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以四乙酰基二苄基六氮杂异伍兹烷为基质,经亚硝解脱苄合成了四乙酰基二亚硝基六氮杂异伍兹烷(TADNSIW);用纯硝酸氧化TADNSIW制备四乙酰基二硝基六氮杂异伍兹烷(TADNIW),收率93.0%,以上两步反应均在室温下完成。在85℃条件下,TADNIW经硝硫混酸硝解合成了六硝基六氮杂异伍兹烷(HNIW),反应时间50 m in,收率95.1%,质量分数98.80%。用硝硫混酸对TADNSIW进行硝解合成了HNIW,并优化了反应条件,反应温度90℃,反应时间60 m in,硝解剂必须大于14 mL(底物TADNSIW 1.2 g),收率为96.1%,质量分数98.87%。分别用FTIR,1HNMR和元素分析对目标化合物进行了表征。前体TADNSIW和TADNIW分子中只有乙酰基和亚硝基,它们的硝解反应体系较简单,反应时间短、反应条件温和,母液中只含有乙酸和硝解剂,产物易分离。 相似文献
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四乙酰基二苄基六氮杂异伍兹烷亚硝解脱苄反应 总被引:1,自引:3,他引:1
利用市售无机亚硝解试剂,采用3种不同的方法,在温和条件(30℃左右)下,使四乙酰基二苄基六氮杂异伍兹烷(TADBIW)脱除苄基,转化成HNIW的前体——四乙酰基二亚硝基六氮杂异伍兹烷(TADNSIW),并用FT-IR、MS、^1HNMR及元素分析法对TADBIW的脱苄产物进行了结构鉴定。提出了TADBIW亚硝解脱苄反应的机理,TADBIW作为三级胺脱除苄基的反应是以生成烯胺正离子(或称亚胺正离子)为中间体的反应,并由所获得的副产物苯甲醛证明该反应机理。 相似文献
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制备六硝基六氮杂异伍兹烷的硝解工艺近期进展 总被引:3,自引:0,他引:3
六硝基六氮杂异伍兹烷(HN研)是当今已工业化生产的能量水平最高的炸药,HNIW的制备包括基本母体的合成、母体的氢解、氢解产物(硝解底物)的硝解(即生成HN研)及HNIW的转晶4步。综述了近几年来制备HNIW的硝解工艺的进展(包括作者的若干研究成果),详细报道了硝解3种底物([四乙酰基二苄基六氮杂异伍兹烷(TADBIW)、四乙酰基二甲酰基六氮杂杂异伍兹烷(TADFIW)及四乙酰基六氮杂异伍兹烷(TAIW])以制备HNIW的工艺条件,并评价了各自的优、缺点。 相似文献
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四乙酰基二氯乙酰基六氮杂异伍兹烷硝解产物中副产物的分离和鉴定 总被引:1,自引:0,他引:1
硝解四乙酰基二氯乙酰基六氮杂异伍兹烷 (TADCIW)制备四硝基二氯乙酰基六氮杂异伍兹烷 (TNDCIW)时 ,所得产物经薄层色谱 (TL C)检测发现含有少量副产物。采用柱色谱分离出了该副产物 ,经 FTIR、1H- NMR、MS(CI)及元素分析对副产物的结构进行鉴定 ,确定它为五硝基一氯乙酰基六氮杂异伍兹烷 (PNMCIW) ,这为改进 TADCIW的硝解条件提供了依据。 相似文献
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乙烯酮(双乙烯酮)是十分重要的化工中间体,其下游产品较多。江苏某化工厂开发生产乙烯酮(双乙烯酮)下游产品三十多个,年生产规模三万多吨,是国内以乙烯酮(双乙烯酮)为中间体生产精细化学品的综合骨干企业。针对乙烯酮(双乙烯酮)下游产品废水特点,该厂结合企业实际,开展了产品优化,结构调整,清洁生产,资源循环利用,节水降耗等工作,从源头削减了污染物的生产。同时投资二千多万元新建预处理装置三套,6000m3/d废水生化处理装置一套,使全厂乙烯酮(双乙烯酮)下游产品的废水得到了有效的治理。 相似文献
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D. G. Gordeev L. F. Gudarenko M. V. Zhernokletov V. G. Kudel’kin M. A. Mochalov 《Combustion, Explosion, and Shock Waves》2008,44(2):177-189
A semi-empirical equation of state for metals is described. Its capabilities are demonstrated by the example of the equation
of state for aluminum. New experimental data are presented on the location of the isentrope of aluminum for unloading from
the state at p = 229.71 GPa on the shock adiabat to an aerogel (SiO2) of density 0.08 g/cm3.
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Translated from Fizika Goreniya i Vzryva, Vol. 44, No. 2, pp. 61–75, March–April, 2008. 相似文献
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Jorge Marcelo Romero Soledad Bustillo Hugo Enrique Ramirez Maisuls Nelly Lidia Jorge Manuel Eduardo Gómez Vara Eduardo Alberto Castro Alicia H. Jubert 《International journal of molecular sciences》2007,8(7):688-694
A thermochemical rather simple experimental technique is applied to determine the enthalpy of formation of Diperoxide of ciclohexanone. The study is complemented with suitable theoretical calculations at the semiempirical and ab initio levels. A particular satisfactory agreement between both ways is found for the ab initio calculation at the 6–311G basis This set level. Some possible extensions of the present procedure are pointed out. 相似文献
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A perturbation viscometer is a differential capillary viscometer that measures the logarithmic viscosity gradient of the viscosity-composition curve for gas mixtures. Measurements are made at different gas mixture compositions. Integration of the logarithmic viscosity gradients measured over the full composition range gives the mixture viscosity relative to the viscosity of one of the pure components of the gas mixture. This method is attractive because, for measurements of equal precision, integration of the gradients is potentially an order of magnitude more precise than measurement of the viscosities directly. It can also work at high and low temperatures and perhaps high pressures.The perturbation viscometer has been used to make measurements on ideal gas mixtures at ambient and elevated temperatures. The situation is more complicated when the gas mixtures are non-ideal. Extra effects due to density differences, molar volume change on mixing and differential thermal expansion may be measured in addition to the desired viscosity change producing systematic errors in the results. Thus, a more sophisticated apparatus is required. The standard perturbation viscometer has been modified to separate out the extra effects to permit measurement of the true change in viscosity. In addition, the theoretical operation of the modified apparatus has been revised to account for the design changes to permit calculation of the viscosity-composition profiles from the results.The apparatus has been tested using helium-HFC-125 mixtures and two new viscosity-composition profiles are presented for these mixtures at 23 and . Internal consistency tests have been used to confirm that the data produced are of high quality with an estimated uncertainty in the viscosity ratio data at of 0.9% and at of 1.5%. 相似文献
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塔设备改造选型的分析 总被引:2,自引:0,他引:2
就当前扩产增容中塔设备设计和改造时板式塔和填料塔的选型问题加以分析。在评述目前国内常用的几种塔板和新型填料之后,着重介绍一种新型塔板(导向梯形浮阀塔板)和一种新型填料(波环填料——乾隆帕克)。 相似文献