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间苯三酚合成研究进展 总被引:1,自引:0,他引:1
间苯三酚是一种比较昂贵的重要中间体,工业合成具有一定的技术难度.阐述了国内外间苯三酚合成技术的研究进展,包括(异丙)苯法、三硝基甲苯法、氯代苯法、苯胺法等具有工业化价值的几种工艺路线的收率、工艺条件及工业化可行性.#建议国内企业应该采用较为先进的(异丙)苯法或氯代苯法工艺提高产品质量. 相似文献
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为了提高六硝基六氮杂异伍兹烷(CL-20)的安全性,采用机械混合法和重结晶法分别制备了CL-20/TATB混合物;通过光学显微镜、扫描电子显微镜(SEM)、X-射线衍射(XRD)、差示扫描量热仪(DSC)、感度测试仪对其形貌、晶型、热稳定性、机械感度进行测试分析。结果表明,机械混合后CL-20表面无明显包覆物,而重结晶混合粒子表面有一层致密的黄色薄膜,同时两种混合物中CL-20的晶型仍为ε型,未发生晶型转变;两种混合物的热分解表观活化能较原料CL-20分别提高了17.3、117.36kJ/mol,热爆炸临界温度分别提高了0.12、3.8℃,重结晶混合粒子的热稳定性明显提高;两种混合物的撞击感度(H50)较原料CL-20分别提高了10.4、54.5cm,摩擦感度的临界载荷分别提高了80、60N,表明重结晶混合粒子的机械感度显著降低。 相似文献
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以苯胺为原料,经废氢溴酸溴化、脱胺基、甲氧基化、路易斯酸脱甲基四步合成间苯三酚,总收率为67.5%。考察了各种影响因素对合成反应的影响,获得了较佳工艺条件,并对产品后处理作了相应的研究。 相似文献
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研究了间苯三酚在非质子极性溶剂中,以18-冠醚-6作催化剂的Williamson反应,轩合成了间苯三酚的单辛基、二辛基和三辛基醚,并对反应条件和产物组成关系进行了讨论。 相似文献
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为考察声化学胺化法合成1,3,5-三氨基-2,4,6-三硝基苯(TATB)的应用前景,以1,3,5-三氯-2,4,6-三硝基苯(TCTNB)和氨水为原料,用声化学胺化法合成了TATB,考察了超声波作用方式对TATB粒径的影响。得到的目标产物TATB的质量分数达到97%以上,产率达到90%。采用红外光谱、核磁共振氢谱、质谱、X射线衍射及元素分析鉴定了TATB的结构。DSC测定其分解点为383.8℃;激光粒度仪测试其粒径,由探头式超声波得到的TATB平均粒径为2.46μm,由水槽式超声波得到的TATB平均粒径为14.07μm;氧瓶燃烧法测得TATB中氯质量分数低于0.2%。各项指标均达到了TATB国军标要求。声化学胺化法制备TATB反应条件温和、粒径可控、能耗低、基本排除了安全隐患。 相似文献
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用DSC-TG研究了TATB的热分解过程。根据升温速率分别为5、10、15、20K/min的DSC和TG-DTG曲线计算了分解反应的活化能(E)、指前因子(A)和120℃时的速率常数(k120),并计算了升温速率为5K/min时,TATB分解峰值温度时的分解反应活化焓、活化熵和活化自由能,用小容量测试法研究了TATB在1-乙基-3-甲基咪唑醋酸盐/二甲基亚砜([Emim]Ac/DMSO)溶剂中的热爆炸特性。结果表明,采用Kissinger法和Ozawa法计算得到TATB分解反应的活化能分别为212.1和212.0kJ/mol,采用Rogers公式和Arrhenius公式计算得到A和k120值分别为5.87×1016s-1和3.87×10-12s-1;升温速率为5K/min条件下,TATB分解峰值温度时的分解反应活化焓、活化熵和活化自由能分别为206kJ/mol、61.42J/(K·mol)和167.39kJ/mol,TATB粉末的临界爆炸温度为336.6℃;TATB在[Emim]Ac/DMSO溶剂中不爆炸。 相似文献
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Guangcheng Yang Fude Nie Hui Huang Lin Zhao Wanting Pang 《Propellants, Explosives, Pyrotechnics》2006,31(5):390-394
Nano‐TATB was prepared by solvent/nonsolvent recrystallization with concentrated sulfuric acid as solvent and water as nonsolvent. Transmission Electron Microscopy (TEM) and Atomic Force Microscopy (AFM) were used to characterize the appearance and the size of the particles. The results revealed that nano‐TATB particles have the shape of spheres or ellipsoids with a size of about 60 nm. Due to their small diameter and high surface energy, the particles tended to agglomerate. By using X‐ray powder diffraction (XRD), broadening of diffraction peaks and decreasing intensity were observed, when the particle sizes decreases to the nanometer size range. The corrected average particle size of nano‐TATB was estimated using the Scherrer equation and the size ranged from 27 nm to 41 nm. Furthermore, the specific surface area and pore diameter of nano‐TATB were determined by BET method. The values were 22 m2/g and 1.7 nm respectively. Thermogravimetric (TG) and Differential Scanning Calorimetric (DSC) curves revealed that thermal decomposition of nano‐TATB occurs in the range of 356.5 °C–376.5 °C and its weight loss takes place at about 230 °C. Furthermore, a slight increase in the weight loss was observed for nano‐TATB in comparison with micro‐TATB. 相似文献
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Alan K. Burnham Keith R. Coffee Gregory L. Klunder Adele F. Panasci-Nott John G. Reynolds 《Propellants, Explosives, Pyrotechnics》2024,49(2):e202300121
