自升压-热聚合法制备蒽油基软沥青

Preparation of anthracene oil based soft pith by autogenous pressurizing and thermal polymerization

蒽油基软沥青具有分子量分布较窄、灰分低、碳含量高、芳香性较高等特点,是制备高品质炭素材料的优质前驱体。本文以蒽油为原料,采用自升压-热聚合法制备蒽油基软沥青。利用单因素法考察了反应条件对蒽油基软沥青性质的影响。当反应温度为450℃、反应压力为0.5 MPa、反应时间为7.5 h,制备出的蒽油基软沥青软化点(SP)为37℃、甲苯不溶物(TI)为11.91%、喹啉不溶物(QI)为0.72%、结焦值(CV)为28.51%。在此基础上,通过正交优化实验,发现自升压-热聚合法制备蒽油基软沥青最佳条件为:反应温度为455℃、反应时间为8h、反应压力为0.5 MPa,蒽油基软沥青的SP为48℃、TI为16.6%、QI为0.7%、CV为36.8%,蒽油基沥青的收率为62.4%。通过元素分析法、FTIR法和TGA法对蒽油基软沥青进行了表征研究。

Anthracene oil based soft pitch is a good precursor for production of high-quality carbon materials owing to its unique characteristics such as narrow distribution of molecular weight,low content of ash,high content of carbon,and moderately high aromaticity,etc. In the present work,anthracene oil based soft pitch has been produced by using the method of autogenous pressurizing and thermal polymerization. Through single factor analysis,the influence of reaction conditions on the properties of anthracene oil based soft pitch have been determined. The results show that,under the conditions of reaction temperature at 450 ℃,holding time of 7.5 h and reaction pressure of 0.5 MPa,the prepared anthracene oil based soft pitch has the softening point (SP) of 37 ℃,toluene insoluble (TI) of 11.91%,quinoline insoluble (QI) of 0.72%,and coking value (CV) of 28.51%. On this basis,through carrying out orthogonal optimization experiments the optimum condition for preparation of anthracene oil based soft pitch is found to be the reaction temperature of 455 ℃,holding time of 8 h and reaction pressure of 0.5 MPa,and the obtained anthracene oil based soft pitch has SP of 48 ℃,TI of 16.6%,QI of 0.7% and CV of 36.8% together with a yield of 62.4%. Moreover,the anthracene oil based soft pitch has also been characterized by using elemental analysis,FTIR and TGA analyses.