A kind of preparation method of characteristic hexanitrohexaazaisowurtzitane

A technology of hexanitrohexaazane and isowurtzitane is applied in the field of preparation of special hexanitrohexaazaisowurtzitane, which can solve the problems of small particle size, difficulty in meeting the requirements of particle size and crystal morphology, and the like

Active Publication Date: 2017-12-12
SHANXI BEIHUA GUANLYU CHEM IND
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  • Claims
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AI Technical Summary

Problems solved by technology

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 hexanitrohexaazaisowurtzitane is produced by the direct nitration reaction of the hexasubstituted hexaazaisowurtzitane Based on hexaazaisowurtzitane, the obtained hexanitrohexaazaisowurtzitane is in the ε crystal form, and the crystal shape is mostly elongated bipyramid, with a median particle size of about 40 microns and a small particle size, which is difficult to meet the requirements of pouring mixed explosives. Requirements for Particle Size and Crystal Morphology of Hexanitrohexaazaisowurtzitane

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

[0023] The invention provides a method for preparing special hexanitrohexaazaisowurtzitane, comprising the following steps:

[0024] Provide hexanitrohexaazaisowurtzitane solution;

[0025] Dilute and crystallize the hexanitrohexaazaisowurtzitane solution sequentially by diluting the diluted solution in order of concentration from high to low to obtain special hexanitrohexaazaisowurtzitane.

[0026] In the method provided by the invention, the raw material CL-20 solution is recrystallized with a dilute solution, and the special CL-20 product obtained has large particle size, narrow distribution, smooth crystal surface, no obvious edges and corners, long-short axis ratio ≤ 1.5, and roundness value ≥ 0.85, suitable for particle size gradation, improving the charge performance, insensitivity performance, charge density and explosive power of molten injection and cast explosives.

[0027] The invention uses a dilute solution to dilute and crystallize the hexanitrohexaazaisowurtzi...

Embodiment 1

[0044] Taking a 400-liter spherical crystallization kettle as an example to prepare special CL-20, the specific process is as follows:

[0045] 1. At room temperature, add 78kg of ethyl acetate into the dissolution kettle, and add 30kg of raw material CL-20 into the dissolution kettle under stirring conditions, and filter the solution after all the dissolution to obtain the CL-20 solution;

[0046] 2. Add the obtained CL-20 solution into the spherical crystallization kettle, at 35°C to 50°C, add the measured ethyl acetate n-octane solution: 72% in the order of adding high concentration first and then adding low concentration Ethyl acetate n-octane solution 39kg, 50% ethyl acetate n-octane 78kg, 33% ethyl acetate n-octane 58.5kg, finally add n-octane 78kg, control flow speed, slow first and then fast, 36-48 hours After the internal addition is completed, the crystallization temperature is controlled to not be lower than 35°C, and the crystallization temperature is adjusted by t...

Embodiment 2

[0055] The special CL-20 was prepared according to the scheme of Example 1, the difference is that in this example, the solvent for dissolving CL-20 is methyl acetate, and the diluting solution is methyl acetate n-octane.

[0056] The present invention conducts the microstructure detection of the obtained idiosyncratic CL-20, and the results show that the idiosyncratic CL-20 crystals prepared by the present invention have a smooth surface, no obvious edges and corners, a small major-to-minor axis ratio, high roundness value, and large particle size.

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Abstract

The invention provides a special hexanitrohexaazaisowurtzitane preparation method. The method comprises the following steps: providing a hexanitrohexaazaisowurtzitane solution; diluting the hexanitrohexaazaisowurtzitane solution with the dilute solutions according to concentration of the dilute solutions with a sequence from high to low in order, and then crystallizing the hexanitrohexaazaisowurtzitane solution to obtain the special hexanitrohexaazaisowurtzitane. The method can realize dilution and crystallization of the hexanitrohexaazaisowurtzitane solution by the dilute solutions according to concentration of the dilute solutions with the sequence from high to low in order, crystal concentration of a simple-substance explosive can be increased through dilution and crystallization processes, internal defect of the crystal is reduced, surface flaw is eliminated, crystal shape and granularity can be controlled, so that quality of the simple-substance explosive is enhanced, and usage requirement can be satisfied.

Description

technical field [0001] The invention relates to the field of explosives, in particular to a preparation method of special hexanitrohexaazaisowurtzitane. Background technique [0002] Hexanitrohexaazaisowurtzitane was first synthesized in 1987 by Nielen and others at the U.S. Naval Weapons Center after years of hard work, and is a typical representative of energetic materials with high energy density. The crystal density and oxygen balance of hexanitrohexaazaisowurtzitane are better than those of HMX. It has excellent energy characteristics and good chemical stability. It can be used for high energy such as missile warhead charge, solid rocket propellant and atomic bomb priming Density energetic materials field. [0003] Hexanitrohexaazaisowurtzitane (CL-20) is a polymorph. There are four crystal forms at normal temperature and pressure: α, β, γ and ε. Crystal density up to 2.04g / cm 3 ~2.05g / cm 3 . The existing process usually synthesizes hexanitrohexaazaisowurtzitane ac...

Claims

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Application Information

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IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 毋文莉焦清介贾宏选郭学永刘波崔超侯鹤卫涌
Owner SHANXI BEIHUA GUANLYU CHEM IND
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