同步氢化/热缩聚法制备中间相沥青的工艺研究

The technological conditions of preparation of mesophase pitch by simultaneous hydrogenation-thermal condensation

系统地研究了在氢化剂量固定情况下,反应温度与时间对同步氢化/热缩聚法所制得的中间相沥青(MP)性质的影响,并制得了可纺MP。研究表明反应时间同为4h时,MP的软化点和不溶分含量随反应温度的提高而升高;偏光结果显示,低温产物为中间相小球和各向同性基质的混合物,高温产物为连续中间相。反应温度同为410℃时,MP软化点和不溶分含量均随反应时间的延长而显著提高,经历了从中间相小球到小球发生融并,最后形成了马赛克织构的中间相。纺丝性能测试表明,反应温度为410或420℃,反应4h制得的中间相沥青,可以熔融纺丝,经氧化和碳化后制得两组碳纤维。

In this work,the spinnable mesophase pitch was prepared through simultaneous hydrogenation-thermal condensation of coal tar pitch with tetralin as hydrogenation agent.The influences of reaction temperature and soaking time on the properties of mesophase pitch were systematically investigated.Results showed that with the reaction temperature increasing,the softening point and insoluble content of mesophase pitch were increased;the MP prepared at lower temperature is the mixture of isotropic pitch and mesophase spheres and at higher temperature is the pitch with anisotropic pitch as continuous phase.Furthermore,fixing the reaction temperature（410℃）,with the reaction time increasing,softening point and insoluble content of mesophase pitch were improved remarkably.Accordingly,the mesophase texture was experienced from mesophase sphere to mosaic texture.The test of spinning property showed that the mesophase pitch prepared in 410 and 420℃ for 4h could be melt spun into fibers,which was made into carbon fibers through melt spun,oxidation and carbonization.