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Preparation method of characteristic benzotrifuroxan

A special technology of benzofurazan trioxide, which is applied in the field of preparation of special benzofurazan trioxide, can solve the problems of difficult control, difficult to meet the particle size requirements, cumbersome operation, etc.

Inactive Publication Date: 2017-02-15
SHANXI BEIHUA GUANLYU CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, in the prior art, recrystallized BTF is usually obtained by adding the mother liquor of propionic acid of BTF to ice water, which not only requires ice making in advance, manual stirring, and cumbersome operation, but also the particle size of the obtained product fluctuates between 8 μm and 25 μm, which is difficult to control. Difficult to meet the particle size requirement of benzofurazan for primary explosives of special weapon types

Method used

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  • Preparation method of characteristic benzotrifuroxan

Examples

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preparation example Construction

[0022] The invention provides a preparation method of special benzofurazan, comprising the following steps:

[0023] Provide benzofuroxan raw material solution;

[0024] Adding the benzofurazan trioxide raw material solution into dilution water for stirring to obtain special benzofurazan; the particle diameter of the special benzofurazan is 10-14 μm.

[0025] The method provided by the present invention, the method provided by the present invention controls the size and distribution of the crystal particle size by adding the benzofurazan raw material solution into the dilution water to carry out recrystallization technology, improves the explosive quality of BTF through a simple method, and satisfies special requirements. Weapon type primer requirements. The results of the examples of the present application show that the special benzofurazan prepared according to the technical solution of the present invention has a volume average particle size of 10-14 μm, and the particle ...

Embodiment 1

[0040] Taking a 50-liter glass kettle as an example, the preparation of 10 μm ~ 14 μm BTF is carried out as follows:

[0041] 1. Add 30 liters of propionic acid to a 50-liter glass kettle, under stirring conditions, add 1.2 kg of BTF to dissolve until transparent, and set aside;

[0042] 2. Add 30 liters of dilution water to another 50 liters of glass kettle, cool to 0 ℃ ~ 3 ℃ through the jacket, and add 10 liters of BTF propionic acid mother liquor evenly to crystallization in dilution water;

[0043] 3. After adding the BTF propionic acid mother liquor, continue stirring at a stirring speed of 200rpm for 5 minutes to complete the crystallization;

[0044] 4. Discharge the crystallization mother liquor to a vacuum filter for solid-liquid separation, wash the material several times until the pH reaches 5.0-7.0, and collect the material after draining;

[0045] 5. Repeat 2 to 4 operations twice to completely crystallize the BTF raw material solution;

[0046] 6. Dry the collec...

Embodiment 2

[0049] Adopt the scheme of Example 1 to prepare characteristic BTF, the difference is that in this embodiment, the volume ratio of dilution water to BTF solution is 7:3, wherein, the mass ratio of solute and solvent in BTF solution is 1:25, and 15L BTF Add the propionic acid solution to 35L dilution water at a uniform speed within 8 minutes, control the stirring speed during the feeding process to 200rpm, the mass ratio of BTF to propionic acid in the BTF propionic acid solution is 1:25, dilute at 3°C ​​for 8 minutes During the crystallization process, the stirring speed was controlled to be 200 rpm.

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Abstract

The invention provides a preparation method of characteristic benzotrifuroxan (BTF), wherein the preparation method comprises the following steps: providing a benzotrifuroxan raw material solution; and adding the benzotrifuroxan raw material solution to dilution water in a flowing manner, and diluting and crystallizing, to obtain the characteristic benzotrifuroxan. According to the method provided by the invention, the crystal granularity and distribution are controlled by a recrystallization technology of adding the benzotrifuroxan raw material solution to the dilution water in the flowing manner for dilution and crystallization, the quality of the BTF explosive is improved through the simple method, and the requirements of special weapon type initiating explosives are met. The results of the embodiment indicate that the characteristic benzotrifuroxan prepared by the method has the volume average particle size of 10 to 14 [mu]m, and has the advantages of uniform particle size and small fluctuation.

Description

technical field [0001] The invention relates to the field of explosives, in particular to a preparation method of special benzofurazan trioxide. Background technique [0002] Benzotris[1,2,5]-diazol-(1,4,7) trioxide, also known as benzotrioxide furazan (BTF), is a light yellow crystalline powder with high Density and energy, due to its good explosive performance and suitable sensitivity, it is used as the primary explosive for special weapon models. During the use of BTF, the uniformity of particle size determines its performance. Studies have shown that the particle size of BTF products is controlled within 10 μm to 14 μm, and when the particle size is uniform, the performance is the best, which is the quality assurance during the use of explosives. [0003] However, in the prior art, recrystallized BTF is usually obtained by adding the mother liquor of propionic acid of BTF to ice water, which not only requires ice making in advance, manual stirring, and cumbersome operat...

Claims

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Application Information

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IPC IPC(8): C07D271/12
CPCC07D271/12
Inventor 姚新民贾宏选杨琨王卫星卫涌侯鹤谢利鹏杨芬
Owner SHANXI BEIHUA GUANLYU CHEM IND