二硝酰胺铵的结晶控制研究
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摘要
通过溶剂—非溶剂重结晶法制备了短棒状的二硝酰胺铵(ADN),采用扫描电镜(SEM)、激光粒度仪分析了加料方式、超声波振荡、晶体生长控制剂等因素在重结晶过程中对ADN晶体形貌和粒度的影响。结果表明:超声波辅助沉积技术可明显改善ADN的晶体形貌和防止晶体团聚;采用无机硝酸盐为晶形控制剂可显著减小ADN晶体的长径比;经晶形控制后,ADN晶体的形貌呈现规则化,表面光滑无棱角,颗粒大小更加均匀、平均粒径为(80±1)μm,粒度分布范围变窄、可控制在33～142μm;按GJB 772A—97测试的摩擦感度由16%降低至4%,撞击感度提高了4.2 J,安全性能明显优于最初样品,吸湿性也得到明显改善。
The ammonium dinitramide(ADN) with short rod-like shape was prepared by the solventnonsolvent recrystallization method. The influence of the factors including feeding mode, ultrasonic wave oscillation, crystal growth controlling agent, etc. on the morphology and particle size of ADN crystal during the recrystallization was analyzed by using the scanning electron microscopy(SEM) and laser particle size analyzer. The results show that the ultrasonic wave assisted deposition technology can significantly improve the morphology of ADN crystal and prevent crystal agglomeration. The length-diameter ratio of ADN crystal can be significantly reduced by using inorganic nitrate as the crystal controlling agent. After controlling the morphology of crystal, the morphology of ADN crystal is regular, its surface is smooth without edges,the particle size is more uniform, the average particle size is(80±1) μm, the particle size distribution range becomes narrower, and can be controlled in 33～142 μm. The friction sensitivity testing in accordance with GJB 772 A—97 reduces from 16% to 4%, the impact sensitivity increases by 4.2 J, the safety performance is significantly superior to that of the original samples, and the hygroscopicity is also obviously improved.
The ammonium dinitramide(ADN) with short rod-like shape was prepared by the solventnonsolvent recrystallization method. The influence of the factors including feeding mode, ultrasonic wave oscillation, crystal growth controlling agent, etc. on the morphology and particle size of ADN crystal during the recrystallization was analyzed by using the scanning electron microscopy(SEM) and laser particle size analyzer. The results show that the ultrasonic wave assisted deposition technology can significantly improve the morphology of ADN crystal and prevent crystal agglomeration. The length-diameter ratio of ADN crystal can be significantly reduced by using inorganic nitrate as the crystal controlling agent. After controlling the morphology of crystal, the morphology of ADN crystal is regular, its surface is smooth without edges,the particle size is more uniform, the average particle size is(80±1) μm, the particle size distribution range becomes narrower, and can be controlled in 33～142 μm. The friction sensitivity testing in accordance with GJB 772 A—97 reduces from 16% to 4%, the impact sensitivity increases by 4.2 J, the safety performance is significantly superior to that of the original samples, and the hygroscopicity is also obviously improved.
引文
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[16] WANG Dongxu, CHEN Shusen, LI Yanyue, et al. An investigation into the effects of additives on crystal characteristics and impact sensitivity of RDX[J]. Journal of Energetic Materials, 2014, 32(3):184-198.
[2] PAGORIA P F, LEE G S, MITCHELL A R, et al. A review of energetic materials synthesis[J]. Thermochimica Acta,2002,384(1):187-204.
[3] VENKATACHALAM S,SANTHOSH G,NINAN K.An overview on the synthetic routes and properties of ammonium dinitramide(ADN)and other dinitramide salts[J]. Propellants, Explosives, Pyrotechnics, 2004,29(3):178-187.
[4]任晓雪,赵凤起,郑斌.ADN推进剂的研究发展[J].飞航导弹,2007(12):53-55.
[5] MATSUNAGA Hiroki, HABU Hiroto, MIYAKE Atsumi.Thermal decomposition of the high-performance oxidizer ammonium dinitramide under pressure[J]. Journal of Thermal Analysis and Calorimetry,2014,116(3):1 227-1 232.
[6] NAGAO L M. Toward a habit modification of ammonium dinitramide[D]. Yale University, 1998.
[7] BENAZET S, JACOB G. Preparation of ammonium dinitramide(ADN)crystals, ADN crystals and energetic composites containing them:US7789980B2[P]. 2010-09-07.
[8]李晓东,杨荣杰. ADN重结晶研究[C]//第二届ADN合成与应用研讨会.北京,2013:62-68.
[9]兰艳花,翟进贤,杨荣杰.含能氧化剂二硝酰胺铵重结晶的理论计算与实验研究[C]//第二届ADN合成与应用研讨会.北京,2013:55-61.
[10] KIM Kwang-Joo, Microparticle formation of1,3,5,7-tetranitro-1,3,5,7-tetraazcy-looctane by crystallizations with ultrasound[C]//Proc of 31th Int Ann Conf. ICT, 2000.
[11] SIVABALAN R, GORE G M,NAIR U R, et al. Study on ultrasound assisted precipitation of CL-20 and its effect on morphology and sensitivity[J]. Journal of Hazardous Materials, 2007, 139(2):199-203.
[12]郭志超,李鸿,王静康,等.超声波对结晶过程的作用及机理[J].天津化工,2003,17(3):1-3.
[13] THOMPSON C, Davies M C, Roberts C J, et al. The effects of additives on the growth and morphology of paracetamol(acetaminophen)crystals[J]. International Journal of Pharmaceutics, 2004, 280(1/2):137-150.
[14] VASILEVA Anna A,DASHKO Dmitry V, DUSHENOK Sergey A, et al. Preparing and some properties of spheroidε-HNIW[C]//New Trends in Research of Energetic Materials. Czech Republic, 2013:955-966.
[15] KIM Hyoun-Soo, CHAE Joo-Seung, Han Sang-Keun, et al. Formation of spherical cyclotrimethylene trinttramine by cooling crystallization[C]//45th International Annual Conference of the Fraunhofer ICT. Congress Center,Stadthalle Karlsruhe, Germany, 2014.
[16] WANG Dongxu, CHEN Shusen, LI Yanyue, et al. An investigation into the effects of additives on crystal characteristics and impact sensitivity of RDX[J]. Journal of Energetic Materials, 2014, 32(3):184-198.