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Nano epsilon crystal form hexanitrohexaazaisowurtzitane (CL-20) explosive and massive preparation method thereof

A technology of heteroisopentazine explosive and hexanitrohexanitrogen, which is applied in nitroalkane composition, organic chemistry method, organic chemistry and other directions, can solve the problems of unsuitable industrial amplification of supercritical fluid method and introduction of mechanical impurities, etc. To achieve the effect of simple operation and simple process

Active Publication Date: 2017-03-22
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

[0006] Among the aforementioned refinement methods, the ball milling method has a large amount of preparation, but it may introduce mechanical impurities; the supercritical fluid method is not suitable for industrial scale-up; the microemulsion method generates β crystal form CL-20; the conventional solvent / non-solvent method is due to rapid crystallization. It is very easy to generate β crystal form CL-20 while reducing the particle size

Method used

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  • Nano epsilon crystal form hexanitrohexaazaisowurtzitane (CL-20) explosive and massive preparation method thereof
  • Nano epsilon crystal form hexanitrohexaazaisowurtzitane (CL-20) explosive and massive preparation method thereof
  • Nano epsilon crystal form hexanitrohexaazaisowurtzitane (CL-20) explosive and massive preparation method thereof

Examples

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Effect test

Embodiment 1

[0033] Add 2000mL toluene to the beaker, put it in the refrigerator to pre-freeze to -30°C; measure 100mL DMF, add 60g CL-20 to it, stir to dissolve it, and heat it to 65°C to prepare the explosive solution; put the beaker in a low temperature Turn on the ultrasound in the ultrasonic tank, use a stirrer to vigorously stir the toluene in the beaker, spray the heated explosive solution into the toluene, and the system temperature after the spraying is -16°C; the obtained material is washed with -20°C toluene several times, filtered , and dried at room temperature to obtain 52g of ε crystal form CL-20 explosive with an average particle diameter of 320nm.

Embodiment 2

[0035] Add 3000mL of n-heptane into the beaker, put it in the refrigerator to pre-freeze to -25°C; measure 250mL of ethyl acetate, add 100g of CL-20 into it, stir to dissolve it, and heat it to 50°C to prepare the explosive solution; Put the beaker into a low-temperature ultrasonic pool and turn on the ultrasound, use a stirrer to stir the n-heptane in the beaker vigorously, spray the heated explosive solution into the n-heptane, and the temperature of the system after the injection is -10°C; the obtained materials are used- Washed several times with n-heptane at 15°C, filtered, and freeze-dried at -40°C to obtain 88 g of ε crystal form CL-20 explosive with an average particle size of 380 nm.

Embodiment 3

[0037] Add 1000mL dichloroethane into the beaker, put it in the refrigerator to pre-freeze to -20°C; measure 100mL acetone, add 40g CL-20 into it, stir to dissolve, and heat to 45°C to prepare the explosive solution; put the beaker Put it into a low-temperature ultrasonic pool and turn on the ultrasound, use a stirrer to stir the dichloroethane in the beaker vigorously, spray the heated explosive solution into the dichloroethane, and the system temperature after the spray is -8°C; the obtained material is Wash with dichloroethane at -10°C several times, filter, and vacuum-dry at 60°C to obtain 34 g of ε crystal form CL-20 explosive with an average particle size of 350 nm.

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Abstract

The invention discloses a nano epsilon crystal form hexanitrohexaazaisowurtzitane (CL-20) explosive and a massive preparation method thereof. The preparation method is characterized by comprising the following steps: dissolving CL-20 explosive into a solvent to prepare an explosive solution; pre-cooling a non-solvent; heating the explosive solution to a certain temperature, ejecting the explosive solution into the pre-cooled non-solvent under stirring and ultrasonic waves, and finally carrying out solid-liquid separation, washing, purification, and drying to obtain the nano epsilon crystal form hexanitrohexaazaisowurtzitane (CL-20) explosive. The problem solves the problem that in a conventional solvent-non-solvent rapid crystallization method, crystal transformation of CL-20 happens easily; the epsilon crystal form hexanitrohexaazaisowurtzitane (CL-20) explosive is obtained through direct crystallization; the technical process is simple, the operation is convenient, moreover, the epsilon crystal form hexanitrohexaazaisowurtzitane (CL-20) explosive can be produced in batches, and the yield of each batch can reach 100 grams. By optimizing the technological parameters, epsilon crystal form CL-20 powder with an average particle size less than 500 nm can be obtained.

Description

technical field [0001] The invention belongs to the field of energetic material preparation, and in particular relates to a nano-ε crystal hexanitrohexaazaisopentazane explosive with a particle diameter below 500 nm and a batch preparation method thereof. Background technique [0002] After the explosives are refined, most of them show the advantages of reduced critical diameter, reduced mechanical sensitivity, improved short-pulse detonation sensitivity, faster and more complete release of detonation energy, higher combustion efficiency, faster and more stable detonation wave propagation, etc., submicron / Nano-explosives have great application prospects in weapon systems. [0003] Hexanitrohexaazaisopentazane (HNIW or CL-20) is a cage-like nitramine structure high-energy compound composed of two five-membered rings and one six-membered ring, and its molecular formula is C 6 h 6 N 12 o 12 , first synthesized by A.T.Nielsen in 1987. The performance of CL-20 is superior t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/22C06B25/40
CPCC06B25/40C07B2200/13C07D487/22
Inventor 吴鹏谯志强黄纪春孟力逄万亭陈瑾张丽媛杨光成
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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