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Preparation method of large-particle hexanitrohexaazaisowurtzitane explosive

A technology of isowurtzane explosives and hexanitrohexanitrogen, which is applied in organic chemistry and other fields, can solve the problems of high brittleness of crystal particles, difficulty in obtaining CL-20, and no public literature reports on the preparation method, and achieve good application prospects and operation The effect of convenience and simple process

Active Publication Date: 2014-01-29
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, due to the high brittleness of CL-20 crystal particles, it is difficult to obtain large CL-20 by ordinary recrystallization methods, and only CL-20 with an average particle size of 100-150 μm can be obtained. Therefore, it is difficult to obtain more than 75% CL-20 by gradation. Solid content of CL-20 pouring formula, so it is difficult to play the high-energy characteristics of CL-20, inhibiting its application in high energy density charging
[0004] The present invention uses the method of adding seed crystals in the supersaturated region of CL-20 solution to prepare large particle CL-20 with a particle size greater than 400 μm. At present, there is no public literature report on the preparation method of large particle CL-20 explosives

Method used

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Embodiment 1

[0025] At room temperature, add 300ml of ethyl acetate into the beaker, then add 100g of raw material CL-20 under stirring, after complete dissolution, filter to obtain a saturated solution of CL-20. At 25-50°C, under stirring, add 250ml of n-heptane for the first time, then add 10g of seed crystals with an average particle size of 123μm, stir at 300rpm for 30min, then add the remaining 750ml of n-heptane dropwise at a rate of 6mL / min. Heptane, after the addition of n-heptane is completed, continue to stir for 30 minutes, filter, wash with distilled water for 5-6 times, and dry in a vacuum oven at 60°C for 6-8 hours to obtain large particles of CL with an average particle size of 349.5 μm -20.

Embodiment 2

[0027] At room temperature, add 580ml of ethyl acetate into the beaker, then add 200g of raw material CL-20 under stirring, after complete dissolution, filter to obtain a saturated solution of CL-20. At 25-50°C, under stirring, add 500ml of toluene for the first time, then add 20g of seed crystals with an average particle size of 165μm, stir at 300rpm for 30min, then add the remaining 1300ml of toluene dropwise at a rate of 8mL / min, and wait After adding toluene dropwise, continue to stir for 50 minutes, filter, wash with distilled water for 5-6 times, and dry in a vacuum oven at 60°C for 6-8 hours to obtain large particles of CL-20 with an average particle size of 402.4 μm.

Embodiment 3

[0029] At room temperature, add 350ml of acetone into the beaker, then add 200g of raw material CL-20 under stirring, after complete dissolution, filter to obtain a saturated solution of CL-20. At 25-50°C, under stirring, add 450ml of n-hexane for the first time, then add 20g of seed crystals with an average particle size of 186μm, stir at 300rpm for 30min, then add the remaining 1000ml of n-hexane dropwise at a rate of 15mL / min. Hexane, after the addition of n-hexane is completed, continue to stir for 40 minutes, filter, wash with distilled water for 5-6 times, and dry in a vacuum oven at 60°C for 6-8 hours to obtain large particles of CL with an average particle size of 422.6 μm -20.

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Abstract

The invention discloses a preparation method of a large-particle hexanitrohexaazaisowurtzitane explosive, and the preparation method comprises the following steps: adding enough hexanitrohexaazaisowurtzitane into a recrystallization solvent at 25-50 DEG C, dissolving and filtering to obtain a hexanitrohexaazaisowurtzitane saturated solution; putting the hexanitrohexaazaisowurtzitane saturated solution into a three-necked flask, wherein the temperature is 25-50 DEG C, and the stirring speed is 200-500 rpm (revolutions per minute); adding a non-solvent for the first time so that the solvent is at a supersaturation concentration and no crystal is precipitated; adding a hexanitrohexaazaisowurtzitane seed crystal, and stirring; dropwise adding the non-solvent for the second time by use of a peristaltic pump, wherein the dropwise adding time is 1-3 hours; after the dropwise adding, stirring, filtering, washing and drying to obtain large-particle hexanitrohexaazaisowurtzitane explosive. By adopting the preparation method disclosed by the invention, the hexanitrohexaazaisowurtzitane explosive with average particle size over 350 microns can be prepared; the preparation method is simple in process and convenient to operate.

Description

technical field [0001] The invention belongs to the field of energetic materials, and in particular relates to a preparation method of a large particle hexanitrohexaazaisowurtzitane explosive. The invention has good application prospects in high-energy and low-sensitivity pouring explosives. Background technique [0002] Hexanitrohexaazaisowurtzitane (HNIW, CL-20) is known as "the breakthrough fourth-generation energetic material" and "the most powerful non-nuclear explosive" so far. It is of great significance in high-energy charge and improving the efficient damage of weapons and ammunition. Its wide application will greatly promote the technological progress of strategic and tactical weapons. However, in practical applications, especially in casting formulations, in order to obtain high energy, it is necessary to use particles of different particle sizes, especially CL-20 with large particles for grading, so as to obtain PBX casting formulations with high solid content. ...

Claims

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Application Information

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IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 徐容杨志剑李金山王述存聂福德
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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