CF_3SO_3H/H_2O喷射结晶制备纳米TATB

为获得粒度可控、纯度较高的纳米1,3,5-三氨基-2,4,6-三硝基苯(TATB),采用三氟甲磺酸为溶剂,去离子水为非溶剂,通过喷射结晶法制备了纳米TATB。研究了制备工艺及p H对TATB粒度和纯度的影响规律。用场发射扫描电镜(FE-SEM)、BET(Brunauer-Emmett-Teller)比表面积测试、X射线衍射(XRD)、高效液相色谱(HPLC)和差示扫描量热(DSC)等对纳米TATB的形貌、比表面积、晶体结构、纯度和热分解特性进行了表征。结果表明,喷射过程中溶剂-非溶剂的体积比可以影响纳米TATB形貌和粒度,随着溶剂/非溶剂比例的减小,样品的粒径变小,颗粒更均匀;在溶剂与非溶剂的体积比为1∶50的条件下,可以获得粒径为60nm、颗粒均匀、比表面积为31.6 m~2·g~(-1)的纳米TATB。p H值对纳米TATB的纯度影响很关键,用水洗至p H=7,样品纯度可以达到98.1%。

Preparation of Nano-TATB from CF3SO3H/H2O by Spraying Crystallization

To obtain nano-1, 3, 5-triamino-2, 4, 6-trinitrobenzene(TATB) with controllable particle size and higher purity, nano-TATB was prepared by a spraying recrystallization method with trifluoromethanesulfonic acid as solvent and deionized water as non-solvent. The influence of preparation technology and pH on the particle size and purity of nano-TATB was studied. The morphology, specific surface area, crystal structure, purity and thermal decomposition characteristics of nano-TATB were characterized by field emission scanning electron microscopy(FE-SEM), BET(brunauer-emmett-teller) specific surface area test, high performance liquid chromatography(HPLC) and differential scanning calorimetry(DSC), etc. Results show that the volume ratio of solvent to non-solvent can affect the morphology and particle size of nano-TATB. With the decreasing volume ratio of solvent to non-solvent, the particle size of the sample becomes smaller and the size distribution is more uniform. Under the condition of volume ratio 1:50 and pH=7, nano-TATB particles with the size of 60 nm, uniform particles and specific surface area of 31.6 m²·g^-1 are obtained. The effect of pH value on the purity of nano-TATB is very important, with water washing to pH=7, the purity of the sample can reach 98.1%.