A kind of preparation method of characteristic hexanitrohexaazaisowurtzitane

A technology of hexanitrohexaazane and isowurtzitane, which is applied in the field of preparation of special hexanitrohexaazaisowurtzitane, can solve the problems of wide particle size distribution, uneven particle size distribution, etc., and achieve crystal The effect of regular and smooth shape and narrow particle size distribution

Active Publication Date: 2018-01-02
SHANXI BEIHUA GUANLYU CHEM IND
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0004] The CL-20 produced by the existing process is mostly ε crystal form, and its crystal shape is mostly elongated bipyramid, with a median particle size of about 40 microns, and a wide and uneven particle size distribution.
For example, the existing process usually synthesizes hexanitrohexaazaisowurtzitane according to a two-step method: firstly, the hexasubstituted hexaazaisowurtzitane is synthesized by the original amine, and then the hexasubstituted hexaazaisowurtzitane is produced by direct nitration reaction Hexanitrohexaazaisowurtzitane, to obtain hexanitrohexaazaisowurtzitane in the ε crystal form, with uneven particle size distribution and poor controllability

Method used

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  • A kind of preparation method of characteristic hexanitrohexaazaisowurtzitane
  • A kind of preparation method of characteristic hexanitrohexaazaisowurtzitane
  • A kind of preparation method of characteristic hexanitrohexaazaisowurtzitane

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preparation example Construction

[0027] The present invention provides a method for preparing special hexanitrohexaazaisowurtzitane, which comprises the following steps: providing a hexanitrohexaazaisowurtzitane raw material solution; combining the hexanitrohexaazaisowurtzitane raw material The solution stream is added to the diluent and stirred to obtain the characteristic hexanitrohexaazaisowurtzitane; the particle size of the characteristic hexanitrohexaazaisowurtzitane is 100-110μm; the stirring speed is 500-600rpm ; The diluent is a low carbon alkane.

[0028] In the method provided by the present invention, the CL-20 solution stream is added to the low-carbon alkane diluent combined with the restriction of the stirring speed of 500-600rpm, which improves the mobility of the CL-20 solute in the solution and promotes the dissolution of the metastable crystal form. Thereby it is beneficial to stabilize the growth of the crystal form, and is beneficial to reduce the difference in the growth rate of the crystal...

Embodiment 1

[0046] Taking a 50-liter glass crystallization kettle as an example, the CL-20 is manufactured using the following steps:

[0047] 1. At room temperature, add 10kg ethyl acetate to the dissolving kettle;

[0048] 2. Under stirring conditions of 300rpm speed, add 4㎏ CL-20 and observe that all CL-20 is dissolved;

[0049] 3. Filter the dissolving liquid and add the dissolving liquid to the upper tank,

[0050] 3. Add 16kg of n-octane into the crystallization kettle, and raise the temperature to 42℃~45℃;

[0051] 4. Add the CL-20 solution at a speed of 1.0kg / min under 500rpm speed, continue to stir for 110min, and control the crystallization temperature to not be lower than 38℃;

[0052] 5. Discharge and drain the solvent in the filter layer;

[0053] 6. Place the crystalline material in a drying cabinet for drying, and dry it at 50°C until the moisture content is less than 0.10%;

[0054] 7. After the moisture content of the dried material is qualified, the mixed batch is packed;

[0055] 8. ...

Embodiment 2

[0062] Taking a 50-liter glass crystallization kettle as an example, the CL-20 is manufactured using the following steps:

[0063] 1. At room temperature, add 10kg ethyl acetate to the dissolving kettle;

[0064] 2. Under the stirring condition of 300rpm speed, add 4㎏ CL-20 and observe that all CL-20 is dissolved;

[0065] 3. Filter the dissolving liquid and add the dissolving liquid to the upper tank,

[0066] 3. Add 16kg of n-octane into the crystallization kettle and raise the temperature to 38℃;

[0067] 4. At 500rpm, add CL-20 solution at 1.0kg / min and continue stirring for 1h; then add 3.5kg n-octane at 1.kg / min and continue stirring at 700rpm for 1h to control the crystallization temperature Not lower than 38℃;

[0068] 5. Discharge and drain the solvent in the filter layer;

[0069] 6. Place the crystalline material in a drying cabinet for drying, and dry it at 50°C until the moisture content is less than 0.10%;

[0070] 7. After the moisture content of the dried material is quali...

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Abstract

The invention provides a method for preparing idiosyncratic hexanitrohexaazaisowurtzitane. The method comprises the following steps: providing a hexanitrohexaazaisowurtzitane raw material solution; feeding the hexanitrohexaazaisowurtzitane raw material solution into a diluent in batches and then stirring to obtain idiosyncratic hexanitrohexaazaisowurtzitane, wherein the particle size of the idiosyncratic hexanitrohexaazaisowurtzitane is 100 to 110 mum, the stirring speed is 500 to 600rpm, and the diluent is a lower carbon alkane. The method provided by the invention has the advantages of improving the activity of a CL-20 solute in the solution, promoting the dissolution of a metastable crystal form, being favorable for stabilizing the growth of the crystal form, and reducing the difference of the growth rate among crystals in the crystallization process, thus further improving the uniformity of particle size; the idiosyncratic CL-20 is prepared in the defined feed-batch order at the stirring speed, and the natural growth habit of the crystals is changed so that the crystal faces can grow synchronously as much as possible to obtain the spherical-like crystal particles.

Description

Technical field [0001] The invention relates to the field of explosives, in particular to a method for preparing special hexanitrohexaazaisowurtzitane. Background technique [0002] Hexanitrohexaazaisowurtzitane was first synthesized in 1987 by Nielen and others of the US Naval Weapons Center after years of hard work. It is a typical representative of high energy density energetic materials. [0003] Hexanitrohexaazaisowurtzitane (CL-20) is a polymorphic substance. There are four crystal forms of α, β, γ and ε under normal temperature and pressure. The ε-type hexanitrohexaazaisowurtzitane Crystal density up to 2.04g / cm 3 ~2.05g / cm 3 , Has excellent energy characteristics. Due to its good chemical stability, it has attracted more attention in the field of energetic materials at home and abroad. It can be used in energy-containing fields such as missile warhead charges, solid rocket propellants and atomic bomb detonators. [0004] The CL-20 produced by the existing technology is mostl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 毋文莉贾宏选王卫星姚新民刘波王博侯鹤杨芬介二林
Owner SHANXI BEIHUA GUANLYU CHEM IND
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