各向异性沥青的制备及其纺丝性能研究  

Preparation and spinning properties of anisotropic asphalt

作　　者：廖烈榜 陈彦君 王朝晖 LIAO Liebang;CHEN Yanjun;WANG Chaohui(Port Department of SINOPEC Hunan Petrochemical Co.,Ltd.,Yueyang 414014)

机构地区：[1]中石化湖南石油化工有限公司港口部,湖南岳阳414014

出　　处：《合成纤维工业》2024年第6期36-41,共6页China Synthetic Fiber Industry

基　　金：中国石化科技部资助项目(120030)。

摘　　要：以催化澄清油浆与渣油为原料,通过调控原料化学组成,采用热缩聚法调制各向异性沥青,再经纺丝、氧化、碳化、石墨化制得各向异性沥青基碳纤维,研究了调控前后原料的化学组成变化,热缩聚时间、温度对各向异性沥青物性的影响,并对各向异性沥青基碳纤维的热导率及力学性能进行了表征。结果表明:以催化澄清油浆与渣油为原料的混合料经过脱固、加氢等调控处理后,混合料中硫、氮含量下降,饱和脂肪烃的含量增大,芳烃含量降低;采用热缩聚法制备各向异性沥青,当热缩聚时间由2 h增加至12 h时,沥青中间相含量增大,当热缩聚温度由360℃升至420℃时,沥青的软化点提高,中间相、喹啉不溶物、甲苯不溶物含量增大,但收率降低;在热缩聚温度420℃下反应12 h制得的各向异性沥青的软化点为273℃、中间相质量分数为96.8%,且在光学下呈广域流线型;以制备的中间相质量分数为96.8%的各向异性沥青为前驱体进行纺丝,再经氧化、碳化、石墨化制得的高性能碳纤维直径为13μm,拉伸模量为648 GPa、拉伸强度为2.74 GPa、热导率为1128 W/(m·K)。Using catalytic clarified oil slurry and residual oil as raw materials,anisotropic asphalt was modulated by adjusting the chemical composition of raw materials and thermal polymerization and was produced into anisotropic asphalt based carbon fibers by spinning,oxidation,carbonization and graphitization.The change in the chemical composition of raw materials was studied before and after regulation,as were the effects of thermal polymerization time and temperature on the physical properties of anisotropic asphalt.And the thermal conductivity and mechanical properties of anisotropic asphalt based carbon fibers were characterized.The results showed that the sulfur and nitrogen contents decreased,the saturated fatty hydrocarbon content increased,and the aromatic hydrocarbon content decreased when the mixture of catalytic clarified oil slurry and residual oil as raw materials was subjected to modulation including desolidation and hydrogenation;the anisotropic asphalt was prepared by thermal polymerization method,the content of intermediate phase in the asphalt increased when the thermal polymerization time increased from 2 h to 12 h,and the softening point of the asphalt increased,and the contents of intermediate phase,quinoline insoluble matter and toluene insoluble matter increased,but the yield decreased when the thermal polymerization temperature increased from 360℃to 420℃;the anisotropic asphalt,which was obtained by reacting at a thermal polymerization temperature of 420℃for 12 h,had a softening point of 273℃and an intermediate phase mass fraction of 96.8%and showed a wide streamline shape under optical conditions;and a high-performance carbon fiber could be produced with a diameter of 13μm,tensile modulus of 648 GPa,tensile strength of 2.74 GPa and thermal conductivity of 1128 W/(m·K)by spinning followed by oxidation,carbonization and graphitization when the obtained anisotropic asphalt with an intermediate phase mass fraction of 96.8%was used as the precursor.

关 键 词：碳纤维 各向异性沥青 热缩聚法 热导率 力学性能 

分 类 号：TQ342.74[化学工程—化纤工业]