由乙烯焦油调制石墨电极用浸渍剂沥青  

Preparation of Impregnating Pitch for Graphite Electrode from Ethylene Tar

作　　者：崔均烜 王艳莉[1] 沈春银[1] 詹亮[1] CUI Junxuan;WANG Yanli;SHEN Chunyin;ZHAN Liang(State Key Laboratory of Chemical Engineering,School of Chemical Engineering,East China University of Science and Technology,Shanghai 200237,China)

机构地区：[1]华东理工大学化工学院,化学工程联合国家重点实验室,上海200237

出　　处：《华东理工大学学报（自然科学版）》2024年第3期346-353,共8页Journal of East China University of Science and Technology

基　　金：国家自然科学基金(51472086,51002051,22075081,20806024);上海市自然科学基金(12ZR1407200)。

摘　　要：以乙烯焦油为原料,采用空气氧化法调制石墨电极用浸渍剂沥青。考察了氧化温度、氧化时间和空气流速对所制浸渍剂沥青物化性质的影响,并与煤系浸渍剂沥青进行比较。实验还采用激光解析质谱、傅里叶变换红外光谱、核磁共振、元素分析和旋转流变仪等表征手段对浸渍剂沥青的理化性质进行分析。结果表明,在乙烯焦油改性过程中,影响浸渍剂沥青物化性质的主要因素依次为:氧化温度>空气流速>氧化时间,较高的氧化温度有利于提高所制浸渍剂沥青的结焦值;较短的氧化时间和较低的空气流速能降低所制浸渍剂沥青的软化点,其相对较低的软化点有助于浸渍过程中的流动性。在氧化温度、氧化时间和空气流速分别为310℃、4 h和0.2 L/min的最佳制备条件下,所制浸渍剂沥青软化点、结焦值分别为93.44℃、46.73%(以质量分数表示),喹啉不溶物(QI)质量分数低于0.1%,并且S、N和O等杂原子的含量很低,具有更好的流动性,有望达到良好的浸渍效果。Impregnating pitch for graphite electrode is synthesized by air oxidation method using ethylene tar as raw material.The effects of oxidation temperature,oxidation time and air flow on the physicochemical properties of impregnating pitch were investigated,and compared with the coal tar-based impregnating pitch.The physicochemical properties of the obtained impregnating pitch were systematically characterized by laser desorption mass spectrometry,Fourier transform infrared spectroscopy,nuclear magnetic resonance,elemental analysis and rotational rheometer.In the process of ethylene tar modification,the main factors that affect the physicochemical properties of the impregnating pitch are:oxidation temperature>air flow>oxidation time.A higher oxidation temperature is beneficial for the increase of the coking value of the obtained impregnating pitch.A lower air flow and a shorter oxidation time are conducive to reducing the softening point of the obtained impregnating pitch,which is favorable for the fluidity during the impregnation.Under the optimized preparation conditions with the oxidation temperature of 310℃,oxidation time of 4 h,and air flow of 0.2 L/min,the softening point and coking value of the obtained impregnating pitch are 93.44℃and 46.73%(mass fraction),respectively.Moreover,there is a quinoline insoluble(QI)mass fraction of less than 0.1%,lower concentrations of S,N and O heteroatoms and better rheological properties,which is expected to achieve good impregnation effect.

关 键 词：乙烯焦油 空气氧化 浸渍剂沥青 喹啉不溶物 石墨电极 

分 类 号：TQ522.65[化学工程—煤化学工程]