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Green Crystallization of HMX Based on Membrane Separation: Preparation and Characterization
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1.Institute of Chemical Materials, CAEP, Mianyang 621999, China;2.School of Environment and Safety Engineering, North University of China,Taiyuan 030051, China

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    Abstract:

    Aiming at the problems that the crystallization methods (evaporation, antisolvent and cooling, etc.) of the conventional explosive are difficult to accurately control the uniformity of supersaturation and the low solvent recovery rate, an organic solvent nanofiltration(OSN) membrane crystallization apparatus based on pressure-driven and cross-flow filtration was designed and used to study the membrane crystallization process of 1,3,5,7-tetranitro-1,3,5,7-tetrazacyclooctane(HMX). The effects of key process parameters (temperature and pressure) on the crystal morphology and particle size were discussed, and the crystal morphology and structure were compared with those of evaporative crystallization. The HMX crystals after recrystallization by both methods were characterized by scanning electron microscopy(SEM),X-ray powder diffractometer(XRD) and thermogravimetric-differential scanning calorimeter(TG-DSC). The long-term operational stability of the nanofiltration membrane was further investigated, and the solvent recovered by permeation was used to re-crystallize. Results show that by the optimal control of temperature and pressure, the membrane crystallization process can obtain β-phase HMX with narrow particle size distribution (coefficient of variation < 46%), high crystal density (ρavg=1.8997-1.9004 g·cm-3) and excellent thermal stability. Compared with evaporation crystallization, the supersaturation control in the membrane crystallization process is easier to operate, and the prepared crystal morphology is more uniform. After repeated use, the rejection of HMX molecules in the solvent still remained above 92%, showing a good permeation selectivity stability. The β-phase HMX crystals with an median particle size of 34.92 μm and a coefficient of variation of 37.22% can still be prepared by membrane crystallization using permeation-recovered solvent, indicating that this technology can realize the efficient recovery and reuse of the crystallization solvent.

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王腾,周鑫,郝世龙,等.基于膜分离的HMX绿色结晶制备与表征[J].含能材料,2023,31(1):8-17.
WANG Teng, ZHOU Xin, HAO Shi-long, et al. Green Crystallization of HMX Based on Membrane Separation: Preparation and Characterization[J]. Chinese Journal of Energetic Materials,2023,31(1):8-17.

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History
  • Received:May 18,2022
  • Revised:October 27,2022
  • Adopted:October 20,2022
  • Online: October 24,2022
  • Published: January 25,2023