溶剂-非溶剂法制备纳米FOX-7及其性能
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摘要
以N,N-二甲基乙酰胺(DMAC)、N-甲基吡咯烷酮(NMP)及两者的混合物为溶剂,通过溶剂-非溶剂法制备了纳米1,1-二氨基-2,2-二硝基乙烯(FOX-7)。通过场发射电子显微镜(FE-SEM)、X射线衍射(XRD)、傅里叶变换红外光谱(FT-IR)、差示扫描量热法(DSC)和热重分析法(TG)对所制备的纳米FOX-7的形貌、物相、结构和热性能进行了表征,并对样品的感度进行了测试;在此基础上,研究了溶剂、表面活性剂对纳米FOX-7性能的影响。结果表明:所制备的纳米FOX-7平均晶粒尺寸小于30 nm。添加表面活性剂有助于降低纳米FOX-7的晶粒尺寸及颗粒尺寸,提高其粒度分布均匀性,改善其分散性。与原料相比,所制备的纳米FOX-7的初始分解温度提高,两个分解放热峰之间温度范围变窄,能量释放效率及分解焓有较大的提高,撞击感度与摩擦感度明显降低。当采用混合溶剂并添加表面活性剂OP-10和Tween 20时,所制备的纳米FOX-7的初始分解温度都提高近15℃,分解焓分别提高了4.97%,4.65%,摩擦感度降低了66.7%,50.0%。
Nano-1,1-diamino-2,2-dinitroethylene(FOX-7)was prepared by the solvent-non-solvent method using N,N-dimethyl-acetamide(DMAC),N-methylpyrrolidone(NMP)and a mixture of the two as solvents. The morphology,phase,structure and thermal performances of the prepared nano-FOX-7 were characterized by field emission scanning electron microscope(FE-SEM),X-ray diffraction(XRD),Fourier transform infrared spectroscopy(FT-IR),differential scanning calorimetry(DSC)and thermogravimetric analysis(TG)method and its sensitivities were tested. On this basis,the effects of solvents and surfactants on the performances of nano-FOX-7 were investigated. The results show that the average grain size of the prepared nano-FOX-7 is less than 30 nm. The addition of surfactant is helpful to reduce the grain size and particle size of the prepared nano-FOX-7,en-hance its uniformity of particle size distribution and improve its dispersity. Compared with the raw material,the initial decompo-sition temperatures of the prepared nano-FOX-7 increase,the temperature ranges between their two decomposition exothermic peaks become narrow,their energy release efficiency and decomposition enthalpy greatly increase and the impact and friction sensitivities significantly reduce. When using the mixed solvents and adding the surfactants OP-10 and Tween 20,the initial de-composition temperatures of the prepared nano-FOX-7 increase nearly by 15 ℃,the enthalpies of decomposition increase by 4.97% and 4.65% respectively. And the friction sensitivities decrease by 66.7% and 50.0% respectively.
Nano-1,1-diamino-2,2-dinitroethylene(FOX-7)was prepared by the solvent-non-solvent method using N,N-dimethyl-acetamide(DMAC),N-methylpyrrolidone(NMP)and a mixture of the two as solvents. The morphology,phase,structure and thermal performances of the prepared nano-FOX-7 were characterized by field emission scanning electron microscope(FE-SEM),X-ray diffraction(XRD),Fourier transform infrared spectroscopy(FT-IR),differential scanning calorimetry(DSC)and thermogravimetric analysis(TG)method and its sensitivities were tested. On this basis,the effects of solvents and surfactants on the performances of nano-FOX-7 were investigated. The results show that the average grain size of the prepared nano-FOX-7 is less than 30 nm. The addition of surfactant is helpful to reduce the grain size and particle size of the prepared nano-FOX-7,en-hance its uniformity of particle size distribution and improve its dispersity. Compared with the raw material,the initial decompo-sition temperatures of the prepared nano-FOX-7 increase,the temperature ranges between their two decomposition exothermic peaks become narrow,their energy release efficiency and decomposition enthalpy greatly increase and the impact and friction sensitivities significantly reduce. When using the mixed solvents and adding the surfactants OP-10 and Tween 20,the initial de-composition temperatures of the prepared nano-FOX-7 increase nearly by 15 ℃,the enthalpies of decomposition increase by 4.97% and 4.65% respectively. And the friction sensitivities decrease by 66.7% and 50.0% respectively.
