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

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...

Examples

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.

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...

Examples

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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