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以4,5-二碘邻苯二甲腈和全氟碘己烷为原料,合成了前驱体4,5-二全氟己基邻苯二甲腈,再合成2,3,9,10,16,17,23,24-八全氟己基钴酞菁(CoPc(C6F13)8)。前驱体结构经1HNMR、19FNMR、IR及MS表征确认,目标产物经HRMS、IR及紫外-可见吸收光谱分析确认。将其应用于氟两相体系催化乙苯氧化反应,考察其催化氧化性能,结果显示:以全氟辛烷为溶剂,催化剂用量为0.03 mmol,反应温度120 ℃,分子氧为氧源,反应6 h,在该条件下乙苯的转化率为41.8%,苯乙酮的选择性为85.3 %。氟碳相可以回收使用5次,催化活性基本保持不变。 相似文献
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以4-硝基邻苯二甲腈和水杨醛为原料,在无水碳酸钾的催化下合成了一种新的酞菁前驱体4-(水杨醛氧基)邻苯二甲腈。产物经IR、UV-Vis、^1HNMR及MS表征确认了其结构,同时对该物质的最佳合成条件进行了优化,产率达94.3%。 相似文献
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[目的] 2-(3-氯-2-氧代基)异吲哚啉-1,3-二酮是合成5-氨基乙酰丙酸的中间体,用催化氧化方法进行了合成。[方法]以邻苯二甲酰亚胺钾为主要原料,经与和环氧氯丙烷反应制备N-(2,3-环氧丙基)邻苯二甲酰亚胺,再经盐酸水解,TEMPO催化下PhI(OAc)_2氧化得到目标产物。[结果]在优化的反应条件下,2-(3-氯-2-氧代基)异吲哚啉-1,3-二酮的反应收率为93.1%。催化剂TEMPO可回收套用2次。结构经氢谱核磁分析确证。[结论] 2-(3-氯-2-氧代基)异吲哚啉-1,3-二酮合成工艺具有污染小、收率高和易于工业化生产等优点。 相似文献
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针对当前广泛使用的全氟辛酸及其盐类(PFOA)等含有C8全氟链段的化合物因对环境和人体健康存在潜在危害等问题,以全氟己基乙基碘为原料出发进行了温和条件下合成其替代品的研究。结果表明,第1步取代反应,当全氟己基乙基碘、H2O与NMP的摩尔比为1:3:22时,可以以86.2%的最高收率得到全氟己基乙醇;第2步氧化反应,当滴加时间和反应时间分别为1 h时,可以以91.3%的最高产率得到全氟己基乙酸。目标化合物的总收率为78.7%。该合成方法具有条件温和、收率高、反应路线短等特点,适用于工业化生产。 相似文献
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通过"一锅法"合成了含芳醚键的低聚双邻苯二甲腈单体,并以4,4'-双(4-氨基苯氧基)二苯砜(p-BAPS)为固化剂获得了具有较高稳定性和热氧稳定性的聚合物树脂。低聚邻苯二甲腈单体制备过程为过量间苯二酚与4'4-二氟二苯甲酮反应,以N,N-二甲基甲酰胺(DMF)/甲苯为溶剂,加入适量K2CO3,最后用4-硝基邻苯二甲腈进行封端。合成的低聚双邻苯二甲腈单体用IR及1H-NMR进行结构表征。该低聚物单体与4,4'-双(4-氨基苯氧基)二苯砜(p-BAPS)进行热交联形成一个密实的热固性材料。通过热重分析和差示扫描量热分析研究该聚合物树脂的固化性能及热氧稳定性,结果表明该聚合物固化温度在450℃左右,在氮气氛下开始分解的温度为330℃,因此该固化物具有优良的热稳定性和氧化稳定性。 相似文献
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以间苯二酚和乙酰乙酸乙酯为原料,在浓硫酸的催化下合成7-羟基-4-甲基香豆素。以4-硝基邻苯二甲酰亚胺为原料,通过氨水催化开环,三氯氧磷脱水制得4-硝基邻苯二甲腈。得到的7-羟基-4-甲基香豆素和4-硝基邻苯二甲腈经过亲核取代反应得到7-(3,4-二氰基苯氧基)-4-甲基香豆素。考察了7-羟基-4-甲基香豆素和4-硝基邻苯二甲腈的投料比、缚酸剂用量、反应温度和反应时间对反应的影响,最优反应条件为:n(7-羟基-4-甲基香豆素)∶n(4-硝基邻苯二甲腈)∶n(无水碳酸钾)=1.4∶1.0∶1.5,反应温度30℃,反应时间14 h,收率为63.7%,并通过红外吸收光谱、核磁共振氢谱和高效液相色谱(色谱纯度为99.30%)对合成的化合物的结构进行了确证。在该条件下适当放大实验条件得到收率基本在83.1%,比文献报道收率68%要高。 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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醋酸纤维素取代基分布与性质的关系 总被引:9,自引:0,他引:9
分析了以吡啶为溶剂的醋酸纤维素的13C-NMR核磁共振谱,得出了三种不同位置羟基的取代度。结合X—射线和DSC分析,初步说明具有相同取代度但未经水解和经过水解的醋酸纤维素(CA) 性质上的差异是由于三个羟基上的取代度分布不同及消晶程度差异所致。 相似文献