Preparation method of super-large particle hexanitrohexaazaisowurtzitane

A technology of hexanitrohexaazane and isowurtzitane is applied in the field of preparation of super-large particle hexanitrohexaazaisowurtzitane, and can solve the problems of low yield, poor morphology consistency, easy occurrence of twinning phenomenon and the like

Active Publication Date: 2020-06-05
SHANXI BEIHUA GUANLYU CHEM IND
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  • Abstract
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  • Claims
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Problems solved by technology

[0006] Although the above two methods can prepare hexanitrohexaazaisowurtzitane crystals in a specific particle size range, the maximum experimental scale is only 100 grams. When the process is enlarged to the kilogram level, the prepared hexanitrohexaazaisowurtzitane Crystals are prone to twinning, poor shape consistency, and low yield, making it difficult to achieve the goal of industrial mass production

Method used

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  • Preparation method of super-large particle hexanitrohexaazaisowurtzitane

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preparation example Construction

[0030] The invention provides a method for preparing super-large particle hexanitrohexaazaisowurtzitane, comprising the following steps:

[0031] (1) dissolving a saturated amount of hexanitrohexaazaisowurtzitane in a recrystallization solvent to obtain a saturated solution of hexanitrohexaazaisowurtzitane;

[0032] (2) adding large particle hexanitrohexaazaisowurtzitane seed crystals to the saturated solution of hexanitrohexaazaisowurtzitane to obtain hexanitrohexaazaisowurtzitane suspension, the large The average particle size of the granular hexanitrohexaazaisowurtzitane seed crystals ranges from 250 to 300 μm;

[0033] (3) Adding a non-solvent to the hexanitrohexaazaisowurtzitane suspension in a natural feeding manner, after heat preservation, solid-liquid separation to obtain super-large particle hexaazaisowurtzitane, the The flow speed of the non-solvent is 20-40L / min, and the adding position of the non-solvent is located below the liquid level of the hexanitrohexaazais...

Embodiment 1

[0062] At room temperature, add 80 L of ethyl acetate into the dissolving machine, add 30 kg of raw material CL-20 under stirring, and after complete dissolution, filter to obtain a saturated solution of CL-20. Put the saturated solution into the crystallizer, control the temperature to 40°C, and the stirring rate to 150rpm, add 5kg of seed crystals with an average particle size of 150μm, stir for 10min, add 200L n-octane to the high level tank, and place the outlet below the liquid level of the saturated solution. Open the high-position tank bottom valve and add n-octane at a uniform speed for 5 minutes. After the addition, time and keep warm for 48 hours, filter, and dry to obtain large particles of hexanitrohexaazaisowurtzitane.

[0063] The screened hexanitrohexaazaisowurtzitane with an average particle size of 300 μm was used as the seed crystal; at room temperature, 80 L of ethyl acetate was added to the dissolving machine, and 30 kg of raw material CL-20 was added under ...

Embodiment 2

[0065] At room temperature, add 80L of acetone into the dissolving machine, add 30kg of raw material CL-20 under stirring, after completely dissolving, filter to obtain a saturated solution of CL-20. Add the saturated solution into the crystallizer, control the temperature at 40°C, and the stirring rate at 250rpm, add 5kg of seed crystals with an average particle size of 150μm, stir for 10min, add 200L of n-heptane to the head tank, and place the outlet below the liquid level of the saturated solution. Open the bottom valve of the high tank and add n-heptane at a uniform speed at one time, and the feeding time is 5 minutes. After the addition, time and keep warm for 48 hours, filter, and dry to obtain large particles of hexanitrohexaazaisowurtzitane.

[0066] The screened hexanitrohexaazaisowurtzitane with an average particle size of 300 μm was used as the seed crystal; at room temperature, 80 L of acetone was added into the dissolving machine, and 30 kg of raw material CL-20 w...

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Abstract

The invention belongs to the field of energetic materials, and particularly relates to a preparation method of super-large-particle hexanitrohexaazaisowurtzitane. According to the preparation method of the super-large-particle hexanitrohexaazaisowurtzitane, the seed crystal in a specific particle size range is added into a saturated solution, and then a non-solvent is rapidly added into the solution, so that the non-solvent and the mixed solution are rapidly and uniformly mixed to form a uniform supersaturated state in the whole range, and uniform growth of the seed crystal in the whole rangeis realized. The crystal size of the seed crystal is adjusted so that the super-large particle hexanitrohexaazaisowurtzitane crystal with the average particle size in the range of 400 to 600 microns can be prepared. The result of the embodiment shows that the experimental magnitude can be up to 50 kg at most, the prepared hexanitrohexaazaisowurtzitane crystals are good in morphology consistency, the yield can reach 60% or above, and the purpose of industrial batch production is achieved.

Description

technical field [0001] The invention belongs to the field of energetic materials, and in particular relates to a preparation method of super-large particle hexanitrohexaazaisowurtzitane. Background technique [0002] Hexanitrohexaazaisowurtzitane (HNIW, CL-20) is a white crystalline compound with high energy density and a caged polycyclic ammonium nitrate structure. Strong non-nuclear elemental explosives have been widely concerned by the world since they were synthesized for the first time by Dr. Nielsen of the United States in 1987. [0003] 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 casting formulations with high solid content. [0004] Chinese patent CN101624394 provides a spherical ε-hexanitrohexaazaisowurtzitane crystal and a preparation method thereof. By adding a crystal production contr...

Claims

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Application Information

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IPC IPC(8): C06B25/34
CPCC06B25/34
Inventor 侯鹤谢利鹏苗菲刘波刘雪朵
Owner SHANXI BEIHUA GUANLYU CHEM IND
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