石油炼制与化工 ›› 2025, Vol. 56 ›› Issue (11): 41-46.

• 基础研究 • 上一篇    下一篇

氧化温度对中间相沥青结构的影响

杨靖宇,焦玉凯,李明   

  1. 青岛农业大学化学与药学院
  • 收稿日期:2025-03-04 修回日期:2025-07-16 出版日期:2025-11-12 发布日期:2025-10-24
  • 通讯作者: 李明 E-mail:liming041424@163.com
  • 基金资助:
    中国博士后科学基金;山东省博士后创新项目

EFFECTS OF OXIDATION TEMPERATURES ON THE STRUCTURE OF MESOPHASE PITCH


  • Received:2025-03-04 Revised:2025-07-16 Online:2025-11-12 Published:2025-10-24

摘要: 对中间相沥青进行氧化交联处理可使其表现出优异的电化学性能,用于生产高性能碳材料。采用直接热缩聚法,以催化裂化油浆的富芳烃组分为原料制备中间相沥青,在不同温度下对其进行氧化处理。采用扫描电子显微镜、傅里叶变换红外光谱、X射线衍射和同步热分析等手段对氧化前后中间相沥青的微观结构、官能团、晶体结构以及热稳定性进行表征,探究氧化过程对中间相结构的影响。结果表明,经过氧化处理后中间相沥青的热稳定性显著提高。当氧化温度为130 ℃及130 ℃以下时,体系中主要发生脂肪族的脱除反应和芳烃的开环反应,并伴随芳香族小分子片层结构的增加。体系层间距最低为0.344 0 nm,结构最致密,分子层间的有序度下降。当氧化温度为160 ℃及160 ℃以上时,体系中以氧化交联反应为主。与氧化温度为130 ℃时相比,体系的芳香性降低,同时分子片层堆叠高度和有序度增加,微观结构中出现大量微团状的中间相沥青。

关键词: 中间相沥青, 氧化交联, 催化裂化油浆, 有序度, 晶体结构, 锂离子电池, 负极材料

Abstract: Oxidative cross-linking treatment of mesophase pitch can endow it with excellent electrochemical properties, enabling its use in the production of high-performance carbon materials. Mesophase pitch was prepared from the aromatic-rich fraction of FCC slurry and oxidized at different temperatures. Scanning electron microscope,fourier transform infrared spectroscopy,X-ray diffraction spectroscopy,and thermogravimetric analyzer were used to analyze the microstructure,functional groups, crystal structure,and thermal stability of the mesophase pitch before and after oxidation,respectively. The effect of the oxidation process on the structural properties of the mesophase pitch was investigated. The results showed that the thermal stability of the mesophase pitch significantly improved after oxidation treatment. When the oxidation temperature was 130 ℃ or below, the primary reactions occurring in the system were the removal of aliphatic groups and the ring-opening reactions of aromatic hydrocarbons, accompanied by an increase in the small aromatic molecular lamellar structures. The lowest interlayer spacing in the system was 0.3440 nm, indicating the most compact structure, while the orderliness between molecular layers decreased. When the oxidation temperature was 160 ℃ or above, oxidative cross-linking reactions dominated in the system. Compared to the case at an oxidation temperature of 130 ℃, the aromaticity of the system decreased, while the stacking height and orderliness of the molecular lamellae increased, and a large number of micro-globular mesophase pitch structures emerged in the microstructure.

Key words: mesophase pitch, oxidation cross-linking, FCC slurry, orderliness, crystal structure, lithium-ion battery, anode material