1.School of Environmental and Safety Engineering， North University of China， Taiyuan 030051 China;2.Shanxi Engineering Technology Research Center for Ultrafine Powder， Taiyuan 030051 China
利用液滴微流控技术，以活性剂浓度为0.5%的水溶液为连续相，以DAAF的乙酸乙酯溶液为分散相，通过流体聚焦式微通道制备了DAAF/F2602复合微球，研究了两相流速比、分散相浓度以及活性剂种类对DAAF/F2602复合微球的颗粒形貌、粒径以及圆形度的影响，得出了最佳工艺条件，并与水悬浮法进行了对比。研究结果显示，流体聚焦式微通道制备的最佳工艺为悬浮液浓度为4%、两相流速比为16∶1、活性剂为CTAB。2种制备方法所得样品的DAAF晶型均未发生改变，撞击感度均大于100 J，摩擦感度均为0%大于360 N，表明2种样品安全性能良好。其中液滴微流控法所得DAAF/F2602复合微球的粒径为20.22~53.85 μm，小于水悬浮法所得复合粒子的粒径（121~356 μm），且粒径分布更加均匀，热分解峰峰温也延后了6.45 ℃，活化能增加了6.12 kJ·mol-1，热稳定性提高。液滴微流控法所得DAAF/F2602复合微球堆积形成的锥角为34°，小于水悬浮法所得复合粒子堆积形成的锥角（40°），流散性好。
Using droplet microfluidics technology， an aqueous solution of the active agent at a concentration of 0.5% was used as the continuous phase， and an ethyl acetate solution of DAAF was employed as the dispersed phase. DAAF/F2602 composite microspheres were prepared by fluid-focused microchanneling. The effects of two-phase flow rate ratio， concentration of dispersed phase， and type of active agent on particle morphology， particle size， and roundness of DAAF/F2602 composite microspheres were investigated. The optimal process conditions， including a suspension concentration of 4%， a two-phase flow rate ratio of 16∶1 and an active agent of CTAB， were obtained and compared with the aqueous suspension method. The results show that the DAAF crystalline shape of the samples obtained from two preparation methods are unchanged， the impact sensitivity is higher than 100 J， and the friction sensitivity is 0% and the friction sensibility are more than 360 N， indicating that the two samples have good safety performance. Among them， the particle sizes of DAAF/F2602 composite microspheres which obtained by the droplet microfluidization method were in the range of 20.22 to 53.85 μm， which were smaller than that obtained by the aqueous suspension method （121-356 μm）.Furthermore， the particle sizes distribution was observed to be more uniform. Thethermal decomposition exhibited a delayed peak temperature by 6.45 ℃， and the activation energy was increased by 6.12 kJ·mol-1， which lead to improved thermal stability. The cone angle generated by the stacking of DAAF/F2602 composite microspheres which obtained by the droplet microfluidization method， is 34°. This angle is smaller than that of composite particles obtained by the water suspension method （40°）， which indicate better dispersion property.
朱瑞,刘意,张东旭,等.液滴微流控技术制备DAAF/氟橡胶复合微球[J].含能材料, 2023, 31(11):1105-1115. DOI:10.11943/CJEM2023082.
ZHU Rui, LIU Yi, ZHANG Dong-xu, et al. Preparation of DAAF/Fluororubber Composite Microspheres by Droplet Microfluidic Technology[J]. Chinese Journal of Energetic Materials, 2023, 31(11):1105-1115. DOI:10.11943/CJEM2023082.