest energy level and the best comprehensive performance. Explosives, based on which mixed explosives are used for the warhead charge of missiles, nuclear weapons and anti-tank shells, or as heat-resistant explosives for deep well perforating bombs, and are also used as high-performance solid propellants and gun propellants components. HMX has four crystal forms, namely α, β, γ, and δ. The β-type is a stable crystal form. The crystal form, purity, particle size and distribution of HMX will affect its performance, and these properties are affected by the crystallization process used. At the same time, the solvent used for crystallization wil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C06B25/34
Inventor 郭学永张静元焦清介崔超卢佳骥
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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