富勒烯对甲基苯胺衍生物的合成及其对硝化棉安定性的影响

Synthesis of Fullerene p-Methylaniline Derivative and Its Effect on the Stability of Nitrocellulose

以富勒烯(C_(60))、溴素(Br_(2))、八溴富勒烯(C_(60)Br_(8))及对甲基苯胺(C_(7)H_(9)N)为原料,经两步反应合成了富勒烯对甲基苯胺衍生物C_(60)(NC_(6)H_(4)CH_(3))_(n);采用核磁共振碳谱(^(13)C-NMR)、质谱(MS)、X射线光电子能谱(XPS)、傅里叶变换红外光谱仪(FT-IR)以及紫外-可见光分光光度计(UV-Vis)对合成得到的富勒烯对甲基苯胺衍生物结构进行了表征;采用差热分析(DTA)、真空安定性测试(VST)、热重分析(TGA)、甲基紫实验等热分析方法,并结合电子顺磁共振波谱法研究了富勒烯对甲基苯胺衍生物与硝化棉的相互作用规律和机理。结果表明,富勒烯对甲基苯胺衍生物将甲基紫试纸的变色时间由56min延长至95min;将单位质量硝化棉热分解释放的气体量由2.67mL/g降至1.46mL/g;将硝化棉的热失重率由17.17%降至5.46%;当富勒烯对甲基苯胺衍生物的质量浓度为0.76g/L时,其对氮氧自由基的清除率达到50%。表明富勒烯对甲基苯胺衍生物提高了硝化棉的安定性,且安定性能明显优于传统安定剂DPA和C2。

Fullerene p-methylaniline derivative C_(60)(NC_(6)H_(4)CH_(3))_(n)was synthesized via a two-step reaction by using fullerene,Br_(2),C_(60)Br_(8)and p-toluidine as raw materials.The structure of fullerene p-methylaniline derivative was characterized by nuclear magnetic resonance(^(13)C NMR),mass spectrometry(MS),X-ray photoelectron spectroscopy(XPS),Fourier transform infrared spectroscopy(FT-IR)and ultraviolet-visible spectrophotometer(UV-Vis).Thermal analysis methods such as differential thermal analysis(DTA),vacuum stability test(VST),thermogravimetric analysis(TGA)and methyl violet test were used to study the interactive mechanism between fullerene p-methylaniline derivative and nitrocellulose.The results show that C_(60)(NC_(6)H_(4)CH_(3))_(n)can prolong the discoloration time of methyl violet test paper from 56min to 95min.The gas released by the thermal decomposition of nitrocellulose is reduced from 2.67mL/g to 1.46mL/g,and the thermal mass loss rate of nitrocellulose is decreased from 17.17%to 5.46%.When the concentration of C_(60)(NC_(6)H_(4)CH_(3))_(n)is 0.76g/L,the scavenging rate of nitroxide radical reaches to 50%.It reveals that C_(60)(NC_(6)H_(4)CH_(3))_(n) can enhance the stability of nitrocellulose,and its stability is better than DPA and C2.