溶剂气氛调控制备TATB

Preparation and Regulation of TATB by Solvent Atmosphere

为调控制备不同粒径TATB,提出了一种基于溶剂气氛诱导的试验方法,将纳米TATB暴露在溶剂二甲基亚砜(DMSO)气氛中,利用溶剂气氛诱导控制TATB粒子成长;利用场发射扫描电子显微镜观察了制备的TATB晶体形貌;利用拉曼光谱仪(Raman)和傅里叶变换红外光谱仪测量了TATB的特征峰变化;利用差示扫描量热-热重联用仪(TG-DSC)分析了TATB的热分解性能;研究了溶剂气氛、试验温度以及反应时间对TATB粒径形貌的影响。结果表明,溶剂气氛试验法可诱导纳米TATB生长,调控微观形貌,制备出粒径范围1~17μm的TATB;同时,溶剂气氛试验法制备TATB残余溶剂脱附量较小,仅为4.7mg/g,同溶剂重结晶法制备TATB相比,约为其残余溶剂脱附量的1/21;试验温度和溶剂溶解度是调控纳米TATB晶体生长的两个关键控制条件,通过调控试验温度和溶剂溶解度,可实现TATB粒径的控制生长;拉曼光谱结果显示TATB物相结构未发生变化;热分解结果表明随着TATB平均粒径从3μm增至17μm,其对应的热分解表观活化能E_(a)从208.366kJ/mol增至211.753kJ/mol。

To prepare TATB with different particle sizes,nano-TATB was exposed to the solvent dimethyl sulfoxide(DMSO) atmosphere,which was used to induced and controlled the growth of TATB particles.And then,the morphology of the prepared TATB crystals was observed by field emission scanning electron microscope.The characteristic peaks of TATB were measured by Raman spectroscopy and Fourier transform infrared spectroscopy.The thermal decomposition performance of TATB was analyzed by differential scanning calorimetry(TG-DSC).A solvent atmosphere induction method was proposed,and the effects of solvent atmosphere,test temperature and reaction time on TATB particle size and morphology were studied.The experimental results show that the solvent atmosphere induction method can induce the growth of nano-TATB with a particle size range of 1—17μm and regulate the microscopic morphology.Compared with the method of preparing TATB in solvent,the desorption amount of residual solvent in the preparation of TATB by solvent atmosphere induction method is significantly less,only 4.7mg/g,which is about 1/21 of the former.It is also found that the test temperature and solvent solubility are two key control conditions for regulating the growth of nano-TATB crystals,and the growth of TATB particle size can be controlled by adjusting the test temperature and solvent solubility.Raman spectroscopy results show that the phase structure of TATB prepared by solvent atmosphere induction does not change.The thermal decomposition results show that with the increase of the average particle size of TATB from 3μm to 17μm,the apparent activation energy E_(a) of thermal decomposition increases from 208.366kJ/mol to 211.753kJ/mol.