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CL-20 explosive crystal refinement method based on counter solvent ultrasonic extraction technology

An extraction technology and crystal refinement technology, which is applied in solvent extraction, solid solvent extraction, gaseous solvent extraction, etc., can solve the problems of high cost, harsh experimental conditions, unfavorable batch preparation, etc., and achieve good reproducibility and production high rate effect

Active Publication Date: 2017-06-20
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

) reported a supercritical carbon dioxide anti-solvent method (SAS) to prepare CL-20 ultrafine particles under the extreme conditions of 50 ° C and 12 Mpa. The obtained crystal surface is round and the average particle size is 1.33 μm. The conditions are harsh, the cost is high, and it is not conducive to batch preparation

Method used

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  • CL-20 explosive crystal refinement method based on counter solvent ultrasonic extraction technology
  • CL-20 explosive crystal refinement method based on counter solvent ultrasonic extraction technology
  • CL-20 explosive crystal refinement method based on counter solvent ultrasonic extraction technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] (1) Take 70ml of N,N-dimethylformamide (DMF) and place it in a 150ml three-neck flask, weigh 10g of CL-20 raw material and add it, heat it in a water bath to 90°C, and stir it mechanically until the crystals are completely dissolved. The solution was naturally cooled by the cooling crystallization method, and after crystallization for 1 h, it was filtered and washed to obtain CL-20 solvate crystals, about 12 g.

[0053] (2) XRD was used to characterize the phase of the solvate, and after confirming that all the obtained crystals were solvate, they were placed in an airtight container for use.

[0054] (3) The CL-20 solvate crystals are quickly added to 150ml of ethanol anti-solvent (the mass ratio of solvate to anti-solvent is about 1:10), and the solution is ultrasonically treated at the same time, and the ultrasonic power is 300W. For agglomeration, 0.02 g of sorbitan monooleate surfactant was added dropwise in the anti-solvent.

[0055] (4) After ultrasonication for...

Embodiment 2

[0057] (1) Measure 120ml of dimethyl carbonate (DMC) into a 250ml rotary evaporating flask, weigh 10g of CL-20 raw material and add it, heat it in a water bath to 60°C, stir mechanically until the crystals are completely dissolved, and use the solvent evaporation method The solution was rotary evaporated, crystallized for 1 h, filtered and washed to obtain CL-20 / DMC solvate crystals.

[0058] (2) XRD was used to characterize the phase of the solvate, and after confirming that all the obtained crystals were solvate, they were placed in an airtight container for use.

[0059] (3) Quickly add CL-20 solvate crystals into 180ml of diethyl ether anti-solvent, and at the same time, ultrasonically treat the solution with an ultrasonic power of 700W. alcohol surfactants.

[0060] (4) After ultrasonication for 5 minutes, filter, wash, and dry, take a small amount of samples for XRD characterization to confirm that the solvent has been completely removed, and confirm that the refined CL...

Embodiment 3

[0062] (1) Measure 30ml of dioxane (DIO) into a 250ml three-neck flask, weigh 10g of CL-20 raw material and add it. At room temperature (20°C), mechanically stir until the crystals are completely dissolved. Solvent method 100ml of deionized water was used as a non-solvent, added at a rate of 5ml / min, stirred for 1 hour to crystallize, filtered and washed to obtain CL-20 / DIO solvate crystals.

[0063] (2) XRD was used to characterize the phase of the solvate, and after confirming that all the obtained crystals were solvate, they were placed in an airtight container for use.

[0064] (3) CL-20 solvate crystals are quickly added in 150ml of n-heptane anti-solvent, and the solution is ultrasonically treated at the same time. The ultrasonic power is 100W. Vinylpyrrolidone surfactant.

[0065] (4) After ultrasonication for 30 minutes, filter, wash, and dry, take a small amount of samples for XRD characterization to confirm that the solvent has been completely removed, and confirm t...

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Abstract

The invention discloses a CL-20 explosive crystal refinement method based on a counter solvent ultrasonic extraction technology. The method comprises the following steps: complexing a raw material CL-20 and solvent to prepare CL-20 solvent compound crystals; adding the CL-20 solvent compound crystals into counter solvent, and simultaneously performing ultrasonic treatment; and after solvent molecules of the CL-20 solvent compound crystals are removed, stopping ultrasonic treatment, then filtering, washing, and drying to obtain refined CL-20 crystals. The refined CL-20 crystals have a favorable particle shape, the crystals are in an epsilon crystal form, the average particle diameter is smaller than 5 mu m, the crystal purity is greater than 99.6%, and the apparent density of the crystals reaches 99.5% or above of the theoretical density of the crystals.

Description

technical field [0001] The invention relates to a method for preparing explosive crystals, in particular to a method for refining CL-20 explosive crystals based on anti-solvent ultrasonic extraction technology. Background technique [0002] Traditional energetic materials have been difficult to meet the stringent requirements of precise strike, high-efficiency damage and high survivability, and are facing severe challenges at this stage. In order to break through the limitations of traditional energetic materials, the research on the micro-nanoization of energetic materials has become one of the current research hotspots and has attracted extensive attention. Micro-nano energetic materials usually refer to ultrafine explosive powders with a particle size of less than 10 μm. Due to their small particle size and large specific surface area, they produce many unique properties different from traditional energetic materials. They have high energy release rate, reliable detonatio...

Claims

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Application Information

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IPC IPC(8): B01D11/02B01D11/00B01D9/00C06B25/34
CPCB01D9/0054B01D11/0265B01D2011/007C06B25/34
Inventor 徐金江刘渝孙杰张浩斌刘晓峰
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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