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Preparation method of cubic short rod-shaped 1-oxo-diamino-3,5-dinitropyrazine explosive

A technology of dinitropyrazine explosives and short rods, which is applied in the direction of nitrated acyclic/alicyclic/heterocyclic amine explosive compositions, etc., which can solve the problems of uneven forming powder columns, impact sensitivity, late formula processing, particle shape and Particle size influence, difficult binder and other problems, to achieve the effect of eliminating defects, improving subsequent processing and molding performance, and narrow particle size distribution

Active Publication Date: 2015-08-19
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

T.D. Tran of the LLNL laboratory in the United States prepared 4 kinds of LLM-105 crystal materials with different particle shapes by using different crystallization methods, and their shapes are very irregular. research, but the obtained particle shape is mainly needle-shaped and "X"-shaped, and the particle fluidity is poor
In addition, using several other recrystallization solvents, including DMF, DMF / water, NMP, and NMP / water, can only obtain needle-shaped LLM-105 crystals, and the different particle shapes LLM-105 crystals obtained by these recrystallization methods are all sensitive to heat Stable, insensitive to sparks and friction; however, impact sensitivity and post-formulation processing properties are significantly affected by particle shape and particle size
The main performance is that the shape of the long needle-shaped or cross-shaped luanite LLM-105 crystal particles is poor, and it is difficult to mix evenly with the binder in the subsequent formulation process, and the LLM-105 crystal is easy to separate from the binder during processing and molding, resulting in The inside of the shaped powder column is uneven; the luan crystal structure also makes it difficult to increase the density of the booster powder formula
Simultaneously the LLM-105 purity that above-mentioned recrystallization method obtains is not high, has hindered the application of LLM-105 explosive in wider military field

Method used

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  • Preparation method of cubic short rod-shaped 1-oxo-diamino-3,5-dinitropyrazine explosive
  • Preparation method of cubic short rod-shaped 1-oxo-diamino-3,5-dinitropyrazine explosive
  • Preparation method of cubic short rod-shaped 1-oxo-diamino-3,5-dinitropyrazine explosive

Examples

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Embodiment 1

[0028] Take 5g LLM-105 and 150mL HNO with a mass percentage concentration of 30% respectively 3 , stir and heat up to 50°C to completely dissolve LLM-105, and filter to remove insoluble impurities to obtain LLM-105 / HNO 3 Explosive solution; LLM-105 / HNO 3 Put the explosive solution into the explosive injection kettle, tighten the explosive injection kettle cover, fill the explosive injection kettle with high-purity nitrogen with a purity of 99.5%, and keep the internal pressure of the explosive injection kettle at 1Mpa.

[0029] Weigh 1g of polyoxyethylene sorbitan monolaurate surfactant and add it to 300L ultrapure water, mix well, and configure LLM-105 explosive non-solvent; put LLM-105 explosive non-solvent into a low-temperature refrigerator, Pre-freeze at -10°C for 12 hours. Then the frozen LLM-105 explosive non-solvent is packed into the non-solvent storage tank, the cover of the non-solvent storage tank is tightened, and 99.5% high-purity nitrogen is charged into the n...

Embodiment 2

[0036]Take 5g LLM-105 and 100mL HNO with a mass percentage concentration of 45% respectively 3 , stir and heat up to 50°C to completely dissolve LLM-105, and filter to remove insoluble impurities to obtain LLM-105 / HNO 3 Explosive solution; LLM-105 / HNO 3 Put the explosive solution into the explosive injection kettle, tighten the explosive injection kettle cover, fill the explosive injection kettle with high-purity nitrogen with a purity of 99%, and keep the internal pressure of the explosive injection kettle at 0.5Mpa.

[0037] Weigh 2g of hexadecylamine bromide surfactant and add it to a mixture of 30L of ultrapure water and 500L of ammonia water with a concentration of 1% by mass, mix evenly to dissolve the cetylamine bromide, and configure it into LLM -105 explosive non-solvent; put LLM-105 explosive non-solvent in a low-temperature refrigerator, and pre-freeze at 0°C for 12 hours. Then put the frozen LLM-105 explosive non-solvent into the non-solvent storage tank, tighten...

Embodiment 3

[0043] Take 5g LLM-105 and 500mL HNO with a mass percentage concentration of 60% respectively 3 , stirred at room temperature to dissolve LLM-105 completely, and filtered to remove insoluble impurities to obtain LLM-105 / HNO 3 Explosive solution; LLM-105 / HNO 3 Put the explosive solution into the explosive injection kettle, tighten the explosive injection kettle cover, fill 99.7% high-purity nitrogen into the explosive injection kettle, and keep the internal pressure of the explosive injection kettle at 0.2Mpa.

[0044] Weigh 7g of OP-10 surfactant and add it to 30L ultrapure water, and weigh 300g of sodium hydroxide to make it into a solution of 5% sodium hydroxide by mass percentage, mix it evenly, and make it into LLM-105 explosive non-toxic Solvent; put the LLM-105 explosive non-solvent in a low-temperature refrigerator, and pre-freeze at -5°C for 12 hours. Then put the frozen LLM-105 explosive non-solvent into the non-solvent storage tank, tighten the cover of the non-sol...

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Abstract

The invention discloses a preparation method of a cubic short rod-like 1-oxygen-diamido-3,5-dinitro pyrazine (or 2,6-diamido-3,5-dinitro pyrazine-1-oxide with a code being LLM-105) explosive. According to the method, a solvent-non-solvent impinging jet crystallization mode is adopted; nitric acid (HNO3) is taken as a good solvent of LLM-105; the LLM-105 crystal is rapidly crystallized and separated out in a non-solvent containing a surfactant. By adopting the method disclosed by the invention, the cubic short rod-like LLM-105 crystal with regular crystal morphology can be obtained; the rod length of the LLM-105 crystal is 2-3 microns. The thermal performance of the LLM-105 crystal prepared by the method disclosed by the invention is obviously changed; thermal decomposition peak temperature is reduced to 343 DEG C from 350 DEG C; the LLM-105 crystal prepared by the method disclosed by the invention can be applied to a booster explosive.

Description

technical field [0001] The embodiment of the present invention relates to the technical field of military pyrotechnic agents, more specifically, the embodiment of the present invention relates to a preparation method of cubic short rod-shaped 1-oxo-diamino-3,5-dinitropyrazine explosive. Background technique [0002] 1-Oxo-diamino-3,5-dinitropyrazine (LLM-105) was a major breakthrough in the field of explosive synthesis in the 1990s. LLM-105 has a high crystal density (1.913g / cm 3 ), excellent physical properties, good safety performance, and 20% higher energy than TATB. Due to the π-conjugated system and strong intramolecular hydrogen bonding in the molecule, LLM-105 has excellent heat resistance (DSC exothermic peak temperature is 354°C, heating rate is 10°C·min -1 ), insensitive to impact, spark, friction and shock wave stimulation, is a typical high-energy low-sensitivity explosive (characteristics fall high H 50 =117cm, the detonation velocity is 8560m / s). These exce...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C06B25/34
Inventor 张娟吴鹏谯志强杨光成聂福德
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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