【作者】 徐安营；

【导师】 罗立文；

【作者基本信息】 中国石油大学 ， 化学工程与技术， 2011， 硕士

【摘要】 21世纪是环保的世纪，降低轻质油品的硫含量已成为一项迫切而重要的任务。目前各国都在加紧研究轻质油非加氢脱硫的新技术，超声波氧化脱硫技术是其中的研究热点之一。高铁酸钾是一种新型的强氧化剂，具有见效快、无残留毒性和不造成二次污染等突出优点，在氧化脱硫方面具有巨大的潜力。本论文使用次氯酸钾氧化法进行高铁酸钾的合成，研究显示：在0℃，次氯酸钾和硝酸铁的物料比为3:1，稳定剂的用量为0.043 g/g铁盐时具有较佳反应效果。其中，铁盐的分批加入时间为60 min；加完后继续反应45 min。产品经一次纯化后纯度即达到95 %以上，这为高铁酸钾工业化生产的实现提供了一定的参考依据。利用自制的高铁酸钾对正丁硫醇-环己烷模型化合物进行脱硫研究，得到的较优条件为：助剂为草酸调节pH值为4.0；高铁酸钾用量为0.003 g/mL模型化合物；超声波处理时间为7 min，脉冲时间为4 s；反应温度为50℃；与模型化合物等体积的甲醇萃取一次，萃取时间为45 min。紫外-可见光谱的标准曲线显示脱硫率能够达到85 %左右，气相色谱仪得到的结果与此基本一致。本文利用高铁酸钾对劣质柴油也进行了脱硫研究，结果显示：实验较优条件与上述体系基本相似，但高铁酸钾加入量为0.04 g/mL柴油，萃取时间为60 min。分光光度法的结果表明，当萃取液的吸光度值达到最大值时，相应的柴油吸光度值达到最低值。通过X-射线荧光光谱分析仪与气相色谱仪对脱硫效率进行表征，显示脱硫率能够达到72.0 %以上。在此条件下，柴油收率能够达到91.2 %左右。更多还原

【Abstract】 Environmental protection is one theme in the 21st century，desulfurization has been animportant and stringent mission. At present, the development of new technologies aboutnon-hydrogenation desulfurization is being studied in all countries. The oxidationdesulfurization is one of research hotspot. Potassium ferrate is a new type of strong oxidant,which bears many advantages such as rapidity, non-residual toxicity and non-secondarypollution. Hence, it exhibits great potential in the oxidation desulfurization.In this thesis , potassium ferrate was synthesized by the hypochlorite oxidation method.The studies display that the reaction has the best effect at 0℃when the molar ration ofpotassium hypochlorite and ferric nitrate is 3, and the weight ratio of stabilizer and ferric saltis 0.043. Meanwhile, the ferric salt is gradually added in 60 minutes, and the reaction is keptfor 45 minutes at 0℃. The purity quotient of product reaches 95% after the purification isconducted only one time, which provide some data for realizing the industrializationproduction of potassium ferrate.The desulfurization studies were conducted by adding above potassium ferrate to themodel mixture consisting of n-butyl mercaptan and cyclohexane. The optimum conditions areas follows: the pH value is 4.0, the ratio of potassium ferrate and model mixture is 0.003g/mL, the ultrasonic time is 7 minutes, the reaction temperature is 50℃, the impulse time is 4seconds, and the mixture is extracted for 45 minutes by using isometrical methanol. Theresults derived from the standard curve of UV-vis spectra show that the desulfurizationefficiency reaches 85 %, which is similar to result from the gas chromatograph.The desulfurization studies were also conducted by adding potassium ferrate to the baddiesel. The optimum conditions are similar to those of above-mentioned system, but theaddition value of potassium ferrate is 0.04 g/mL for the diesel, and the extraction time is 60 minutes. The results of spectrophotometry display that the absorbance of diesel reaches thesmallest value when the absorbance of the related extraction solution reaches the largest value.The desulfurization efficiency was characterized by X-ray fluorescence spectrometer and gaschromatography after extraction, and the results show that the rate of desulphurizationreaches72.0 %. Based on above conditions, the yield of diesel gets to 91.2 %.更多还原