【作者】 毛峰；

【导师】 许文林；

【作者基本信息】 扬州大学 ， 应用化学， 2007， 硕士

【摘要】 蒽、菲、咔唑是煤焦油中的主要组分,是精细化工的重要原料。在我国大多数的工厂中,由粗蒽制取精蒽、精菲和精咔唑常使用溶剂萃取结晶法。因此,蒽、菲和咔唑在有机溶剂中的溶解度数据对其工艺的改进具有重要的指导意义。但迄今为止有关这方面的研究甚少,使用的有机溶剂不多,且实用性不强。虽然蒽、菲、咔唑在有些有机溶剂中的溶解度报道过,但是它们都缺乏理论上的探讨,不能从根本上了解这些溶剂之间的差别。本文实验测定了蒽、菲和咔唑在DMF(N,N–二甲基甲酰胺)、DMA(N,N–二甲基乙酰胺)和NMP(1–N–2甲基吡咯烷酮)中的溶解度数据,理论分析了蒽、菲和咔唑在溶剂中溶解度大小差异的原因,并用溶解度-温度经验关系式lnx=A +BlnT进行了关联。同时应用基团贡献法建立了蒽、菲、咔唑在DMF,DMA和NMP中的溶解度的模型方程,采用MATLAB语言对模型方程进行了求解,计算得到了蒽和菲在DMF、DMA和NMP中的溶解度,并将计算结果与实验测得到的结果进行了比较。蒽在DMF、DMA和NMP中溶解度的计算值与实验值的平均相对偏差分别为43.23%,36.38%和27.49%,菲在DMF、DMA和NMP中溶解度的计算值与实验值的平均相对偏差分别为6.80%,5.07%和0.97%,但两者总体规律一致,随着温度的升高溶解度都急剧增加,且它们在DMF、DMA和NMP中的溶解度大小顺序一致。因此,UNIFAC可以较好的预测蒽和菲在DMF,DMA和NMP中的溶解特性,应用UNIFAC计算可以为粗蒽的分离选取合适的溶剂和优化工艺提供一定的理论依据。最后,本文对用溶剂结晶分离蒽、菲和咔唑的结晶条件进行了研究,得到了结晶分离蒽、菲和咔唑的最佳结晶条件。蒽、菲和咔唑中的大量的菲可以先由苯在常温下溶解萃取除去,DMF在溶解温度80℃,结晶温度20℃,养晶时间1h,固液比1.8g/ml时候对分离蒽和咔唑混合物中的咔唑效果最好。更多还原

【Abstract】 Anthracene,phenanthrene and carbazole is the main component of coal tar and the important raw material of fine chemical. During the process of the separation and extraction of anthracene,phenanthrene and carbazole from coal tar by solvent extraction, the optimization of process conditions and the rational choice of solvents are closely related to the solubility of anthracene,phenanthrene and carbazole in solvents. It is very important to measure the solubility of anthracene,phenanthrene and carbazole in different solvents for improving the extraction process.The solubility of anthracene, phenanthrene and carbazole in N , N-dimethyformamide (DMF), N,N-dimethylacetamide(DMA) and N–methyl- 2-pyrrolidone (NMP) was determined in the temperature range from 20 to 95℃using a liquid-solid phase equilibrium method. The solubility behavior of anthracene ,phenanthrene and carbazole in DMF、DMA and NMP was also obtained using the UNIFAC group contribution method and the model equations were solved by MATLAB. The comparative average error between the calculated results and experimental data of anthracene is 43.23%,36.38% and 27.49% in DMF、DMA and NMP respectively, which is 6.80%,5.07% and 0.97% for phenanthrene. The UNIFAC model can be applied to predict the solubility of anthracene in DMF、DMA and NMP. The work provides a elementary basis for selecting a solvent and optimizing process during the separation and purification of crude anthracene process by solvent methods.Through the experiment, it is known that the dissolving effect of benzene to Phenanthrene in some studied organic solvent is best, moreover DMF to carbazole is best. So benzene and DMF from the some solvents can be used to separate crude anthracene. At 80℃,crystal-keeping time 60min, the solvent ratio 1.8g / m1, the effect of DMF is the best to separate carbazole from the compound of anthracene and carbazole.更多还原