TATB (1,3,5-triamino-2,4,6-trinitrobenzene) was thermally degraded by two small-scale analytical methods – simultaneous differential scanning calorimetry and thermogravimetric analysis (SDT) and a hot-stage microscope with Fourier Transform Infrared (FTIR) analysis capabilities. SDT used ramped heating, isothermal soaking, and thermal pretreatment at various conditions. The heat flow and mass loss were monitored during various treatment conditions to derive chemical decomposition kinetics and Arrhenius parameters. FTIR experiments used isothermal heating, and changes were monitored spectroscopically. Solid samples generated at specific conditions were collected from both methods and were analyzed by DMSO extraction followed by chemical speciation by optical and mass spectrometric methods. Characterization provided the following reaction insights: 1. TATB decreases in a sigmoidal pattern in isothermally heated samples. Other soluble products gradually increase in concentration and then abruptly decline in concentration during the second exotherm, such as diamino-dinitro-benzofurazan and amino-nitro-benzodifurazan. 2. FTIR showed gradual changes in the amino and nitro functionality, shifting positions and decreasing intensity for the first 40 min. Then the solid gradually appeared more like an amorphous C with N incorporated, similar to previous studies on thermally degraded TATB-type materials. 3. Extracted residues (DMSO-soluble components removed) examined by FTIR showed an abrupt change in chemical composition between 40- and 45-min isothermal treatment, indicating early forming solids are different than later forming residues. 4. A reliable mass- and energy-balanced global reaction network must include at least two autocatalytic reactions, either in parallel or series, and at least one must have an explicit initiation reaction having a low activation energy. 相似文献
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采用溶剂/非溶剂法,在超声辅助的情况下,制备了TATB/HMX共晶炸药;探究了TATB/HMX共晶技术的影响因素;计算了TATB/HMX共晶炸药的理论密度和理论爆速;采用扫描电子显微镜(SEM)、X射线衍射仪(XRD)和差示扫描热量法(DSC)对其进行表征和热分析,并测试了其撞击感度。结果表明,制备TATB/HMX共晶的最佳工艺条件为:以[Emim]Ac/DMSO为复合溶剂,TATB和HMX投料比(摩尔比)为3∶7,温度为80℃,搅拌速率为500r/min;与原料相比,TATB/HMX共晶分子在结构上发生改变;TATB/HMX共晶炸药颗粒大小约为2μm,形貌为六边形晶体;共晶炸药的热安定性优于原料HMX,其特性落高比原料HMX高74cm,撞击感度明显降低;理论密度为1.891g/cm~3,理论爆速为8.758km/s,表明其爆炸性能良好。 相似文献
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Batikan Koroglu Alan K. Burnham Imren Mashiana Ana Racoveanu Christopher Arose Jonathan C. Crowhurst John G. Reynolds 《Propellants, Explosives, Pyrotechnics》2024,49(2):e202300124
This experimental study investigated the effects of confinement, starting mass, and heating rate on TATB thermal decomposition and sublimation using a combined Thermo-Gravimetric Analyzer and Differential Scanning Calorimetry (TGA/DSC) instrument. The confinement of volatile products was varied using different pinhole sizes with TGA/DSC pans. The measurements showed the open pan experiments without lids/pinholes resulted in complete sublimation of TATB between 320 °C and 360 °C. The heat of sublimation was determined to be 176 kJ/mol (42 kcal /mol), consistent with literature data obtained from other experimental techniques. The use of pinholes suppressed the sublimation of TATB such that the decrease in pinhole size resulted in 1) an increase in the enthalpy of reaction and an increase in the amount of carbonaceous material remaining at the end of decomposition, and 2) convergence of the two peak temperatures corresponding to maximum heat flow and maximum weight loss. Also, a transition from a two-exotherm thermal decomposition behavior towards a single-exotherm occurred as the pinhole size was decreased for a given starting mass or as the starting mass was increased for a given pinhole size. These results indicate the kinetics of TATB sublimation, TATB thermal decomposition, and gas diffusion out of a TGA/DSC pan can all compete and result in significantly different enthalpies, amounts of remaining materials, and peak temperatures depending on the pinhole size and starting mass used in the measurements. The results also indicate precise control of process variables (pinhole size, starting mass, and heating rate) in TGA/DSC measurements is required for thermal safety assessment of explosives. 相似文献