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A kind of preparation method of fine particle NTO

A fine particle and solution technology, applied in organic chemistry, nitrated acyclic/alicyclic/heterocyclic amine explosive composition, etc., can solve problems such as complex process and wide range of NTO crystal particle size distribution

Active Publication Date: 2020-07-31
SHANXI BEIHUA GUANLYU CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above technology is not only complicated in process, but although the particle size can be refined to a certain extent, the NTO obtained by recrystallization still has the problem of a wide range of crystal particle size distribution.

Method used

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  • A kind of preparation method of fine particle NTO
  • A kind of preparation method of fine particle NTO
  • A kind of preparation method of fine particle NTO

Examples

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Effect test

preparation example Construction

[0023] The invention provides a kind of preparation method of fine particle NTO, comprises the following steps:

[0024] Add the solution of raw material NTO dropwise into cold water under stirring condition, and filter the obtained mixed material liquid to obtain fine particle NTO;

[0025] The solvent of the dissolving liquid is nitrogen methyl pyrrolidone; the temperature of the dissolving liquid is 60-80° C.; the temperature of the cold water is 0-5° C.; the stirring rate is 300-500 r / min.

[0026] In the present invention, the solution solution of raw material NTO is added dropwise into cold water under stirring condition, and the obtained mixed material solution is filtered to obtain fine particle NTO. In the present invention, the solvent of the dissolving solution is nitrogen-methylpyrrolidone; the volume ratio of the nitrogen-methylpyrrolidone and cold water is preferably 1:5-8, more preferably 1:7-8; The mass percent concentration of the raw material NTO is preferab...

Embodiment 1

[0033] Dissolve 1000 g of NTO raw material in 1.8 L of nitrogen methyl pyrrolidone, and the temperature of the constant temperature water bath is 80 ° C. Add 14L of pure water into the crystallizer, start stirring, the stirring speed is 400r / min, turn on the refrigeration cycle, so that the temperature of the pure water in the crystallizer drops to 0°C, and use a constant pressure dropping funnel to drop the solution to control the temperature in the crystallizer The temperature is 0-5°C, and the dropwise addition time is 5 minutes. After the dropwise addition is completed, filter and dry to obtain fine particles of NTO.

[0034] Carry out electron microscope test to the NTO raw material of embodiment 1 and the fine particle NTO that obtains, test result is as follows figure 1 and figure 2 shown. figure 1 is the electron microscope picture of the NTO raw material, figure 2 Electron microscope image of fine-grained NTO. figure 1 The results show that before crystalliza...

Embodiment 2

[0037] Dissolve 1000g of NTO raw material in 1.8L of nitrogen methyl pyrrolidone, and the temperature of the constant temperature water bath is 70°C. Add 14L of pure water to the crystallizer, start stirring, the stirring speed is 500r / min, turn on the refrigeration cycle, so that the temperature of the pure water in the crystallizer drops to 3°C, and use a constant pressure dropping funnel to drop the solution to control the temperature in the crystallizer The temperature is 0-5°C, and the dropwise addition time is 15 minutes. After the dropwise addition is completed, filter and dry to obtain fine particles of NTO.

[0038] The fine-grained NTO obtained in Example 2 was subjected to an electron microscope test, and the test result was similar to the electron microscope image of the fine-grained NTO obtained in Example 1. The NTO after crystallization was a flaky crystal with a narrow particle size range, an average of 30 μm, and The crystal shape is relatively regular and the...

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Abstract

The invention belongs to the technical field of energetic materials and particularly relates to a preparation method of a fine particle NTO. The preparation method comprises: adding a raw material NTOsolution into cold water drop by drop under the stirring condition, and sequentially filtering and drying the mixed liquid to obtain fine particles NTO. The solvent of the solution is N-methyl pyrrolidone, the temperature of the solution is 60 to 80 DEG C, the temperature of the cold water is 0 to 5 DEG C and the stirring rate is 300 to 500 r / min. The preparation method has simple processes. Theprepared NTO particles have small sizes and a narrow particle size distribution range.

Description

technical field [0001] The invention relates to the technical field of energetic materials, in particular to a method for preparing fine particle NTO. Background technique [0002] 3-Nitro-1,2,4-triazol-5-one (NTO for short) is a high-energy, low-sensitivity, easy-to-form single-substance explosive. Its density is as high as 1.93g / cm 3 , the energy is close to cyclotrimethyltrinitramine (referred to as RDX), and the sensitivity is close to triaminotrinitrobenzene (referred to as TATB). It is mainly used in the manufacture of low-vulnerability plastic bonded explosives, and can replace TATB as a cyclotetramethylene Tetranitramine (abbreviated as HMX) is an active desensitizing agent for mixed explosives, so it is more attractive than ordinary explosives RDX and HMX in practical applications. [0003] Most of the NTO crystals prepared by reaction today have a typical rod-like structure, which is sensitive to shock wave stimulation. Moreover, its particle size distribution i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D249/14C06B25/34
CPCC06B25/34C07D249/14
Inventor 侯鹤毋文莉王卫星贾宏选张茂林
Owner SHANXI BEIHUA GUANLYU CHEM IND
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