引文
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[28]Qingping Luo,Chonghua Pei,Guixiang Liu,et al.Insensitive High Cyclotrimethylenetrinitramine(RDX)nanostructured ex-plosives derived from solvent/nonsolvent method in a bacterial cellulose(BC)gelatin matrix[J].Nano,2015,10(3):1550033-1-1550033-8.
[29]付秋菠.1,1-二氨基-2,2-二硝基乙烯的合成及其性能研究[D].成都:四川大学,2007:34-40.FU Qiu-bo.Synthesis and properties of 1,1-diamino-2,2-dini-troethylene[D].Chengdu:Sichuan University,2007:34-40.
[30]Wang K,Zhang W,Phelan R,et al.Direct fabrication of well-aligned free-standing mesoporous carbon nanofiber ar-rays on silicon substrates[J].Journal of the American Chemical Society,2007,129(44):13388-13389.
[31]Prodan E A.Localization phenomena of topo chemical reac-tions[J].Journal of Thermal Analysis,1984,29(5):941-948.
[32]Zohari N,Keshavarz M H,Seyedsadjadi S A.The advantages and shortcomings of using nano-sized energetic materials[J].Central European Journal of Energetic Materials,2013,10(1):135-147.
[2]Bellamy A J.FOX-7(1,1-diamino-2,2-dinitroethene):high en-ergy density materials[M].Springer Berlin Heidelberg,2007:1-33.
[3]Latypov N V,Bergman J,Langlet A,et al.Synthesis and reac-tions of 1,1-diamino-2,2-dinitroethylene[J].Cheminform,1998,30(1):11525-11536.
[4]Hudson R J,Zioupos P,Gill P P,et al.Investigating the me-chanical properties of RDX crystals using nano-indentation[J].Propellants,Explosives,Pyrotechnics,2012,37(2):191-197.
[5]Zhang C,Peng Q,Wang L,et al.Thermal sensitivity of HMXcrystals and HMX-based explosives treated under various con-ditions[J].Propellants,Explosives,Pyrotechnics,2010,35(6):561-566.
[6]However.Nano-CL-20/HMX cocrystal explosive for significant-ly reduced mechanical sensitivity[J].Journal of Nanomaterials,2017,2017(5):1-7.
[7]于佳莹,王建华,刘玉存,等.CL-20/GO纳米复合含能材料的制备与性能研究[J].科学技术与工程,2017,17(12):93-96.YU Jia-ying,WANG Jian-hua,LIU Yu-cun,et al.Preparation and properties of CL-20/GO nanocomposite energetic materi-als[J].Science Technology and Engineering,2017,17(12):93-96.
[8]Han Gao,Xiao-ting Hou,Xiang Ke,et al.Effects of na-no-HMX on the properties of RDX-CMDB propellant:higher energy and lower sensitivity[J].Defence Technology,2017(5):323--326.
[9]Makhov M N.Energy content of HMX-silicon nano-powder mixtures[J].Russian Journal of Physical Chemistry B,2018,12(1):115-119.
[10]Liu J,Bao X Z,Rong Y B,et al.Preparation of na-no-RDX-based PBX and its thermal decomposition properties[J].Journal of Thermal Analysis&Calorimetry,2017(3):1-6.
[11]Doukkali M,Patel R B,Stepanov V,et al.The effect of ionic strength and ph on the electrostatic stabilization of nano-RDX[J].Propellants,Explosives,Pyrotechnics,2017,42(9).
[12]徐哲,李小东,边红莉,等.初始裂解产物对FOX-7裂解通道影响的理论研究[J].科学技术与工程,2017,17(10):36-39.XU Zhe,LI Xiao-dong,BIAN Hong-li,et al.Theoretical study on the effect of initial cracking products on FOX-7 cracking channel[J].Science Technology and Engineering,2017,17(10):36-39.
[13]孟增睿,尚丽平,杜宇,等.FOX-7太赫兹波吸收特性及理论计算[J].光谱学与光谱分析,2015,44(7):1121-1125.MENG Zeng-rui,SHANG Li-ping,DU Yu,et al.Absorption characteristics and theoretical calculation of FOX-7 terahertz wave[J].Infrared and Laser Engineering,2015,44(7):1121-1125.
[14]Taylor D E,Rob F,Rice B M,et al.A molecular dynamics study of 1,1-diamino-2,2-dinitroethylene(FOX-7)crystal us-ing a symmetry adapted perturbation theory-based intermolec-ular force field[J].Physical Chemistry Chemical Physics,2011,13(37):16629-16636.
[15]蔡华强,舒远杰,郁卫飞,等.FOX-7的合成和反应机理研究[J].化学学报,2004,62(3):295-301.CAI Hua-qiang,SHU Yuan-jie,YU Wei-fei,et al.Study on the synthesis and reaction mechanism of FOX-7[J].Acta Chimica Sinica,2004,62(3):295-301.
[16]宗和厚.FOX-7热分解机理及晶体特性的理论研究[D].绵阳:中国工程物理研究院,2007:44-50.ZONG He-hou.Theoretical study on thermal decomposition mechanism and crystal properties of FOX-7[D].Mianyang:China Academy of Engineering Physics,2007:44-50.
[17]Burnham A K,Weese R K,Wang R,et al.Thermal properties of FOX-7[J].Office of Scientific&Technical Information Technical Reports,2005:211114-211119.
[18]Huang B,Qiao Z,Nie F,et al.Fabrication of FOX-7 qua-si-three-dimensional grids of one-dimensional nanostructures via a spray freeze-drying technique and size-dependence of thermal properties[J].Journal of Hazardous Materials,2010,184(1-3):561-566.
[19]Cai H,Tian L,Huang B,et al.1,1-Diamino-2,2-dintroethene(FOX-7)nanocrystals embedded in mesoporous carbon FDU-15[J].Microporous&Mesoporous Materials,2013,170(4):20-25.
[20]Gao B,Wu P,Huang B,et al.Preparation and characteriza-tion of nano-1,1-diamino-2,2-dinitroethene(FOX-7)explo-sive[J].New Journal of Chemistry,2014,38(6):2334-2341.
[21]储峰,邓潘,樊祥,等.溶剂-非溶剂法在含能材料中的应用[J].化学推进剂与高分子材料,2010,8(3):38-41.CHU Feng,DENG pan,FAN xiang,et al.Application of sol-vent-non solvent method in energetic materials[J].Chemical Propellants&Polymeric Materials,2010,8(3):38-41.
[22]Fernandez E J,Laguna A,Lopez-De-Luzuriaga J M,et al.Gold-thallium supramolecular arrays with 4,4′-bipyridine sol-vent induction of luminescent networks[J].Dalton Transactions,2004,4(12):1801-1806.
[23]Celebre G,De L G,Maiorino M,et al.Solute-solvent interac-tions and chiral induction in liquid crystals[J].Journal of the American Chemical Society,2005,127(33):11736-11744.
[24]Yagi S,Morinaga T,Nomura T,et al.Solvent effect on helici-ty induction of zinc bilinone bearing a chiral auxiliary at the helix terminal[J].Journal of Organic Chemistry,2001,66(11):3848-3853.
[25]Bakshi M S,Sachar S,Kaur G,et al.Dependence of crystal growth of gold nanoparticles on the capping behavior of sur-factant at ambient conditions[J].Crystal Growth&Design,2008,8(5):1713-1719.
[26]Mitarai M,Kishimoto M,Suh D,et al.Surfactant effects on the crystal growth of clathrate hydrate at the interface of water and hydrophobic-guest Liquid[J].Crystal Growth&Design,2015,15(2):812-821.
[27]Gómez-Cisneros M,Trevi?o M E,Peralta R D,et al.Surfac-tant concentration effects on the microemulsion polymeriza-tion of vinyl acetate[J].Polymer,2005,46(9):2900-2907.
[28]Qingping Luo,Chonghua Pei,Guixiang Liu,et al.Insensitive High Cyclotrimethylenetrinitramine(RDX)nanostructured ex-plosives derived from solvent/nonsolvent method in a bacterial cellulose(BC)gelatin matrix[J].Nano,2015,10(3):1550033-1-1550033-8.
[29]付秋菠.1,1-二氨基-2,2-二硝基乙烯的合成及其性能研究[D].成都:四川大学,2007:34-40.FU Qiu-bo.Synthesis and properties of 1,1-diamino-2,2-dini-troethylene[D].Chengdu:Sichuan University,2007:34-40.
[30]Wang K,Zhang W,Phelan R,et al.Direct fabrication of well-aligned free-standing mesoporous carbon nanofiber ar-rays on silicon substrates[J].Journal of the American Chemical Society,2007,129(44):13388-13389.
[31]Prodan E A.Localization phenomena of topo chemical reac-tions[J].Journal of Thermal Analysis,1984,29(5):941-948.
[32]Zohari N,Keshavarz M H,Seyedsadjadi S A.The advantages and shortcomings of using nano-sized energetic materials[J].Central European Journal of Energetic Materials,2013,10(1):135-147.